dr89用户手册 - PDF 무료 다운로드

DR890 48470-22 1

5AluVer 3 6 TIMER ENTER 4

1.5 / PH 2 6 5.0 N PH 3.5-4.5 a) 50 / Aluminum Voluette Ampule b) 3 0.1 0.2 0.3 c) 0.1 0.1 / d) 1.00 100 / 3 AL 250 0.4 / 0.4 / TenSette0.850/Voluette Ampule 100 0.4/ 0.013/ 10.013 / 6

300 mg/lcaco 3 300 mg/lcaco 3 a) 3 b) 5.0 N c) 5.25 N 1000 mg/l CaCO 3 a) 3 b) 5.25N 20 mg/l 50 mg/l 7

(100 Tests)... 22420-00 : (1) 14290-99, (1) 14577-99, (1) 14294-49. AluVer 3......1... 100/pkg...14290-99...1... 100/pkg...14577-99 Bleaching 3....1... 100/pkg...14294-49 50... 1......1896-41 10-20-25 ml, w/ cap... 2... 6/pkg...24019-06 OPTIONAL REAGENTS Aluminum Standard Solution, 100 mg/l...100 ml...14174-42 Aluminum Standard Solution, Voluette ampule, 50 mg/l as Al, 10 ml... 16/pkg...14792-10 Hydrochloric Acid Solution, 6N (1:1)...500 ml...884-49 m-nitrophenol Indicator Solution, 10 g/l...100 ml...2476-32 Nitric Acid, ACS...500 ml...152-49 Nitric Acid Solution, 1:1...500 ml...2540-49 Sodium Hydroxide Standard Solution, 5.0 N...100 ml MDB...2450-32 Sodium Hydroxide Standard Solution, 5.0 N... 50 ml SCDB...2450-26 Sulfuric Acid Standard Solution, 5.25 N...100 ml MDB...2449-32 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS Ampule Breaker Kit... each...21968-00 Brush... each...690-00 Flask, volumetric, Class A, 100 ml... each...14574-42 Flask, volumetric, Class A, 250 ml... each...14574-46 Fluoride Combination Electrode... each...50265-00 Fluoride Analysis Package... each...50269-00 ph Indicator Paper, 1 to 11 ph... 5 rolls/pkg...391-33 ph/ise Meter, sension 2, portable... each...51725-00 Pipet, TenSette, 0.1 to 1.0 ml... each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet... 50/pkg...21856-96 Pipet, Volumetric, Class A, 1.00 ml... each...14515-35 Thermometer, -10 to 110 C... each...1877-01 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 8

8079 9

... 1...100/pkg...21412-99 UV...1......21134-00 10-20-25 ml, w/cap...2...6/pkg...24019-06 :, 115 V, 60 Hz...1......20828-00, 230 V, 50 Hz...1......20828-02 OPTIONAL REAGENTS Benzotriazole Standard Solution, 500 mg/l... 100 ml...21413-42 Rochelle Salt Solution...29 ml* DB...1725-33 Sulfuric Acid Standard Solution, 1.00 N... 100 ml MDB...1270-32 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS Flask, volumetric, Class A, 1000 ml...each...14574-53 Lamp, UV (lamp only)...each...20823-00 ph Paper, 1 to 11 ph...5 rolls/pkg...391-33 ph Meter, sension 1, portable...each...51700-00 Pipet Filler, safety bulb...each...14651-00 Pipet, TenSette, 0.1 to 1.0 ml...each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet...50/pkg...21856-96 Pipet Tips, for 19700-01 TenSette Pipet...1000/pkg...21856-28 Pipet, volumetric, 10.0 ml, Class A...each...14515-38 Stopwatch...each...14645-00 Thermometer, mercury-filled, -20 to 110 C...each...566-01 Timer, interval, 1 second to 99 hours...each...23480-00 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 12

0 to 1.60 mg/l as B10061 -H Boron 13

1.0/ 0.04/ 40.03/ 16

(mg/l) ( 3+ ) 10 20 120 Isothiazolin-type 120 Quat-type 90 60 1000CaCO 3 2500 2+ 20 1000 ( CaCO 3 ) ( 7+ ) 5 (Mo 6+ ) 60, AMP 20,, HEDP 20 Polyacrylates 20 (as Acumer 1000, 1100) Polymaleic Acid 40 (as Belcene 200) 120 1800 40 Tolyltriazole 20 ( 2+ ) 10 >500 mg/l (+ -) 11.0NpH5 7 25 (+) ()(+) 17

(Fe 3+ or Fe 2+ ), 8 mg/l (+),(+) (+) 18

BoroTrace...26669-00 : (1) 26666-69, (1) 26667-46, (1) 22419-26, (1) 25946-49 BoroTrace 2...2...100/pkg...26666-69 BoroTrace 3...2...100/pkg... 26667-99, 1 M... 20...50 ml SCDB...22419-26,... 25 ml... 500 ml...25946-49, for opening powder pillows...1......968-00,, 50-mL, w/cap.2......20898-41, 10-20-25 ml, w/cap...2...6/pkg...24019-06 OPTIONAL REAGENTS Boron Standard Solution, 250 mg/l as B, 10-mL Voluette Ampule...16/pkg...14249-10 Boron Standard Solution, 1000 mg/l as B... 100 ml...1914-42 Dechlorinating Reagent Powder Pillows...100/pkg...14363-69 Eluant Solution... 1 L...22256-53 Phosphate Buffer Solution, ph 7.2... 1 L...431-53 Sodium Hydroxide Standard Solution, 5.0 N...50 ml DB...2450-26 Sulfamic Acid...113 g...2344-14 Sulfuric Acid Standard Solution, 1.000 N... 100 ml MDB...1270-32 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS Ampule Breaker Kit (for 10-mL ampules)...eacu...21968-00 Filter Holder Assembly...each...2468-00 Flask, volumetric, polypropylene, 100 ml, w/cap...each...14060-42 Flask, volumetric, polypropylene, 1000 ml, w/cap...each...14060-53 Membrane Filters, 3-micron...25/pkg...25940-25 ph Paper, ph 1-11...each...391-33 Pipet, Mohr-type, polypropylene, 5 ml...each...2106-37 Pipet, TenSette, 0.1 to 1.0 ml...each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet...each...21856-96 Spoon, measuring, 0.1 g...each...511-00 Syringe, 30-cc...each...22258-00 Thermometer, -10 to 110 C...each...1877-01 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 19

Br2 Br2 20

0.1( mg / L 2.25 mg / L) 10.1( 0.2( mg / L 2.25 mg / L) 25.2( 22

Pollution Prevention and Waste Management Samples treated with sodium arsenite for manganese or chromium interference will be hazardous wastes as regulated by Federal RCRA for arsenic (D004). See Section 3 for more information on proper disposal of these materials. 23

() DPD....1.... 100/pkg...21056-69 () DPD AccuVac.....1... 25/pkg...25030-25 (), 10-20-25-mL, w/ cap... 6/pkg...24019-06 (), 50 ml... 1... each...500-41 OPTIONAL REAGENTS Chlorine Standard Solution, PourRite ampule, 25-30 mg/l, 2 ml... 20/pkg...26300-20 Potassium Iodide Solution, 30 g/l...100 ml* MDB...343-32 Sodium Arsenite, 5 g/l...100 ml* MDB...1047-32 Sodium Hydroxide Standard Solution, 1.000 N...100 ml* MDB...1045-32 Sulfuric Acid Standard Solution, 1 N...100 ml* MDB...1270-32 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS AccuVac Snapper Kit... each...24052-00 PourRite Ampule Breaker... each...24846-00 Cylinder, graduated, 25 ml... each...508-40 ph Meter, sension 1, portable... each...51700-00 ph Indicator Paper, 1 to 11 ph units... 5 rolls/pkg...391-33 Pipet, TenSette, 0.1 to 1.0 ml... each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet... 50/pkg...21856-96 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. * Contact Hach for larger sizes 24

10126 25

PH 27

11 5 10 DPD 11/ 1 a 14268-10 b(50-75 /) c 100 2 a1 5%1 2#8021. 3 6 ) 4 2.45 DPD 5 6 ) 0.10. 28

(EDL) 29

() DPD/ (100 tests)...27709-00 : DPD llows, 10 ml.. 1...100/pkg... 21055-69... 4... 29 ml... 27621-33 (AccuVac ) DPD/AccuVac (25 tests)... 27710-00 : DPD AccuVac... 1...25/pkg... 25020-25... 16... 29 ml...27621-33 OPTIONAL REAGENTS Chlorine Standard Solution, Voluette ampule, 50-75 mg/l, 10 ml... 16/pkg... 14268-10 DPD Free Chlorine Reagent w/dispensing cap... 250 tests... 21055-29 Potassium Iodide Solution, 30 g/l...100 ml* MDB... 343-32 Sodium Arsenite, 5 g/l...100 ml* MDB... 1047-32 Sodium Hydroxide Standard Solution, 1.000 N...100 ml* MDB... 1045-32 Sulfuric Acid Standard Solution, 1.000 N...100 ml* MDB... 1270-32 Water, deionized... 4 L... 272-56 Water, sterile, chlorine dioxide-free... 500 ml... 26415-49 OPTIONAL APPARATUS AccuVac Snapper Kit... each... 24052-00 Cylinder, graduated, 25 ml... each... 508-40 ph Meter, sension 1, portable... each... 51700-10 ph Paper, 1 to 11 ph units... 5 rolls/pkg... 391-33 Pipet, TenSette, 0.1 to 1.0 ml... each... 19700-01 Pipet Tips, for 19700-01 TenSette Pipet... 50/pkg... 21856-96 PourRite Ampule Breaker... each... 24846-00 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. * Marked Dropper Bottle - contact Hach for larger sizes. 31

8345 ENTER 32

25.0/ 0.3/ 77.3/, 10-20-25 ml, w/ cap... 2... 6/pkg...24019-06... 10 ml... 4 L...272-56 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 33

0.00 mg/l Cl2 34

PH 5 10 a) LR Chlorine PourRite Ampule b) TenSette0.110 c) d) / 35

0.1( mg / L mg / L) 10.1( e) d f) 2.40/ 0.06/ 80.03/2/ 8021 Federal RCRA for arsenic (D004) (Mn4+, Mn7+) (Cr6+) 1 1. ph to 6 7. 2. 3(30 g/l)10-ml. 3. 1 4. 3(5 g/l) 5. 6. 36

(NH2Cl) ph NH2ClHR Free Cl2 (1 mg/l Cl2): C ( F) NH2Cl 5 (41) 10 (50) 20 (68) 30 (86) 1.2 mg/l +0.15 0.19 0.30 0.29 2.5 mg/l +0.35 0.38 0.55 0.61 3.5 mg/l +0.38 0.56 0.69 0.73 5.0 mg/l +0.68 0.75 0.93 1.05 ph6-7 DPD... 1... 100/pkg...14070-99... 30 ml... 4 L...272-56, 10-20-25 ml, w/ caps...2...6/pkg...24019-06 OPTIONAL REAGENTS Chlorine Standard Solution, PourRite ampule, 50-75 mg/l, 2 ml...20/pkg... 14268-20 Potassium Iodide Solution, 30 g/l... 100 ml* MDB... 343-32 Sodium Arsenite, 5 g/l... 100 ml* MDB...1047-32 Sodium Hydroxide Standard Solution, 1.000 N... 100 ml* MDB... 1045-32 Sulfuric Acid Standard Solution, 1.000 N... 100 ml* MDB... 1270-32 OPTIONAL APPARATUS Cylinder, graduated, mixing, 25 ml...each...20886-40 ph Meter, sension 1, portable...each...51700-00 ph Paper, 1 to 11 ph units...5 rolls/pkg...391-33 Pipet, TenSette, 0.1 to 1.0 ml...each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet...50/pkg...21856-96 PourRite Ampule Breaker...each...24846-00 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. * Marked Dropper Bottle (contact Hach for larger sizes) 37

0.00 mg/l Cl2 38

PH 5 10 a) LR Chlorine PourRite Ampule b) TenSette0.110 c) d) / 0.1( mg / L mg / L) 10.1( 39

e) d f) 2.40/ 0.06/ 80.03/2/ 8167 Federal RCRA for arsenic (D004) (Mn4+, Mn7+) (Cr6+) ph 1 1. ph to 6 7. 2. 3(30 g/l)10-ml. 3. 1 4. 3(5 g/l) 5. 6. ph6-7 40

DPD... 1... 100/pkg...14064-99... 30 ml...500ml...272-49, 10-20-25 ml, w/ caps...2...6/pkg...24019-06 OPTIONAL REAGENTS Description Unit Cat. No. Chlorine Standard Solution, PourRite ampule, 50-75 mg/l, 2 ml...20/pkg... 14268-20 Potassium Iodide Solution, 30 g/l... 100 ml* MDB... 343-32 Sodium Arsenite, 5 g/l... 100 ml* MDB...1047-32 Sodium Hydroxide Standard Solution, 1.000 N... 100 ml* MDB... 1045-32 Sulfuric Acid Standard Solution, 1.000 N... 100 ml* MDB... 1270-32 OPTIONAL APPARATUS Cylinder, graduated, mixing, 25 ml...each...20886-40 ph Meter, sension 1, portable...each...51700-00 ph Paper, 1 to 11 ph units...5 rolls/pkg...391-33 Pipet, TenSette, 0.1 to 1.0 ml...each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet...50/pkg...21856-96 PourRite Ampule Breaker...each...24846-00 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 41

(0-2.00 mg/l) : 8021 42

PH 5 10 a) LR Chlorine PourRite Ampule b) TenSette0.1 c) d) READ e) / 0.1( mg / L mg / L) 10.1( f) d e g) a) LR Chlorine PourRite Ampule b) 25 c) 0.2( ) d) DPD e) f) / 0.2( mg / L mg / L) 25.2( 43

g) f h) 1.00/ 0.01/ 1.00/ 0.01/ 9110.02/ Federal RCRA for arsenic (D004) DPD 44

() DPD, 10 ml... 1... 100/pkg...21055-69 l, 10, 20, 25 ml, w/ cap... 2... 6/pkg...24019-06 () DPD AccuVac... 1... 25/pkg...25020-25, 50 ml... 1... each...500-41 OPTIONAL REAGENTS Description Unit Cat. No. Chlorine Standard Solution, PourRite ampule, 25-30 mg/l, 2 ml... 20/pkg... 26300-20 DPD Free Chlorine Reagent w/dispensing cap... 250 tests...21055-29 Potassium Iodide Solution, 30 g/l...100 ml* MDB... 343-32 Sodium Arsenite, 5 g/l...100 ml* MDB...1047-32 Sodium Hydroxide Standard Solution, 1.000 N...100 ml* MDB... 1045-32 Sulfuric Acid Standard Solution, 1.000 N...100 ml* MDB... 1270-32 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS AccuVac Snapper Kit... each... 24052-00 Cylinder, graduated, 25 ml... each...508-40 ph Meter, sension 1, portable... each...51700-00 ph Paper, 1 to 11 ph units... 5 rolls/pkg...391-33 Pipet, TenSette, 0.1 to 1.0 ml... each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet... 50/pkg...21856-96 45

PourRite Ampule Breaker... each... 24846-00 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 46

: 8167 47

PH 5 10 a) LR Chlorine PourRite Ampule b) TenSette0.1 c) d) READ e) / 0.1( mg / L mg / L) 10.1( f) d e g) a) LR Chlorine PourRite Ampule b) 25 c) 0.2( ) d) DPD e) f) / 48

0.2( mg / L mg / L) 25.2( g) f h) 1.00/ 0.01/ 1.00/ 0.01/ 9110.02/ Federal RCRA for arsenic (D004) 49

() DPD, 10 ml... 1... 100/pkg... 21056-69 l, 10, 20, 25 ml, w/ cap... 2... 6/pkg...24019-06 () DPD AccuVac... 1... 25/pkg... 25030-25, 50 ml... 1... each...500-41 OPTIONAL REAGENTS Description Unit Cat. No. Chlorine Standard Solution, PourRite ampule, 25-30 mg/l Cl2... 20/pkg...26300-20 DPD Total Chlorine Reagent w/dispensing cap... 250 tests...21056-29 Potassium Iodide Solution, 30 g/l...100 ml* MDB...343-32 Sodium Arsenite, 5 g/l... 100 ml* MDB...1047-32 Sodium Hydroxide Standard Solution, 1 N... 100 ml* MDB...1045-32 Sulfuric Acid Standard Solution, 1 N... 100 ml* MDB...1270-32 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS AccuVac Snapper Kit... each...24052-00 PourRite Ampule Breaker... each...24846-00 Cylinder, graduated, 25 ml... each...508-40 ph Indicator Paper, 1 to 11 ph units... 5 rolls/pkg...391-33 ph Meter, sension 1, portable... each...51700-00 50

Pipet, TenSette, 0.1 to 1.0 ml... each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet... 50/pkg...21856-96 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 51

Test N Tube TM 52

PH 5 10 a) LR Chlorine PourRite Ampule b) TenSette0.1 c) 8 d) / 0.1( mg / L mg / L) 10.1( e) d e f) 53

2.53/ 0.14/ 100.03/ Federal RCRA for arsenic (D004) 54

Test N Tube DPD...1... 50/pkg...21055-45 Test N Tube...1 l... 6/pkg...22758-06 COD/TNT... 1... each...48464-00 OPTIONAL REAGENTS Chlorine Standard Solution, PourRite ampule, 50-75 mg/l, 2 ml... 20/pkg...14268-20 Potassium Iodide Solution, 30 g/l...100 ml* MDB...343-32 Sodium Arsenite, 5 g/l...100 ml* MDB...1047-32 Sodium Hydroxide Standard Solution, 1.000 N...100 ml* MDB...1045-32 Sulfuric Acid Standard Solution, 1.000 N...100 ml* MDB...1270-32 OPTIONAL APPARATUS Beaker, 50 ml... each...500-41 ph Meter, sension 1, portable... each...51700-00 ph Paper, ph 1 to 11 ph... 5 rolls/pkg...391-33 Pipet, TenSette, 0.1 to 1.0 ml... each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet... 50/pkg...21856-96 PourRite Ampule Breaker... each... 24846-00 Test Tube Rack... each...18641-00 55

Test N Tube TM 56

PH 5 10 a) LR Chlorine PourRite Ampule b) TenSette0.1 c) 8 d) / 0.1( mg / L mg / L) 10.1( e) d e f) 57

2.53/ 0.14/ 100.03/ Federal RCRA for arsenic (D004) 58

Test N Tube DPD...1... 50/pkg...21056-45 Test N Tube...1... 6/pkg...22758-06 COD/TNT... 1......48464-00 OPTIONAL REAGENTS Chlorine Standard Solution, 2-mL PourRite ampule, 50-75 mg/l... 20/pkg...14268-20 Potassium Iodide Solution, 30 g/l...100 ml* MDB...343-32 Sodium Arsenite Solution, 5 g/l... 100 ml* MDB...1047-32 Sodium Hydroxide Standard Solution, 1.00 N... 100 ml* MDB...1045-32 Sulfuric Acid Standard Solution, 1.000 N... 100 ml* MDB...1270-32 OPTIONAL APPARATUS Beaker, 50 ml... each...500-41 PourRite Ampule Breaker... each...24846-00 ph Indicator Paper, ph 1 to 11... 5 rolls/pkg...391-33 ph Meter, sension 1, portable... each...51700-00 Pipet, TenSette, 0.1 to 1.0 ml... each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet... 50/pkg...21856-96 Test Tube Rack... each...18641-00 59

() a) PourRite 5/ b) TenSette3100.10.2 0.3 c) 0.1 0.05/ d) a) Voluette12.5/ b) TenSette325 0.10.20.3 c) 0.1 0.05/ d) 1050/1000 0.5/ 0.6/ 0.008/ 61

0.6/ 0.005/ 130.01/ 62

ChromaVer3.. 1...100/pkg...12710-99, 10-20-25 ml, w/ cap...2...6/pkg...24019-06 AccuVac ChromaVer 3 AccuVac... 1...25/pkg...25050-25, 50 ml...1...each...500-41 OPTIONAL REAGENTS Description Unit Cat. No Acid Reagent Powder Pillows... 100/pkg...2126-99 Chromium, Hexavalent, Standard Solution, 50 mg/l Cr6+...100 ml...810-42 Chromium, Hexavalent, Standard Solution, Voluette Ampule, 12.5 mg/l Cr6+, 10 ml... 16/pkg...14256-10 Chromium, Hexavalent, Standard Solution, PourRite Ampule, 5 mg/l Cr6+, 2 ml... 20/pkg...26056-20 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS Description Unit Cat. No. AccuVac Snapper Kit... each...24052-00 Ampule Breaker Kit... each...21968-00 Flask, volumetric, Class A, 1000 ml... each...14574-53 ph Paper, 1 to 11 ph units... 5 rolls/pkg...391-33 ph Meter, EC10, portable... each...50050-00 Pipet, TenSette, 0.1 to 1.0 ml... each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet... 50/pkg...21856-96 Pipet, volumetric, 5.00 ml, Class A... each...14515-37 Pipet Filler, safety bulb... each...14651-00 PourRite Ampule Breaker, 2 ml... each...24846-00 In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 63

c) TenSette30.10.2 0.3 d) 0.1 0.05/ 150/100 0.5/ 0.5/ 0.4/ 0.004/ 150.01/ 1 ph 2 66

(100 Tests)...22425-00 : (1) 2126-99, (1) 12066-99, (1) 2043-99, (1) 2044-99... 1...100/pkg...2126-99 ChromaVer 3... 1...100/pkg...12066-99 Chromium 1... 1...100/pkg...2043-99 Chromium 2... 1...100/pkg...2044-99, 4", 120 V...1......12067-01, 4", 240 V...1......12067-02, 10-20-25 ml, w/ cap... 2...6/pkg...24019-06...1......1955-55 OPTIONAL REAGENTS Chromium, trivalent, Standard Solution, 50 mg/l Cr3+... 100 ml...14151-42 Chromium, trivalent, Standard Solution, PourRite ampule, 12.5 mg/l Cr3+, 2 ml...20/pkg...14257-20 Nitric Acid, ACS... 500 ml...152-49 Nitric Acid Solution 1:1... 500 ml...2540-49 Sodium Hydroxide Standard Solution 5.0 N... 50 ml* DB...2450-26 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS Cylinder, graduated, polypropylene, 25 ml...each...1081-40 Finger Cots...2/pkg...14647-02 ph Paper, 1 to 11 ph units...5 rolls/pkg...391-33 ph Meter, EC10, portable...each...50050-00 Pipet, serological, 2 ml...each...532-36 Pipet, TenSette, 0.1 to 1.0 ml...each...19700-01 Pipet Tips for 19700-01 TenSette Pipet...50/pkg...21856-96 Pipet, volumetric, Class A, 1.00 ml...each...14515-35 Pipet Filler, safety bulb...each...14651-00 PourRite Ampule Breaker...each...24846-00 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 67

8025 68

250Pt-Co Pt-Co 1925Pt-Co 69

... 50 ml... 4 L...272-56...1...each...2131-00, 47 mm, 300 ml...1...each...13529-00, 47 mm, 0.45...1...100/pkg...13530-00, 500 ml...1...each...546-49,10-20-25 ml, w/cap...2...6/pkg...24019-06, No. 7, one hole...1...6/pkg...2119-07 OPTIONAL REAGENTS Color Standard Solution, 500 platinum-cobalt units... 1 L...1414-53 OPTIONAL APPARATUS Cylinder, graduated, 50-mL, glass...each...508-41 Flask, volumetric, Class A, 100 ml...each...14574-42 Pipet, volumetric, Class A, 50 ml...each...14515-41 Thermometer, -10 to 110 C...each...1877-01 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 70

(0 to 5.00 mg/l) : 8506 71

Sampling and Storage Collect samples in acid-cleaned glass or plastic containers. Adjust the ph to 2 or less with nitric acid (about 2 ml per liter). Store preserved samples up to six months at room temperature. Before analysis, adjust the ph to 4 to 6 with 8 N potassium hydroxide. Do not exceed ph 6, as copper may precipitate. Correct the test result for volume additions; see Correction for Volume Additions in Section 1 for more information. If only dissolved copper is to be determined, filter the sample before acid addition using the labware listed under Optional Apparatus. Accuracy Check Standard Additions Method a) Fill three 25-mL graduated mixing cylinders with 25 ml of sample. b) Snap the neck off a Copper Voluette Ampule Standard, 75 mg/l as Cu. c) Use the TenSette Pipet to add 0.1, 0.2, and 0.3 ml of standard, respectively, to the mixing cylinders. Stopper and mix thoroughly. d) For analysis with AccuVac Ampuls, transfer the solutions to dry, clean 50-mL beakers to fill the ampules. For analysis with powder pillows, transfer only 10 ml of the solution to 10-mL sample cells. e) Analyze each sample as described in the procedure. The copper concentration should increase about 0.3 mg/l for each 0.1 ml of standard added. f) If these increases do not occur, see Standard Additions in Section 1 for more information. Standard Solution Method Prepare a 1.00 mg/l copper standard by pipetting 1.00 ml of Copper Standard Solution, 100 mg/l as Cu, into 100-mL volumetric flask. Dilute to volume with deionized water and mix well. Prepare this solution daily. Using this solution as the sample, perform the copper procedure as described above. Method Performance Precision In a single laboratory, using a standard solution of 2.25 mg/l Cu and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of ±0.02 mg/l Cu. In a single laboratory, using a standard solution of 2.25 mg/l Cu and two representative lots of AccuVac Ampuls with the instrument, a single operator obtained a standard deviation of ±0.02 mg/l Cu. 73

() CuVer 1... 1......100/pkg...21058-69, 10-20-25 ml, w/cap... 2... 6/pkg...24019-06 () CuVer 2 AccuVac... 1... 25/pkg...25040-25, 50 ml... 1... each...500-41 OPTIONAL REAGENTS Copper Standard Solution, 100 mg/l... 100 ml...128-42 Copper Standard Solution, Voluette Ampule, 75 mg/l Cu, 10 ml...16/pkg...14247-10 CuVer 2 Reagent Powder Pillows...100/pkg...21882-99 Formaldehyde, 37%, ACS...100 ml* MDB...2059-32 Free Copper Reagent Powder Pillows...100/pkg...21186-69 Hydrochloric Acid Solution, 6.0 N... 500 ml...884-49 Hydrosulfite Reagent Powder Pillows...100/pkg...21188-69 Nitric Acid, ACS... 500 ml...152-49 Nitric Acid Solution, 1:1... 500 ml...2540-49 Potassium Chloride Solution, saturated...50 ml SCDB...765-26 Potassium Hydroxide Standard Solution, 8.0 N... 100 ml* MDB...282-32 Sodium Hydroxide Standard Solution, 5.0 N... 100 ml* MDB...2450-32 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS Description Unit Cat. No. AccuVac Snapper Kit...each...24052-00 Ampule Breaker Kit...each...21968-00 Cylinder, graduated, mixing, 25 ml...each...20886-40 Cylinder, graduated, polypropylene, 25 ml...each...1081-40 Cylinder, graduated, 100 ml...each...508-42 Filter Paper, folded, 12.5 cm...100/pkg...1894-57 Filter Pump...each...2131-00 Flask, volumetric, 100 ml...each...547-42 Funnel, polypropylene, 65 mm...each...1083-67 Hot Plate, 4" diameter, 120 V...each...12067-01 Hot Plate, 4" diameter, 240 V...each...12067-02 ph Indicator Paper, 1 to 11 ph...5 rolls/pkg...391-33 ph Meter, EC10, portable...each...50050-00 Pipet, TenSette, 0.1 to 1.0 ml...each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet...50/pkg...21856-96 Pipet, volumetric, Class A, 1.00 ml...each...14515-35 Pipet Filler, safety bulb...each...14651-00 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 74

μ μg/l, CuZERO 75

0.0 μg/l Cu μ 60 mg/l 10 mg/l 15000 mg/l 90,000 mg/l Cr6+ 110 mg/l 100 mg/l 30000 mg/l Fe2+ 6 mg/l 3mg/L 10000 mg/l 140 mg/l 3 mg/l 11mg/L 60mg/L 60000 mg/l 90000 mg/l 9mg/L EDTA PH 76

Sampling and Storage Collect samples in acid-washed plastic bottles. To preserve, adjust the ph to 2 or less with nitric acid (about 5 ml per liter). Store preserved samples up to six months at room temperature. Before testing, adjust the ph of the sample to between 2 and 6. If the sample is too acidic, adjust the ph with 5.0 N Sodium Hydroxide Standard Solution. Correct test results for volume additions; see Correction for Volume Additions in Section 1 for more information. Accuracy Check Standard Additions Method a) Fill six (3 pairs) 25-mL graduated mixing cylinders with 25 ml of sample. Properly mark each pair of cylinders as sample and blank. b) Using a TenSette Pipet, add 0.1 ml of Copper Standard Solution, 10.0 mg/l Cu, to two of the cylinders. Add 0.2 ml of standard to two more of the cylinders. Add 0.3 ml of standard to the other two cylinders, making a total of six samples (2 for each volume of standard). c) Analyze the samples as described above. The copper concentration reading should increase by 40 μg/l for each 0.1 ml of standard added. d) If these increases do not occur, see Standard Additions in Section 1 for more information. Standard Solution Method To assure the accuracy of the test, prepare a 100 μg/l copper standard: a) Pipet 1.00 ml of Copper Standard Solution, 10.0 mg/l Cu, into a 100-mL volumetric flask. b) Dilute to volume with copper-free, reagent-grade water. c) Use this standard in place of the sample in the procedure. The reading should be 100 μg/l Cu. d) Prepare this solution daily. Method Performance Precision In a single laboratory, using a standard solution of 100 μg/l copper and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of 3.4 μg/l copper. Estimated Detection Limit The estimated detection limit for program 22 is 5.4 μg/l Cu. For more information on the estimated detection limit, see Section 1. Summary of Method The porphyrin method is very sensitive to trace amounts of free copper. Due to the sensitivity of the method, a masking agent is used to prepare a blank for each sample. The method is free from most interferences and does not require any sample extraction or preconcentration. Interferences from other metals are eliminated by the copper 77

masking reagent. The porphyrin indicator forms an intense, yellow-colored complex proportional to any free copper present in the sample. Total copper may be determined if a digestion is performed prior to analysis., 10-mL (100 tests)...26033-00 : (1) 26034-49, (2) 26035-49, (2) 26036-49, (1) 129-02... 1...100/pkg...26034-49 1..... 2...100/pkg...26035-49 2... 2...100/pkg...26036-49 l, 10-20-25 ml, w/ caps...2...6/pkg...24019-06 OPTIONAL REAGENTS Copper Standard Solution, 10 mg/l Cu... 100 ml MDB...129-32 Hydrochloric Acid Solution, 1:1 (6 N)... 500 ml...884-49 Nitric Acid, ACS... 500 ml...152-49 Nitric Acid Solution, 1:1... 500 ml...2540-49 Sodium Hydroxide Standard Solution, 5 N... 1 L...2450-53 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS Beaker, 100 ml...each...500-42 Cylinder, mixing, graduated, 25 ml...each...20886-40 Flask, volumetric, Class A, 100 ml...each...14574-42 Hot Plate, 7 x 7 inches, 120 V...each...23441-00 Hot Plate, 7 x 7 inches, 240 V...each...23441-02 ph Paper, 1 to 11 ph units...5 rolls/pkg...391-33 ph Meter, sension 1, portable...each...51700-00 Pipet, Mohr, 5 ml...each...20934-37 Pipet, TenSette, 0.1 to 1.0 ml...each...19700-01 Pipet Tips, for 19700-01...50/pkg...21856-96 Pipet, volumetric, 1.0 ml, Class A...each...14515-35 Pipet Filler, safety bulb...each...14651-00 Watch Glass, Pyrex, 100 ml...each...578-70 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 78

- 79

CyaniVer 5 312 a)2.5n 25mL ph 7 9 b) c) d) 25mLa e) c 4 a)2.5n 25mL ph 7 9 b) c) d) 25mLa e)c f) 4 1mg/L4 CyaniVer 3 HexaVer20 mg/l 5 mg/l14 Sampling and Storage Collect samples in glass or plastic bottles and analyze as soon as possible. The presence of oxidizing agents, sulfides and fatty acids can cause cyanide loss during sample storage. Samples containing these substances must be pretreated as described in the following procedures before preservation with sodium hydroxide. If the sample contains sulfide and is not pretreated, it must be analyzed within 24 hours. Preserve the sample by adding 4.0 ml of 5.0 N Sodium Hydroxide Standard Solution to each liter (or quart) of sample, using a glass serological pipet and pipet filler. Check the sample ph. Four ml of sodium hydroxide are usually enough to raise the ph of most water and wastewater samples to 12. Add more 5.0 N sodium hydroxide if necessary. Store the samples at 4 C (39 F) or less. Samples preserved in this manner can be stored for 14 days. 81

Before testing, samples preserved with 5.0 N sodium hydroxide or samples that are highly alkaline due to chlorination treatment processes or distillation procedures should be adjusted to approximately ph 7 with 2.5 N Hydrochloric Acid Standard Solution. If significant amounts of preservative are used, correct for the volume added; see Correction for Volume Additions in Section 1 for more information. Oxidizing Agents Oxidizing agents such as chlorine decompose cyanides during storage. To test for their presence and eliminate their effect, pretreat the sample as follows: a) Take a 25-mL portion of the sample and add one drop of m-nitrophenol Indicator Solution, 10 g/l. Swirl to mix. b) Add 2.5 N Hydrochloric Acid Standard Solution drop-wise until the color changes from yellow to colorless. Swirl the sample thoroughly after the addition of each drop. c) Add two drops of Potassium Iodide Solution, 30 g/l, and two drops of Starch Indicator Solution, to the sample. Swirl to mix. The solution will turn blue if oxidizing agents are present. d) If Step c suggests the presence of oxidizing agents, add two level 1-g measuring spoonfuls of ascorbic acid per liter of sample. e) Withdraw a 25-mL portion of sample treated with ascorbic acid and repeat Steps a to c. If the sample turns blue, repeat Steps d and e. f) If the 25-mL sample remains colorless, adjust the remaining sample to ph 12 for storage with 5 N Sodium Hydroxide Standard Solution (usually 4 ml/l). g) Perform the procedure given under Interferences, Reducing Agents, to eliminate the effect of excess ascorbic acid, before following the cyanide procedure. Sulfides Sulfides quickly convert cyanide to thiocyanate (SCN). To test for the presence of sulfide and eliminate its effect, pretreat the sample as follows: a) Place a drop of sample on a disc of hydrogen sulfide test paper that has been wetted with ph 4 Buffer Solution. b) If the test paper darkens, add a 1-g measuring spoon of lead acetate to the sample. Repeat Step a. c) If the test paper continues to turn dark, keep adding lead acetate until the sample tests negative for sulfide. d) Filter the black lead sulfide precipitate using the apparatus listed under Optional Apparatus. Preserve the sample for storage with 5 N Sodium Hydroxide Standard Solution or neutralize to a ph of 7 for analysis. Fatty Acids Caution perform this operation in a hood as quickly as possible. When distilled, fatty acids will pass over with cyanide and form soaps under the alkaline conditions of the absorber. If the presence of fatty acid is suspected, do not preserve samples with sodium hydroxide until the following pretreatment is performed. The effect of fatty acids can be minimized as follows: a) Acidify 500 ml of sample to ph 6 or 7 with Acetic Acid Solution. 82

b) Pour the sample into a 1000-mL separatory funnel and add 50 ml of hexane. c) Stopper the funnel and shake for one minute. Allow the layers to separate. d) Drain off the sample (lower) layer into a 600-mL beaker. If the sample is to be stored, add 5 N Sodium Hydroxide Standard Solution to raise the ph to above 12. Accuracy Check Standard Solution Method Caution Cyanides and their solutions, and the hydrogen cyanide liberated by acids, are very poisonous. Both the solutions and the gas can be absorbed through the skin. Prepare a 100 mg/l cyanide stock solution weekly by dissolving 0.1884 grams of sodium cyanide in deionized water and diluting to 1000 ml. Immediately before use, prepare a 0.10 mg/l cyanide working solution by diluting 1.00 ml of the 100 mg/l stock solution to 1000 ml using deionized water. Use this prepared standard in place of sample in Step 3. Results should be 0.10 mg/l CN-. Method Performance Precision In a single laboratory, using a standard solution of 0.19 mg/l CN- and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of ±0.017 mg/l CN-. Estimated Detection Limit (EDL) The estimated detection limit for program 23 is 0.008 mg/l CN. For more information on the estimated detection limit, see Section 1. Acid Distillation For USEPA reporting purposes, samples must be distilled. All samples should be treated by acid distillation except when experience has shown that there is no difference in results obtained with or without distillation. With most compounds, a one-hour reflux is adequate. If thiocyanate is present in the original sample, a distillation step is absolutely necessary as thiocyanate causes a positive interference. High concentrations of thiocyanate can yield a substantial quantity of sulfide in the distillate. The rotten egg smell of hydrogen sulfide will accompany the distillate when sulfide is present. The sulfide must be removed from the distillate prior to testing. If cyanide is not present, the amount of thiocyanate can be determined. The sample is not distilled and the final reading is multiplied by 2.2. The result is mg/l thiocyanate. The distillate can be tested and treated for sulfide after the last step of the distillation procedure by using the following lead acetate treatment procedure. 83

a) Place a drop of the distillate (already diluted to 250 ml) on a disc of hydrogen sulfide test paper that has been wetted with ph 4.0 Buffer Solution. b) If the test paper darkens, add 2.5 N Hydrochloric Acid Standard Solution drop-wise to the distillate until a neutral ph is obtained. c) Add a 1-g measuring spoon of lead acetate to the distillate and mix. Repeat Step a. d) If the test paper continues to turn dark, keep adding lead acetate until the distillate tests negative for sulfide. e) Filter the black lead sulfide precipitate through filter paper and funnel. This sample should now be neutralized to ph 7 and analyzed for cyanide without delay. Distillation Procedures A detailed procedure for the distillation of cyanide samples is included with the Hach Distillation Apparatus. Three detailed procedures, Free Cyanides, Cyanides Amenable to Chlorination, and Total Cyanides, are included with the four- and ten-position Midi-Dist Distillation System. See the Optional Apparatus listing. Summary of Method The pyridine-pyrazolone method gives an intense blue color with free cyanide. A sample distillation is required to determine cyanide from transition and heavy metal cyanide complexes. (100 Tests), 10 ml...24302-00 : (1) 21068-69, (1) 21069-69, (1) 21070-69 CyaniVer 3... 1...100/pkg...21068-69 CyaniVer 4... 1...100/pkg...21069-69 CyaniVer 5... 1...100/pkg...21070-69, 10-20-25, w/cap...2...6/pkg...24019-06 OPTIONAL REAGENTS Description Unit Cat. No. Acetic Acid Solution, 10%... 500 ml...14816-49 Ascorbic Acid...100 g...6138-26 Bromine Water... 25 ml...2211-20 Buffer Solution, ph 4.0... 500 ml...12223-49 Hexanes, ACS... 4 L...14478-17 HexaVer Chelating Reagent Powder Pillows...100/pkg...243-99 Hydrochloric Acid Standard Solution, 2.5 N... 100 ml MDB...1418-32 Lead Acetate, trihydrate, ACS...500 g...7071-34 84

Magnesium Chloride Solution... 1 L...14762-53 m-nitrophenol Indicator... 100 ml MDB...2476-32 Potassium Iodide Solution, 30 g/l... 100 ml MDB...343-32 Sodium Arsenite Solution, APHA... 100 ml MDB...1047-32 Sodium Cyanide, ACS...28 g...184-20 Sodium Hydroxide Standard Solution, 0.25 N... 1 L...14763-53 Sodium Hydroxide Standard Solution, 5.0 N... 1 L...2450-53 Starch Indicator Solution... 10 ml MDB...349-32 Sulfuric Acid Standard Solution, 19.2 N... 500 ml...2038-49 Water, deionized... 4 L... 272-56 OPTIONAL APPARATUS Description Unit Cat. No. Beaker, glass, 600 ml...each...500-52 Bottle, wash, 500 ml...each... 620-11 Cylinder, graduated, 50 ml...each... 508-41 Cylinder, graduated, 250 ml...each... 508-46 Distillation Apparatus, cyanide accessories...each...22658-00 Distillation Apparatus, general purpose accessories...each...22653-00 OPTIONAL APPARATUS, continued Description Unit Cat. No. Distillation Apparatus Heater and Support Apparatus, 115 Vac, 60 Hz... each...22744-00 Distillation Apparatus Heater and Support Apparatus, 230 Vac, 50 Hz... each...22744-02 Dropper, plastic... each...6080-00 Filter Paper, folded, 12.5 cm... 100/pkg...1894-57 Flask, volumetric, Class A, 1000 ml... each... 14574-53 Flask, volumetric, Class A, 250 ml... each...14574-46 Funnel, poly, 65 mm... each...1083-67 Funnel, separatory, 500 ml... each... 520-49 Hydrogen Sulfide Test Papers... 100/pkg...25377-33 Midi-Dist Distillation System, 4-position... each...26384-00 Midi-Dist Distillation System, 10-position... each...26385-00 ph Meter, sension 1, portable... each...51700-00 Pipet, volumetric, Class A, 1.00 ml... each...14515-35 Pipet Filler, safety bulb... each...14651-00 Scoop, double ended... each...12257-00 Spoon, measuring, 1.0 g... each...510-00 Support Ring, 4 inch... each... 580-01 Support Stand... each...563-00 Thermometer, -10 to 110 C... each...1877-01 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 85

8139 86

Sampling and Storage Collect samples in clean plastic or glass bottles. Samples must be analyzed within 24 hours. Accuracy Check Standard Solution Method a) Dissolve 1.000 gram of cyanuric acid in 1000 ml of deionized water to make a 1000 mg/l solution. It takes several hours for the cyanuric acid to dissolve. This solution is stable for several weeks. b) Dilute 2.00 ml of the 1000 mg/l solution to 100 ml with deionized water to make a 20 mg/l solution. Prepare fresh daily. c) Testing the 20 mg/l solution should give test results of about 20 mg/l cyanuric acid. Method Performance Precision In a single laboratory, using a standard solution of 25.0 mg/l cyanuric acid and two lots of reagent with the instrument, a single operator obtained a standard deviation of ±1.2 mg/l cyanuric acid. 87

Estimated Detection Limit The estimated detection limit for program 24 is 7.0 mg/l cyanuric acid. For more information on the estimated detection limit, see Section 1. Summary of Method The test for cyanuric acid uses the turbidimetric method. Cyanuric Acid 2 Reagent precipitates any cyanuric acid present and holds it in suspension. The amount of turbidity caused by the suspended particles is directly proportional to the amount of cyanuric acid present. Due to the nature of the precipitation reaction, low levels of cyanuric acid (less than 7 mg/l) are not detected by this method.... 1...50/pkg...2460-66, 10-20-25 ml, w/cap...2...6/pkg...24019-06 OPTIONAL REAGENTS Cyanuric Acid...25 g... 7129-24 Water, deionized... 4 L... 272-56 OPTIONAL APPARATUS Balance, Analytical, 115 V, Scientech, Model SA 120...each...26103-00 Balance, Analytical, 230 V, Scientech, Model SA 120...each...26103-02 Filter Paper, folded 12.5 cm...100/pkg...1894-57 Flask, volumetric, Class A, 100 ml...each... 14574-42 Flask, volumetric, Class A, 1000 ml...each... 14574-53 Funnel, poly, 65 mm...each... 1083-67 Pipet, volumetric, Class A, 2.00 ml...each...14515-36 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 88

μ8140 μ 89

μ μ Sampling and Storage Most oxygen scavengers will react quickly with atmospheric oxygen. Collect samples in acid-rinsed plastic or glass containers, allowing the sample to overflow. Cap the container so there is no head space above the sample. Rinse each sample cell several times with sample, then carefully fill to the fill mark. Analyze the sample immediately. Other Oxygen Scavengers To determine other oxygen scavengers, perform the test as directed above, then multiply the DEHA result by the appropriate factor below: 90

Method Performance Precision In a single laboratory, using a standard solution of 242 μg/l DEHA and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of ±6.2 μg/l DEHA. Estimated Detection Limit The estimated detection limit for program 25 is 9 μg/l DEHA. For more information on the estimated detection limit, see Section 1. Summary of Method Diethylhydroxylamine (DEHA) or other oxygen scavengers present in the sample react with ferric iron in DEHA Reagent 2 Solution to produce ferrous iron in an amount equivalent to the DEHA concentration. This solution then reacts with DEHA 1 Reagent, which forms a purple color with ferrous iron. The color is proportional to the concentration of oxygen scavenger in the sample. Using this procedure other oxygen scavengers can be determined by multiplying the DEHA results by the appropriate multiplier. (100 tests)...24466-00 : (2) 21679-69, (1) 21680-49 1... 2... 100/pkg...21679-69 2... 1 ml...500 ml...21680-49... 25 ml... 4 L... 272-56,, 0.5 and 1.0-mL... 1... 20/pkg...21247-20, 10-20-25 ml, w/ cap... 2... 6/pkg...24019-06 OPTIONAL REAGENTS Hydrochloric Acid, 1:1 (6 N)...500 ml... 884-49 OPTIONAL APPARATUS Bottle, wash, 250-mL... each...620-31 Cylinder, graduated, polypropylene, 25 ml... each...1081-40 ph Paper, 1 to 11 ph units... 5 rolls/pkg...391-33 Thermometer, -10 to 110 C... each...1877-01 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 91

8029 SPADNS Method μ 92

Sampling and Storage Collect samples in plastic bottles. Samples may be stored up to 28 days. Accuracy Check Standard Solution Method A variety of standard solutions covering the entire range of the test are available from Hach. Use these in place of sample to verify technique. Minor variations between lots of reagent become measurable above 1.5 mg/l. While results in this region are usable for most purposes, better accuracy may be obtained by diluting a fresh sample 1:1 with deionized water and retesting. Multiply the result by 2. Standard Adjust To adjust the calibration curve using the reading obtained with a 1.80-mg/L Standard Solution, press SETUP and use the arrow keys to scroll to the STD setup option. Press ENTER to activate the option. Then enter 1.80 to edit the standard concentration to match that of the standard used. Press ENTER to complete the adjustment. See Standard Curve Adjustment in Section 1 for more information. Method Performance Precision In a single laboratory, using standard solutions of 1.00 mg/l fluoride and two lots of SPADNS Reagent with the instrument, a single operator obtained standard deviations of ±0.035 mg/l fluoride. In a single laboratory, using standard solutions of 1.00 mg/l fluoride and two lots of SPADNS AccuVac Reagent with the instrument, a single operator obtained standard deviations of ±0.040 mg/l fluoride. Estimated Detection Limit (EDL) The EDL for programs 27 and 28 is 0.05 mg/l F-. For more information on derivation and use of Hach s estimated detection limit, see Section 1. Summary of Method The SPADNS Method for fluoride determination involves the reaction of fluoride with a red zirconium-dye solution. The fluoride combines with part of the zirconium to form 94

a colorless complex, thus bleaching the red color in an amount proportional to the fluoride concentration. Seawater and wastewater samples require distillation. See Optional Apparatus for Distillation Apparatus listing. Pollution Prevention and Waste Management SPADNS Reagent contains sodium arsenite. Final solutions will contain sodium arsenite (D004) in sufficient concentration to be regulated as hazardous waste for Federal RCRA. See Section 3 for more information on disposal of these materials. () SPADNS... 4 ml... 500 ml... 444-49... 10 ml... 4 L...272-56 ()...1......14651-00, Class A, 10.00 ml...1......14515-38, Class A, 2.00 ml...1......14515-36, 10-20-25 ml w/ cap...2...6/pkg...24019-06, -10 to 110 C...1......1877-01 ( ACCUVAC ) SPADNS.. 2...25/pkg...25060-25...... 4 L...272-56 ( ACCUVAC ), 50 ml...2......500-41 OPTIONAL REAGENTS Fluoride Standard Solution, 0.2 mg/l F-... 500 ml...405-02 Fluoride Standard Solution, 0.4 mg/l F-... 500 ml...405-04 Fluoride Standard Solution, 0.5 mg/l F-... 500 ml...405-05 Fluoride Standard Solution, 0.6 mg/l F-... 500 ml...405-06 Fluoride Standard Solution, 0.8 mg/l F-... 500 ml...405-08 Fluoride Standard Solution, 1.0 mg/l F-... 1000 ml...291-53 Fluoride Standard Solution, 1.0 mg/l F-... 500 ml...291-49 Fluoride Standard Solution, 1.2 mg/l F-... 500 ml...405-12 Fluoride Standard Solution, 1.4 mg/l F-... 500 ml...405-14 Fluoride Standard Solution, 1.5 mg/l F-... 500 ml...405-15 Fluoride Standard Solution, 1.6 mg/l F-... 500 ml...405-16 Fluoride Standard Solution, 1.8 mg/l F-... 500 ml...405-18 Fluoride Standard Solution, 2.0 mg/l F-... 500 ml...405-20 Silver Sulfate, ACS...113 g...334-14 Sodium Arsenite Solution... 100 ml MDB...1047-32 StillVer Distillation Solution... 500 ml... 446-49 95

OPTIONAL APPARATUS AccuVac Snapper Kit... each...24052-00 Cylinder, graduated, 100 ml... each...508-42 Cylinder, graduated, 250 ml... each...508-46 Distillation Heater and Support Apparatus Set, 115 V, 50/60 Hz... each...22744-00 Distillation Heater and Support Apparatus Set, 230 V, 50/60 Hz... each...22744-02 Distillation Apparatus General Purpose Accessories... each...22653-00 ph Meter, sension 1, portable... each...51700-00 Pipet, TenSette, 1.0 to 10.0 ml... each...19700-10 Pipet Tips, for 19700-10 TenSette Pipet... 50/pkg...21997-96 Stopper... 6/pkg...1731-06 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 96

; CLG 97

1.00.25 mg/l CaCO3 (3+) 0.25 mg/l (2+) 0.75 mg/l EDTA, 0.2 mg/l CaCO3 EDTA EGTA (2+) 1.4 mg/l (3+) 2.0 mg/l (2+) 0.20 mg/l (2+) 0.050 mg/l 98

Sampling and Storage Collect samples in acid-washed plastic bottles. Adjust the sample ph to 2 or less with nitric acid (about 5 ml per liter). Preserved samples can be stored up to six months. Adjust the sample ph to between 3 and 8 with 5.0 N Sodium Hydroxide Standard Solution just before analysis. Correct the test results for volume additions; see Correction for Volume Additions in Section 1 for more information. Accuracy Check Using a 2.00 mg/l (as CaCO3) standard solution as sample, perform the hardness procedure described above. The results should be 2.00 mg/l calcium (as CaCO3). Method Performance Precision In a single laboratory using a standard solution of 2.00 mg/l Mg as CaCO3 and 1.88 mg/l Ca as CaCO3 with the instrument, a single operator obtained a standard deviation of ± 0.09 mg/l Mg as CaCO3 and ± 0.08 mg/l Ca as CaCO3. Estimated Detection Limit The estimated detection limit for program 30 is 0.13 mg/l magnesium hardness and 0.08 mg/l calcium hardness. For more information on the estimated detection limit, see Section 1. Summary of Method The colorimetric method for measuring hardness supplements the conventional titrimetric method because it can measure very low levels of calcium and magnesium. Also some interfering metals (those listed above) in the titrimetric method are inconsequential in the colorimetric method when diluting the sample to bring it within the range of this test. The indicator dye, calmagite, forms a purplish-blue color in a strongly alkaline solution and changes to red when it reacts with free calcium or magnesium. Calcium is chelated with EGTA to destroy any red color due to calcium and then the sample is chelated with EDTA to destroy the red color due to both calcium and magnesium. Measuring the red color in the different stages of chelation gives results as the calcium and magnesium hardness concentrations. 99

(100 Tests)...23199-00 : (1) 22417-32, (1) 22418-32, (1) 22419-26, (1) 22297-26... 1 ml... 100 ml MDB...22417-32... 1 ml... 100 ml MDB...22418-32 EDTA, 1 M...1... 50 ml...22419-26 EGTA...1... 50 ml...22297-26, 100-mL...1......1896-42, 0.5 and 1.0 ml...2...20/pkg...21247-20, 10-20-25 ml, w/cap...3...6/pkg...24019-06 OPTIONAL REAGENTS Calcium Standard Solution, 2.0 mg/l as CaCO3... 946 ml...20581-16 Nitric Acid, ACS... 500 ml...152-49 Nitric Acid Solution, 1:1... 500 ml...2540-49 Sodium Hydroxide Standard Solution 5.0 N... 100 ml MDB...2450-32 OPTIONAL APPARATUS ph Meter, sension 1, portable...each...51700-00 Thermometer, -10 to 110 C...each...1877-01 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 100

μ8141 p- (N2H4) HydraVer 2 0 μg/l N2H4 101

μg/l 11 240mL 3 10 mg/l20mg/l 10 mg/l Sampling and Storage Collect samples in glass or plastic containers. Fill the containers completely and cap them tightly. Avoid excessive agitation or exposure to air. Samples must be analyzed immediately after collection and cannot be preserved for later analysis. Accuracy Check Standard Solution Method To assure the accuracy of the test, prepare the following solutions: a) Prepare a 25 mg/l hydrazine stock solution by dissolving 0.1016 g of hydrazine sulfate in 1000 ml of oxygen-free deionized water. Use Class A glassware. Prepare this stock solution daily. b) Prepare a 100 μg/l hydrazine working solution by diluting 4.00 ml of the 25 mg/l stock solution to 1000 ml with deionized oxygen-free water. Prepare just before analysis. c) Use the working solution in place of the sample in Step 4. The result should be 100 μg/l hydrazine. Method Performance Precision In a single laboratory using a standard solution of 250 μg/l hydrazine (N2H4) and two representative lots of reagent with the instrument, a single operator obtained a standard 102

deviation of ±9 μg/l hydrazine. In a single laboratory using a standard solution of 250 μg/l hydrazine (N2H4) and two lots of AccuVac Ampuls with the instrument, a single operator obtained a standard deviation of ±3 μg/l hydrazine. Estimated Detection Limit The estimated detection limit for program 31 is 16 μg/l N2H4, and the estimated detection limit for program 32 is 10 μg/l N2H4. For more information on the estimated detection limit, see Section 1. Summary of Method Hydrazine reacts with the p-dimethylaminobenzaldehyde from the HydraVer 2 Reagent to form a yellow color which is proportional to the hydrazine concentration. () HydraVer 2... 1 ml...100 ml* MDB...1790-32... 10 ml... 4 L...272-56 () 25 ml...1......508-40 10-, 20- and 25 ml, w/ caps...2...6/pkg...24019-06 ( AccuVac) AccuVac...2...25/pkg...25240-25... 10 ml... 4 L...272-56 ( AccuVac), 50 L...2......500-41 OPTIONAL REAGENTS Hydrazine Sulfate, ACS...100 g...742-26 OPTIONAL APPARATUS AccuVac Snapper Kit...each...24052-00 Balance, AccuLab PocketPro, portable...each...25568-00 Cylinder, graduated, mixing, 25 ml...each...1896-40 Flask, volumetric, 100 ml, Class A...each...14574-42 Flask, volumetric, 1000 ml, Class A...each...14574-53 Pipet, serological, 1 ml...each...532-35 Pipet, TenSette, 0.1 to 1.0 ml...each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet...50/pkg...21856-96 Pipet, volumetric, Class A, 1.00 ml...each...14515-35 Pipet, volumetric, Class A, 4.00 ml...each...14515-04 Pipet Filler, safety bulb...each...14651-00 Thermometer, -10 to 110 C...each...1877-01 Weighing Boat, 67/46 mm, 8.9 cm sq....500/pkg...21790-00 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 103

0 mg/l Fe 104

Sampling and Storage Ferrous iron must be analyzed immediately and cannot be stored. Analyze samples as soon as possible to prevent oxidation of ferrous iron to ferric iron, which is not measured. Accuracy Check Standard Solution Method Prepare a ferrous iron stock solution (100 mg/l Fe2+) by dissolving 0.7022 grams of ferrous ammonium sulfate, hexahydrate, in deionized water. Dilute to 1 liter. Prepare immediately before use. Dilute 1.00 ml of this solution to 100 ml with deionized water to make a 1.00 mg/l standard solution. Prepare immediately before use. Run the test using the 1.00 mg/l Fe2+ Standard Solution by following either the powder pillow or AccuVac procedure. Results should be between 0.90 mg/l and 1.10 mg/l Fe2+. Method Performance Precision In a single laboratory using an iron standard solution of 2.00 mg/l Fe2+ and two representative lots of powder pillow reagents with the instrument, a single operator obtained a standard deviation of ±0.017 mg/l Fe2+. In a single laboratory using a standard solution of 2.00 mg/l Fe2+ and two representative lots of AccuVac ampuls with the instrument, a single operator obtained a standard deviation of ±0.009 mg/l Fe2+. Estimated Detection Limit The estimated detection limit for program 33 (powder pillows and AccuVac Ampuls) is 0.03 mg/l Fe. For more information on the estimated detection limit, see Section 1. 105

Summary of Method The 1,10-phenanthroline indicator in Ferrous Iron Reagent reacts with ferrous iron in the sample to form an orange color in proportion to the iron concentration. Ferric iron does not react. The ferric iron (Fe3+) concentration can be determined by subtracting the ferrous iron concentration from the results of a total iron test. ()... 1...100/pkg...1037-69, 10-20-25 ml, w/ cap...2...6/pkg...24019-06 ( ACCUVAC ) AccuVac... 1...25/pkg...25140-25, 50 ml...1......500-41 OPTIONAL REAGENTS Ferrous Ammonium Sulfate, hexahydrate, ACS...113 g... 11256-14 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS AccuVac Snapper Kit...each...24052-00 Balance, analytical, 115 V...each...26103-00 Balance, analytical, 230 V...each...26103-02 Clippers, for opening powder pillows...each...968-00 Flask, volumetric, 100 ml, Class A...each...14574-42 Flask, volumetric, 1000 ml, Class A...each...14574-53 Pipet, volumetric, Class A, 1.00 ml...each...14515-35 Pipet Filler, safety bulb...each...14651-00 Weighing Boat, 67/46 mm, 8.9 cm square...500/pkg...21790-00 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 106

107

108

Sampling and Storage Collect samples in acid-cleaned glass or plastic containers. No acid addition is necessary if analyzing the sample immediately. To preserve samples, adjust the ph to 2 or less with nitric acid (about 2 ml per liter). Preserved samples may be stored up to six months at room temperature. Adjust the ph to between 3 and 5 with 5.0 N Sodium Hydroxide Standard Solution before analysis. Correct the test result for volume additions; see Correcting for Volume Additions in Section 1 for more information. If only dissolved iron is to be determined, filter the sample before adding the acid. Accuracy Check Standard Additions Method a) Snap the neck off a 50 mg/l Iron PourRite Ampule Standard Solution. b) Use the TenSette Pipet to add 0.1, 0.2, and 0.3 ml of standard, respectively, to three 25-mL samples and mix thoroughly. c) For analysis using AccuVac Ampuls, transfer solutions to dry, clean 50-mL beakers to facilitate filling of the ampuls. For analysis with powder pillows, transfer only 10 ml of solution to the 10-mL sample cells. d) Analyze each standard addition sample as described above. The iron concentration should increase 0.2 mg/l for each 0.1 ml of standard added. e) If these increases do not occur, see Standard Additions in Section 1 for troubleshooting information. Standard Solution Method Prepare a 1.0-mg/L iron standard by diluting 1.00 ml of Iron Standard Solution, 100 mg/l Fe, to 100 ml with deionized water. Or, dilute 1.00 ml of an Iron PourRite Ampule Standard Solution (50 mg/l) to 50 ml in a volumetric flask. Prepare this solution daily. Run the test following the procedure for powder pillows or AccuVac Ampuls. Results should be between 0.90 mg/l and 1.10 mg/l Fe. Method Performance Precision In a single laboratory, using a standard solution of 2.00 mg/l Fe and two representative lots of powder pillow reagents with the instrument, a single operator obtained a standard deviation of ±0.017 mg/l. In a single laboratory, using a standard solution of 2.00 mg/l Fe and two representative lots of AccuVac ampuls with the instrument, a single operator obtained a standard eviation of ±0.009 mg/l Fe. Estimated Detection Limit (EDL) The EDL for program 33 is 0.03 mg/l Fe. For more information on derivation and use of Hach s estimated detection limit, see Section 1. Summary of Method FerroVer Iron Reagent reacts with all soluble iron and most insoluble forms of iron in the sample to produce soluble ferrous iron. This reacts with 1,10-phenanthroline indicator in the reagent to form an orange color in proportion to the iron concentration. 109

() FerroVer... 1... 100/pkg...21057-69, 10-20-25 ml, with screw cap... 1... 6/pkg...24019-06 REQUIRED REAGENTS & APPARATUS (Using AccuVac Ampuls) FerroVer AccuVac...1... 25/pkg...25070-25, 50 ml... 1......500-41 OPTIONAL REAGENTS Description Unit Cat. No. Ammonium Hydroxide, ACS...500 ml...106-49 Hydrochloric Acid Standard Solution, 6 N...500 ml...884-49 Hydrochloric Acid, ACS...500 ml...134-49 Iron Standard Solution, 100 mg/l...100 ml...14175-42 Iron PourRite Ampule Standard, 50 mg/l... 20/pkg...14254-20 Nitric Acid, ACS...500 ml...152-49 Nitric Acid Solution, 1:1...500 ml...2540-49 RoVer Rust Remover... 454 g...300-01 Sodium Hydroxide Standard Solution, 5.0 N...100 ml MDB...2450-32 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS AccuVac Snapper Kit... each...24052-00 Ampule Breaker, PourRite Ampules... each...24826-00 Clippers, Shears 71/4 "... each...23694-00 Cylinder, graduated, poly, 25 ml... each...1081-40 Cylinder, graduated, poly, 100 ml... each...1081-42 Digesdahl Digestion Apparatus, 115 V... each...23130-20 Digesdahl Digestion Apparatus, 230 V... each...23130-21 Filter Discs, glass, 47 mm... 100/pkg...2530-00 Filter Holder, membrane... each...2340-00 Filter Pump... each...2131-00 Flask, Erlenmeyer, 250 ml... each...505-46 Flask, filtering, 500 ml... each...546-49 OPTIONAL APPARATUS (continued) Description Unit Cat. No. Flask, volumetric, Class A, 50 ml...each...14574-41 Flask, volumetric, Class A, 100 ml...each...14574-42 Hot Plate, 4" diameter, 120 VAC...each...12067-01 Hot Plate, 4" diameter, 240 VAC...each...12067-02 ph Meter, sension 1, portable...each...51700-00 ph Indicator Paper, 1 to 11 ph...each...391-33 Pipet Filler, safety bulb...each...14651-00 Pipet, serological, 2 ml...each...532-36 Pipet, serological, 5 ml...each...532-37 110

Pipet, TenSette, 0.1 to 1.0 ml...each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet...50/pkg...21856-96 Pipet, volumetric, Class A, 1.00 ml...each...14515-35 Spoon, measuring, 0.1 g...each...511-00 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 111

0 mg/l Fe 112

(EDTA) g/l FerroVer TPTZTPTZ 4FerroZine 24 C (75 F)5 25mL2 1) 25-mL25 ml 2) 125-mL 3) FerroZine 4) 5) 2030 6) 25-mL 7) 25mL 8) 9) 92 4FerroZine 24 C (75 F)5 25mL2 113

Sampling and Storage Collect samples in acid-washed glass or plastic bottles. To preserve samples, adjust the sample ph to 2 or less with nitric acid (about 2 ml per liter). Samples preserved in this manner can be stored up to six months at room temperature. If only dissolved iron is to be reported, filter sample immediately after collection and before the addition of nitric acid. Before testing, adjust the sample ph to 3 5 with ammonium hydroxide, ACS. Do not exceed ph 5 as iron may precipitate. Correct test results for volume additions; see Correction for Volume Additions in Section 1 for more detailed information. Accuracy Check Standard Additions Method a) Snap the neck off an Iron Voluette Ampule Standard, 25 mg/l Fe. b) Use the TenSette Pipet to add 0.1 ml of standard to the prepared sample measured in Step 10. c) Swirl to mix and allow another five-minute reaction period, then measure the iron concentration as in Step 10. d) Add two additional 0.1-mL standard increments, taking a concentration reading after allowing the five-minute reaction period for each increment. e) Each 0.1 ml of standard added should cause a 0.1 mg/l increase in the concentration reading. f) If these increases do not occur, see Standard Additions in Section 1 for more information. Standard Solution Method Prepare a 0.4 mg/l iron working solution as follows: a) Pipet 1.00 ml of Iron Standard Solution, 100 mg/l Fe, into a 250-mL volumetric flask. b) Dilute to volume with deionized water. This solution should be prepared daily. Analyze the working solution according to the above procedure. Method Performance Precision In a single laboratory, using a standard solution of 0.80 mg/l iron and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of ±0.004 mg/l iron. Estimated Detection Limit The estimated detection limit for program 37 is 0.011 mg/l Fe. For more information on the estimated detection limit, see Section 1. Summary of Method The FerroZine Iron Reagent forms a purple colored complex with trace amounts of iron in samples that are buffered to a ph of 3.5. This method is applicable for determining trace levels of iron in chemical reagents and glycols and can be used to analyze samples containing magnetite (black iron oxide) or ferrites after treatment as described in Interferences. 114

() FerroZine... 1...50/pkg...2301-66...1......968-00, 10-20-25, w/cap...2...6/pkg...24019-06 OPTIONAL REAGENTS Ammonium Hydroxide, ACS... 500 ml...106-49 Hydrochloric Acid Solution, 1:1 (6N)... 500 ml...884-49 FerroZine Iron Reagent Solution... 1000 ml...2301-53 Iron Standard Solution, 100 mg/l Fe... 100 ml...14175-42 Iron Standard Solution, Voluette Ampule, 25 mg/l Fe, 10 ml...16/pkg...14253-10 Nitric Acid, ACS... 500 ml...152-49 Nitric Acid Solution, 1:1... 500 ml...2540-49 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS Ampule Breaker Kit...each...21968-00 Clippers, shears, 7¼-inch...each...20658-00 Cylinder, graduated, 25 ml...each...508-40 Dropper, calibrated, 0.5-mL & 1.0-mL mark...6/pkg...23185-06 Flask, erlenmeyer, 125 ml...each...505-43 Flask, volumetric, 250 ml, Class A...each...14574-46 Hot plate, 3 ½" diameter, 120 V...each...12067-01 Hot plate, 3 ½" diameter, 240 V...each...12067-02 ph Indicator Paper, 1 to 11 ph...5 rolls/pkg...391-33 Pipet, serological, 2 ml...each...532-36 ph Meter, EC10, portable...each...50050-00 Pipet, TenSette, 0.1 to 1.0 ml...each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet...50/pkg...21856-96 Pipet, volumetric, 1.00 ml, Class A...each...14515-35 Thermometer, -10 to 110 C...each...1877-01 Water Bath, with sample cell rack...each...1955-55 For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 115

116

0.00 mg/l Fe ph34 1.0N 1.0NpH35 Sampling and Storage Collect samples in acid-cleaned plastic or glass bottles. If prompt analysis is impossible, preserve the sample by adjusting to ph 2 or less with hydrochloric acid (about 2 ml per liter). Preserved samples may be stored up to six months at room temperature. If reporting only dissolved iron, filter the sample immediately after collection and before adding the acid. Before analysis, adjust the sample ph to between 3 and 4 with 5.0 N Sodium Hydroxide Standard Solution. Do not exceed ph 5 as iron may precipitate. Correct the test result for volume; see Correction for Volume Additions in Section 1. Accuracy Check Standard Additions Method a) Snap the top off an Iron PourRite Ampule Standard Solution, 25 mg/l Fe. b) Use the TenSette Pipet to add 0.2, 0.4 and 0.6 ml of standard to three 50-mL samples. Swirl gently to mix. c) Analyze each sample as described above. The iron concentration should increase by 0.1 mg/l for each 0.2 ml of standard added. d) If these increases do not occur, see Standard Additions in Section 1 for more Information. 117

Standard Solution Method Prepare a 0.4 mg/l iron working solution as follows: a) Pipet 1.00 ml of Iron Standard Solution, 100 mg/l Fe, into a 250-mL volumetric flask. b) Dilute to volume with deionized water. Prepare this solution daily. Analyze this working solution according to the above procedure. Results should be between 0.36 and 0.44 mg/l Fe. Method Performance Precision In a single laboratory, using a standard solution of 1.00 mg/l Fe and two representative lots of reagents with the instrument, a single operator obtained a standard deviation of À0.006 mg/l Fe. Estimated Detection Limit The estimated detection limit for program 38 is 0.03 mg/l Fe. For more information on the estimated detection limit, see Section 1. Summary of Method FerroMo Iron Reagent 1 contains a reducing agent combined with a masking agent. The masking agent eliminates interference from high levels of molybdate. The reducing agent converts precipitated or suspended iron (rust) to the ferrous state. FerroMo Iron Reagent 2 contains the indicator combined with a buffering agent. The indicator reacts with the ferrous iron in the sample, buffered between ph 3-4, resulting in a deep blue-purple color. FerroMo (100 tests)...25448-00 : (4) 25437-68, (2) 25438-66 FerroMo 1...1... 25/pkg...25437-68 FerroMo 2...1... 50/pkg...25438-66...1...968-00, 50 ml... 1......1896-41, 10-20-25 ml, w/cap... 2... 6/pkg...24019-06 OPTIONAL REAGENTS Hydrochloric Acid Solution, 6.0 N (1:1)...500 ml...884-49 Hydrochloric Acid, ACS...500 ml...134-49 Iron Standard Solution, 100 mg/l Fe...100 ml...14175-42 Iron Standard Solution, PourRite Ampule, 118

25 mg/l Fe, 2 ml... 20/pkg...24629-20 Sodium Hydroxide Standard Solution, 1.0 N...100 ml MDB...1045-32 Sodium Hydroxide Standard Solution, 5.0 N...100 ml MDB...2450-32 Sulfuric Acid Standard Solution, 1.0 N...100 ml MDB...1270-32 Water, deionized... 4 L... 272-56 OPTIONAL APPARATUS Ampule Breaker Kit... each...24846-00 Flask, volumetric, Class A, 250 ml... each...14574-46 ph Indicator Paper, 1 to 11 ph... 5 rolls/pkg...391-33 ph Meter, Sension.1, portable... each...51700-10 Pipet Filler, safety bulb... each...14651-00 Pipet, TenSette, 0.1 to 1.0 ml... each...19700-01 Pipet Tips, for 19700-01 Pipet... 50/pkg...21856-96 Pipet, volumetric, Class A, 1.00 ml... each...14515-35 For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 119

TPTZ 0.00 mg/l Fe 120

121

Sampling and Storage Collect samples in acid-washed glass or plastic bottles. Adjust the sample ph to 2 or less with nitric acid (about 2 ml per liter). Store samples preserved in this manner up to six months at room temperature. If reporting only dissolved iron, filter sample immediately after collection and before addition of nitric acid. Before testing, adjust the ph of the stored sample to between 3 and 4 with 5.0 N Sodium Hydroxide Standard Solution. Do not exceed ph 5 as iron may precipitate. Correct the test result for volume additions; see Correction for Volume Additions in Section 1. Accuracy Check Standard Additions Method (Powder Pillows) a) Snap the neck off a PourRite Iron Ampule Standard, 25 mg/l Fe. b) Use the TenSette Pipet to add 0.1 ml of standard to the prepared sample measured in Step 10. Swirl to mix. c) Measure the iron concentration as in Step 10. The measurement does not require the three-minute waiting period. d) Add two additional 0.1-mL aliquots of standard, measuring the concentration after each addition. The iron concentration should increase by 0.25 mg/l for each 0.1-mL addition of standard. e) If these increases do not occur, see Standard Additions in Section 1 for more information. Standard Additions Method (AccuVac Ampuls) a) Use a graduated cylinder to measure 25.0 ml of sample into each of three 50-mL beakers. b) Snap the neck off an Iron Ampule Standard, 25 mg/l Fe. c) Using a TenSette Pipet, add 0.1, 0.2 and 0.3 ml of standard, respectively, to the 50-mL beakers. Swirl to mix. d) Fill a TPTZ AccuVac Ampul from each beaker. e) Measure the concentration of each ampul according to the procedure. The iron concentration should increase by 0.1 mg/l for each 0.1 ml addition of standard. f) If these increases do not occur, see Standard Additions in Section 1 for more information. Standard Solution Method Prepare a 0.4 mg/l iron working solution as follows: a) Using Class A glassware, pipet 1.00 ml of Iron Standard Solution, 100 mg/l Fe, into a 250-mL volumetric flask. b) Dilute to volume with deionized water. Stopper and invert repeatedly to mix. Prepare this solution daily. 122

Method Performance Precision In a single laboratory using a standard solution of 1.00 mg/l Fe and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of À0.017 mg/l Fe. In a single laboratory using a standard solution of 1.00 mg/l Fe and one representative lot of AccuVac Ampuls with the instrument, a single operator obtained a standard deviation of À0.022 mg/l Fe. Estimated Detection Limit The estimated detection limit for program 39 is 0.04 mg/l Fe. For more information on the estimated detection limit, see Section 1. Summary of Method The TPTZ Iron Reagent forms a deep blue-purple color with ferrous iron. The indicator is combined with a reducing agent which converts precipitated or suspended iron, such as rust, to the ferrous state. The amount of ferric iron present can be determined as the difference between the results of a ferrous iron test and the concentration of total iron. () TPTZ... 1... 100/pkg...26087-99, 10-20-25 ml, w/cap... 1... 6/pkg...24019-06 ( ACCUVAC ) TPTZ AccuVac...1... 25/pkg...25100-25, 50 ml... 1......500-41, 10-20-25 ml, w/cap... 1... 6/pkg...24019-06 OPTIONAL REAGENTS Hydrochloric Acid Solution, 1:1, 6.0 N...500 ml...884-49 Iron Standard Solution, 100 mg/l Fe...100 ml...14175-42 Iron Standard Solution, PourRite Ampule, 25 mg/l Fe, 2 ml... 20/pkg...24629-20 Nitric Acid, ACS...500 ml...152-49 Nitric Acid Solution, 1:1...500 ml...2540-49 RoVer Rust Remover... 454 g...300-01 Sodium Hydroxide Standard Solution, 1.0 N...100 ml MDB...1045-32 Sodium Hydroxide Standard Solution, 5.0 N...100 ml MDB...2450-32 Sulfuric Acid Standard Solution...100 ml MDB...1270-32 Water, deionized... 4 L...272-56 123

8034 0 mg/l Mn 124

g/l Sampling and Storage Collect samples in acid-washed plastic bottles. Manganese may be lost by adsorption to glass container walls. Adjust the ph to less than 2 with nitric acid (about 2 ml per liter). Preserved samples may be stored up to six months at room temperature. Adjust the ph to 4 to 5 with 5.0 N sodium hydroxide before analysis. Do not exceed ph 5, as manganese may be lost as a precipitate. Correct the test result for volume additions; see Correction for Volume Additions in Section 1 for more information. If only dissolved Mn is to be determined, filter before acid addition. Accuracy Check Standard Additions Method a) Snap the neck off a Manganese Voluette Ampule Standard Solution, 250 mg/l Mn. b) Use the TenSette Pipet to add 0.1, 0.2 and 0.3 ml of standard, respectively, to the three 25-mL water samples. Swirl to mix. 125

c) Transfer only 10 ml of each solution to the 10-mL sample cells. d) Analyze each standard addition sample as described in the procedure. The manganese concentration should increase 1.0 mg/l for each 0.1 ml of standard added. e) If these increases do not occur, see Standard Additions in Section 1 for troubleshooting information. Standard Solution Method Prepare a 5.0 mg/l manganese standard solution by pipetting (use a TenSette or Class A volumetric pipet) 5.00 ml of Manganese Standard Solution, 1000 mg/l Mn, into a 1000-mL volumetric flask. Dilute to the mark with deionized water. Or, prepare this standard by diluting 1.00 ml of a High Range Manganese Standard Voluette Ampule, 250 mg/l, to 50 ml. Prepare these solutions daily. Use these solutions as the sample in the procedure. Method Performance Precision In a single laboratory, using a standard solution of 10.00 mg/l Mn and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of 0.18 mg/l Mn. Estimated Detection Limit The estimated detection limit for program 41 is 0.12 mg/l Mn. For more information on the estimated detection limit, see Section 1. Summary of Method Manganese in the sample is oxidized to the purple permanganate state by sodium periodate, after buffering the sample with citrate. The purple color is directly proportional to the manganese concentration. (100 tests) 10 ml...24300-00 : (1) 21076-69, (1) 21077-69 ()... 1... 100/pkg...21076-69... 1... 100/pkg...21077-69, 10-20-25 ml, w/cap...2... 6/pkg...24019-06 126

OPTIONAL REAGENTS Hydrochloric Acid, 6 N...500 ml...884-49 Manganese Standard Solution, 1000 mg/l Mn...100 ml...12791-42 Manganese Standard Solution, Voluette ampule, High Range, 250 mg/l Mn, 10 ml... 16/pkg...14258-10 Nitric Acid, ACS...500 ml...152-49 Nitric Acid Solution 1:1...500 ml...2540-49 Sodium Hydroxide Solution, 5.0 N...100 ml MDB...2450-32 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS Ampule Breaker Kit... each...21968-00 Flask, Erlenmeyer, 250 ml... each...505-46 Flask, volumetric, Class A, 50 ml... each...14574-41 Flask, volumetric, Class A, 100 ml... each...14574-42 Flask, volumetric, Class A, 1000 ml... each...14574-53 ph Indicator Paper, 1 to 11 ph... 5 rolls/pkg...391-33 ph Meter, sension.1, portable... each...51700-10 Pipet, serological, 5 ml... each...532-37 Pipet, TenSette, 0.1 to 1.0 ml... each...19700-01 Pipet, TenSette, 1.0 to 10.0 ml... each...19700-10 Pipet Tips, for 19700-01 TenSette Pipet... 50/pkg...21856-96 Pipet Tips, for 19700-10 TenSette Pipet... 50/pkg...21997-96 Pipet, volumetric, Class A, 5.00 ml... each...14515-37 Pipet, volumetric, Class A, 1.00 ml... each...14515-35 Pipet Filler, safety bulb... each...14651-00 For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 127

8149 128

0 mg/l Mn g/l Sampling and Storage Collect samples in a clean glass or plastic container. Adjust the ph to 2 or less with nitric acid (about 2 ml per liter). Preserved samples can be stored up to six months at room temperature. Adjust the ph to 4.0-5.0 with 5.0 N sodium hydroxide before analysis. Correct the test result for volume additions; see Correction for Volume Additions in Section 1. 129

Accuracy Check Standard Additions Method Note: Volume accuracy is very important when performing standard additions with 10-mL volumes. The fill mark on the 10-mL sample cell is not intended to measure standard addition volumes. a) Fill three 10-mL graduated mixing cylinders with 10.0 ml of sample. b) Snap the neck off a Manganese Voluette Ampule Standard, 10 mg/l Mn. c) Use the TenSette Pipet to add 0.1 ml, 0.2 ml and 0.3 ml of standard, respectively, to the three mixing cylinders. Stopper and mix each thoroughly. d) Analyze each sample as described in the procedure. The manganese concentration should increase 0.1 mg/l for each 0.1 ml of standard added. e) If these increases do not occur, see Standard Additions in Section 1 for more information. Note: An alternative to the above procedure is to pipet 10.0 ml of sample into dry sample cells before performing standard additions. A volumetric pipet or a TenSette Pipet can be used to deliver the sample volume. Standard Solution Method Prepare a 0.5 mg/l manganese standard solution as follows: a) Pipet 5.00 ml of Manganese Standard Solution, 1000 mg/l Mn, into a 1000-mL volumetric flask. b) Dilute to the mark with deionized water. Prepare this solution daily. c) Pipet 10.00 ml of the solution from Step b into a 100-mL volumetric flask. d) Dilute to the mark with deionized water. This second dilution is equivalent to 0.5 mg/l Mn. Method Performance Precision In a single laboratory using a standard solution of 0.5 mg/l Mn and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of À0.013 mg/l Mn. Estimated Detection Limit The estimated detection limit for program 43 is 0.007 mg/l Mn. For more information on the estimated detection limit, see Section 1. Waste Management The alkaline cyanide solution contains cyanide. Cyanide solutions should be collected for disposal as reactive (D003) waste. Store all cyanide solutions in a caustic solution with ph >11 to prevent release of hydrogen cyanide gas. In case of a spill, clean up the area as outlined below: 1. Use a fume hood or self-contained breathing apparatus. 2. While stirring, add the waste to a beaker containing a strong solution of sodium hydroxide and calcium hypochlorite or sodium hypochlorite (household bleach). 3. Maintain a strong excess of hydroxide and hypochlorite. Let the solution stand for 24 hours. 4. Flush the solution down the drain with a large excess of water. 130

Summary of Method The PAN method is a highly sensitive and rapid procedure for detecting low levels of manganese. An ascorbic acid reagent is used initially to reduce all oxidized forms of manganese to Mn2+. An alkaline-cyanide reagent is added to mask any potential interferences. PAN Indicator is then added to combine with the Mn2+ to form an orange-colored complex. (100 tests) 10 ml...24333-00 : (2) 21223-32, (2) 14577-99, (2) 21224-32, (1) 21128-02...30...50 ml SCDB...21223-26... 2...100/pkg...14577-99 PAN 0.1%....42... 50 ml SCDB...21224-26... 10 ml... 4 L...272-56 REQUIRED APPARATUS 25 ml...1.......508-40 10-20-25 ml, w/cap...2...6/pkg...24019-06 OPTIONAL REAGENTS Hydrochloric Acid Solution, 1:1 (6 N)... 500 ml...884-49 Manganese Standard Solution, 1000 mg/l Mn... 100 ml...12791-42 Manganese Standard Sol n, PourRite Ampule, 20 mg/l Mn, 2 ml...20/pkg.... 21128-20 Nitric Acid Solution, 1:1... 500 ml...2540-49 Rochelle Salt Solution...29 ml DB...1725-33 Sodium Hydroxide Solution, 50%... 500 ml...2180-49 Nitric Acid, ACS... 500 ml...152-49 OPTIONAL APPARATUS Ampule Breaker, PourRite Ampule...each...24846-00 Beaker, glass, 1000 ml...each...500-53 Cylinder, graduated, mixing, 10 ml...each...20886-38 Dropper, plastic, calibrated, 1.0 ml...20/pkg...21247-20 Flask, volumetric, Class A, 1000 ml...each...14574-53 Flask, volumetric, Class A, 100 ml...each...14574-42 Pipet, TenSette, 0.1 to 1.0 ml...each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet...50/pkg...21856-96 Pipet, volumetric, Class A, 10.0 ml...each...14515-38 Pipet, volumetric, Class A, 5.0 ml...each...14515-37 Pipet Filler, safety bulb...each...14651-00 For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 131

8036 132

0 mg/l Mo6 g/l Sampling and Storage Collect samples in clean plastic bottles. Adjust the ph to 2 or less with nitric acid (about 2 ml per liter). Preserved samples can be stored up to 6 months at room temperature. Adjust the ph to 7 with 5.0 N sodium hydroxide before analysis. Correct the test result for volume additions; see Volume Additions (Section 1) for more information. Accuracy Check Standard Additions Method a) Fill three 25-mL graduated mixing cylinders with 25 ml of sample. b) Snap the neck off a Molybdenum Voluette Ampule Standard Solution, 500 mg/l Mo6+. 133

c) Use the TenSette Pipet to add 0.1, 0.2 and 0.3 ml of standard, respectively, to the three mixing cylinders. Stopper each and mix thoroughly. d) For analysis with AccuVac Ampuls, transfer solutions to dry, clean 50-mL beakers. For analysis with powder pillows, transfer only 10 ml of solution to the sample cells. e) Analyze each standard addition sample as described in the procedure. The molybdenum concentration reading should increase 2.0 mg/l for each 0.1 ml of standard added. f) If these increases do not occur, see Standard Additions in Section 1 for troubleshooting information. Standard Solution Method To assure the accuracy of the test, use a Molybdenum Standard Solution, 10.0 mg/l Mo6+. Follow the procedure for powder pillows or AccuVac Ampuls. Results should be between 9.0 and 11.0 mg/l Mo6+. Standard Adjust To adjust the calibration curve using the reading obtained with the 10.0-mg/L standard solution, press the SETUP key and scroll (using the arrow keys) to the STD setup option. Press ENTER to activate the standard adjust option. Then enter 10.0 to edit the standard concentration to match that of the standard used. Press ENTER to complete the adjustment. See Section 1, Standard Curve Adjustment for more information. Method Performance Precision In a single laboratory using a standard solution of 20.0 mg/l Mo6+ and two representative lots of powder pillows with the instrument, a single operator obtained a standard deviation of À0.3 mg/l Mo6+. In a single laboratory using a standard solution of 20.0 mg/l Mo6+ and two representative lots of AccuVac Ampuls with the instrument, a single operator obtained a standard deviation of À0.1 mg/l Mo6+. Estimated Detection Limit The estimated detection limit for program 44 is 0.2 mg/l Mo6+. For more information on the estimated detection limit, see Section 1. Summary of Method Powder Pillows MolyVer 1 and 2 Reagents are added to buffer and condition the sample. MolyVer 1 contains a buffer to control the ph in addition to a chelating agent to mask interferences. MolyVer 3 provides the mercaptoacetic acid, which reacts with molybdate molybdenum to form a yellow color proportional to the molybdenum concentration. AccuVac Ampuls The CDTA Solution masks metal interferences. The MolyVer 6 reagent provides the mercaptoacetic acid, which reacts with molybdate molybdenum to form a yellow color proportional to the molybdenum concentration. 134

(), 10 ml (100 tests)... 26041-00 : (1) 26042-99, (1) 26043-99, (1) 26044-99, (1) 14265-02 MolyVer 1...1... 100/pkg...26042-99 MolyVer 2...1... 100/pkg...26043-99 MolyVer 3...1... 100/pkg...26044-99 ( ACCUVAC ) MolyVer 6AccuVac (25 tests)... 25220-98 : (1) 25220-25, (1) 26154-36 CDTA 0.4M... 4... 15 ml SCDB...26154-36 MolyVer 6 AccuVac... 1... 25/pkg...25220-25 ().........968-00, 10-20-25 ml, w/cap... 2... 6/pkg...24019-06 ( ACCUVAC ), 50 ml... 2......500-41 10-20-25 ml, w/cap... 1... 6/pkg...24019-06 OPTIONAL REAGENTS Molybdenum Standard Solution, 10 mg/l Mo6+...100 ml...14187-42 Molybdenum Standard Solution, Voluette Ampule, 500 mg/l Mo6+, 10 ml... 16/pkg...14265-10 Nitric Acid, ACS...500 ml...152-49 Sodium Hydroxide Standard Solution, 5.0 N...100 ml MDB...2450-32 Sulfamic Acid Powder Pillows... 100/pkg...1055-99 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS AccuVac Snapper Kit... each...24052-00 Ampule Breaker Kit... each...21968-00 Cylinder, graduated, mixing, 25 ml... each...20886-40 Filter Paper, folded, 12.5 cm... 100/pkg...1894-57 Flask, Erlenmeyer, 250 ml... each...505-46 Funnel, poly, 65 mm... each...1083-67 Pipet, serological, 5 ml... each...532-37 Pipet, TenSette, 0.1 to 1.0 ml... each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet... 50/pkg...21856-96 For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 135

8169 136

0 mg/l Mo6 g/l 137

HEDP30g/L10 90.9HEDP 30mg/L Sampling and Storage Collect samples in glass or plastic bottles. Accuracy Check Standard Addition Method a) Add 25 ml of sample to three 25-mL mixing cylinders. b) Snap the neck off a Molybdenum PourRite Ampule Standard Solution, 75 mg/l Mo6+. c) Use the TenSette Pipet to add 0.1, 0.2 and 0.3 ml of standard, respectively, to three 25-mL samples. Mix thoroughly. d) Analyze 20 ml of each spiked sample as described in the procedure. The molybdenum concentration reading should increase by 0.3 mg/l for each 0.1 ml addition of standard. e) If these increases do not occur, see Standard Additions in Section 1 for more information. Standard Solution Method Prepare a 2.0-mg/L molybdenum standard solution by pipetting 10 ml of a 10-mg/L Molybdenum Standard Solution into a 50-mL graduated mixing cylinder. Dilute to the mark with deionized water and mix thoroughly. Analyze 20 ml of this solution according to the procedure. 138

Method Performance Precision In a single laboratory using standard solutions of 2.00 mg/l Mo6+ and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of À0.009 mg/l Mo6+. Estimated Detection Limit The estimated detection limit for program 47 is 0.07 mg/l Mo6+. For more information on the estimated detection limit, see Section 1. Summary of Method The ternary complex method for molybdenum determination is a method in which molybdate molybdenum reacts with an indicator and sensitizing agent to give a stable blue complex. t, 20 ml (100 tests)...24494-00 : (1) 23524-49, (1) 23525-12, (1) 25575-02 1...1...100/pkg...23524-49 2... 0.5 ml....50 ml MDB...23525-12, 25 ml... 1......1896-40, 10-20-25 ml, w/cap... 2...6/pkg...24019-06 OPTIONAL REAGENTS Hydrochloric Acid Solution, 1:1, 6.0 N... 500 ml...884-49 Molybdenum Standard Solution, PourRite Ampule 75 mg/l Mo6+, 2 ml...20/pkg...25575-20 Molybdenum Standard Solution, 10 mg/l Mo6+... 100 ml...14187-42 Sodium Hydroxide Standard Solution, 1.0 N... 100 ml MDB...1045-32 Water, deionized...4 L...272-56 OPTIONAL APPARATUS Cylinder, mixing, graduated, 50 ml...each...1896-41 Filter Paper, folded, 12.5 cm...100/pkg...1894-57 Funnel, poly, 65 mm...each...1083-67 ph Paper, 1-11 ph units...5 rolls/pkg...391-33 Pipet, TenSette, 0.1 to 1.0 ml...each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet...50/pkg...21856-96 Pipet, volumetric, 10.00 ml, Class A...each...14515-38 Pipet Filler, safety bulb...each...12189-00 PourRite Ampule Breaker...each...24846-00 For Technical Assistance, Price and Ordering In the U.S.A. call 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 139

140

141

Sampling and Storage Collect samples in acid-washed plastic bottles. Adjust the sample ph to 2 or less with nitric acid (about 5 ml per liter). Preserved samples can be stored up to six months at room temperature. Adjust the sample ph to between 3 and 8 with 5.0 N Sodium Hydroxide Standard Solution just before analysis. Do not exceed ph 8 as this may cause some loss of nickel as a precipitate. Correct test results for volume additions, see Correcting for Volume Additions, (Section 1) for more information. Accuracy Check Standard Solution Method Prepare a 0.5 mg/l nickel standard solution by diluting 10.0 ml of a 5 mg/l working stock solution to 100 ml in a 100-mL volumetric flask. The working stock solution should be prepared daily by diluting 5.00 ml of Nickel Standard Solution, 1000 mg/l as Ni, to 1000 ml with deionized water. Or, using the TenSette Pipet, add 0.2 ml of a Nickel Voluette Ampule Standard Solution, 300 mg/l Ni, into a 100-mL volumetric flask. Dilute to volume with deionized water. This is a 0.6 mg/l standard solution. Method Performance Precision In a single laboratory using a standard solution of 0.50 mg/l nickel and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of À0.008 mg/l nickel. Estimated Detection Limit The estimated detection limit for program 48 is 0.013 mg/l Ni. For more information on the estimated detection limit, see Section 1. Summary of Method After buffering the sample and masking any Fe3+ with pyrophosphate, the nickel is reacted with 1-(2-Pyridylazo)-2-Naphthol indicator. The indicator forms complexes with most metals present. After color development, EDTA is added to destroy all metal-pan complexes except nickel and cobalt., 25 ml (100 tests)... 22426-00 : (2) 7005-99, (4) 21501-66, (2) 21502-32 EDTA...2... 100/pkg...7005-99 -...2... 50/pkg...21501-66 P.A.N., 0.3%... 2 ml...100 ml MDB...21502-32, 10-20-25, w/caps... 2... 6/pkg...24019-06... 10 ml... 4 L...272-56 142

,... 1......968-00, 25 ml... 1......20886-40 OPTIONAL REAGENTS Nickel Standard Solution, 1000 mg/l Ni...100 ml...14176-42 Nickel Standard Solution, Voluette Ampule, 300 mg/l Ni, 10 ml... 16/pkg...14266-10 Nitric Acid, ACS...500 ml...152-49 Nitric Acid Solution, 1:1...500 ml...2540-49 Sodium Hydroxide Standard Solution, 5.0 N...100 ml MDB...2450-32 OPTIONAL APPARATUS Ampule Breaker Kit... each...21968-00 Flask, volumetric, Class A, 100 ml... each...14574-42 Flask, volumetric, Class A, 1000 ml... each...14574-53 ph Paper, 1 to 11 ph units... 5 rolls/pkg...391-33 ph Meter, EC10, portable... each...50050-00 Pipet, serological, 1 ml... each...532-35 Pipet, serological, 5 ml... each...532-37 Pipet, TenSette, 0.1 to 1.0 ml... each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet... 50/pkg...21856-96 Pipet, volumetric, Class A, 5.0 ml... each...14515-37 Pipet, volumetric, Class A, 10.0 ml... each...14515-38 Pipet Filler, safety bulb... each...14651-00 Thermometer, -10 to 110 ãc... each...1877-01 For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 143

144

1 2 145

Sampling and Storage Collect samples in clean plastic or glass bottles. Store at 4 C (39 F) or lower if the sample is to be analyzed within 24 to 48 hours. Warm to room temperature before running the test. For longer storage periods, adjust sample ph to 2 or less with sulfuric acid, ACS (about 2 ml per liter). Sample refrigeration is still required. Before testing the stored sample, warm to room temperature and neutralize with 5.0 N Sodium Hydroxide Standard Solution. Do not use mercury compounds as preservatives. Correct the test result for volume additions; see Correction for Volume Additions (Section 1) for more information. Accuracy Check Standard Additions Method a) Fill three 25-mL mixing cylinders with 25 ml of sample. b) Snap the neck off a Nitrate Nitrogen Ampule Standard, 500 mg/l nitrate nitrogen. c) Use the TenSette Pipet to add 0.1, 0.2, and 0.3 ml of Nitrate Nitrogen Standard Solution to the three samples. Stopper and mix thoroughly. d) For AccuVac analysis, transfer the solutions to clean, dry 50-mL beakers. For analysis with powder pillows, transfer only 10 ml of solution to clean, dry sample cells. e) Analyze each sample as described above. The nitrate nitrogen (NO3 --N) concentration should increase 2.0 mg/l for each 0.1 ml of standard added. f) If these increases do not occur, see Standard Additions (Section 1) for more information. Standard Solution Method Use a Hach Nitrate-Nitrogen Standard Solution, 10.0 mg/l NO3-N, listed under Optional Reagents as the sample and perform the procedure as described above. Standard Adjust To adjust the calibration curve using the reading obtained with the 10.0-mg/L standard solution, press the SETUP key and scroll (using the arrow keys) to the STD setup option. Press ENTER to activate the standard adjust option. Then enter 10.0 to edit the standard concentration to match that of the standard used. Press ENTER to complete the curve adjustment. See Section 1, Standard Curve Adjustment for more information. If you are using a reagent blank correction, the blank correction should be entered before the Standard Adjust value is entered. Method Performance Precision In a single laboratory using standard solutions of 25.0 mg/l nitrate nitrogen (NO3 --N) and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of +0.3 mg/l nitrate nitrogen for program #50 and ±1.7 mg/l nitrate nitrogen for program # 51. 146

Estimated Detection Limit The estimated detection limit for program 50 is 0.5 mg/l NO3 -N and 0.8 mg/l NO3 -N for program 51. For more information on the estimated detection limit, see Section 1. Summary Of Method Cadmium metal reduces nitrates present in the sample to nitrite. The nitrite ion reacts in an acidic medium with sulfanilic acid to form an intermediate diazonium salt which couples to gentisic acid to form an amber-colored product. Pollution Prevention and Waste Management NitraVer 5 contains cadmium metal. Both samples and reagent blanks will contain cadmium (D006) at a concentration regulated as hazardous wastes by the Federal RCRA. Do not pour these solutions down the drain. See Section 3 for more information on proper disposal of these materials. () NitraVer 5...1...100/pkg...21061-69, 10-20-25 ml, w/cap... 2...6/pkg...24019-06 ( ACCUVAC ) NitraVer 5...1...25/pkg...25110-25, 50 ml... 1...each...500-41... 1...6/pkg...1731-06 OPTIONAL REAGENTS Bromine Water 30 g/l... 29 ml*...2211-20 Nitrate Nitrogen Standard Solution, 10.0 mg/l as (NO3--N)... 500 ml...307-49 Nitrate Nitrogen Standard Solution, 1000 mg/l as (NO3--N)... 500 ml...12792-49 Nitrate Nitrogen Standard Solution, PourRite ampule, 500 mg/l as NO3--N, 2 ml...20/pkg...14260-20 Phenol Solution... 29 ml...2112-20 Sodium Hydroxide Standard Solution, 5.0 N... 50 ml*...2450-26 Sulfuric Acid, ACS... 500 ml*...979-49 Water, deionized...4 L...272-56 OPTIONAL APPARATUS AccuVac Snapper Kit... each... 24052-00 Cylinder, graduated, mixing, 25 ml... each... 1896-40 Dropper, for 29-mL bottle... each... 2258-00 ph Indicator Paper, 1 to 11 ph... 5 rolls/pkg... 391-33 ph Meter, sension 1, portable... each... 51700-10 Pipet Filler, safety bulb... each... 14651-00 Pipet, serological, 2 ml... each... 532-36 Pipet, TenSette, 0.1 to 1.0 ml... each... 19700-01 147

Pipet Tips, for 19700-01 TenSette Pipet... 50/pkg... 21856-96 PourRite Ampule Breaker... each... 24846-00 Thermometer, -10 to 110 C... each...1877-01 For Technical Assistance, Price and Ordering In the U.S.A. call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 148

NitraVer 5 NO3-N (NO3) 5:00 TIMER 2 149

0 mg/l NO3-N NO3-N (or NO3) g/l 1 2 150

Sampling and Storage Collect samples in clean plastic or glass bottles. Store at 4 C (39 F) or lower if the sample is to be analyzed within 24 to 48 hours. Warm to room temperature before running the test. For longer storage periods, adjust sample ph to 2 or less with sulfuric acid, ACS (about 2 ml per liter). Sample refrigeration is still required. Before testing the stored sample, warm to room temperature and neutralize with 5.0 N Sodium Hydroxide Standard Solution. Do not use mercury compounds as preservatives. Correct the test result for volume additions; see Correction for Volume Additions, (Section 1) for more information. Accuracy Check Standard Additions Method a) Fill three 25-mL graduated mixing cylinders with 25 ml of sample. b) Snap the neck off a Nitrate Nitrogen Ampule Standard Solution, 100 mg/l NO3-N. c) Use the TenSette Pipet to add 0.1, 0.2, and 0.3 ml of the standard to the three samples. Stopper and mix well. d) For analysis with AccuVac Ampuls, transfer the solutions to dry, clean 50 ml beakers. For analysis with powder pillows, transfer only 10 ml of the solution to dry, clean sample cells. e) Analyze each sample as described above. The nitrate nitrogen (NO3-N) concentration should increase 0.4 mg/l for each 0.1 ml of standard added. f) If these increases do not occur, see Standard Additions (Section 1) for more information. Standard Solution Method A 1.0 mg/l Nitrate Nitrogen Standard Solution is available from Hach. Use this standard in place of sample in the above procedure. Standard Adjust To adjust the calibration curve using the reading obtained with the 1.00-mg/L standard solution, press the SETUP key and scroll (using the arrow keys) to the STD setup option. Press ENTER to activate the standard adjust option. Then enter 1.0 to edit the standard concentration to match that of the standard used. Press ENTER to complete the adjustment. See Section 1, Standard Curve Adjustment for more information. Method Performance Precision In a single laboratory using a standard solution of 3.0 mg/l nitrate nitrogen (NO3--N) and two representative lots of powder pillows with the instrument, a single operator obtained a standard deviation of +0.2 mg/l nitrate nitrogen. In a single laboratory using a standard solution of 3.0 mg/l NO3-N and two representative lots of AccuVac Ampuls with the instrument, a single operator obtained a standard deviation of +0.1 mg/l nitrate nitrogen. 151

Estimated Detection Limit The estimated detection limit for programs 53 and 54 is 0.2 mg/l NO3-N. For more information on the estimated detection limit, see Section 1. Summary of Method Cadmium metal reduces nitrates present in the sample to nitrite. The nitrite ion reacts in an acidic medium with sulfanilic acid to form an intermediate diazonium salt which couples to gentisic acid to form an amber-colored product. Pollution Prevention and Waste Management NitraVer 5 contains cadmium metal. Both samples and reagent blanks will contain cadmium (D006) at a concentration regulated as hazardous waste by the Federal RCRA. Do not pour these solutions down the drain. See Section 3 for more information on proper disposal of these materials. () NitraVer 5...1...100/pkg...21061-69, 10-20-25 ml, w/cap...2...6/pkg...24019-06 ( ACCUVAC ) NitraVer 5...1...25/pkg...25110-25, 50 ml... 1...each...500-41... 1...6/pkg...1731-06 OPTIONAL REAGENTS Bromine Water 30 g/l... 29 ml*...2211-20 Nitrate Nitrogen Standard Solution, 1.0 mg/l as NO3-N...500 ml...2046-49 Nitrate Nitrogen Standard Solution, 100 mg/l as NO3-N...500 ml...1947-49 Nitrate Nitrogen Standard Solution, PourRite Ampule, 100 mg/l as NO3-N, 2 ml... 20/pkg...1947-20 Phenol Solution, 30 g/l...29 ml...2112-20 Sodium Hydroxide Standard Solution, 5.0 N... 50 ml SCDB*...2450-26 Sulfuric Acid, ACS...500 ml*...979-49 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS AccuVac Snapper Kit... each...24052-00 Cylinder, graduated, mixing, 25 ml... each...20886-40 Dropper, for 1-oz bottle... each...2258-00 ph Paper, 1 to 11 ph units... 5 rolls/pkg...391-33 ph Meter, sension 1, portable... each...51700-10 Pipet Filler, safety bulb... each...14651-00 Pipet, serological, 2 ml... each...532-36 Pipet, TenSette, 0.1 to 1.0 ml... each...19700-01 152

Pipet Tips, for 19700-01 TenSette Pipet... 50/pkg...21856-96 PourRite Ampule Breaker... each...24846-00 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 153

NO3-N (NO3) 154

15:00 TIMER 3 0 mg/l NO3-N NO3-N (or NO3) g/l 155

Standard Solution Method Prepare a 0.20 mg/l nitrate nitrogen standard by diluting 2.00 ml of a 10.0 mg/l Nitrate Nitrogen Standard Solution to 100.0 ml with deionized water. Use this standard in place of sample in Step 3. Standard Adjust To adjust the calibration curve using the reading obtained with the 0.20-mg/L standard solution, press the SETUP key and scroll (using the arrow keys) to the STD setup option. Press ENTER to activate the standard adjust option. Then enter 0.20 to edit the standard concentration to match that of the standard used. Press ENTER to complete the curve adjustment. If you are using a reagent blank correction, the blank correction should be entered before the Standard Adjust feature is entered. See Section 1, Standard Curve Adjustment for more information. Method Performance Precision In a single laboratory using a standard solution of 0.25 mg/l nitrate nitrogen (NO3-N) and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of +0.03 mg/l nitrate nitrogen. Estimated Detection Limit The estimated detection limit for program 55 is 0.01 mg/l NO3-N. For more information on the estimated detection limit, see Section 1. Summary of Method Cadmium metal reduces nitrates present in the sample to nitrite. The nitrite ion reacts in an acidic medium with sulfanilic acid to form an intermediate diazonium salt which couples to chromotropic acid to form a pink-colored product. Pollution Prevention and Waste Management NitaVer 6 contains cadmium metal. Both samples and reagent blanks will contain cadmium (D006) at a concentration regulated as hazardous wastes by the Federal RCRA. Do not pour these solutions down the drain. See Section 3 for more information on proper disposal of these materials. (100 tests)..... 24298-00 : (1) 21071-69, (1) 21072-49 NitriVer 3...1... 100/pkg...21071-69 NitraVer 6...1... 100/pkg...21072-49 25 ml... 1......1896-40 10-20-25 ml, w/ cap... 2... 6/pkg...24019-06 157

OPTIONAL REAGENTS Description Unit Cat. No. Bromine Water, 30 g/l...29 ml*...2211-20 Nitrate Nitrogen Standard Solution, 10.0 mg/l as NO3--N...500 ml...307-49 Nitrate Nitrogen Standard Solution, Voluette ampule, 12 mg/l as NO3--N, 2 ml... 20/pkg...25587-20 Phenol Solution, 30 g/l...29 ml...2112-20 Pretreatment Kit, contains: (1) 2112-20, (1) 2211-20... each...2268-00 Sodium Hydroxide Standard Solution, 5.0 N... 50 ml* SCDB...2450-26 Sulfuric Acid, ACS...500 ml*...979-49 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS Ampule Breaker, PourRite Ampules... each...24846-00 Dropper, for 29-mL bottle... each...2258-00 Flask, volumetric, Class A, 100 ml... each...14574-42 ph Indicator Paper, 1 to 11 ph... 5-roll/pkg...391-33 ph Meter, sension 1, portable... each...51700-10 Pipet, serological, 2 ml... each...532-36 Pipet, TenSette, 0.1 to 1.0 ml... each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet... 50/pkg...21856-96 Pipet, volumetric, Class A, 2.00 ml... each...14515-36 Pipet Filler, safety bulb... each...14651-00 Thermometer, -10 to 110 C... each... 1877-01 Nitrate at these levels can be determined directly using the Nitrate Ion Selective Electrode (Cat. No. 50235-00). For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 158

NO3-N 159

0.0 mg/l NO3-N 1 mg/l 1000 mg/l 12 mg/l100mg/l 400mg10mL 160

Sampling and Storage Collect samples in clean plastic or glass bottles. Store at 4 C (39 F) or lower if the sample is to be analyzed within 24 to 48 hours. Warm to room temperature before running the test. For longer storage periods (up to 14 days), adjust sample ph to 2 or less with sulfuric acid, ACS (about 2 ml per liter). Sample refrigeration is still required. Before testing the stored sample, warm to room temperature and neutralize with 5.0 N Sodium Hydroxide Standard Solution. Do not use mercury compounds as preservatives. Correct the test result for volume additions; see Correction for Volume Additions in Section 1 for more information. Accuracy Check Standard Additions Method a) Fill three 25-mL graduated mixing cylinders with 25 ml of sample. b) Snap the neck off a fresh High Range Nitrate Nitrogen Voluette Ampule Standard, 500 mg/l NO3-N. c) Use the TenSette Pipet to add 0.1, 0.2, and 0.3 ml of standard to the three mixing cylinders, respectively. Mix each thoroughly. d) Analyze each sample as described in the procedure; use a 1-mL aliquot of the spiked sample in each test. The nitrogen concentration should increase 2.0 mg/l for each 0.1 ml of standard added. e) If these increases do not occur, see Standard Additions (Section 1) for more information. Standard Solution Method To test accuracy, prepare a 20.0 mg/l nitrate nitrogen standard solution by pipetting 2.00 ml of a High Range Nitrate Nitrogen Voluette Ampule Standard Solution, 500 mg/l NO3--N, into a 50 ml Class A volumetric flask. Dilute to the line with deionized water. Substitute this standard for the sample and perform the test as described in the procedure. Method Performance Precision In a single laboratory, using a standard solution of 25.0 mg/l nitrate nitrogen (NO3-N) and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of ± 0.5 mg/l NO3-N. Estimated Detection Limit The estimated detection limit for program 57 is 0.3 mg/l NO3-N. For more information on the estimated detection limit, see Section 1. Summary of Method Nitrate in the sample reacts with chromotropic acid under strongly acidic conditions to yield a yellow product with a maximum absorbance at 410 nm. 161

NitraVer Test N Tube (50 tests)... 26053-45 : (1) 26055-46, (1) 272-42, *(50) Nitrate... 1... 50/pkg... * NitraVer B... 1... 50/pkg...26055-46 COD... 1...48464-00... 1...25843-35 TenSette, 0.1 to 1.0 ml... 1...19700-01 Pipet Tips, for 19700-01 TenSette Pipet... varies... 50/pkg...21856-96...1-3...18641-00 OPTIONAL REAGENTS Nitrate-Nitrogen Standard Solution, Voluette Ampules, 500 mg/l N... 16/pkg...14260-10 Sodium Hydroxide Standard Solution, 5.0 N...50 ml...2450-26 Sulfuric Acid, ACS, concentrated...500 ml...979-49 Urea, ACS... 100 g...11237-26 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS Ampule Breaker Kit... each...21968-00 Cylinder, graduated, mixing, 25-mL (3 required)... each...26363-40 Flask, volumetric, Class A, 50 ml... each...14574-41 ph Paper, 1 to 11 ph units... 5 rolls/pkg...391-33 Pipet, volumetric, Class A, 2 ml... each...14515-36 Spoon, measuring, 0.5 g... each...907-00 For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 162

163

Sampling and Storage Collect samples in clean plastic or glass bottles. If prompt analysis is impossible, store at 4 ãc (39 ãf) or lower if the sample is to be analyzed within 48 hours. Warm to room temperature before running the test. Do not use acid preservatives. Remove suspended solids by filtration. Accuracy Check Standard Solution Method Dissolve 0.150 grams of fresh sodium nitrite and dilute to 1000 ml with deionized water to prepare a 100 mg/l nitrite standard solution. Prepare this solution daily. Alternatively, make a dilution of a fresh Hach Nitrite Standard Solution, 821 mg/l NO2 (250 mg/l NO2-N) using Class A glassware. Dilute 10mL of this standard to 100 ml with deionized water to give an 82 mg/l nitrite standard. Prepare this solution just before use. Using this solution as the sample, perform the nitrite procedure as described above. Method Performance Precision In a single laboratory using a standard solution of 123 mg/l nitrite and two representative lots of reagents with the instrument, a single operator obtained a standard deviation of +1 mg/l nitrite. Estimated Detection Limit The estimated detection limit for program 59 is 2 mg/l NO2. For moreinformation on the estimated detection limit, see Section 1. 164

Interferences This test does not measure nitrates nor is it applicable to glycol based samples. Dilute glycol based samples and follow the Low Range Nitrite Procedure. Summary of Method The method uses ferrous sulfate in an acidic medium to reduce nitrite to nitrous oxide. Ferrous ions combine with the nitrous oxide to form a greenish-brown complex in direct proportion to the nitrite present. NitriVer 2.....1...100/pkg...21075-69, 10-20-25, w/ cap...2...6/pkg... 24019-06 OPTIONAL REAGENTS Nitrite Standard Solution, 821 mg/l NO2 (250 mg/l NO2-N)... 500 ml...23402-49 Sodium Nitrite, ACS...454 g...2452-01 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS Balance, analytical, 110 V...each...26103-00 Balance, analytical, 220 V...each...26103-02 Flask, volumetric, 1000 ml...each...547-53 Flask, volumetric, 100 ml, Class A...each...14574-42 Pipet, volumetric, 10.00 ml, Class A...each...14515-38 Pipet Filler, safety bulb...each...14651-00 For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 165

(0 to 0.350 mg/l NO2--N) 8507 166

the sample. Results should be between 0.090 and 0.110 mg/l NO2-N. Method Performance Precision In a single laboratory, using a standard solution of 0.250 mg/l nitrite nitrogen and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of À0.001 mg/l NO2 N for the powder pillow method and À0.003 mg/l NO2 --N for the AccuVac method. Estimated Detection Limit The estimated detection limit for programs 60 and 62 is 0.005 mg/l NO2-N. For more information on derivation and use of Hach s estimated detection limit, see Section 1. Summary of Method Nitrite in the sample reacts with sulfanilic acid to form an intermediate diazonium salt. This couples with chromotropic acid to produce a pink colored complex directly proportional to the amount of nitrite present. NitriVer 3... 1... 100/pkg... 21071-69 NitriVer 3 AccuVac... 1... 25/pkg... 25120-25, 50 ml (for AccuVac procedure)...1...... 500-41 or, 10-20-25 ml (powder pillow procedure)...2... 6/pkg... 24019-06 OPTIONAL REAGENTS Nitrite Standard Solution, 250 mg/l as NO2--N...500 ml... 23402-49 Water, deionized...4 L... 272-56 OPTIONAL APPARATUS Description Unit Cat. No. AccuVac Snapper Kit... each... 24052-00 Flask, volumetric, 250 ml... each... 14574-46 Flask, volumetric, 500 ml... each... 14574-49 Pipet, serological, 10 ml... each... 532-38 Pipet, TenSette, 1 to 10 ml... each... 19700-01 Pipet Tips for 19700-01 TenSette Pipet... 50/pkg... 21856-96 Pipet, volumetric, Class A, 5.00 ml... each... 14515-37 Pipet, volumetric, Class A, 10.00 ml... each... 14515-38 Pipet Filler, safety bulb... each... 14651-00 Thermometer, -10 to 110 ãc... each... 1877-01 For Technical Assistance, Price and Ordering In the U.S.A. call 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 168

NO3-N Test N Tube Test N Tube5 169

0.0 mg/l NO3-N 170

Sampling and Storage Collect samples in clean plastic or glass bottles. Store at 4 ãc (39 ãf) or lower and analyze within 48 hours. Warm to room temperature before running the test. Do not use acid preservatives. Remove suspended solids by filtration. Accuracy Check Standard Solution Method Pipet 5.00 ml of a fresh Hach standard, 250 mg/l as NO2 -N into a Class A 250-mL volumetric flask. Dilute to the line with deionized water to make a 5.00-mg/L intermediate standard. Pipet 10.00 ml of the 5.0-mg/L intermediate standard into a Class A 500-mL volumetric flask. Dilute to the line with deionized water to make a 0.100 mg/l NO2-N standard solution. Prepare immediately before use. Run the test using the 0.100 mg/l NO2-N standard in place of the sample.results should be between 0.090 and 0.110 mg/l NO2 -N. Method Performance Precision In a single laboratory, using a standard solution of 0.250 mg/l nitrite nitrogen and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of À0.004 mg/l NO2-N. Estimated Detection Limit The estimated detection limit for program 63 is 0.006 mg/l NO2-N. For more information on derivation and use of Hach s estimated detection limit, see Section 1. Summary of Method Nitrite in the sample reacts with sulfanilic acid to form an intermediate diazonium salt. This couples with chromotropic acid to produce a pink-colored complex directly proportional to the amount of nitrite present. NitriVer. 3 Test N Tube Set (50 tests)...26083-45 : (50) NitriVer. 3 Test N...*, 6 x 10 mm,6/pkg...22758-06, for 22758-06 vials, 6/pkg...22411-06, 100-mL...272-42 COD/TNT...1...... 48464-00... 1-3...... 18641-00, TenSette, 1 to 10 ml...1...... 19700-10 Pipet Tips for 19700-10 TenSette Pipet...1... 50/pkg... 21997-96 171

OPTIONAL REAGENTS Nitrite Standard Solution, 250 mg/l as NO2--N...500 ml... 23402-49 Water, deionized...4 L... 272-56 OPTIONAL APPARATUS Flask, volumetric, 250 ml... each... 14574-46 Flask, volumetric, 500 ml... each... 14574-49 Pipet, volumetric, Class A, 10.00 ml... each... 14515-38 For Technical Assistance, Price and Ordering In the U.S.A. call 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 172

8155 173

174

Sampling and Storage Collect samples in clean plastic or glass bottles. Most reliable results are obtained when samples are analyzed as soon as possible after collection. If chlorine is known to be present, the sample must be treated immediately with sodium thiosulfate. Add one drop of Sodium Thiosulfate Standard Solution, 0.1 N, for each 0.3 mg of chlorine present in a one liter sample. To preserve the sample, adjust the ph to 2 or less with concentrated sulfuric acid (about 2 ml per liter). Store samples at 4 ãc or less. Samples preserved in this manner can be stored up to 28 days. Just before testing the stored sample, warm to room temperature and neutralize with 5.0 N Sodium Hydroxide Standard Solution. Correct the test result for volume additions; see Correction for Volume Additions, in Section 1 for more detailed information. Accuracy Check Standard Additions Method a) Fill three 25-mL mixing cylinders with 20 ml of sample. b) Use the TenSette Pipet to add 0.1, 0.2, and 0.3 ml of Ammonium Nitrogen Standard, 10 mg/l as NH3-N to the three samples. Stopper the cylinders and mix well. c) Analyze a 10-mL portion of sample as described above. The ammonia nitrogen concentration should increase 0.05 mg/l for each 0.1 ml of standard added. d) If these increases do not occur, see Standard Additions (Section 1) for more information. Standard Solution Method Prepare a 0.40 mg/l ammonia nitrogen standard by diluting 4.00 ml of the Ammonia Nitrogen Standard Solution, 10 mg/l, to 100 ml with deionized water. Or, using the TenSette Pipet, prepare a 0.40 mg/l ammonia nitrogen standard by diluting 0.8 ml of a Ammonia Nitrogen Voluette Standard Solution, 50 mg/l as NH3-N, to 100 ml with deionized water. Method Performance Precision In a single laboratory using a standard solution of 0.40 mg/l ammonia nitrogen (NH3-N) and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of +0.02 mg/l ammonia nitrogen. Estimated Detection Limit The estimated detection limit for program 64 is 0.02 mg/l NH3-N. For more information on the estimated detection limit, see Section 1. Summary of Method Ammonia compounds combine with chlorine to form monochloramine. Monochloramine reacts with salicylate to form 5-aminosalicylate. The 5-aminosalicylate is oxidized in the presence of a sodium nitroprusside catalyst to form a blue-colored compound. The blue color is masked by the yellow color from the excess reagent present to give a final greencolored solution. 175

() for 10-mL (100 tests)...26680-00 : (2) 26531-99, (2) 26532-99 Ammonia Cyanurate... 2...100/pkg...26531-99 Ammonia Salicylate... 2...100/pkg...26532-99, 10-20-25 ml, w/ cap...2...6/pkg...24019-06 OPTIONAL REAGENTS Ammonia Nitrogen Standard Solution, 10 mg/l as NH3-N... 500 ml...153-49 Ammonia Nitrogen, PourRite Ampules, 50 mg/l as NH3-N, 2 ml...20/pkg...14791-20 Cylinder, graduated, mixing, 25 ml...each...20886-40 Sodium Hydroxide Standard Solution, 1.0 N... 100 ml MDB...1045-32 Sodium Hydroxide Standard Solution, 5.0 N...50 ml SCDB...2450-26 Sodium Thiosulfate Standard Solution, 0.1 N... 100 ml MDB...323-32 Sulfide Inhibitor Reagent Powder Pillows...100/pkg...2418-99 Sulfuric Acid, concentrated, ACS... 500 ml...979-49 Sulfuric Acid Standard Solution, 1.0 N... 100 ml MDB...1270-32 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS Cylinder, graduated, polypropylene, 500 ml...each...1081-49 Distillation Heater and Support Apparatus, 115 V...each...22744-00 Distillation Heater and Support Apparatus, 230 V...each...22744-02 Distillation Set, General Purpose...each...22653-00 Filter Paper, folded, 12.5 cm...100...1894-57 Flask, Erlenmeyer, polypropylene, 500 ml...each...1082-49 Flask, volumetric, Class A, 100 ml...each...14574-42 Funnel, poly, 65 mm...each...1083-67 ph Meter, sension.1, portable...each...51700-10 Pipet Filler, safety bulb...each...14651-00 Pipet, TenSette, 0.1 to 1.0 ml...each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet...50/pkg...21856-96 Pipet, volumetric, Class A, 2.0 ml...each...14515-36 PourRite Ampule Breaker Kit...each...24846-00 Thermometer, -10 to 110 ãc...each...1877-01 For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 176

8075 mg/l, TKNZERO 177

178

179

Sampling and Storage Collect samples in a cleaned glass or plastic container. Adjust the ph to 2 or less with sulfuric acid (about 2 ml per liter) and cool to 4 ãc. Preserved samples can be stored up to 28 days. Accuracy Check Kjeldahl Nitrogen Standard Method This procedure checks digestion efficiency and indicates that amount of bound nitrogen that is freed during digestion. The methods and standards available to check digestion technique are found in the Accuracy Check section following the procedures in the Digesdahl Digestion Apparatus Instruction Manual. Using the digested Kjeldahl standard, perform the above TKN analysis on the colorimeter. The TKN value should come within about À3% of the value of the prepared Kjeldahl standard. Standard Solution Method (to check calibration accuracy only) Add one drop of TKN Indicator to each of two 25-mL graduated mixing cylinders. Fill one cylinder to the 20-mL mark with deionized water. Fill the other cylinder to the 20-mL mark with a 1.0 mg/l Ammonia Nitrogen Solution. Add 3 drops of Mineral Stabilizer to each cylinder. Invert several times to mix. Add 3 drops of Polyvinyl Alcohol Dispersing agent to each cylinder. Perform the TKN procedure as described in Steps 9 to 16. This display should show 26-27 mg/l TKN. User Calibration For most accurate results, use a user-calibrated program. The Standard Adjust feature should not be used with a user-entered calibration; it will hinder performance. A one-time setup of a program for TKN is recommended for each new lot of reagents. A new calibration may be performed for each lot of Nessler Reagent by following these instructions: Standard Preparation Use the following standards to make a calibration curve. See Preparing a User-Entered Calibration Curve on page 49, for more information and instructions. Prepare standards representing concentrations of 20, 60, 80, 100, 140 and 160 mg/l NH3-N as follows: a) Using volumetric pipets, transfer 5.0, 15.0, 20.0, 25.0, 35.0, and 40.0 ml of 100 mg/l NH3-N standard solution into six separate 100-mL volumetric flasks. Dilute to volume with deionized water, stopper, and invert to mix. b) Begin at step 4 of the procedure using a 3-mL aliquot for the sample volume. Also prepare a blank solution by substituting a 3 ml aliquot of deionized water for sample in Step 4. Note: Standard solutions are prepared as if a 25-mL volume was used for the digestion. Actual concentrations prepared in Step 1 are 5, 15, 20, 25, 35, and 40 mg/l NH3-N. These represent original concentrations of 20, 60, 80, 100, 140, and 160 mg/l NH3-N, based on the 25 to 100 ml dilution in the digestion. User Entered Calibration Settings For TKN Program # = 101 to 105 Wavelength = 420 nm Resolution = 0 mg/l 180

Method Performance Precision In a single laboratory using a standard solution of 64 mg/l TKN and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of À1.0 mg/l TKN. Estimated Detection Limit The estimated detection limit for program 65 is 2 mg/l TKN. For more information on the estimated detection limit, see Section 1. Summary of Method Total Kjeldahl Nitrogen ± (also called crude protein) refers to the combination of ammonia and organic nitrogen. Organically-bound in the trinegative state, it is converted into ammonium salts by the action of sulfuric acid and hydrogen peroxide. The ammonia is then analyzed by a modified nessler method test. The Mineral Stabilizer complexes calcium and magnesium. The Polyvinyl Alcohol Dispersing Agent aids the color formation in the reaction of Nessler Reagent with ammonium ions. A yellow color forms, proportional to the ammonia concentration. Pollution Prevention And Waste Management Nessler reagent contains mercuric iodide. Both the sample and blank will contain mercury (D009) at concentrations regulated as a hazardous waste by the Federal RCRA. Do not pour these solutions down the drain. See Section 3 for more information on proper disposal of these materials.... 24953-00 : (1) 21196-49, (1) 23766-26, (1) 21194-49, (1) 23765-26, (1) 282-32, (1) 23144-26, (1) 979-49, (1) 22519-26, 50%... 20 ml...490 ml...21196-49... 6......50 ml SCDB...23766-26 Nesslers t... 2 ml...500 ml...21194-49 Polyvinyl... 6... 50 ml SCDB...23765-26, 8.0 N......100 ml MDB...282-32, 1.0 N...... 50 ml SCDB...23144-26, ACS... 6 ml...500 ml...979-49 TKN... 2... 50 ml SCDB...22519-26...... 4 L...272-56 Boiling Chips,...2-3... 500 g...20557-34, 25 ml... 2......21190-40, TenSette, 0.1 to 1.0 ml... 1......19700-01, 19700-01 TenSette... 2... 50/pkg...21856-96 181

... 1......20974-00, 10-20-25 ml, w/ cap... 2... 6/pkg...24019-06 :, 115 V... 1......23130-20, 230 V... 1......23130-21 OPTIONAL REAGENTS Ammonia Nitrogen Standard Solution, 1 mg/l NH3-N...500 ml...1891-49 Ammonia Nitrogen Standard Solution, Voluette Ampule, 150 mg/l NH3-N, 10 ml... 16/pkg...21284-10 Ammonia Nitrogen Standard Solution, 100 mg/l NH3-N...500 ml...24065-49 OPTIONAL APPARATUS Description Unit Cat. No. Ampule Breaker Kit...each...21968-00 Balance, AccuLab Pocket Pro...each...25568-00 Bottle, glass dispenser, 118 ml...each...591-00 Bottle, plastic wash, 1000 ml...each...620-16 Cylinder, graduated, 50 ml...each...508-41 Flask, volumetric, 100 ml, Class A...each...14574-42 Mini Grinder, 120 V...each...20991-00 ph Paper, 1 to 11 ph units...5 rolls/pkg...391-33 Pipet, volumetric, Class A, 0.50 ml...each...14515-34 Pipet, volumetric, Class A, 1.00 ml...each...14515-35 Pipet, volumetric, Class A, 2.00 ml...each...14515-36 Pipet, volumetric, Class A, 5.00 ml...each...14515-37 Pipet, volumetric, Class A, 10.00 ml...each...14515-38 Pipet, volumetric, Class A, 15.00 ml...each...14515-39 Pipet, volumetric, Class A, 20.00 ml...each...14515-20 Pipet, volumetric, Class A, 25.00 ml...each...14515-40 Safety Glasses...each...18421-00 For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 182

NO3-N AmVer 183

0.00 mg/l NH3-N 184

Sampling and Storage Collect samples in clean plastic or glass bottles. Best results are obtained with immediate analysis. If chlorine is known to be present, add one drop of 0.1 N sodium thiosulfate for each 0.3 mg/l Cl2 in a one liter sample. Preserve the sample by reducing the ph to 2 or less with hydrochloric acid (at least 2 ml). Store at 4 C (39 F) or less. Preserved samples may be stored up to 28 days. Before analysis, warm samples to room temperature and neutralize with 5.0 N sodium hydroxide. Correct the test result for volume additions. See Correcting for Volume Additions on page 22 for more information. Accuracy Check Standard Additions Method a) Snap the neck off a Nitrogen, Ammonia Ampule Standard Solution, 50 mg/l NH3-N. b) Use the TenSette Pipet to add 0.1, 0.2, and 0.3 ml of standard to three 25 ml samples. Mix thoroughly. c) Analyze each sample as described above. The nitrogen concentration should increase 0.20 mg/l for each 0.1 ml of standard added. d) If these increases do not occur, see Standard Additions, Section 1, for more information. Standard Solution Method To check accuracy, use a 1.0 mg/l Nitrogen, Ammonia Standard Solution listed under Optional Reagents. Or, dilute 1 ml of solution from a 50 mg/l Ampule Standard for Nitrogen, Ammonia to 50 ml with deionized water using a 50-mL volumetric flask. Method Performance Precision In a single laboratory, using a standard solution of 1.0 mg/l ammonia nitrogen and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of +0.02 mg/l NH3-N. Estimated Detection Limit The estimated detection limit for program 66 is 0.08 mg/l NH3-N. For more information on the estimated detection limit, see Section 1. Summary of Method Ammonia compounds combine with chlorine to form monochloramine. Monochloramine reacts with salicylate to form 5-aminosalicylate. The 5-aminosalicylate is oxidized in the presence of a sodium nitroprusside catalyst to form a blue-colored compound. The blue color is masked by the yellow color from the excess reagent present to give a final green-colored solution. Pollution Prevention And Waste Management The ammonia salicylate reagent contains sodium nitroferricyanide. Cyanide solutions are regulated as hazardous wastes by the Federal RCRA. Collect cyanide solutions for disposal as reactive (D001) waste. Be sure cyanide solutions are stored in a caustic solution with ph >11 to prevent release of hydrogen cyanide gas. See Section 3 for further information in proper disposal of these materials. 185

AmVer (25 tests)...26045-45 : (1) 23952-66, (1) 23954-66, (1) 272-42, *(50) AmVer Low Range Vials AmVer, Test N Tube... 2... 50/pkg... *, 5 ml sample... 2... 50/pkg...23952-66 Cyanurate Reagent Powder Pillows, 5 ml sample... 2... 50/pkg...23954-66 COD... 1......48464-00...1-3......18641-00 TenSette, 0-10 ml... 1......19700-10... 2... 50/pkg...21997-96... 1......25843-35 OPTIONAL REAGENTS Nitrogen, Ammonia Standard Solution, 1.0 mg/l NH3-N... 500 ml...1891-49 Nitrogen, Ammonia Standard Solution, 10 ml Voluette ampules, 50 mg/l NH3-N...16/pkg...14791-10 Nitrogen, Ammonia Standard Solution, 2 ml PourRite ampules, 50 mg/l NH3-N......20/pkg...14791-20 Hydrochloric Acid, ACS... 500 ml...134-49 Sodium Hydroxide Standard Solution, 5.0 N...50 ml SCDB... 2450-26 Sodium Hydroxide, 1.000 N... 100 ml MDB...1045-32 Sodium Thiosulfate Standard Solution, 0.1 N... 100 ml MDB...323-32 Sulfide Inhibitor Reagent Powder Pillows...100/pkg...2418-99 Sulfuric Acid, 1.00 N... 100 ml MDB...1270-32 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS Ampule Breaker Kit...each...21968-00 Cylinder, graduated, mixing, 25 ml, Class A...each...508-40 Distillation Apparatus Set...each...22653-00 Heater and Support Apparatus (for distillation), 115 Vac...each...22744-00 Heater and Support Apparatus (for distillation), 230 Vac...each...22744-02 Filter Paper, folded...100/box...1894-57 Flask, Erlenmeyer, 500 ml...each...505-49 Flask, volumetric, 50 ml, Class A...each...14547-41 Funnel, analytical (for filtering)...each...1083-68 Jack, laboratory (use with distillation apparatus)...each...22743-00 ph Indicator Paper, 1 to 11 ph...5 rolls/pkg...391-33 Ampule Breaker Kit, PourRite...each...24846-00 Thermometer, -20 to 110 ãc...each...566-01 Thermometer, -10 to 260 ãc...each...26357-01 For Technical Assistance, Price and Ordering 186

NO3-N AmVer 187

0.00 mg/l NH3-N 188

Method Performance Precision In a single laboratory, using a standard solution of 50 mg/l ammonia nitrogen (NH3-N) and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of +5 mg/l NH3-N. Estimated Detection Limit The estimated detection limit for program 67 is 1 mg/l NH3-N. For more information on the estimated detection limit, see Section 1. Summary of Method Ammonia compounds combine with chlorine to form monochloramine. Monochloramine reacts with salicylate to form 5-aminosalicylate. The 5-aminosalicylate is oxidized in the presence of a sodium nitroprusside catalyst to form a blue-colored compound. The blue color is masked by the yellow color from the excess reagent present to give a green-colored solution. Safety Good safety habits and laboratory techniques should be used throughout the procedure. Consult the Material Safety Data Sheets for information specific to the reagents used. For additional information, refer to Section 3. Pollution Prevention And Waste Management The ammonia salicylate reagent contains sodium nitroferricyanide. Cyanide solutions are regulated as hazardous wastes by the Federal RCRA. Collect cyanide solutions for disposal as reactive (D001) waste. Be sure cyanide solutions are stored in a caustic solution with ph >11 to prevent release of hydrogen cyanide gas. See Section 3 for further information in proper disposal of these materials. AmVer., TNT (25 tests)...26069-45 : (1) 23952-66, (1) 23954-66, (1) 272-42, *(50) AmVer HR Vials AmVer. HR Test N Tube.... 2...50/pkg...*... 2...50/pkg...23952-66... 2...50/pkg...23954-66 COD/TNT...1...48464-00 TenSette., 0-1 ml...1...19700-01... varies... 50/pkg...21856-96... 1-3...18641-00...1...25843-35 190

OPTIONAL REAGENTS Nitrogen, Ammonia Standard Solution, 50 mg/l NH3-N... 500 ml...14791-50 Nitrogen, Ammonia Standard Solution, 10 mg/l NH3-N... 500 ml...153-49 Ammonia Standard Solution, PourRite. ampules, 150 mg/l NH3-N, 2 ml...20/pkg...21284-20 Hydrochloric Acid, ACS... 500 ml...134-49 Sodium Hydroxide Standard Solution, 5.0 N... 50 ml...2450-26 Sodium Hydroxide Standard Solution, 1.0 N... 100 ml...1045-32 Sodium Thiosulfate Standard Solution, 0.1 N... 100 ml...323-32 OPTIONAL REAGENTS (continued) Quantity Required Description Per Test Unit Cat. No. Sulfide Inhibitor Powder Pillows... 100/pkg...2418-99 Sulfuric Acid, 1.00 N...100 ml MDB...1270-32 Water, deionized... 4 L... 272-56 OPTIONAL APPARATUS Cylinder, 25 ml, graduated, mixing... each...20886-40 Distillation Apparatus Set, general purpose... each...22653-00 Heater and Support Apparatus (for distillation), 115 VAC... each...22744-00 Heater and Support Apparatus (for distillation), 230 VAC... each...22744-02 Filter Paper, folded... 100/pkg...1894-57 Flask, Erlenmeyer, 500 ml... each...505-49 Funnel, analytical (for filtering)... each...1083-68 Jack, laboratory (use with distillation apparatus)... each...22743-00 ph Indicator Paper, 1 to 11 ph... 5 rolls/pkg...391-33 PourRite. Ampule Breaker... each...24846-00 Sample Cell, 10-20-25 ml, w/cap... 6/pkg...24019-06 For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 191

N 192

AmVer 15:00 TIMER 2 0.0 mg/l N 193

194

Sampling And Storage Collect samples in clean plastic or glass bottles. Best results are obtained with immediate analysis. If chlorine is known to be present, add 1 drop of 0.1 N sodium thiosulfate for each 0.3 mg/l Cl2 in a 1 liter sample. Preserve the sample by reducing the ph to 2 or less with concentrated hydrochloric acid (at least 2 ml). Store at 4 C (39 F) or less. Preserved samples may be stored up to 28 days. Warm samples to room temperature and neutralize with 5 N Sodium Hydroxide before analysis. Correct the test result for volume additions; see Correcting for Volume Additions in Section 1. Accuracy Check Standard Additions Method a) Fill three 25-mL graduated mixing cylinders with 25 ml of sample. b) Snap the neck off a fresh High Range Nitrate Nitrogen PourRite Ampule Standard, 500 mg/l NO3 -N. c) Use the TenSette Pipet to add 0.1, 0.2, and 0.3 ml of standard, respectively, to 3 25-mL mixing cylinders. Mix thoroughly. d) Analyze each sample as described in the procedure; use a 1-mL aliquot of the prepared sample in Step 5. The nitrogen concentration should increase about 1.8 to 1.9 mg/l for each 0.1 ml of standard added. e) If these increases do not occur, see Standard Additions in Section 1 for more information. Standard Solution Method To check accuracy, use a 10.0 mg/l Nitrate Nitrogen Standard Solution listed under Optional Reagents. Alternatively, a 20.0 mg/l nitrate nitrogen standard can be prepared by diluting 2 ml of solution from a PourRite Ampule Standard for High Range Nitrate Nitrogen, 500 mg/l NO3 -N, to 50 ml with deionized water. Substitute this standard for the sample and perform the test as described. The recovery of the standards should be about 90-95%. Method Performance Precision/Accuracy The total inorganic nitrogen test provides an estimate of the total nitrite, nitrate, and ammonia nitrogen load in water or wastewater samples. This test is most applicable for monitoring an industrial process stream or a wastewater treatment stream where it is important to track the inorganic nitrogen load as it passes through the treatment process. The test exhibits different recoveries of each of the three nitrogen species, as summarized below. This test is not recommended for quantifying only one of the three species. In that case, use a specific procedure for each particular analyte. Ammonia Nitrogen In a single laboratory, using a standard solution of 20.0 mg/l NH3-N and 2 representative lots of reagent with the instrument, a single operator obtained a mean recovery of 21.3 mg/l with a standard deviation of À 0.77 mg/l N (replicate number = 7 per reagent lot). 195

Nitrate Nitrogen In a single laboratory, using a standard solution of 20.0 mg/l NO3-N and2 representative lots of reagent with the instrument, a single operator obtained a mean recovery of 18.9 mg/l with a standard deviation of À 0.55 mg/l N (replicate number = 7 per reagent lot). Nitrite Nitrogen In a single laboratory, using a standard solution of 20.0 mg/l NO2-N and 2 representative lots of reagent with the instrument, a single operator obtained a mean recovery of 14.6 mg/l with a standard deviation of À 0.77 mg/l N (replicate number = 7 per reagent lot). Estimated Detection Limit The estimated detection limit for program 68 is 0.7 mg/l N. For more information on the estimated detection limit, see Section 1. Summary of Method Titanium (III) ions reduce nitrate and nitrite to ammonia in a basic environment. After centrifugation to remove solids, the ammonia is combined with chlorine to form monochloramine. Monochloramine reacts with salicylate to form 5-aminosalicylate. The 5-aminosalicylate is oxidized in the presence of a sodium nitroprusside catalyst to form a blue-colored compound. The blue color is masked by the yellow color from the excess reagent present to give a final green-colored solution. REQUIRED REAGENTS (TiCl3 ) (25 tests)... 26049-45 : (1) 26051-50, (1) 2040-59, *(50) TIN Pretreatment Diluent Vials AmVer. (25 tests)26045-45 : (1) 23952-66, (1) 23954-66, (1) 272-42, *(50) AmVer. Diluent LR Vials...2... 50/pkg... *...2... 50/pkg...26051-50...2 ml...50 ml...2040-59 AmVer....2... 50/pkg... *... 2...50/pkg...23952-66... 2...50/pkg...23954-66 REQUIRED APPARATUS, 115V...1......26765-00, 230V...1......26765-02 COD/TNT r...1......48464-00...1......25843-35 TenSette., 0.1 to 1.0...1......19700-01...2... 50/pkg...21856-96...1...18641-00 196

OPTIONAL REAGENTS Hydrochloric Acid, ACS...500 ml...134-49 Nitrate Nitrogen Standard Solution, 10 mg/l NO3 --N...500 ml...307-49 Nitrate Nitrogen Standard Solution, PourRite Ampules, 500 mg/l NO3--N, 2 ml... 20/pkg...14260-20 Sodium Hydroxide Standard Solution, 5.0 N... 50 ml SCDB...2450-26 Sodium Thiosulfate Standard Solution, 0.1 N...100 ml MDB...323-32 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS Cylinder, graduated, mixing, 25 ml... each...20886-40 Flask, volumetric, Class A, 50.0 ml... each...14574-41 ph Indicator Paper, 1 to 11 ph... 5 rolls/pkg...391-33 Pipet, volumetric, Class A, 2.0 ml... each...14515-36 PourRite Ampule Breaker... each...24846-00 For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 197

103-106 C N 02:00 Timer 2 198

05:00 Timer 3 199

10% >60ppm >1000 ppm mg/l) mg/l 2.6 300 (3+) 0.5 2 6.6 ppb 500 150 ph 13 ph 100 150 0.9 1.5 Hach chemists tested this chemistry on standard nitrogen solutions prepared from the following compounds and obtained 95% recovery:. Ammonium chloride. Ammonium sulfate. Ammonium acetate. Urea. Glycine Ammonium chloride or nicotinic-ptsa spikes in domestic influent, effluent and the ASTM standard specification for substitute wastewater (D 5905-96) also resulted in 95% recovery. Large amounts of nitrogen-free organic compounds in some samples may decrease digestion efficiency by consuming some of the persulfate reagent. Samples known to contain high levels of organics should be diluted and re-run to verify digestion efficiency. Sampling and Storage Collect samples in clean plastic or glass bottles. Best results are obtained with immediate analysis. Preserve the sample by reducing the ph to 2 or less with concentrated sulfuric acid (at least 2 ml). Store at 4 ãc (39 ãf) or less. Preserved samples may be stored up to 28 days. Warm samples to room temperature and neutralize with 5 N sodium hydroxide before analysis. Correct the test result for volume additions; see Correcting for Volume Additions in Section 1. 200

Accuracy Check This method generally yields 95-100% recovery on organic nitrogen standards. For proof of accuracy Hach offers a set of three Primary Standards for Kjeldahl Nitrogen. 1. Prepare one or more of the following three solutions. Each preparation is for an equivalent 25 mg/l N standard. Use water that is free of all organic and nitrogen-containing species. a) Weigh 0.3379 g of Ammonium p-toluenesulfonate (PTSA). Dissolve in a 1000-mL volumetric flask with deionized water. Add deionized water to the 1000-mL mark. b) Weigh 0.4416 g of Glycine p-toluenesulfonate. Dissolve in a 1000-mL volumetric flask with deionized water. Add deionized water to the 1000-mL mark. c) Weigh 0.5274 g of Nicotinic p-toluenesulfonate. Dissolve in a 1000-mL volumetric flask with deionized water. Add deionized water to the 1000-mL mark. 2. Analyze each of these solutions using the test procedure above. Calculate the percent recovery for each using this formula: Hach analysts have found Ammonia-PTSA to be the most difficult to digest. Other compounds may yield different percent recoveries. Standard Solution Method Substitute 2 ml of a 20 mg/l ammonia nitrogen standard solution for the sample. To prepare a 20-mg/L standard, use a 20-mL Class A pipet to transfer 20 ml of a 100-mg/L Ammonia Nitrogen Standard (see Optional Reagents) to a 100-mL Class A volumetric flask. Dilute to the line with organic-free water. A single analyst should obtain less than 5% variation on replicates. Comparison of the user-obtained value with the standard concentration is an indication of test performance for this user. Standard Additions Method a) Fill three 25-mL graduated mixing cylinders with 25 ml of sample. b) Snap the neck off an Ammonia Nitrogen Voluette Ampule Standard Solution, 160 mg/l as NH3-N. c) Use the TenSette Pipet to add 0.3 ml, 0.6 ml, and 0.9 ml of standard, respectively, to the three mixing cylinders. d) Stopper each cylinder and mix thoroughly. e) Add 2 ml of each prepared solution, respectively, to three TN Hydroxide Reagent Sample Digestion Vials. 201

f) Analyze each standard addition sample as described in the procedure. The nitrogen concentration should increase 2 mg/l for each 0.3 ml of standard added. g) If these increases do not occur, see Standard Additions in Section 1 for troubleshooting information. Blanks for Colorimetric Measurement The reagent blank may be used up to 7 days for measurements using the same lots of reagents. Store the reagent blank in the dark at room temperature (18-25 ãc). If a small amount of white floc appears prior to the end of one week, discard the reagent blank and prepare a new one. Method Performance Precision A Hach chemist analyzed two independent nutrient standards. The lowest average percent recovery was 95% with a standard deviation of À2%. In a single laboratory, using a standard solution of 15.0 mg/l N and two lots of reagent with the instrument, a single operator obtained a standard deviation of less than À0.5 mg/l N. For more information on Hach s precision statement, see Section 1. Estimated Detection Limit The estimated detection limit for program 58 is 2 mg/l N. For more information on the estimated detection limit, see Section 1. Summary of Method An alkaline persulfate digestion converts all forms of nitrogen to nitrate. Sodium metabisulfite is added after the digestion to eliminate halogen oxide interferences. Nitrate then reacts with chromotropic acid under strongly acidic conditions to form a yellow complex with an absorbance maximum near 420 nm. REQUIRED REAGENTS Description Cat. No. Test N Tube (100 vials)... 26722-45 : TN Reagent C, *, 25/pkg.....26721-25 TN*, 25/pkg... 26717-25 TN ()...2... 100/pkg...26718-49 TN Reagent A,...2... 100/pkg...26719-49 TN Reagent B,...2... 100/pkg...26720-49 COD, 115/230 V, North American Plug... 1...45600-00 COD, 230 V, European Plug... 1......45600-02 COD/TNT... 1......48464-00... 1......25843-35...1-3......18641-00 TenSette, 0-10 ml... 1......19700-10 202

... 2... 50/pkg...21997-96... 1.........25843-35.... 1......23810-00...1-3......18641-00 OPTIONAL REAGENTS Nitrogen, Ammonia, 100 mg/l NH3-N...500 ml...24065-49 Nitrogen, Ammonia, Voluette Ampule, 160 mg/l NH3-N, 10 ml... 16/pkg...21091-10 Sulfuric Acid, ACS...500 ml...979-49 Primary Standards for Kjeldahl Nitrogen...set of 3...22778-00 Ammonium p-toluenesulfonate... 25 g... 22779-24 Glycine p-toluenesulfonate... 25 g... 22780-24 Nicotinic Acid p-toluenesulfonate... 25 g... 22781-24 Sodium Hydroxide Standard Solution, 5.0 N...50 ml MDB...2450-26 Water, organic-free...500 ml...26415-49 OPTIONAL APPARATUS Ampule Breaker Kit...each...21968-00 Balance, analytical, 115 VAC...each...26103-00 Balance, analytical, 230 VAC...each...26103-02 Cots, finger...2/pkg...14647-02 Cylinder, graduated, mixing, 25 ml (3 required)...each...26363-40 Flask, volumetric, Class A, 1000 ml (3 required)...each...14574-53 Flask, volumetric, Class A, 100 ml...each...14574-42 Pipet, volumetric, Class A, 20 ml...each...14515-20 ph Paper, 1 to 11 ph units...5 rolls/pkg...391-33 203

10.0 to 150.0 mg/l N 103-106 C 204

mg/l, NZERO 02:00 Timer 2 05:00 Timer 3 205

0 mg/l N 206

10% >240ppm >3000 ppm mg/l) mg/l 10.4 1200 (3+) 2 4 26.4 ppb 2000 600 ph 13 ph 400 650 3.69 6 Sampling and Storage Collect samples in clean plastic or glass bottles. Best results are obtained with immediate analysis. Preserve the sample by reducing the ph to 2 or less with concentrated sulfuric acid (at least 2 ml/l). Store at 4 ãc (39 ãf) or less. Preserved samples may be stored up to 28 days. Warm samples to room temperature and neutralize with 5 N sodium hydroxide before analysis. Correct the test result for volume additions; see Correcting for Volume Additions in Section 1. Accuracy Check This method generally yields 95-100% recovery on organic nitrogen standards. For proof of accuracy Hach offers a set of three Primary Standards for Kjeldahl Nitrogen. 1. Prepare one or more of the following three solutions. Each preparation is for an equivalent 120 mg/l N standard. Use water that is free of all organic and nitrogen-containing species. a) Weigh 1.6208 g of Ammonium p-toluenesulfonate (PTSA). Dissolve in a 1000-mL volumetric flask with deionized water. Add deionized water to the 1000-mL mark. b) Weigh 2.1179 g of Glycine p-toluenesulfonate. Dissolve in a 1000-mL volumetric flask with deionized water. Add deionized water to the 1000-mL mark. c) Weigh 2.5295 g of Nicotinic p-toluenesulfonate. Dissolve in a 1000-mL volumetric flask with deionized water. Add deionized water to the 1000-mL mark. 207

2. Analyze each of these solutions using the test procedure above. Calculate the percent recovery for each using this formula: Hach analysts have found Ammonia-PTSA to be the most difficult to digest. Other compounds may yield different percent recoveries. Standard Solution Method For proof of accuracy, substitute 0.5 ml of a 125 mg/l ammonia nitrogen standard solution for the sample in the procedure. To prepare a 125-mg/L standard, use a 25-mL Class A pipet to transfer 25.00 ml of a 1000-mg/L Ammonia Nitrogen Standard (see OPTIONAL REAGENTS on page 370) to a 200-mL Class A volumetric flask. Dilute to the line with organic-free water. Standard Additions Method a) Fill three 25-mL graduated mixing cylinders with 25 ml of sample. b) Snap the neck off an Ammonia Nitrogen Voluette. Ampule Standard Solution, 1000 mg/l as NH3-N. c) Use the TenSette. Pipet to add 0.1 ml, 0.2 ml, and 0.3 ml of standard, respectively, to the three mixing cylinders. d) Stopper each cylinder and mix thoroughly. e) Add 0.5 ml of each prepared solution, respectively, to three HR Total Nitrogen Hydroxide Digestion Vials. f) Analyze each standard addition sample as described in the procedure. The nitrogen concentration should increase 4 mg/l N for each 0.1 ml of standard added. g) If these increases do not occur, see Standard Additions in Section 1 for troubleshooting information. Blanks for Colorimetric Measurement The reagent blank may be used repeatedly for measurements using the same lots of reagents. Store the reagent blank in the dark at room temperature (18 C25 ãc) for a maximum of seven days. If a small amount of white floc appears prior to the end of one week, discard the reagent blank and prepare a new one. Method Performance Precision In a single laboratory, using a standard solution of 125 mg/l N and two lots of reagent with the instrument, a single operator obtained a standard deviation of less than 3 mg/l N. For more information on Hach s precision statement, see Section 1. 208

Estimated Detection Limit The estimated detection limit for program 69 is 7 mg/l N. For more information on the estimated detection limit, see Section 1. Summary of Method An alkaline persulfate digestion converts all forms of nitrogen to nitrate. Sodium metabisulfite is added after the digestion to eliminate halogen oxide interferences. Nitrate then reacts with chromotropic acid under strongly acidic conditions to form a yellow complex with an absorbance maximum near 420 nm. REQUIRED REAGENTS Test N Tube HR (50 vials)...27141-00 : (1) 26718-46, (1) 26719-46, (1) 26720-46, *(50) Hydroxide Digestion Vials, *(50) Acid Solution Vials HR...1... 50/pkg... * ()...1... 50/pkg... 26718-46 A,...1... 50/pkg... 26719-46 B,.1... 50/pkg... 26720-46 C,...1... 50/pkg... * COD, 115/230 V, North American Plug... 1...... 45600-00 COD, 230 V, European Plug... 1...... 45600-02 COD... 1......48464-00...1-3......18641-00 TenSette, 0-10 ml... 1......19700-10... 2... 50/pkg...21997-96... 1............25843-35... 1...... 23810-00...1-3...... 18641-00 OPTIONAL REAGENTS Nitrogen, Ammonia, 1000 mg/l NH3-N... 1 L... 23541-53 Nitrogen, Ammonia, Voluette Ampule, 1000 mg/l NH3-N, 10 ml... 16/pkg... 23541-10 Sulfuric Acid, ACS... 500 ml... 979-49 Primary Standards for Kjeldahl Nitrogen...set of 3... 22778-00 Ammonium p-toluenesulfonate...25 g... 22779-24 Glycine p-toluenesulfonate...25 g... 22780-24 Nicotinic Acid p-toluenesulfonate...25 g... 22781-24 Sodium Hydroxide Standard Solution, 5.0 N...50 ml MDB... 2450-26 Water, organic-free... 500 ml... 26415-49 209

OPTIONAL APPARATUS Description Unit Cat. No. Ampule Breaker Kit...each...21968-00 Balance, analytical, 115 Vac...each...26103-00 Balance, analytical, 230 Vac...each...26103-02 Cots, finger... 2/pkg...14647-02 Cylinder, graduated, mixing, 25 ml... 3...each...26363-40 Flask, volumetric, Class A, 1000 ml...3...each...14574-53 Flask, volumetric, Class A, 200 ml...each...14574-45 Pipet, volumetric, Class A, 25 ml...2...each...14515-40 ph Paper, 1 to 11 ph units...5 rolls/pkg...391-33 For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224. Out side the U.S.A ª Contact the Hach office or distributor serving you. Outside the U.S.A. ªContact the Hach office or distributor serving you. 210

10129 211

212

0 mg/l C 213

600ml/L PH7 50NTU Sampling and Storage Collect samples in clean glass bottles. Rinse the sample bottle several times with the sample to be collected. Fill the bottle with minimum headspace before capping. Test samples as soon as possible. Acid preservation is not recommended. Homogenize samples containing solids to assure representative samples 214

Accuracy Check Standard Solutions Method a. Prepare a 1000 mg/l organic carbon stock standard by dissolving 2.1254 g dry primary standard Potassium Acid Phthalate in Organic-Free Reagent Water and dilute to 1000 ml. This stock standard is stable for about 1 month at room temperature. Alternatively, open one ampule of TOC Standard Solution (Cat. No. 27915-05). b. Prepare a 10.0 mg/l C standard by transferring 10.00 ml of the stock standard to a 1000-mL Class A volumetric flask. Dilute to volume using Organic-Free Reagent Water. Stopper and mix thoroughly. Prepare this standard fresh daily. Standard Additions Method a. Prepare a 150 mg/l C standard by transferring 15.00 ml of 1000 mg/l C stock solution to a 100-mL Class A volumetric flask. Dilute to volume with organic-free water. Mix. b. Use the TenSette Pipet to add 0.1, 0.2, and 0.3 ml of the 150 mg/l C standard to each of three Acid Digestion vials. c. Add the contents of one TOC Persulfate powder pillow to each vial. d. Add 3.0 ml of sample to each vial. Swirl to mix. e. Proceed with the procedure starting at step 8. f. The mg/l C concentration should increase by 5.0 mg/l for each 0.1 ml increment. Method Performance Precision In a single laboratory, using a standard solution of 9.0 mg/l C and one lot of reagents, a single operator obtained a standard deviation of À0.5 mg/l C. Estimated Detection Limit The estimated detection limit for Method 10129 is 0.3 mg/l C. Sensitivity At mid-range, the sensitivity, expressed as the concentration change per 0.010 absorbance change, is 0.2 mg/l C. Summary of Method The total organic carbon (TOC) is determined by first sparging the sample under slightly acidic conditions to remove the inorganic carbon. In the outside vial, organic carbon in the sample is digested by persulfate and acid to form carbon dioxide. During digestion, the carbon dioxide diffuses into a ph indicator reagent in the inner ampule. The adsorption of carbon dioxide into the indicator forms carbonic acid. Carbonic acid changes the ph of the indicator solution which, in turn, changes the color. The amount of color change is related to the original amount of carbon present in the sample. 215

Test N Tube...50 vials...27603-45 :... 1... 50/pkg...*...0.4 ml..25 ml...452-33... 1...25843-35, Low Range TOC... 1... 10/pkg...* TOC()... 1... 50/pkg...* **...3.0 ml.500 ml...26415-49 COD, 115/230 V ac (U.S.A. and Canada)... 1...45600-00 COD, 115/230 V ac (Europe)... 1...45600-02,10-mL... 1... 508-38, 50-mL... 1... 505-41... 1...23436-00... 1... 50030-00...1-3...18641-00 TenSette., 0.1 to 1.0 ml... 1... 19700-01 TenSette., 1.0 to 10.0 ml... 1...19700-10, for 19700-01 TenSette. Pipet... 2... 50/pkg...21856-96, for 19700-10 TenSette. Pipet... 2... 50/pkg...21997-96...... 1... 45315-00 Wipes, Disposable, Kimwipes... 1... 280/pkg...20970-00 OPTIONAL REAGENTS TOC Standard Solution (KHP Standard, 1000 mg/l C)... 5/pkg...27915-05 Potassium Acid Phthalate... 500 g...315-34 Sulfuric Acid Reagent Solution, 5.25 N... 100 ml MDB...2449-32 OPTIONAL APPARATUS Analytical Balance...each...26103-00 Flask, volumetric, 1000-mL...each...14574-53 Flask, volumetric, 100-mL...each...14574-42 Pipet, Class A, 10.00-mL...each...14515-38 Pipet, Class A, 15.00-mL...each...14515-39 216

10128 217

218

0 mg/l C 219

Accuracy Check Standard Solutions Method a. Prepare a 1000 mg/l organic carbon stock standard by dissolving 2.1254 g dry primary standard Potassium Acid Phthalate in Organic-Free Reagent Water and dilute to 1000 ml. This stock standard is stable for about 1 month at room temperature. Alternatively, open one ampule of TOC Standard Solution (Cat. No. 27945-05). b. Prepare a 300 mg/l C standard by transferring 15.00 ml of the stock standard to a 50-mL Class A volumetric flask. Dilute to volume using Organic-Free Reagent Water. Stopper and mix thoroughly. Prepare this standard fresh weekly. Standard Additions Method a. Prepare a 300 mg/l C standard by transferring 18.00 ml of 1000 mg/l C stock solution to a 50-mL Class A volumetric flask. Dilute to volume with Organic-Free Water. Mix. b. Use the TenSette Pipet to add 0.1, 0.2, and 0.3 ml of the 300 mg/l C standard to each of three Acid Digestion vials. c. Add the contents of one TOC Persulfate powder pillow to each vial. d. Add 0.3 ml of sample to each vial. Swirl to mix. e. Proceed with the procedure starting at step 8. f. The mg/l C concentration should increase by 100 mg/l for each 0.1 ml increment. Method Performance Precision In a single laboratory, using a standard solution of 360 mg/l C and one lot of reagents, a single operator obtained a standard deviation of À8 mg/l C. Estimated Detection Limit Use Method Number 10129 to test TOC levels below 20 mg/l C. Sensitivity At mid-range, the sensitivity, expressed as the concentration change per 0.010 absorbance change, is 6 mg/l C. Summary of Method The total organic carbon (TOC) is determined by first sparging the sample under slightly acidic conditions to remove the inorganic carbon. In the outside vial, organic carbon in the sample is digested by persulfate and acid to form carbon dioxide. During digestion, the carbon dioxide diffuses into a ph indicator reagent in the inner ampule. The adsorption of carbon dioxide into the indicator forms carbonic acid. Carbonic acid changes the ph of the indicator solution which, in turn, changes the color. The amount of color change is related to the original amount of carbon present in the sample. 221

Test N Tube...50 vials...27604-45 :... 1... 50/pkg...*...0.4 ml..25 ml...452-33... 1...25843-35, Low Range TOC... 1... 10/pkg...* TOC()... 1... 50/pkg...* **...3.0 ml..500 ml...26415-49 COD, 115/230 V ac (U.S.A. and Canada)... 1...45600-00 COD, 115/230 V ac (Europe)... 1...45600-02,10-mL... 1... 508-38, 50-mL... 1... 505-41... 1...23436-00... 1... 50030-00...1-3...18641-00 TenSette., 0.1 to 1.0 ml... 1... 19700-01 TenSette., 1.0 to 10.0 ml... 1...19700-10, for 19700-01 TenSette. Pipet... 2... 50/pkg...21856-96, for 19700-10 TenSette. Pipet... 2... 50/pkg...21997-96...... 1... 45315-00 Wipes, Disposable, Kimwipes... 1... 280/pkg... 20970-00 OPTIONAL REAGENTS TOC Standard Solution (KHP Standard, 1000 mg/l C)... 5/pkg...27915-05 Potassium Acid Phthalate... 500 g...315-34 Sulfuric Acid Reagent Solution, 5.25 N... 100 ml MDB...2449-32 OPTIONAL APPARATUS Analytical Balance...each...26103-00 Flask, volumetric, 1000-mL...each...14574-53 Flask, volumetric, 100-mL...each...14574-42 Pipet, Class A, 10.00-mL...each...14515-38 Pipet, Class A, 15.00-mL...each...14515-39 222

223

224

0 mg/l COD 225

226

0 mg/l COD 227

COD COD 2COD 0.50g COD 3 Cl (mg/l) Cl mg/l 2000 1000 8000 2000 1000 4000 20,000 10,000 40,000 Cl- 0.5g HgSO4 mg/l Sampling and Storage Collect samples in glass bottles. Use plastic bottles only if they are known to be free of organic contamination. Test biologically active samples as soon as possible. Homogenize samples containing solids to assure representative samples. Samples treated with sulfuric acid to a ph of less than 2 (about 2 ml per liter) and refrigerated at 4 C can be stored up to 28 days. Correct results for volume additions; see Correction for Volume Additions (Section 1) for more information. Accuracy Check Standard Solution Method Check the accuracy of the 0 to 150 mg/l range with a 100 mg/l standard. Prepare by dissolving 85 mg of dried (120 C, overnight) potassium acid phthalate (KHP) in 1 liter of deionized water. Use 2.0 ml as the sample volume. The expected result will be 100 mg/l COD. As an alternative, dilute 10 ml of 1000-mg/L COD Standard Solution to 100 ml to make a 100-mg/L standard. Check the accuracy of the 0 to 1,500 mg/l range by using either a 300 mg/l or 1000 mg/l COD Standard Solution. Alternatively, prepare a 500 mg/l standard by dissolving 425 mg of dried (120 C, overnight) KHP. Dilute to 1 liter with deionized water. Use 2.0 ml of one of these solutions as the sample volume. Check the accuracy of the 0 to 15,000 mg/l range by using a 10,000 mg/l COD standard solution. Prepare the 10,000 mg/l solution by dissolving 8.500 g of dried (120 C, overnight) KHP in 1 liter of deionized water. Use 0.2 ml of this solution as the sample volume; the expected result will be 10,000 mg/l COD. Method Performance Precision Program #16: In a single laboratory, using a standard solution of 100 mg/l COD and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of 2 mg/l COD. Program #17: In a single laboratory, using a standard solution of 1000 mg/l COD and 228

two representative lots of reagent with the instrument, a single operator obtained a standard deviation of 16 mg/l COD. For more information on Hach s precision statement, see Section 1. Estimated Detection Limit (EDL) The EDL for program 16 is 4 mg/l COD. The EDL for program 17 is 30 mg/l COD. For more information on derivation and use of Hach s estimated detection limit, see Section 1. Blanks for Colorimetric Determination The blank may be used repeatedly for measurements using the same lot of vials. Store it in the dark. Monitor decomposition by measuring the absorbance at the appropriate wavelength (420 or 610 nm). Zero the instrument in the absorbance mode, using a vial containing 5 ml of deionized water and measure the absorbance of the blank. Record the value. Prepare a new blank when the absorbance has changed by about 0.01 absorbance units. Summary of Method The mg/l COD results are defined as the mg of O2 consumed per liter of sample under conditions of this procedure. In this procedure, the sample is heated for two hours with a strong oxidizing agent, potassium dichromate. Oxidizable organic compounds react, reducing the dichromate ion (Cr2O72-) to green chromic ion (Cr3+). When the 0-150 mg/l colorimetric method is used, the amount of Cr6+ remaining is determined. When the 0-1,500 mg/l or 0-15,000 mg/l colorimetric method is used, the amount of Cr3+ produced is determined. The COD reagent also contains silver and mercury ions. Silver is a catalyst, and mercury is used to complex the chloride interference. Pollution Prevention and Waste Management Final samples will contain mercury (D009), silver (D011), and chromium (D007) at concentration levels regulated by the Federal RCRA. Please see Section 3 for further information on proper disposal of these materials. COD :, 0 to 150 mg/l COD... 1 to 2...25/pkg... 21258-25, 0 to 1,500 mg/l COD... 1 to 2...25/pkg... 21259-25 Plus, 0 to 15,000 mg/l COD... 1 to 2...25/pkg... 24159-25...... 4 L... 272-56 REQUIRED APPARATUS, 120 V, 14 speed...1...... 26747-00 COD, 115/230 V... 1...... 45600-00 COD, 230 V, European-style plug...1...... 45600-02 COD/TNT...1...... 48464-00 229

TenSette., 0.1 to 1.0 ml... 1... 19700-01, for 19700-01 TenSette. Pipet... 1... 50/pkg...21856-96 Pipet, volumetric, Class A, 2.00 ml...1...... 14515-36 Pipet Filler, safety bulb...1...... 14651-00... 1 to 2 racks...... 18641-00 OPTIONAL REAGENTS Description Unit Cat. No. COD Digestion Reagent Vials, 0 to 150 mg/l COD... 150/pkg...21258-15 COD Digestion Reagent Vials, 0 to 1,500 mg/l COD... 150/pkg...21259-15 COD Standard Solution, 300 mg/l...200 ml...12186-29 COD Standard Solution, 1000 mg/l...200 ml...22539-29 Mercuric Sulfate...28.3 grams...1915-20 Potassium Acid Phthalate, ACS... 500 g...315-34 Potassium Dichromate Standard Solution, 0.25 N...1000 ml*...1809-53 Sulfuric Acid, ACS...500 ml*...979-49 OPTIONAL APPARATUS Balance, analytical, 115 V... each...26103-00 Balance, analytical, 230 V... each... 26103-02 Beaker, 250 ml... each...500-46 Cylinder, graduated, 5 ml... each...508-37 Electromagnetic Stirrer, 120 V, with electrode stand... each...45300-01 Electromagnetic Stirrer, 230 V, with electrode stand... each...45300-02 Flask, volumetric, Class A, 1000 ml... each...14574-53 Flask, volumetric, Class A, 100 ml... each...14574-42 ph Paper, 1 to 11 ph units... 5 rolls/pkg...391-33 Pipet, serological, 5 ml... each...532-37 Pipet Tips, for 19700-01 TenSette Pipet... 50/pkg*...21856-96 Pipet, volumetric, Class A, 10 ml... each...14515-38 Safety shield, for laboratory bench... each...23810-00 Spoon, measuring, 0.5 g... each...907-00 Stir Bar, 22.2 x 4.76 mm (7/8" x 3/16")... each...45315-00 Stir Bar Retriever... each...15232-00 Timer... each...26304-00 For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 230

III COD 231

0 mg/l COD 232

Sampling and Storage Collect samples in clean glass bottles. Use plastic bottles only if they are known to be free of organic contamination. Test biologically active samples as soon as possible. Homogenize samples containing solids to assure representative samples. Samples treated with concentrated sulfuric acid to a ph of less than 2 (about 2 ml per liter) and refrigerated at 4 ãc may be stored up to 28 days. Correct results for volume additions; see Correcting for Volume Additions (Section 1) for more information. Accuracy Check Standard Solution Method Prepare an 800 mg/l COD standard solution by adding 0.6808 g of dried (103 ãc, overnight) potassium acid phthalate (KHP) to 1 liter of deionized water. Use 0.50 ml of this solution (0.60 ml for the chloride removal procedure) as the sample volume. The result should be 800 À26 mg/l COD. An 800 mg/l COD solution can also be purchased directly from Hach (see Optional Reagents). Method Performance (for Manganic III COD without the chloride removal procedure) Precision In a single laboratory, using a standard solution of 800 mg/l COD and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of 23 mg/l COD. Estimated Detection Limit (EDL) The EDL for program 18 is 14 mg/l COD. For more information on derivation and use of Hach s estimated detection limit, see Section 1. Summary of Method Chemical oxygen demand (COD) is defined as... a measure of the oxygen equivalent of the organic matter content of a sample that is susceptible to oxidation by a strong chemical oxidant ± (APHA Standard Methods, 19th ed., 1995). Trivalent manganese is a strong, noncarcinogenic chemical oxidant that changes quantitatively from purple to colorless when it reacts with organic matter. It typically oxidizes about 80% of the organic compounds. Studies have shown that the reactions are highly reproducible and test results correlate closely to Biochemical Oxygen Demand (BOD) values and hexavalent chromium COD tests. None of the oxygen demand tests provide 100% oxidation of all organic compounds.a calibration is provided which is based on the oxidation of Potassium Acid Phthalate (KHP). A different response may be seen in analyzingvarious wastewaters. The KHP calibration is adequate for mostapplications. The highest degree of accuracy is obtained when test resultsare correlated to a standard reference method such as BOD or one of thechromium COD methods. Special waste streams or classes will require aseparate calibration to obtain a direct mg/l COD reading or to generate a correction factor for the precalibrated KHP response. The sampledigestion time can be extended up to 4 hours for samples which are difficult to oxidize. 233

COD, 20-1000 mg/l. 1... 25/pkg...26234-25... 1 ml... 4 Kg...979-09...... 4 L...272-56 COD/TNT... 1......48464-00, 120 Vac, 14-speed... 1......26747-00, 118 ml... 1... 2/pkg...26748-00, with inert Teflon liner, for mixing bottle... varies... 12/pkg...24018-12 COD, 115 V... 1......45600-00 COD r, 230 V, European-style plug... 1...45600-02, extra fine point... 1......26696-00, for sample + acid... 1......24276-06 TenSette., 0.1 to 1.0 ml... 1... 19700-01 TenSette., 1.0 to 10.0 ml... 1...19700-10, for 19700-01 TenSette. Pipet... 2... 50/pkg...21856-96, for 19700-10 TenSette. Pipet... 2... 50/pkg...21997-96... 1......23810-00... 1......18641-00 OPTIONAL REAGENTS AND APPARATUS COD Standard Solution, 800 mg/l COD...200 ml...26726-29 Potassium Acid Phthalate... 500 g...315-34 Dispenser for sulfuric acid... each...25631-37 For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 234

TenSette C. 235

236

23. 0 mg/l COD 237

Method Performance (for Manganic III COD without the chloride removal procedure) Precision In a single laboratory, using a standard solution of 800 mg/l COD and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of 23 mg/l COD. Estimated Detection Limit (EDL) The EDL for program 18 is 14 mg/l COD. For more information on derivation and use of Hach s estimated detection limit, see Section 1. Summary of Method Chemical oxygen demand (COD) is defined as... a measure of the oxygen equivalent of the organic matter content of a sample that is susceptible to oxidation by a strong chemical oxidant ± (APHA Standard Methods, 19th ed., 1995). Trivalent manganese is a strong, noncarcinogenic chemical oxidant that changes quantitatively from purple to colorless when it reacts with organic matter. It typically oxidizes about 80% of the organic compounds. Studies have shown that the reactions are highly reproducible and test results correlate closely to Biochemical Oxygen Demand (BOD) values and hexavalent chromium COD tests. None of the oxygen demand tests provide 100% oxidation of all organic compounds. A calibration is provided which is based on the oxidation of Potassium Acid Phthalate (KHP). A different response may be seen in analyzing various wastewaters. The KHP calibration is adequate for most applications. The highest degree of accuracy is obtained when test results are correlated to a standard reference method such as BOD or one of the chromium COD methods. Special waste streams or classes will require a separate calibration to obtain a direct mg/l COD reading or to generate a correction factor for the precalibrated KHP response. The sample digestion time can be extended up to 4 hours for samples which are difficult to oxidize. (CRC)...1...25/pkg...26618-25 COD, 20-1000 mg/l...1...25/pkg...26234-25... 1 ml...4 Kg...979-09...... 4 L...272-56 COD/TNT... 1......48464-00, 120 Vac, 14-speed... 1......26747-00, 118 ml... 1... 2/pkg...26748-00, with inert Teflon liner, for mixing bottle... varies... 12/pkg...24018-12 COD, 115 V... 1......45600-00 COD r, 230 V, European-style plug... 1...45600-02 239

, extra fine point... 1......26696-00, for sample + acid... 1......24276-06 TenSette., 0.1 to 1.0 ml... 1... 19700-01 TenSette., 1.0 to 10.0 ml... 1...19700-10, for 19700-01 TenSette. Pipet... 2... 50/pkg...21856-96, for 19700-10 TenSette. Pipet... 2... 50/pkg...21997-96... 1......23810-00... 1......18641- (VPD)...1......49000-00, 115 V...1......14697-00, 230V...1......14697-02 OPTIONAL REAGENTS AND APPARATUS COD Standard Solution, 800 mg/l COD... 200 ml...26726-29 Potassium Acid Phthalate...500 g...315-34 Dispenser for sulfuric acid...each...25631-37 For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 240

241

0.0 mg/l O2 Cr3+ Cu2+ Fe2+ Mg2+ Mn2+ Ni2+ NO2 Sampling and Storage The main consideration in sampling with the High Range Dissolved Oxygen AccuVac Ampul is to prevent the sample from becoming contaminated with atmospheric oxygen. This is accomplished by capping the ampul with an ampul cap in the interval between breaking open the ampul and reading the absorbance. If the ampul is securely capped, it should be safe from contamination for several hours. The absorbance will decrease by approximately 3% during the first hour and will not change significantly afterwards. Sampling and sample handling are important considerations in obtaining meaningful results. The dissolved oxygen content of the water beingtested can be expected to change with depth, turbulence, temperature, sludge deposits, light, microbial action, mixing, travel time and other factors. A single dissolved oxygen test rarely reflects the accurate over-all condition of a body of water. Several samples taken at different times, locations and depths are recommended for most reliable results. Samples must be tested 242

immediately upon collection although only a small error results if the absorbance reading is taken several hours later. Accuracy Check The results of this procedure may be compared with the results of a titrimetric procedure (request lit. code number 8042) or dissolved oxygen meter (Cat. No. 50175-00). Method Performance Precision In a single laboratory, using a standard solution of 8.0 mg/l O2 determined by the Winkler method and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of À0.41 mg/l O2. Estimated Detection Limit The estimated detection limit for program 70 is 0.10 mg/l O2. For more information on the estimated detection limit, see Section 1. Summary of Method The High Range Dissolved Oxygen AccuVac Ampul contains reagent vacuum sealed in a 12-mL ampul. When the AccuVac ampul is broken open in a sample containing dissolved oxygen, a yellow color forms, which turns purple as the oxygen reacts with the reagent. The color developed is proportional to the concentration of dissolved oxygen. AccuVac...1... 25/pkg...25150-25, 50 ml... 1......500-41...... 25/pkg...1731-25, 10-20-25 ml, w/ cap... 1... 6/pkg...24019-06 OPTIONAL REAGENTS AND APPARATUS AccuVac Dissolved Oxygen Sampler... each...24051-00 AccuVac Snapper Kit... each...24052-00 AccuVac Drainer... each...41036-00 BOD bottle and stopper, 300 ml... each...621-00 Dissolved Oxygen Meter, sension.6, Portable... each...50175-00 Dissolved Oxygen Reagent Set (Buret Method)... 100 tests...23514-00 Dissolved Oxygen Reagent Set (Digital Titrator Method)... 50 tests...22722-00 Dissolved oxygen may also be determined by titrimetric methods. Request Publication 8042 for additional information. For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 243

0 μg/l O2 μ 244

Sampling and Storage The main consideration in this procedure is to prevent contaminating the sample with atmospheric oxygen. Sampling from a stream of water that is hard plumbed to the sample source is ideal. Use a funnel to maintain a continual flow of sample and yet collect enough sample to immerse the ampul. It is important not to introduce air in place of the sample. Rubber tubing, if used, will introduce unacceptable amounts of oxygen into the sample unless the length of tubing is minimized and the flow rate is maximized. Flush the sampling system with sample for at least 5 minutes. Accuracy Check The reagent blank for this test can be checked by following these steps: a) Fill a 50-mL beaker with sample and add approximately 50 mg sodium hydrosulfite. b) Immerse the tip of a Low Range Dissolved Oxygen AccuVac Ampul in the sample and break the tip. Keep the tip immersed while the ampul fills completely. c) Determine the dissolved oxygen concentration according to the preceding procedure. The result should be 0 À1 Ìg/L. Method Performance Precision In a single laboratory, using a standard solution of 500 Ìg/L O2 and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of 2 Ìg/L O2. For more information on Hach s precision statement, see Section 1. Estimated Detection Limit The estimated detection limit for program #71 is 10 Ìg/L O2. For more information on the estimated detection limit, see Section 1. Summary of Method When the vacuum-sealed AccuVac ampul is broken open in a sample containing dissolved oxygen, the yellow reagent solution turns blue. The blue color is proportional to the dissolved oxygen concentration. AccuVac... 1...25/pkg...25010-25, 50 ml...1......500-41, 10-20-25 ml, w/cap...1...6/pkg...24019-06 OPTIONAL REAGENTS AND APPARATUS AccuVac Snapper Kit...each...24052-00 Sodium Hydrosulfite, technical grade...500 g...294-34 For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 245

246

Sampling The chief consideration when collecting a sample is to prevent the escape of ozone from the sample. The sample should be collected gently and analyzed immediately. Warming the sample or disturbing the sample by stirring or shaking will result in ozone loss. After collecting the sample, do not transfer it from one container to another unless absolutely necessary. Stability of Indigo Reagent Indigo is light-sensitive. Therefore, the AccuVac Ampuls should be kept in the dark at all times. However, the indigo solution decomposes slowly under room light after filling with sample. The blank ampul can be used for multiple measurements during the same day. Method Performance Precision In a single laboratory, using standard solutions of 0.15, 0.28 and 0.96 mg/l ozone for the low, mid and high range, respectively, and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of 0.01, À0.02 and À0.02 mg/l O3 for the low, mid and high range tests, respectively. For more information on Hach s precision statement, see Section 1. Estimated Detection Limit The estimated detection limit for the programs #72, #73, and #74 is 0.02 mg/l O3. For more information on the estimated detection limit, see Section 1. Summary of Method The reagent formulation adjusts the sample ph to 2.5 after the ampul has filled. The indigo reagent reacts immediately and quantitatively with ozone. The blue color of indigo is bleached in proportion to the amount of ozone present in the sample. Other reagents in the formulation prevent chlorine interference. No transfer of sample is needed in the procedure. Therefore, ozone loss due to sampling is eliminated. 247

AccuVac : 0-0.25 mg/l... 2...25/pkg...25160-25 0-0.75 mg/l... 2...25/pkg...25170-25 0-1.50 mg/l... 2...25/pkg...25180-25...... 4 L...272-56, 50 ml...2......500-41 OPTIONAL APPARATUS AccuVac Snapper Kit...each...24052-00 AccuVac Ampule sampler...each...24051-00 For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 248

0 mg/l PH 249

Sampling and Storage Analyze samples immediately for best results. Accuracy Check Standard Solution Method Using a clear ph 7.0 buffer solution as the sample, perform the ph procedure as described above. Method Performance Precision In a single laboratory using a standard solution of ph 7.0 and two lots of reagent with the instrument, a single operator obtained a standard deviation of less than 0.1 ph units. Estimated Detection Limit The estimated detection limit for program 75 is a ph of 6.5. Standard Adjust To adjust the calibration curve using the reading obtained with the 7.0 buffer solution, press the SETUP key and scroll (using the arrow keys) to the STD setup option. Press ENTER to activate the standard adjust option. Then enter 7.0 to edit the standard concentration to match that of the standard used. See Section 1, Standard Curve Adjustment for more information. Press ENTER to complete the curve adjustment. 250

Summary of Method This method uses a sulfonphthalein indicator (Phenol Red) to determine ph colorimetrically. Phenol Red has a working range of ph 6.8 (yellow) to 8.2 (red)., 0.5 & 1.0 ml marks... 1... 20/pkg...21247-20 Phenol Red, spec grade...1.0 ml...50 ml...26575-12, 10-20-25 ml, w/ cap... 2... 6/pkg...24019-06 OPTIONAL REAGENTS ph 7.0 Buffer Solution...500 ml...12222-49 OPTIONAL APPARATUS Description Units Cat. No. Thermometer, -10 to 110 ãc... each...1877-01 For Technical Assistance, Price and Ordering In the U.S.A. call 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 251

PO4 252

PhosVer 3 2:00 TIMER 2 253

0.0 mg/l PO4 2 254

5mL 5.00mL100 mg/l100 mg/l 10mL50mg/L, CDTA,,, EDTA,,, Diethanoldithiocarbamate, NTA ph 100 mg/l 10mg/L 1000mg/L 5000 mg/l 100 mg/l30 50 mg/l 200 mg/l 250 mg/l 15 mg/l 500 mg/l 10 mg/l Sampling and Storage Collect samples in clean plastic or glass bottles that have been cleaned with 1:1 Hydrochloric Acid Solution and rinsed with deionized water. Do not use a commercial detergent. If prompt analysis is impossible, adjust the ph to 2 or less with about 2 ml of sulfuric acid, ACS, per liter of sample. Store at 4 ãc (39 ãf) or below. Preserved samples can be stored at least 24 hours. See Section 1 for more information on dilution factors, cleaning instructions, etc. Accuracy Check Ideally, a solution containing a known amount of the phosphonate product being used should be prepared. This will check the UV conversion of phosphonate to orthophosphate. Summary of Method This method is directly applicable to boiler and cooling tower samples. The procedure is based on a UV catalyzed oxidation of phosphonate to orthophosphate. Range may be as low as 0 to 2.5 mg/l or as high as 0 to 125 mg/l. Phosphonate is converted to orthophosphate during the UV digestion. Both the sample and the blank will develop color if orthophosphate is present in the sample. The increase in color in the sample is proportional to the phosphate produced in the digestion. 255

(100 tests).... 24297-00 : (2) 21060-69, (1) 20847-69 PhosVer 3... 2...100/pkg... 21060-69 ()...1...100/pkg... 20847-69...... 4 L... 272-56, 50 ml...1...... 1896-41, UV safety...1...... 21134-00, 25 ml...1...... 2066-40 Pipet Filler, safety bulb...1...... 14651-00, 10-20-25 ml, w/cap...2...6/pkg... 24019-06, 115 V...1...... 20828-00, 230 V...1...... 20828-02 OPTIONAL REAGENTS Hydrochloric Acid, 6.0 N (1:1)... 500 ml... 884-49 Sulfuric Acid, ACS... 500 ml... 979-49 OPTIONAL APPARATUS Cord Adapter, single to dual UV lamp...each... 19485-00 ph Paper, 1 to 11 ph units...5 rolls/pkg... 391-33 Pipet, serological, 2 ml...each... 532-36 Pipet, TenSette, 1-10 ml...each... 19700-10 Pipet Tips, for 19700-10 Tensette Pipet...50/pkg... 21997-96 Pipet Tips, for 19700-10 Tensette Pipet...1000/pkg... 21997-28 Thermometer, -10 to 110 ãc...each... 1877-01 UV Lamp, without power supply...each... 20823-00 For Technical Assistance, Price and Ordering In the U.S.A. call 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 256

(0 to 45.0 mg/l) PO4 0.0 mg/l PO4 257

258

Sampling and Storage Collect samples in clean plastic or glass bottles that have been cleaned with 1:1 Hydrochloric Acid Solution and rinsed with deionized water. Do not use a commercial detergent containing phosphate for cleaning glassware used in this test. Analyze samples immediately for best results. If prompt analysis is impossible, preserve samples by filtering immediately and storing at 4 ãc for up to 48 hours. Accuracy Check Standard Additions Method a) Fill three 25-mL graduated mixing cylinders with 25 ml of sample. b) Snap the neck off a Phosphate Voluette Ampule Standard Solution, 500 mg/l as PO4. c) Use the TenSette Pipet to add 0.1 ml, 0.2 ml and 0.3 ml of standard, respectively, to the three mixing cylinders. Stopper and invert to mix well. d) For analysis with AccuVac Ampuls, transfer the spiked samples to clean, dry 50-mL beakers to facilitate filling of the ampuls. For analysis with reagent solution, transfer the spiked samples to 25-mL sample cells. e) Analyze each sample as described in the procedure. Each 0.1-mL addition of standard should cause an increase of 2.0 mg/l PO4 3-. f) If these increases do not occur, see Standard Additions (Section 1) for more information. Standard Solution Method Obtain a Hach Phosphate Standard Solution, 10.0 mg/l as phosphate. Using this solution as the sample, perform the phosphate procedure as described above. Standard Adjust To adjust the calibration curve using the reading obtained with the 10.0 mg/l standard solution, press the SETUP key and scroll (using the arrow keys) to the STD setup option. Press ENTER to activate the standard adjust option. Then enter 10.0 to edit the standard concentration to match that of the standard used. Press ENTER to complete the adjustment. See Standard Curve Adjustment, Section 1 for more information. Method Performance Precision In a single laboratory using a standard solution of 30.0 mg/l PO43-, two lots of reagent, and the instrument, a single operator obtained a standard deviation of À0.1 mg/l PO4 3- for the reagent solution method and a standard deviation of À0.2 for the AccuVac Ampul method. Estimated Detection Limit The estimated detection limit for program 77 is 0.3 mg/l PO4 3- and 0.4 mg/l PO4 3- for program 78. For more information on the estimated detection limit, see Section 1. Summary of Method In the molybdovanadate method, orthophosphate reacts with molybdate in an acid medium to produce a phosphomolybdate complex. In the presence of vanadium, yellow vanadomolybdophosphoric acid is formed. The intensity of the yellow color is proportional to the phosphate concentration. 259

() Molybdovanadate... 2.0 ml...100 ml* MDB...20760-32, 10-20-25 ml, w/ cap... 2... 6/pkg...24019-06... 25 ml... 4 L...272-56 () Molybdovanadate... 2... 25/pkg...25250-25, 50 ml... 2......500-41... 25 ml... 4 L...272-56 OPTIONAL REAGENTS Description Units Cat. No. Bromine Water, 30 g/l...29 ml*...2211-20 Hydrochloric Acid Solution, 1:1 (6.0 N)...500 ml...884-49 Phenol Solution, 30 g/l...29 ml...2112-20 Phosphate Standard Solution, 10.0 mg/l as PO43-... 946 ml...14204-16 Phosphate Standard Solution, Voluette Ampule, 500 mg/l as PO43-, 10 ml... 16/pkg...14242-10 Sodium Hydroxide Standard Solution, 5.0 N... 100 ml* MDB...2450-32 Sulfuric Acid, ACS...500 ml*... 979-49 OPTIONAL APPARATUS AccuVac Snapper Kit... each...24052-00 Ampule Breaker Kit... each...21968-00 Cylinder, graduated, 25 ml... each...508-40 Cylinder, graduated, mixing, 25-mL... each...20886-40 Dispenser, fixed volume, 1.0 ml Repipet Jr.... each...21113-02 Flask, erlenmeyer, 50 ml... each...505-41 Flask, volumetric, Class A, 50 ml... each...14574-41 ph Paper, 1 to 11 ph units... 5 rolls/pkg...391-33 ph Meter, Sension.1, portable... each...51700-00 Pipet, serological, 2.0 ml... each...532-36 Pipet, TenSette, 0.1 to 1.0 ml... each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet... 50/pkg...21856-96 Thermometer, -10 to 110 ãc... each...1877-01 For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 260

~ PO4 PhosVer 3 0.0 mg/l PO4 261

200 mg/l, 100mg/L 10mg/L 300 mg/l 50mg/L 6 mg/l 125mL50mL 2 31 80 mg/l ph Sampling and Storage Collect sample in plastic or glass bottles that have been cleaned with 1:1 Hydrochloric Acid Solution and rinsed with deionized water. Do not use commercial detergents containing phosphate for cleaning glassware used in this test. Analyze samples immediately after collection for best results. If prompt analysis is impossible, preserve samples for up to 48 hours by filtering immediately and storing samples at 4 ãc. Warm to room temperature before testing. 262

Accuracy Check Standard Additions Method a) Fill three 25-mL graduated mixing cylinders with 25 ml of sample. b) Snap the neck off a Phosphate PourRite Ampule Standard Solution, 50 mg/l as PO4 c) Use the TenSette Pipet to add 0.1 ml, 0.2 ml, and 0.3 ml of standard, respectively, to the three mixing cylinders. Stopper each and mix thoroughly. d) For analysis with AccuVacs, transfer solutions to dry, clean 50 ml beakers to fill the AccuVac ampules. For analysis with powder pillows, transfer only 10 ml of solution to the sample cells. e) Analyze each standard addition sample as described in the procedure. The phosphate concentration should increase 0.2 mg/l PO43- for each 0.1 ml of standard added. f) If these increases do not occur, see Standard Additions in Section 1. Standard Solution Method Prepare a 2.0 mg/l PO43- standard solution by pipetting 4.0 ml of Phosphate Standard Solution, 50 mg/l as PO4 3-, into an acid-washed Class A 100-mL volumetric flask. Dilute to volume with deionized water. Stopper and invert to mix. Use this solution in place of the sample in the procedure to insure the accuracy of the test. The mg/l PO4 3- reading should be 2.00 mg/l. Method Performance Precision In a single laboratory using a standard solution of 1.00 mg/l PO43- and two lots of reagents with the instrument, a single operator obtained a standard deviation of À0.05 mg/l PO4 3- In a single laboratory using a standard solution of 1.00 mg/l PO43- and two representative lots of AccuVac ampuls with the instrument, a single operator obtained a standard deviation of À0.03 mg/l PO4 3-. Estimated Detection Limit (EDL) The EDL for program 79 is 0.05 mg/l PO4. For more information on the estimated detection limit, see Section 1. Summary of Method Orthophosphate reacts with molybdate in an acid medium to produce a Phosphomolybdate complex. Ascorbic acid then reduces the complex, giving an intense molybdenum blue color. () PhosVer 3 10 ml sample size...1... 100/pkg...21060-69, 10-20-25 ml, w/cap... 2... 6/pkg...24019-06 () PhosVer 3 AccuVac... 1... 25/pkg...25080-25, 50 ml... 1......500-41 263

... 1... 25/pkg...1731-25, 10-20-25 ml, w/cap... 1... 6/pkg...24019-06 OPTIONAL REAGENTS Hydrochloric Acid Standard Solution, 6.0 N (1:1)...500 ml...884-49 Phosphate Pretreatment Powder Pillows... 50/pkg...14501-66 Phosphate Standard Solution, PourRite ampule, 50 mg/l as PO4 3-, 2 ml... 20/pkg...171-20 Phosphate Standard Solution, Voluette Ampul, 50 mg/l, 10 ml... 16/pkg...171-10 Sodium Hydroxide Standard Solution, 5.0 N...100 ml* MDB...2450-32 Water, deionized...4 L...272-56 OPTIONAL APPARATUS AccuVac Snapper Kit... each...24052-00 Ampule Breaker Kit for 10-ml ampules... each...21968-00 Aspirator, vacuum... each...2131-00 Cylinder, graduated, mixing, 25 ml, tall (3 required)... each...20886-40 Filter Holder, 47 mm, 300 ml, graduated... each...13529-00 Filter, membrane, 47 mm, 0.45 microns... 100/pkg...13530-00 Flask, filtering, 500 ml... each...546-49 Flask, volumetric, Class A, 100 ml... each...14574-42 ph Indicator Paper, 1 to 11 ph... 5 rolls/pkg...391-33 ph Meter, Sension.1, portable... each...51700-00 Pipet, 2 ml serological... each...532-36 Pipet, TenSette, 0.1 to 1.0 ml TenSette Pipet... each...19700-01 Pipet Tips, for 19700-01... 50/pkg...21856-96 Pipet Filler, safety bulb... each...14651-00 Pipet, volumetric, Class A, 4.00 ml... each...14515-04 PourRite Ampule Breaker Kit... each...24846-00 For Technical Assistance, Prices and Ordering In the U.S.A. call 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 264

5 6 2ml 5N 3 25ml * = ++ * 265

Sampling and Storage Collect samples in plastic or glass bottles that have been acid-washed with 1:1 HCl and rinsed with deionized water. Do not use detergents containing phosphates for cleaning glassware used in this test. Analyze samples immediately after collection for best results. If prompt analysis is impossible, preserve samples up to 28 days by adjusting the ph to 2 or less with concentrated sulfuric acid (about 2 ml per liter) and storing at 4 ãc. Warm to room temperature before testing. Correct results for volume additions; see Volume Additions (Section 1) for more information. Interferences For turbid samples, use 50 ml of sample and double the reagent quantities. Use digested sample to zero the instrument in the reactive phosphorus procedure. This compensates for any color or turbidity destroyed by this procedure. For alkaline or highly buffered samples it may be necessary to add additional acid in Step 3 to drop the ph of the solution below 1. Summary of Method Phosphates present in organic and condensed inorganic forms (meta-, pyro- or other polyphosphates) must be converted to reactive orthophosphate before analysis. Pretreatment of the sample with acid and heat provides the conditions for hydrolysis of the condensed inorganic forms. Organic phosphates are converted to orthophosphate by heating with acid and persulfate. Organically bound phosphates are thus determined indirectly by subtracting the result of an acid hydrolyzable phosphorus test from the total phosphorus result. This procedure must be followed by one of the reactive phosphorus(orthophosphate) analysis methods for determination of the phosphorus content of the sample. If the ascorbic acid (PhosVer 3) method is used to measure the reactive phosphorus, this method is EPA approved for NPDES reporting. The following reagents and apparatus are required in addition to those required for the reactive phosphorus test.... 1...100/pkg...2451-99, 5.0 N... 2 ml....100 ml* MDB...2450-32, 5.25 N... 2 ml...100 ml* MDB...2449-32, 25 ml...2......508-40, 50 ml...1......505-41, 10-20-25 ml, w/caps...2...6/pkg...24019-06 OPTIONAL REAGENTS Hydrochloric Acid, 6 N... 500 ml...884-49 266

Sodium Hydroxide Solution, 5.0 N... 1 L...2450-53 Sulfuric Acid... 500 ml...979-49 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS Description Unit Cat. No. Cylinder, graduated, 50 ml... each...508-41 Flask, erlenmeyer, 125 ml... each...505-43 Hot Plate, 4" diameter, 120 Vac... each...12067-01 Hot Plate, 4" diameter, 240 Vac... each...12067-02 Pads, cooling, 4 x 4"...... each...18376-00 ph Indicator Paper, 1 to 11 ph...... 5 rolls/pkg...391-33 ph Meter, Sension.1, portable...... each...51700-00 For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 267

* = + 268

Sampling and Storage Analyze samples immediately after collection for best results. If prompt analysis is not possible, samples may be preserved up to 48 hours by cooling to 4 ãc (39 ãf). Warm to room temperature before testing. Summary of Method This procedure lists the necessary steps to convert condensed phosphate forms (meta-, pyro- or other polyphosphates) to reactive orthophosphate before analysis. The procedure uses acid and heat to hydrolyze the sample. Organic phosphates are not converted to orthophosphate by this process, but a very small fraction may be unavoidably included in the result. Thus, the acid hydrolyzable ± phosphate results are primarily a measure of inorganic phosphorus. This procedure must be followed by one of the reactive phosphorus (orthophosphate) analysis methods for determination of the phosphorous content of the sample. The following reagents and apparatus are required in addition to those required for the reactive phosphorus test., 5.0 N... 2 ml...100 ml* MDB...2450-32, 5.25 N... 2 ml...100 ml* MDB... 2449-32, 25 ml... 2......508-40, 50 ml... 1......505-41 OPTIONAL REAGENTS Hydrochloric Acid, 6 N...500 ml...884-49 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS Cylinder, graduated, 50 ml... each...508-41 Flask, erlenmeyer, 125 ml... each...505-43 Hot Plate, 4" diameter, 120 Vac... each...12067-01 Hot Plate, 4" diameter, 240 Vac... each...12067-02 Pad, cooling, 4" x 4"... each...18376-00 ph indicator Paper, 1 to 11 ph... 5 rolls/pkg...391-33 ph Meter, sension.1, portable... each...51700-00 Thermometer, -10 to 110 ãc... each...1877-01 For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 269

Test N tube PO4 TenSette 5 Test 'N Tube 0.00 mg/l PO4 270

PhosVer 3 PhosVer 3 271

, ph 200 mg/l 100mg/L 10mg/L 300 mg/l 50mg/L 6 mg/l 425mL50mL 5 61 80 mg/l Sampling and Storage Collect samples in plastic or glass bottles that have been acid cleaned with 1:1 Hydrochloric Acid Solution and rinsed with deionized water. Do not use commercial detergents containing phosphate for cleaning glassware used in this test. Analyze samples immediately after collection for best results. If prompt analysis is impossible, preserve samples for up to 48 hours by filtering immediately and storing at 4 ãc. Warm to room temperature before analyzing the sample. Accuracy Check Note: Clean glassware with 1:1 hydrochloric acid solution. Rinse again with deionized water. Do not use detergents containing phosphates to clean glassware. Standard Additions Method a) Fill three 25-mL graduated mixing cylinders with 25 ml of sample. b) Snap the neck off a Phosphate PourRite Ampule Standard, 50 mg/l as PO4 3-. c) Use the TenSette Pipet to add 0.1 ml, 0.2 ml and 0.3 ml, respectively, to the three 25-mL aliquots of sample prepared in step a. Mix well. d) Analyze each sample as described in the procedure; use 5.0 ml of the prepared standard additions for each test. The concentration should increase as follows: 0.2 mg/l, 0.4 mg/l, 0.6 mg/l PO4, respectively. e) If these increases do not occur, see Standard Additions in Section 1 for more information. Standard Solution Method To check accuracy, use a 1.0 mg/l Phosphate Standard Solution listed under Optional Reagents. Or, prepare a 1.0-mg/L PO4 3- standard by pipetting 2 ml of solution from a Phosphate Voluette Ampule Standard for Phosphate, 50 mg/l as PO4-, into an 272

acid-washed, Class A 100-mL volumetric flask. Dilute to the mark with deionized water. Substitute this standard for the sample and perform the procedure as described. Method Performance Precision In a single laboratory, using a standard solution of 5.00 mg/l PO4 3- and two lots of reagent with the instrument, a single operator obtained a standard deviation of À0.08 mg/l PO4 3-. Estimated Detection Limit (EDL) The EDL for program 82 is 0.07 mg/l PO43-. For more information on derivation and use of Hach s estimated detection limit, see Section 1. Sample Disposal Information Final samples will contain molybdenum. In addition, final samples will have a ph less than 2 and are considered corrosive (D002) by the Federal RCRA. Summary of Method Orthophosphate reacts with molybdate in an acid medium to produce a phosphomolybdate complex. Ascorbic acid then reduces the complex, giving an intense molybdenum blue color. Test N Tube...50 tests... 27425-45 : (1) 21060-46, (50) * PhosVer 3...1...50/pkg... 21060-46 50Test N Tube...1...50/pkg... * COD/TNT...1...... 48464-00...1...... 25843-35 TenSette, 1 to 10 ml...1...... 19700-10, for 19700-10 TenSette Pipet...1...50/pkg... 21997-96... 1-3...... 18641-00 OPTIONAL REAGENTS Bromine Water, 30 g/l... 29 ml... 2211-20 Hydrochloric Acid Standard Solution, 6.0 N (1:1)... 500 ml... 884-49 Phenol Solution, 30 g/l... 29 ml... 2112-20 Phosphate Standard Solution, 1 mg/l as PO43-... 500 ml... 2569-49 Phosphate Standard Solution, Voluette ampule, 50 mg/l as PO43-,10mL...16/pkg... 171-10 Phosphate Standard Solution, PourRite ampule, 50 mg/l as PO43-, 2 ml...20/pkg... 171-20 273

Water, deionized... 4 L... 272-56 OPTIONAL APPARATUS Ampule Breaker, Pour Rite (2-mL ampule)... each...24846-00 Ampule Breaker Kit... each...21968-00 Aspirator, vacuum... each...2131-00 Cylinder, graduated, mixing, 25 ml (3 required)... each...20886-40 Dispenser, Repipet Jr., 2 ml... each...22307-01 Filter Holder, 47 mm, 300 ml, graduated... each...13529-00 Filter, membrane, 47 mm, 0.45 microns... 100/pkg...13530-00 Flask, filtering, 500 ml... each...546-49 Flask, volumetric, Class A, 100 ml... each...14574-42 ph Indicator Paper, 1 to 11 ph units... 5 rolls/pkg...391-33 ph Meter, sension.1, portable... each...51700-00 Pipet, TenSette, 0.1 to 1.0 ml... each...19700-01 Pipet Tips, for 19700-01... 50 pkg...21856-96 Pipet Filler, Safety Bulb... each...14651-00 Pipet, volumetric, Class A, 5.00 ml... each...14515-37 Pipet, volumetric, Class A, 2.00 ml... each...14515-36 For Technical Assistance, Price and Ordering In the U.S.A. call 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 274

mg/l, PO4ZERO 275

PhosVer 3 0.00 mg/l PO4 PhosVer 3 276

PhosVer 3 ph, 200 mg/l 100 mg/l 10 mg/l 100 mg/l 300 mg/l ph 50 mg/l 10 mg/l 90 mg/l 80 mg/l Sampling and Storage Collect samples in plastic or glass bottles that have been acid cleaned with 1:1 Hydrochloric Acid Solution and rinsed with deionized water. Do not use commercial detergents containing phosphates for cleaning glassware used in this test. Analyze samples immediately after collection for best results. If prompt analysis is impossible, preserve the sample for up to 28 days by adjusting the ph to 2 or less with 277

concentrated sulfuric acid (about 2 ml per liter) and storing at 4 ãc. Neutralize and warm the sample to room temperature before analysis. Correct test results for volume additions; see Volume Additions in Section 1. Accuracy Check Note: Clean glasswarewith 1:1 hydrochloric acid solution. Rinse again with deionized water. Do not use detergents containing phosphates to clean glassware. Standard Additions Method a) Fill three 25 ml graduated mixing cylinders with 25 ml of sample. b) Snap the neck off a Phosphate PourRite Ampule Standard, 50 mg/l as PO43-. c) Use the TenSette Pipet to add 0.1 ml, 0.2 ml and 0.3 ml, respectively, to the three 25-mL aliquots of sample prepared in step a. Mix well. d) Analyze each sample as described in the procedure using 5.0 ml of the prepared standard additions for each test. The concentration should increase 0.2 mg/l, 0.4 mg/l, and 0.6 mg/l PO4 3-, respectively. e) If these increases do not occur, see Standard Additions (Section 1). Standard Solution Method To check accuracy, use a 1.0 mg/l Phosphate Standard Solution (see Optional Reagents). Or, prepare a standard by pipetting 2 ml of solution a Voluette Ampule Standard for Phosphate Standard, 50 mg/l as PO4 3-, into an acid-cleaned Class A 100-mL volumetric flask. Dilute to the mark with deionized water. Substitute this standard for the sample and perform the procedure as described. The mg/l PO4 3- reading should be 1.0 mg/l. ORPrepare a 2.5 mg/l standard solution by pipetting 5 ml of a 50-mg/L Phosphate Voluette Ampule Standard into an acid-washed 100-mL Class A volumetric flask. Dilute to the mark with deionized water. Method Performance Precision In a single laboratory, using a standard solution of 3.00 mg/l PO43- and two lots of reagent with the instrument, a single operator obtained a standard deviation of À0.06 mg/l PO4 3-. Estimated Detection Limit The estimated detection limit for program 82 is 0.07 mg/l PO4 3-.For more information on the estimated detection limit, see Section 1. Sample Disposal Information Final samples will contain molybdenum. In addition, final samples will have a ph less than 2 and are considered corrosive (D002) by the Federal RCRA. Summary of Method Phosphates present in organic and condensed inorganic forms (meta-, pyro- or other polyphosphates) must be converted to reactive orthophosphate before analysis. Pretreatment of the sample with acid and heat provides the conditions for hydrolysis of the condensed inorganic forms. Organic phosphates are converted to orthophosphate by heating with acid and persulfate. Orthophosphate reacts with molybdate in an acid medium to produce a phosphomolybdate complex. Ascorbic acid then reduces the complex, giving an intense molybdenum blue color. 278

Test N Tube...50 tests... 27426-45 : (1) 272-56, (1) 20847-66, (1) 21060-46, (1) 27430-42, (50) * PhosVer 3...1...50/pkg... 21060-46...1...50/pkg... 20847-66, 1.54 N... 2 ml... 100 ml...27430-42 Test N Tube...1...50/pkg...*... 100 ml...4 liters... 272-56 COD, 115/230 Vac (U.S.A. and Canada)...1...... 45600-00 COD, 115/230 Vac (Europe)...1...... 45600-02 COD/TNT...1... 48464-00...1...... 25843-35...1...... 23810-00... 1-3...... 18641-00 TenSette, 1 to 10 ml...1...... 19700-10, for 19700-10 TenSette Pipet......50/pkg... 21997-96 OPTIONAL REAGENTS Description Unit Cat. No. Total and Acid Hydrolyzable Test N Tube Reagent Set... each...27427-45 Hydrochloric Acid Standard Solution, 6.0 N (1:1)...500 ml...884-49 Phosphate Standard Solution, 1 mg/l as PO43-...500 ml...2569-49 Phosphate Standard Solution, PourRite ampule, 50 mg/l as PO43-, 2 ml... 20/pkg...171-20 Phosphate Standard Solution, Voluette ampule, 50 mg/l as PO43-, 10 ml... 16/pkg...171-10 Sodium Hydroxide Standard Solution, 5.0 N...1 L...2450-53 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS Ampule Breaker Kit... each...21968-00 Ampule Breaker, PourRite ampules... each...24846-00 Cylinder, graduated, mixing, 25 ml (3 required)... each...20886-40 ph Indicator Paper, 1 to 11 ph units... 5 rolls/pkg...391-33 ph Meter, Sension.1, portable... each...51700-00 Pipet Filler, safety bulb... each...14651-00 Pipet, volumetric, Class A, 5.00 ml... each...14515-37 Pipet, volumetric, Class A, 2.00 ml... each...14515-36 Pipet, TenSette, 0.1-1.0 ml... each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet... 50/pkg...21856-96 For Technical Assistance, Price and Ordering In the U.S.A. call 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving 279

PhosVer 3 Test N Tube mg/l, PO4ZERO 280

PhosVer 3 0.00 mg/l PO4 PhosVer 3 10 15 PhosVer 3 281

200 mg/l 100 mg/l 10 mg/l 100 mg/l 300 mg/l ph, ph 50 mg/l 10 mg/l 90 mg/l 80 mg/l PhosVer 3 282

Sampling and Storage Collect samples in plastic or glass bottles that have been acid cleaned with 1:1 Hydrochloric Acid Solution and rinsed with deionized water. Do not use commercial detergents containing phosphate for cleaning glassware used in this test. Analyze samples immediately after collection for best results. If prompt analysis is impossible, the sample may be preserved up to 48 hours by cooling to 4 ãc (39 ãf). Warm to room temperature before testing. Accuracy Check Note: Clean glassware with 1:1 hydrochloric acid solution. Rinse with deionized water. Do not use detergents containing phosphate to clean glassware. Standard Additions Method a) Fill three 25-mL graduated mixing cylinders with 25 ml of sample. b) Snap the neck off a Phosphate PourRite Ampule Standard, 50 mg/l as PO43-. c) Use the TenSette Pipet to add 0.1 ml, 0.2 ml and 0.3 ml, respectively, to the three 25-mL aliquots of sample prepared in step a. Mix well. d) Analyze each sample as described in the procedure. Use 5.0 ml of the prepared standard additions for each test; the concentration should increase as follows: 0.2 mg/l, 0.4 mg/l, and 0.6 mg/l PO43-, respectively. e) If these increases do not occur, see Standard Additions in Section 1 for more information. Standard Solution Method Obtain a 1.0 mg/l Phosphate Standard Solution listed under Optional Reagents. Or, this can be prepared by pipetting 2 ml of a Voluette Ampule Standard for Phosphate, 50 mg/l as PO4 3-, into an acid washed Class A 100-mL volumetric flask. Dilute to the mark with deionized water. Substitute this standard for the sample and perform the procedure as described. Method Performance Precision In a single laboratory, using a standard solution of 3.00 mg/l PO43- and two lots of reagent with the instrument, a single operator obtained a standard deviation of À0.06 mg/l PO43-. Estimated Detection Limit The estimated detection limit for program 82 is 0.07 mg/l PO43-. For more information on the estimated detection limit, see Section 1. Sample Disposal Information Final samples will contain molybdenum. In addition, final samples will have a ph less than 2 and are considered corrosive (D002) by the Federal RCRA. Summary of Method Phosphates present in organic and condensed inorganic forms (meta-, pyro- or other polyphosphates) must be converted to reactive orthophosphate before analysis. Pretreatment of the sample with acid and heat provides the conditions for hydrolysis of 283

the condensed inorganic forms. Organic phosphates are converted to orthophosphate by heating with acid and persulfate. Orthophosphate reacts with molybdate in an acid medium to produce a phosphomolybdate complex. Ascorbic acid then reduces the complex, giving an intense molybdenum blue color. REQUIRED REAGENTS Test N Tube 1...50tests...27427-45 : (1) 272-56, (1) 1045-42, (1) 20847-66, (1) 21060-46, (50) PhosVer 3...1...50/pkg... 21060-46...1...50/pkg... 20847-66, 1.54 N... 2 ml... 100 ml...27430-42 Test N Tube...1...50/pkg...*... 100mL...4...272-56 REQUIRED APPARATUS COD, 115/230 Vac (U.S.A. and Canada)...1...... 45600-00 COD, 115/230 Vac (Europe)...1...... 45600-02 COD/TNT...1... 48464-00...1...... 25843-35...1...... 23810-00... 1-3...... 18641-00 TenSette, 1 to 10 ml...1...... 19700-10, for 19700-10 TenSette Pipet......50/pkg... 21997-96 OPTIONAL REAGENTS Bromine Water, 30 g/l... 29 ml... 2211-20 Hydrochloric Acid Standard Solution, 6.0 N (1:1)... 500 ml... 884-49 Phenol Solution, 30 g/l... 29 ml... 2112-20 Phosphate Standard Solution, 1 mg/l as PO43-... 500 ml... 2569-49 Phosphate Standard Solution, PourRite ampule, 50 mg/l as PO4 3-, 2 ml...20/pkg... 171-20 Phosphate Standard Solution, Voluette ampule, 50 mg/l as PO43-, 10 ml...16/pkg... 171-10 Sodium Hydroxide Standard Solution, 5.000 N... 1000 ml... 2450-53 Sulfuric Acid Standard Solution, 1.000 N... 1 L... 1270-53 Water, deionized... 4 L... 272-56 284

OPTIONAL APPARATUS Description Units Cat. No. Ampule Breaker Kit, Voluette...each... 21968-00 Ampule Breaker, PourRite...each... 24846-00 Cylinder, graduated, mixing, 25 ml (3 required)...each... 20886-40 Flask, volumetric, Class A, 100 ml...each... 14574-42 ph Indicator Paper, 1 to 11 ph units...5 rolls/pkg... 391-33 ph Meter, sension.1, portable...each... 51700-00 Pipet, TenSette, 0.1-1.0 ml...each... 19700-01 Pipet Tips, for 19700-01 TenSette Pipet...50/pkg... 21856-96 Pipet, volumetric, Class A, 5.00 ml...each... 14515-37 Pipet, volumetric, Class A, 2.00 ml...each... 14515-36 Pipet Filler, safety bulb...each... 14651-00 For Technical Assistance, Price and Ordering In the U.S.A. call 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 285

PO4 mg/l PO4 286

0.00 mg/l PO4 10,000 mg/l CaCO 3 150,000 mg/l Cl - 1 ml 10 N25mL pipet filler 40,000 mg/l CaCO 3 0.50g sulfamic 4 100,000 mg/l 5mg/L 125mL 2 3 44 21+3C 1mL 10 N 25mL pipet filler ph 287

Sampling and Storage Collect samples in clean plastic or glass bottles that have been cleaned with 1:1 Hydrochloric Acid Solution and rinsed with deionized water. Do not use a commercial detergent containing phosphate for cleaning glassware used in this test. Analyze samples immediately for best results. If prompt analysis is not possible, preserve samples by filtering immediately and storing the sample at 4 ãc (39 ãf) for up to 48 hours. Accuracy Check Standard Additions Method a) Snap the neck off a Phosphate PourRite Ampule Standard Solution, 500 mg/l as PO43-. b) Use the TenSette Pipet to add 0.1 ml, 0.2 ml and 0.3 ml of standard, respectively, to three 25-mL samples. Mix well. c) Analyze each sample as described in the procedure. Each 0.1-mL addition of standard should cause an increase of 2.0 mg/l orthophosphate (PO43-). d) If these increases do not occur, see Standard Additions (Section 1)for more information. Standard Solution Method Prepare a 10.0-mg/L phosphate standard by pipetting 10.0 ml of a Phosphate Standard Solution, 50 mg/l as PO4 3- into a 50-mL volumetric flask. Dilute to volume with deionized water. Or, prepare a 10.0-mg/L PO43- standard solution by using the TenSette Pipet to add 1.00 ml of Phosphate PourRite Ampule Standard, 500 mg/l as PO43-, into a 50-mL volumetric flask. Dilute to volume with deionized water.substitute this standard for the sample and perform the test as described. The mg/l PO43- reading should be 10 mg/l. Method Performance Precision In a single laboratory using a standard solution of 15.0 mg/l PO43- and two lots of reagent with the instrument, a single operator obtained a standard deviation of À0.12 mg/l PO43-. Estimated Detection Limit The estimated detection limit for program 85 is 0.14 mg/l PO43-. For more information on the estimated detection limit, see Section 1. (100 Test)...22441-00 : (1) 1934-32, (1) 2236-32... 1 ml......100 ml MDB*...1934-32... 1 ml......100 ml MDB*...2236-32, 10-20-25 ml, w/ cap...2...6/pkg...24019-06 288

OPTIONAL REAGENTS Description Units Cat. No. Amino Acid Reagent Powder Pillow...100/pkg...804-99 Bromine Water, 30 g/l... 29 ml...2211-20 Hydrochloric Acid Solution, 1:1 (6 N)... 500 ml...884-49 Phenol Solution, 30 g/l... 29 ml...2112-20 Phosphate Standard Solution, 50 mg/l PO43-... 500 ml...171-49 Phosphate Standard Solution, PourRite ampule, 500 mg/l PO43-, 2 ml...20/pkg...14242-20 Sodium Hydroxide Standard Solution, 5.0 N... 100 ml MDB... 2450-32 Sulfamic Acid...113 g...2344-14 Sulfuric Acid Standard Solution, 10 N... 1 L...931-53 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS Description Unit Cat. No. Ampule Breaker Kit, PourRite... each...24846-00 Aspirator, vacuum... each...2131-00 Cylinder, graduated, 50 ml... each...508-41 Cylinder, graduated, mixing, 25 ml... each...20886-40 Filter Holder, 47 mm, 300 ml, graduated... each...13529-00 Filter, membrane, 47 mm, 0.45 microns... 100/pkg...13530-00 Flask, filtering, 500 ml... each...546-49 Flask, erlenmeyer, 125 ml... each...505-43 Flask, volumetric, Class A, 50 ml... each...14574-41 ph Indicator Paper, 1 to 11 ph... 5 rolls/pkg...391-33 ph Meter, sension.1, portable... each...51700-00 Pipet, serological, 2.0 ml... each...532-36 Pipet, TenSette, 0.1 to 1.0 ml... each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet... 50/pkg...21856-96 Pipet, volumetric, Class A, 10.00 ml... each...14515-38 Pipet Filler, safety bulb... each...12189-00 Spoon, measuring, 0.05 g... each...492-00 Thermometer, -10 to 110 ãc... each...1877-01 For Technical Assistance, Price and Ordering In the U.S.A. ªCall 800-227-4224 Outside the U.S.A. ªContact the Hach office or distributor serving you. 289

Test N Tube TenSette TenSette PO4 C 13 C 15 33 C 2 290

0.00 mg/l PO4 291

100mg/L 100mg/L 550mL 6 71 ph 20 C) 25 C) 1000mg/L Sampling and Storage Collect samples in plastic or glass bottles that have been acid cleaned with 1:1 Hydrochloric Acid Solution and rinsed with deionized water. Do not use commercial detergents containing phosphate for cleaning the glassware used in this test. For best results, analyze the samples immediately after collection. If prompt analysis is impossible, preserve the samples for up to 748 hours by filtering immediately and storing at 4 C. The sample should have a neutral (6 8) ph and be at room temperature before analysis. Accuracy Check Note: Clean glassware with 1:1 hydrochloric acid solution. Rinse again with deionized water. Do not use detergents containing phosphates to clean glassware. Standard Additions Method a. Fill three 10-mL graduated mixing cylinders with 10 ml of sample. b. Snap the neck off a Voluette Ampule of Phosphate Standard Solution, 500 mg/l as PO4 (Cat. No. 14242-10). c. Use the TenSette Pipet to add 0.1 ml, 0.2 ml and 0.3 ml, respectively, to the three 10-mL aliquots of sample prepared in step a. Mix well. d. Analyze each sample from step c as described in the procedure; use 5.0 ml of the prepared sample for each test. The concentration should increase as follows: 5 mg/l, 10 mg/l, and 15 mg/l PO4, respectively. 292

e. If these increases do not occur, see Standard Additions in Section 1 of the DR/890 Procedures Manual for more information. Standard Solution Method To check accuracy, prepare an 80 mg/l PO4 standard by pipetting 8.0 ml of solution from a 10-mL Voluette Ampule of Phosphate Standard Solution, 500 mg/l as PO4, into an acid-cleaned 50-mL Class A volumetric flask. Fill to the line with deionized water. Substitute this standard for the sample and perform the procedure as described. Standard Adjust To adjust the calibration curve using the reading obtained with the 80 mg/ml PO4 standard solution, press the SETUP key and scroll, using the arrow keys, to the STO option. Press ENTER to activate the standard adjust option. Then enter 80.0 to edit the standard concentration to match that of the standard used. Press ENTER to complete the adjustment. See Standard Curve Adjustment, Section 1 of the Procedures Manual for more information. Method Performance Precision In a single laboratory, using a standard solution of 80.0 mg/l PO4 and two lots of reagent with the instrument, a single operator obtained a standard deviation of ±3.0 mg/l PO4. Estimated Detection Limit (EDL) The EDL for program 86 is 7.0 mg/l PO4. For more information on derivation and use of Hach s estimated detection limit, see Section 1 of the DR/890 Procedures Manual. Sample Disposal Information Safety Final samples will contain molybdenum. In addition, final samples will have a ph less than 2 and are considered corrosive (D002) by the Federal RCRA. Consult the Material Safety Data Sheet for information specific to the reagent used. Good safety habits and laboratory techniques should be used throughout the procedure. Consult the Material Safety Data Sheet for information specific to the reagents used. Summary of Method Orthophosphate reacts with molybdate in an acid medium to produce a phosphomolybdate complex. In the presence of vanadium, yellow vanadomolybdophosphoric acid forms. The intensity of the yellow color is proportional to the phosphate concentration. Installing this Program on the DR/800 This procedure will add the current method as a new Hach program to your DR/800. 1. Turn the DR/800 on by pressing the ON key. 293

2. Press the SETUP key. 3. Press the down arrow key two times so that the prompt line shows USER. 4. Press the ENTER key. 5. Enter 8138, followed by ENTER. 6. Enter each of the numbers in the right column, each followed by ENTER. The line numbers in the left column relate to the line number on the display. At any time you may use the arrow keys to scroll back to review or change any number you have already entered. 294

Test N Tube.....50 vials...27673-45 : (50) Test N Tube *, (2) 272-42 Test N Tube... 1... 50/pkg...*...100 ml...272-42 COD/TNT... 1...48464-00 TenSette, 1 to 10 ml... 1...19700-10 s, for 19700-10 TenSette Pipet... 1... 50/pkg...21997-96... 1 3...18641-00 OPTIONAL REAGENTS Bromine Water, 30 g/l...29 ml**...2211-20 Hydrochloric Acid Standard Solution, 6.0 N (1:1)...500 ml...884-49 Phenol Solution, 30 g/l...29 ml...2112-20 Phosphate Standard Solution, PourRite ampule, 500 mg/l as PO4, 2 ml... 20/pkg...14242-20 Phosphate Standard Solution, Voluette ampule, 500 mg/l as PO4, 10 ml... 16/pkg...14242-10 OPTIONAL APPARATUS Ampule Breaker Kit...each...21968-00 Aspirator, vacuum...each...2131-00 Cylinder, graduated, mixing, 10 ml, 3 required...each...20886-38 Filter Holder, 47 mm, 300 ml, graduated...each...13529-00 Filter, membrane, 47 mm, 0.45 microns...200/pkg...13530-00 Flask, filtering, 500 ml...each...546-49 Flask, volumetric, Class A, 50-mL...each...14574-41 ph Indicator Paper, 1 to 11 ph units...5 rolls/pkg...391-33 ph Meter, sension 1, portable...each...51700-10 Pipet, TenSette, 0.1 to 1.0 ml...each...19700-01 Pipet Tips, for 19700-01 TenSette Pipet... 50/pkg...21856-96 Pipet Tips, for 19700-10 TenSette Pipet... 250/pkg...21997-25 Pipet, volumetric, Class A, 5.00-mL...each...14515-37 Pipet, volumetric, Class A, 8.00-mL...each...14515-08 PourRite Ampule Breaker...each...24846-00 295

10127 (0.0 to 100.0 mg/l ) Test N Tube PO4 TenSette TenSette 296

Molybdovanadate 0.0 mg/l PO4 297

100mg/L 100mg/L 850mL 9 10 1 ph 20 C) 25 C) 1000mg/L Sampling and Storage Collect samples in plastic or glass bottles that have been acid cleaned with 1:1 Hydrochloric Acid Solution and rinsed with deionized water. Do not use commercial detergents containing phosphates for cleaning the glassware used in this test. Analyze samples immediately after collection for best results. If prompt analysis is impossible, preserve the sample for up to 28 days by adjusting the ph to 2 or less with concentrated H2SO4 (about 2 ml per liter) and storing at 4 C. Warm the sample to room temperature and neutralize with 5.0 N NaOH before analysis. Correct test results for volume additions; see Volume Additions in Section 1of the DR/890 Procedures Manual. Accuracy Check Note: Clean glassware with 1:1 hydrochloric acid solution. Rinse again with deionized water. Do not use detergents containing phosphates to clean glassware. Standard Additions Method a. Fill each of three 10-mL graduated mixing cylinders with 10 ml of sample. b. Snap the neck off a 10-mL Voluette Ampule of Phosphate Standard Solution, 500 mg/l as PO4 (Cat. No. 14242-10). 298

c. Use a TenSette Pipet to add 0.1 ml, 0.2 ml and 0.3 ml, respectively, to the three 10-mL aliquots of the water sample prepared in step a. Mix well. d. Analyze samples from step c as described in the procedure. Use 5.0 ml of the prepared sample for each test. The concentration should increase: 5 mg/l, 10 mg/l, and 15 mg/l PO4, respectively. e. If these increases do not occur, see Standard Additions (Section 1 of the DR/890 Procedures Manual) for more information. Standard Solution Method To check accuracy, prepare an 80 mg/l standard by pipetting 8.0 ml of solution from a 10-mL Voluette Ampule of Phosphate Standard Solution, 500 mg/l as PO4 into an acid-cleaned, Class A, 50-mL volumetric flask. Dilute to the mark with deionized water. Substitute this standard for the sample and perform the procedure as described. Standard Adjust To adjust the calibration curve using the reading obtained with the 80 mg/l PO4 standard solution, press the SETUP key and scroll, using the arrow keys, to the STO option. Press ENTER to activate the standard adjust option. Then enter 80.0 to edit the standard concentration to match that of the standard used. Press ENTER to complete the adjustment. See Standard Curve Adjustment, Section 1 of the Procedures Manual for more information. Method Performance Safety Precision In a single laboratory, using a standard solution of 80.0 mg/l PO4 and two lots of reagent with the instrument, a single operator obtained a standard deviation of ±3.0 mg/l PO4 Estimated Detection Limit The estimated detection limit for program 87 is 7.0 mg/l PO4. For more information on the estimated detection limit, seesection 1 of the DR/890 Procedures Manual. Good safety habits and laboratory techniques should be used throughout the procedure. Consult the Material Safety Data Sheet for information specific to the reagents used. Sample Disposal Information The final samples will contain molybdenum. In addition, the final samples will have a ph less than 2 and are considered corrosive (D002) by the Federal RCRA. Consult the Material Safety Data Sheet for information specific to the reagent used. Summary of Method Phosphates present in organic and condensed inorganic forms (meta-, pyro- or other polyphosphates) must be converted to reactive orthophosphate before analysis. Pretreatment of the sample with acid and heat provides the conditions for hydrolysis of 299

the condensed inorganic forms. Organic phosphates are converted to orthophosphate by heating with acid and persulfate. Orthophosphate reacts with molybdate in an acid medium to produce a phosphomolybdate complex. In the presence of vanadium, yellow vanadomolybdophosphoric acid forms. The intensity of the yellow color is proportional to the phosphate concentration. Installing this Program on the DR/800 This procedure will add the current method as a new Hach program to your DR/800. 1. Turn the DR/800 on by pressing the ON key. 2. Press the SETUP key. 3. Press the down arrow key two times so that the prompt line shows USER. 4. Press the ENTER key. 5. Enter 8138, followed by ENTER. 6. Enter each of the numbers in the right column, each followed by ENTER. The line numbers in the left column relate to the line number on the display. At any time you may use the arrow keys to scroll back to review or change any number you have already entered. 300

REQUIRED REAGENTS Test N Tube..... 50 vials... 27672-45 : (50) Test N Tube *, (2) 272-42, (1) 20847-66 (1) 20760-26, (1) 7430-42 Molybdovanadate... 0.5 ml..25 ml... 20760-26...1... 50/pkg... 20847-66, 1.54 N...2 ml.. 100 ml... 27430-42 Test N Tube...1... 50/pkg... *... 100 ml... 272-42 COD, 115/230 Vac (U.S.A. and Canada)...1...... 45600-00 COD, 115/230 Vac (Europe)...1...... 45600-02 COD/TNT, DR/800 series...1...... 48464-00, LDPE, 0.5 to 1.0 ml...1... 20/pkg... 21247-20 TenSette 1 to 10 ml...1...... 19700-10, for 19700-10 TenSette Pipet..... 50/pkg... 21997-96...1...... 50030-00...1 3... each... 18641-00 OPTIONAL REAGENTS Description Unit Cat. No. Hydrochloric Acid Standard Solution, 6.0 N (1:1)...500 ml...884-49 Phosphate Standard Solution, PourRite ampule, 500 mg/l as PO4, 2-mL... 20/pkg...14242-20 Phosphate Standard Solution, Voluette ampule, 500 mg/l as PO4, 10-mL... 16/pkg...14242-10 Sodium Hydroxide Standard Solution, 5.0 N...1 L...2450-53 Sulfuric Acid, ACS, concentrated...500 ml...979-491 OPTIONAL APPARATUS Ampule Breaker Kit...each...21968-00 Aspirator, vacuum...each...2131-00 Cylinder, graduated, mixing, 10 ml (3 required)...each...20886-38 Filter Holder, 47 mm, 300 ml, graduated...each...13529-00 Filter, membrane, 47 mm, 0.45 microns...200/pkg...13530-01 Flask, filtering, 500-mL...each...546-49 Flask, volumetric, Class A, 50-mL...each...14574-41 ph Indicator Paper, 1 to 11 ph units...5 rolls/pkg...391-33 ph Meter, sension 1, portable...each...51700-10 Pipet Filler, Safety Bulb...each...14651-00 Pipet, TenSette, 0.- to 1.0-mL...each...19700-01 Pipet Tips, for 19700-01... 50 pkg...21856-96 301

Pipet, volumetric, Class A, 8.00-mL...each...14515-08 Stopper, No. 7 one hole... 6/pkg...2119-07 Tubing, rubber... 12 feet...560-19 302

8186 (SiO2) SiO2 303

0 mg/l SiO2 304

50 mg/l PO460 mg/l PO4 2%75 mg/l PO4-11% Sampling and Storage Collect samples in clean plastic bottles. Analyze samples as soon as possible after collection. If prompt analysis is not possible, store samples for up to 28 days by cooling to 4 C (39 F) or below. Warm samples to room temperature before analysis. Accuracy Check Standard Additions Method a) Open a Low Range Silica Standard Solution Pillow, 50 mg/l SiO2. b) Using the TenSette Pipet, add 0.1, 0.2, and 0.3 ml of standard to three 10-mL samples. Mix thoroughly. c) Analyze each sample as described above. The silica concentration should increase 0.5 mg/l for each 0.1 ml of standard added. d) If these increases do not occur, see Standard Additions in Section 1 for more information. Standard Adjust To adjust the calibration curve using the reading obtained with the 1.00-mg/L Standard Solution (see Optional Reagents), press the SETUP key and scroll (using the arrow keys) to the STD setup option. Press ENTER to activate the standard adjust option. Then enter 1.00 to edit the standard concentration to match that of the standard used. Press ENTER to complete the adjustment. See Section 1, Standard Curve Adjustment for more information. 305

Method Performance Precision In a single laboratory, using standard solutions of 1.00 mg/l silica and two representative lots of reagent and a instrument, a single operator obtained a standard deviation of ±0.025 mg/l silica. Estimated Detection Limit (EDL) The estimated detection limit for program 90 is 0.020 mg/l SiO2. For more information on the estimated detection limit, see Section 1. If testing for very low levels of silica, use the ultra-low range silica method on the Hach DR/2010 or DR/4000 Spectrophotometers. Reagent Preparation To prepare Amino Acid F Reagent Solution, dissolve 11.4 grams of Amino Acid F Reagent Powder in 100 ml of 1.0 N Sodium Hydroxide Solution. The solution is stable for at least one month if stored in a plastic bottle. Summary of Method Silica and phosphate in the sample react with molybdate ion under acidic conditions to form yellow silicomolybdic acid complexes and phosphomolybdic acid complexes. Acid reduces the yellow silicomolybdic acid to an intense blue color, which is proportional to the silica concentration., 10 ml sample (100 tests)...24593-00 : (1) 22540-69, (1) 21062-69 (2) 1995-26 F... 1...100/pkg...22540-69... 2...100/pkg...21062-69 Molybdate 3...,...28...50 ml SCDB...1995-26 REQUIRED APPARATUS, 10-20-25 ml, w/ cap...2...6/pkg...24019-06 OPTIONAL REAGENTS Silica Standard Solution, 1.00 mg/l SiO2... 500 ml...1106-49 Silica Standard Solution Pillows, 20 mg/l as SiO2, 10 ml...16/pkg...14245-10 Sodium Bicarbonate, ACS...454 g...776-01 Sodium Hydroxide Standard Solution, 1.000 N... 900 ml...1045-53 Sulfuric Acid Standard Solution, 1.0 N... 1000 ml...1270-53 OPTIONAL APPARATUS Bottle, 118 ml, polyethylene, oblong...6/pkg...23184-06 Dropper, 0.5- & 1.0-mL marks...6/pkg...23185-06 Pipet, serologic, 2 ml, poly...each...2106-36 Pipet, TenSette, 0.1 to 1.0 ml...each...19700-01 306

Pipet Tips, for 19700-01 Pipet...50/pkg...21856-96 Standard Methods for the Examination of Water and Wastewater...each...22708-00 Thermometer, - 10 to 110 C...each...1877-01 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 307

8185 (SiO2) SiO2 2:00 Timer 2 308

0 mg/l SiO2 50 mg/l PO460 mg/l PO4 2%75 mg/l PO4-11% 309

Sampling and Storage Collect samples in clean plastic or glass bottles. Analyze samples as soon as possible after collection. Store samples up to 28 days at 4 C (39 F) or below. Warm samples to room temperature before analyzing. Accuracy Check Standard Additions Method a) Open a High Range Silica Standard Solution, 1000 mg/l SiO2. b) Use the TenSette Pipet to add 0.1 ml, 0.3 ml, and 0.5 ml of the standard to three 10-mL samples. Mix each thoroughly. c) Analyze each sample as described above. The silica concentration should increase 10.0 mg/l for each 0.1 ml of standard added. d) If these increases do not occur, see Standard Additions in Section 1 for more information. Standard Solution Method To check the accuracy of the method, use the Silica Standard Solutions, 25 and 50 mg/l as SiO2, listed under Optional Reagents. Analyze according to the above procedure using deionized water as the blank. Standard Adjust To adjust the calibration curve using the reading obtained with the 50.0 mg/l standard solution, press the SETUP key and scroll (using the arrow keys) to the STD setup option. Press ENTER to activate the standard adjust option. Then enter 50.0 to edit the standard concentration to match that of the standard used. Press ENTER to complete the adjustment. See Section 1, Standard Curve Adjustment for more information. Method Performance Precision In a single laboratory, using a standard solution of 50.0 mg/l SiO2 and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of 1.0 mg/l silica. Estimated Detection Limit The estimated detection limit for program 89 is 1.00 mg/l SiO2. For more information on the estimated detection limit, see Section 1. Summary of Method Silica and phosphate in the sample react with molybdate ion under acidic conditions to form yellow silicomolybdic acid complexes and phosphomolybdic acid complexes. Addition of citric acid destroys the phosphate complexes. Silica is then determined by measuring the remaining yellow color. 310

, 10 ml sample (100 tests)...24296-00 : (1) 21074-69, (1) 21062-69, (1) 21073-69... 1...100/pkg...22540-69... 2...100/pkg...21062-69 Molybdate...,...28...50 ml SCDB... 21073-69, 10-20-25 ml, w/ cap...2...6/pkg...24019-06 OPTIONAL REAGENTS Silica Standard Solution, 10 mg/l...500 ml...1403-49 Silica Standard Solution, 25 mg/l...236 ml...21225-31 Silica Standard Solution, 50 mg/l...200 ml...1117-29 Silica Standard Solution, 1000 mg/l...500 ml...194-49 Sodium Bicarbonate, ACS... 454 g...776-01 Sulfuric Acid Standard Solution, 1.000 N...100 ml MDB...1270-32 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS Pipet, TenSette, 0.1 to 1.0 ml... each...19700-01 Pipet Tips, for 19700-01 Pipet... 50/pkg...21856-96 Standard Methods for the Examination of Water and Wastewater... each...22708-00 Thermometer, -10 to 110 C... each...1877-01 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 311

10098 (SiO2) SiO2 312

2:00 Timer 2 0 mg/l SiO2 50 mg/l PO460 mg/l PO4 2%75 mg/l PO4-11% 313

Sampling and Storage Collect samples in clean plastic or glass bottles. Analyze samples as soon as possible after collection. Store samples up to 28 days at 4 C (39 F) or below. Warm samples to room temperature before analyzing. Accuracy Check Standard Additions Method a) Open a High Range Silica Standard Solution, 1000 mg/l SiO2. b) Use the TenSette Pipet to add 0.1 ml, 0.3 ml, and 0.5 ml of the standard to three 10-mL samples. Mix each thoroughly. c) Analyze each sample as described above. The silica concentration should increase 4 mg/l for each 0.1 ml of standard added. d) If these increases do not occur, see Standard Additions in Section 1 for more information. Standard Solution Method To prepare a 160-mg/L silica standard, pipet 40.0 ml of a 1000-mg/L Silica Standard Solution into a 250-mL volumetric flask. Dilute to the line with deionized water. Analyze according to the above procedure using deionized water as the blank. Standard Adjust To adjust the calibration curve using the reading obtained with the 160-mg/L standard solution, press the SETUP key and scroll (using the arrow keys) to the STD setup option. Press ENTER to activate the standard adjust option. Then enter 160. to edit the standard concentration to match that of the standard used. Press ENTER to complete the adjustment. See Section 1, Standard Curve Adjustment for more information. Method Performance Precision In a single laboratory, using a standard solution of 100.0 mg/l SiO2 and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of 2.0 mg/l silica. Estimated Detection Limit The estimated detection limit for program 88 is 3.0 mg/l SiO2. For more information on the estimated detection limit, see Section 1. Summary of Method Silica and phosphate in the sample react with molybdate ion under acidic conditions to form yellow silicomolybdic acid complexes and phosphomolybdic acid complexes. Addition of citric acid destroys the phosphate complexes. Silica is then determined by measuring the remaining yellow color. 314

, 25-mL sample (100 tests)...22443-00 : (1) 1042-99, (1) 14548-99, (2) 1041-66...1...100/pkg...1042-99...1...100/pkg...14548-99...1...100/pkg...1041-99... 30 ml... 4 L...272-56 10-20-15 ml,...2...6/pkg...24019-06 OPTIONAL REAGENTS Silica Standard Solution, 10 mg/l... 500 ml...1403-49 Silica Standard Solution, 25 mg/l... 236 ml...21225-31 Silica Standard Solution, 50 mg/l... 200 ml...1117-29 Silica Standard Solution, 1000 mg/l... 500 ml...194-49 Sodium Bicarbonate, ACS...454 g...776-01 Sulfuric Acid Standard Solution, 1.000 N... 100 ml MDB...1270-32 OPTIONAL APPARATUS Flask, volumetric, 250 ml, Class A...each...14574-46 Pipet, TenSette, 0.1 to 1.0 ml...each...19700-01 Pipet Tips, for 19700-01 Pipet...50/pkg...21856-96 Pipet, volumetric, Class A, 100 ml...each...14515-42 Pipet Filler, safety bulb...each...14651-00 Standard Methods for the Examination of Water and Wastewater...each...22708-00 Thermometer, -10 to 110 C...each...1877-01 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 315

8051 316

20000mg/L CaCO3 10000mg/L 40000mg/L 500mg/L User- Entered Calibration There are various programs to determine sulfate, each with a different level of accuracy. Best results are obtained by performing a user-entered calibration with each new lot of reagent. Programs 91 and 92 can be run when a high degree of accuracy is not needed. Use of the Standard Adjust feature will improve performance when using programs 91 and 92. It should NOT be used with a user calibration, as it will hinder performance. Using Class A glassware, prepare standards of 10, 20, 30, 40, 50, 60, and 70 mg/l sulfate by pipetting 1, 2, 3, 4, 5, 6, and 7 ml of a 1000-mg/L sulfate standard into 100-mL volumetric flasks. Dilute to the mark with deionized water and mix well. Zero the instrument with water. The user-entered settings for sulfate are: Program number: #101 to 105 Wavelength: 520 nm Resolution: 0 mg/l See Creating User-Entered Program in the instrument manual for specific instructions on entering a user-entered program. Sampling and Storage Collect samples in clean plastic or glass bottles. Samples may be stored up to 28 days by cooling to 4 C (39 F) or lower. Warm to room temperature before analysis. 317

Accuracy Check Standard Additions Method- Powder Pillows a) Snap the neck off a Sulfate Standard PourRite Ampule,1000 mg/l SO4. b) Use a TenSette Pipet to add 0.1, 0.2 and 0.3 ml of standard to thethree 10-mL samples. Mix thoroughly. c) Analyze each sample as described above. The sulfate concentrationshould increase 10 mg/l for each 0.1 ml of standard added. d) If these increases do not occur, see Standard Additions in Section 1 for more information. Standard Additions Method- AccuVac Ampuls a) Snap the neck off a Sulfate Standard PourRite Ampule, 2500 mg/l SO4 b) Fill three 25- ml graduated cylinders with 25 ml of sample. Use a TenSette Pipet to add 0.1, 0.2 and 0.3 ml of standard to the three cylinders. Mix thoroughly. For AccuVac Ampuls, transfer to a 50-mL beaker. c) Analyze each sample as described above. The sulfate concentration should increase 10 mg/l for each 0.1 ml of standard added. d) If these increases do not occur, see Standard Additions in Section 1 for more information. Standard Solution Method Check the accuracy of the test by using the Sulfate Standard Solution, 50 mg/l, listed under Optional Reagents. Or, prepare this solution by pipetting 1.0 ml of a PourRite Ampule Standard for Sulfate (2500 mg/l) into a 50-mL volumetric flask. Dilute to volume with deionized water. The final concentration is 50 mg/l sulfate. Substitute this standard for the sample and proceed with the test as described in the procedure. Standard Adjust Standard adjust is recommended when using stored programs 91 or 92. It should not be used with a user-entered calibration. To adjust the calibration curve using the reading obtained with the 50-mg/L standard solution, press the SETUP key and scroll (using the arrow keys) to the STD setup option. Press ENTER to activate the standard adjust option. Then enter 50 to edit the standard concentration to match that of the standard used. Press ENTER to complete the adjustment. See Section 1, Standard Curve Adjustment for more information. Method Performance Precision In a single laboratory, using a standard solution of 50 mg/l sulfate and two representative lots of powder pillows with the instrument, a single operator obtained a standard deviation of ±0.5 mg/l sulfate. In a single laboratory, using a standard solution of 50 mg/l sulfate and two representative lots of AccuVac Ampuls with the instrument, a single operator obtained a standard deviation of ±3 mg/l sulfate. Estimated Detection Limit (EDL) The EDL for program 91 is 4.9 mg/l SO4 and the EDL for program 92 is 3 mg/l SO4. 318

For more information on derivation and use of Hach s estimated detection limit, see Section 1. Summary of Method Sulfate ions in the sample react with barium in the SulfaVer 4 Sulfate Reagent to form insoluble barium sulfate. The amount of turbidity formed is proportional to the sulfate concentration. The SulfaVer 4 also contains a stabilizing agent to hold the precipitate in suspension. () SulfaVer 4... 1...100/pkg...21067-69, 10-20-25 ml, w/ cap...2...6/pkg...24019-06 () SulfaVer 4 AccuVac... 1...25/pkg...25090-25, 50-mL...1......500-41 OPTIONAL REAGENTS Sulfate Standard Solution, 50 mg/l... 500 ml...2578-49 Sulfate Standard Solution, 1000 mg/l... 500 ml...21757-49 Sulfate Standard Solution, PourRite Ampule, 2500 mg/l, 2 ml...20/pkg...14252-20 Sulfate Standard Solution, PourRite Ampule, 1000 mg/l, 2 ml...20/pkg...21757-20 Water, deionized... 4 L...272-56 OPTIONAL APPARATUS AccuVac Snapper Kit...each...24052-00 Cylinder, graduated mixing, 25 ml...each...20886-40 Filter Paper, folded, 12.5 cm...100/pkg...1894-57 Flask, volumetric, 50 ml, Class A...each...14574-41 Funnel, poly, 65 mm...each...1083-67 Pipet, TenSette, 0.1 to 1.0 ml...each...19700-01 Pipet Tips, for 19700-01 Pipet...50/pkg...21856-96 Pipet, volumetric, 1.00 ml, Class A...each...14515-35 Pipet, volumetric, 2.00 ml, Class A...each...14515-36 Pipet, volumetric, 3.00 ml, Class A...each...14515-03 Pipet, volumetric, 4.00 ml, Class A...each...14515-04 Pipet, volumetric, 5.00 ml, Class A...each...14515-37 Pipet, volumetric, 6.00 ml, Class A...each...14515-06 Pipet, volumetric, 7.00 ml, Class A...each...14515-07 Pipet Filler, safety bulb...each...14651-00 PourRite Ampule Breaker...each...24846-00 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 319

320

Sampling and Storage Collect samples in clean plastic or glass bottles. Fill completely and cap tightly. Avoid excessive agitation or prolonged exposure to air. Analyze samples immediately. Method Performance Precision In a single laboratory, using standard solutions of 0.73 mg/l sulfide and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of ± 0.02 mg/l sulfide. 321

Estimated Detection Limit (EDL) The EDL for program 93 is 0.01 mg/l S2-. For more information on derivation and use of Hach s estimated detection limit, see Section 1. Soluble Sulfides Determine soluble sulfides by centrifuging the sample in completely filled, capped tubes and analyzing the supernatant. Insoluble sulfides are then estimated by subtracting the soluble sulfide concentration from the total sulfide result. Summary of Method Hydrogen sulfide and acid-soluble metal sulfides react with N, N-dimethyl-p-phenylenediamine oxalate to form methylene blue. The intensity of the blue color is proportional to the sulfide concentration. High sulfide levels in oil field waters may be determined after dilution. Pollution Prevention and Waste Management Sulfide 2 Reagent contains potassium dichromate. The final solution will contain hexavalent chromium (D007) at a concentration regulated as a hazardous waste by Federal RCRA. See Section 3 for more information on proper disposal of these materials. (100 tests)... 22445-00 : (2) 1816-42, (2) 1817-42 1... 2 ml...100 ml MDB...1816-32 2... 2 ml...100 ml MDB...1817-32... 25 ml... 4 L... 272-56, 25 ml... 1...... 508-40, Class A, 25.00 ml... 1......14515-40 Pipet Filler, safety bulb... 1...14651-00, 10-20-25 ml, w/ cap... 2... 6/pkg...24019-06 OPTIONAL REAGENTS Description Units Cat. No. Bromine Water, 30 g/l...29 ml...2211-20 Phenol Solution, 30 g/l...29 ml...2112-20 Sodium Sulfide, hydrate... 114 g...785-14 OPTIONAL APPARATUS Bottle, Wash, 250 ml... each...620-31 Dropper, for 1 oz. bottle... each...2258-00 Flask, erlenmeyer, 50 ml... each...505-41 Standard Methods for the Examination of Water and Wastewater... each...22708-00 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 322

8028 LAS 323

0 mg/l LAS 324

Sampling and Storage Collect samples in clean plastic or glass bottles. Analyze samples as soon as possible, but they may be stored at least 24 hours by cooling to 4 C (39 F). Warm to room temperature before testing. Accuracy Check Standard Additions Method a) Snap the neck off a Detergent Voluette Ampule Standard Solution, 60 mg/l as LAS. b) Using the TenSette Pipet, add 0.1, 0.2, and 0.3 ml of standard to three 300-mL samples. Mix thoroughly. c) Analyze each as described above. The anionic surfactants reading should increase 0.02 mg/l for each 0.1 ml of standard added. d) If these increases do not occur, see Standard Additions (Section 1) for more information. Method Performance Precision In a single laboratory, using a standard solution of 0.150 mg/l LAS, two lots of reagent, and the instrument, a single operator obtained a standard deviation of ±0.010 mg/l LAS as anionic surfactant. Estimated Detection Limit The estimated detection limit for program 26 is 0.020 mg/l LAS. For more information on the estimated detection limit, see Section 1. Summary of Method Detergents, ABS (alkyl benzene sulfonate) or LAS (linear alkylate sulfonate) are determined by association with crystal violet dye and extraction of the ion-pair complex into benzene. Pollution Prevention and Waste Management Benzene (D018) solutions are regulated as hazardous waste by Federal RCRA. Do not pour these materials down the drain. Collect water saturated with benzene solutions for disposal with laboratory solvent wastes. See Section 3 for more information on proper disposal of these materials., ACS... 55 ml...500 ml...14440-49... 10 ml...500 ml... 452-49...1... 25/pkg... 1008-68... 1...... 968-00, 25 ml... 1... 508-40 325

, 50 ml... 1...... 508-41 500 ml... 1...... 508-49, 500 ml... 1...... 520-49 Ring, support, 4 inch... 1...... 580-01, 10-20-25 ml, w/ cap... 2... 6/pkg...24019-06 Stand, support, 127 X 203 mm (5 X 8")... 1...... 563-00 OPTIONAL REAGENTS Acetone, ACS...500 ml...14429-49 Detergent Standard Solution, Voluette ampule, 60 mg/l as LAS, 10 ml... 16/pkg...14271-10 OPTIONAL APPARATUS Ampule Breaker Kit... each...21968-00 Pipet, TenSette, 0.1 to 1.0 ml... each...19700-01 Pipet Tips, for 19700-01 Pipet... 50/pkg...21856-96 Thermometer, -10 to 110 C... each...1877-01 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 326

8006 0 mg/l 327

Sampling and Storage Collect samples in clean plastic or glass bottles. Analyze samples as soon as possible after collection. The sample may be stored seven days by cooling to 4 C (39 F). Method Performance Precision In a single laboratory, using a standard solution of 847.4 mg/l Suspended Solids with the instrument, a single operator obtained a standard deviation of 18.2 mg/l Suspended Solids. For more information on Hach s precision statement, see Section 1. Estimated Detection Limit The estimated detection limit for program 94 is 22.1 mg/l Suspended Solids. For more information on the estimated detection limit, see Section 1. Summary of Method This method of determining suspended solids is a simple, direct measurement which does not require the filtration or ignition and weighing steps that gravimetric procedures do. The USEPA specifies the gravimetric method for solids determinations, while this method is often used for checking in-plant processes. 328

, 600 ml, low form...1...... 1080-52, 1.2 L, 120 V...1...... 26161-00, 1.2 L, 240 V...1......26161-02, 500 ml,...1...... 1081-49, serologic, 25 ml...1...... 2066-40...1......14651-00 OPTIONAL APPARATUS Stirring Rod, glass...3/pkg... 1770-01 Wash Bottle, 250 ml...each...620-31 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 329

8193 330

Sampling and Storage Collect samples in clean plastic or glass bottles. Accuracy Check Standard Solution Method Prepare a 200-mg/L tannic acid standard solution by dissolving 0.200 grams of tannic acid in deionized water and diluting to 1000 ml. Prepare this solution monthly. A 2.0 mg/l tannic acid standard is prepared by diluting 10.00 ml of the stock solution to 1000 ml with deionized water. Prepare this standard daily. Method Performance Precision In a single laboratory, using standard solutions of 4.0 mg/l tannic acid and two representative lots of reagent with the instrument, a single operator obtained a standard deviation of ±0.1 mg/l tannic acid. Estimated Detection Limit The estimated detection limit for program 98 is 0.1 mg/l tannin and lignin. For more information on the estimated detection limit, see Section 1. 331

Summary of Method This test measures all hydroxylated aromatic compounds, including tannin, lignin, phenol and cresol. This method produces a blue color proportional to the amount of these compounds present in the sample. Report results as total tannin and lignin expressed as mg/l tannic acid. (up to 100 tests)....22446-00 : (1) 675-49, (1) 2560-42... 10 ml... 500 ml...675-49 TanniVer 3... 1 ml... 100 ml... 2560-42... 25 ml... 4 L...272-56...1....14651-00, volumetric, Class A, 5.0 ml...1......14515-37, volumetric, Class A, 0.5 ml...1......14515-34, 10-20-25-mL, w/ cap...2...6/pkg...24019-06 OPTIONAL REAGENTS Formaldehyde... 100 ml...2059-32 Sodium Pyrophosphate, ACS...50 g...14295-25 Tannic Acid...113 g...791-14 OPTIONAL APPARATUS Description Unit Cat. No Balance, analytical, 115 V... each...26103-00 Balance, analytical, 230 V... each...26103-02 Cylinder, graduated, 25 ml... each...508-40 Filter Paper, folded, 12.5 cm... 100/pkg...1894-57 Flask, volumetric, 1000 ml... each...547-53 Funnel, poly, 65 mm... each...1083-67 Pipet, TenSette, 0.1 to 1.0 ml... each...19700-01 Pipet Tips, for 19700-01 Pipet... 50/pkg...21856-96 Pipet, volumetric, Class A, 10.00 ml... each...14515-38 Pipet, Filler, safety bulb... each...14651-00 Spoon, measuring, 0.2 g... each...638-00 Weighing Boat, 67/47 mm... 500/pkg...21790-00 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 332

10017 37 C, 1.0mL ( ); 333

1N 0.000 ABS ToxTrak ToxTrak 334

2 5.0mL, 0.5mL ( ),, 1mL 10mL,, 0% 1/10, 18 0 1314,. 0.600.10 4575 335

0.60 0.10 0.000 ABS.. 336

Disposal of Test Cultures Dispose of active bacterial cultures by using one of these methods: 1. Autoclave used test containers at 121 C for 15 minutes at 15 pounds of pressure. Once the containers are sterile, pour the contents down the drain with running water. The reaction tubes may be washed and re-used. 2. Sterilize test containers by using a 1:10 dilution of commercial laundry bleach. Pour the test container contents and test containers into the bleach solution. Allow 10-15 minutes of contact time with the bleach solution. Then pour the liquid down the drain and wash the reaction tubes for re-use. Summary of Method Resazurin is a redox-active dye, which changes from pink to blue when it is reduced. Bacterial respiration occurring in the sample reduces resazurin. If toxic substances are present, they inhibit the rate of resazurin reduction. The sample color is compared to a toxin-free control tube to determine how toxic the sample is to an indigenous culture or a culture of E. coli. A chemical accelerant reduces the reaction time of the procedure. ToxTrak (25 tests)... 25972-00 : (1) 25607-66, (1) 25608-36, (1) 22336-15, (2) 21247-20, (2) 20962-08 ToxTrak... 1... 50/pkg...25607-66 ToxTrak... 2... 15 ml SCDB...25608-36... 1... 15/pkg...22336-15... 1... 10/pkg...20962-08......200 ml...272-29... 1.......936-00 COD/TNT... 1......48464-00, 1 ml...... 10/pkg...21247-20... 1......14537-00, volumetric, 5.00 ml, Class A... 1......14515-37... 1......14651-00 Test N... 1... 25/pkg...25831-25 OPTIONAL REAGENTS Culture Set: (incl. Bactrol Discs and Lauryl Tryptose Broth Tubes)...25 cultures...25978-00 Bactrol Discs, E. coli... 25/bottle...25809-25 Isopropanol...500 ml...14459-49 Lauryl Tryptose Broth Tubes... 15/pkg...21623-15 337

OPTIONAL APPARATUS Burner, Alcohol, 60 ml... each...20877-42 Burner, Bunsen... each...21627-00 Germicidal Cloth... 50/pkg...24632-00 Incubator, Dri Bath, 25 well, 120/230 V... each...45900-00 Incubator, Dri Bath, 25 well, 120/230 V, with European power cord... each...45900-02 Test Tube Rack... each...24979-00 Timer... each...26305-00 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 338

8237 1 FAU=1 NTU=1 FTU Formazin FAU 339

Sampling and Storage Collect samples in clean plastic or glass bottles. Analyze samples as soon as possible. Store samples up to 48 hours by cooling to 4 C (39 F). Analyze the sample at the same temperature as it was collected. Accuracy Check Standard Solution Method The stored program has been calibrated using formazin, the primary standard for turbidity. A 200 FAU formazin solution for checking the accuracy of the test can be prepared using the following procedure. 1. Pipet 5.00 ml of a 4000 NTU Formazin stock solution into a 100-mL volumetric flask. 2. Dilute to the mark with deionized water. Prepare this daily. Convenient stabilized turbidity stock solution (200 NTU StablCal Standard) is available from Hach. Standard Adjust To adjust the calibration curve using the reading obtained with the 200 FAU formazin standard, press the SETUP key and scroll (using the arrow keys) to the STD setup option. Press ENTER to activate the standard adjust option. Then enter 200 to edit the standard concentration to match that of the standard used. Press ENTER to complete the adjustment. See Section 1, Standard Curve Adjustment for more information. Method Precision Precision In a single laboratory, using a turbidity standard solution of 200 FAU with the instrument, a single operator obtained a standard deviation of ±2 FAU. Estimated Detection Limit The estimated detection limit for program 95 is 21 FAU. For more information on the estimated detection limit, see Section 1. Summary of Method This turbidity test measures an optical property of the sample which results from scattering and absorption of light by particles in the sample. The amount of turbidity measured depends on variables such as the size, shape, color, and refractive properties of the particles. This procedure is calibrated using formazin turbidity standards and the 340

readings are in terms of Formazin Attenuation Units (FAU). This test cannot be used for USEPA reporting purposes, but it may be used for daily in-plant monitoring. One FAU is equivalent to one Nephelometric Turbidity Unit (NTU) of Formazin. However, the optical method of measurement for FAU is very different than the NTU method (1 NTU = 1 FTU = 1 FAU when traced to formazin primary standards.), 10-20-25 ml, w/cap...2...6/pkg...24019-06 Formazin, 4000 NTU... 500 ml...2461-49...15 ml DB...1269-36 StablCal Stabilized Turbidity Standard, 200 NTU... 500 ml...26604-49... 4 L... 272-56 OPTIONAL APPARATUS Description Units Cat. No. Bath, ultrasonic... each...24895-00 Bottle, wash, 250 ml... each...620-31 Flask, volumetric, Class A, 100 ml... each...14574-42 Flask, filter, 500 ml... each...546-49 Filter Holder... each...13529-00 Filter Pump, aspirator... each...2131-00 Oiling cloth, for applying silicone oil... each...26873-00 Pipet Filler, safety bulb... each...14651-00 Pipet, volumetric, Class A, 5.0 ml... each...14515-37 Sample Degassing Kit... each...43975-00 Stopper, rubber, one-hole, No. 7... 6/pkg...2119-07 Tubing, rubber, 5/16 I.D... 12 feet...560-19 Tweezers, plastic... each...14282-00 For Technical Assistance, Price and Ordering In the U.S.A. Call 800-227-4224 Outside the U.S.A. Contact the Hach office or distributor serving you. 341

8196 342

343