주관기관 냄새환경학회 국립환경과학원

제출문 국립환경과학원장귀하

제 1 장서 론 제 1 절배경및필요성 제 2 절목표및내용

제 2 장표준화지침에따른공정시험방법검토 제 1 절서론 제 2 절표준화작성지침에맞춘악취공정시험방법의재구성

μ μ μ μ μ μ μ μ μ

μ μ μ μ μ μ

μ μ μ

μ μ μ μ μ μ

μ μ μ

악취공정시험기준일반사항 (ES 09101)

β β

7.2.2 부지경계선시료관능시험절차 7.2.2.1 7.2.2.2 7.2.2.3 7.2.2.4 7.2.2.5 7.2.2.6

7.2.2.7 7.2.2.8 7.2.3 배출구시료관능시험절차 7.2.3.1 7.2.3.2 7.2.3.3 7.2.3.4 7.2.3.5 7.2.3.6 7.2.3.7

7.2.3.8 7.2.3.9 7.2.3.10 7.2.3.11 7.2.3.12 7.2.3.13

8.1 부지경계선시료희석배수산정 8.1.1 관능시험희석배수결정

8.1.2 희석배수산정방법 8.1.3 판정방법

8.1.4 결과표시 8.2 배출구시료희석배수산정 8.2.1 관능시험희석배수결정 8.2.2 희석배수산정방법 8.2.2.1

8.2.2.2 8.2.2.3

악취공정시험기준암모니아 - 붕산용액흡수법 (ES 09301.1) μ

악취공정시험기준암모니아 - 인산함침필터 (ES 09301.2) μ

악취공정시험기준황화합물-저온농축-모세관 GC법 (ES 09302.1) μ μ

악취공정시험기준황화합물-저온농축-모세관 GC법 (ES 09302.1)

악취공정시험기준황화합물-저온농축-모세관 GC법 (ES 09302.1) μ μ

악취공정시험기준황화합물-저온농축-모세관 GC법 (ES 09302.1) μ μ μ μ μ

악취공정시험기준황화합물-저온농축-충전형 GC법 (ES 09302.2) μ

악취공정시험기준황화합물-저온농축-충전형 GC법 (ES 09302.2)

악취공정시험기준황화합물-저온농축-충전형 GC법 (ES 09302.2) μ μ

악취공정시험기준황화합물-저온농축-충전형 GC법 (ES 09302.2) μ μ μ μ μ

악취공정시험기준황화합물-전기냉각저온농축-모세관 GC법 (ES 09302.3)

악취공정시험기준황화합물-전기냉각저온농축-모세관 GC법 (ES 09302.3) μ μ

악취공정시험기준황화합물-전기냉각저온농축-모세관 GC법 (ES 09302.3)

악취공정시험기준황화합물-전기냉각저온농축-모세관 GC법 (ES 09302.3) μ

악취공정시험기준황화합물-전기냉각저온농축-모세관 GC법 (ES 09302.3)

악취공정시험기준황화합물-전기냉각저온농축-모세관 GC법 (ES 09302.3) μ μ μ μ

악취공정시험기준황화합물-전기냉각저온농축-모세관 GC법 (ES 09302.3) μ μ

악취공정시험기준트라이메틸아민 - HS- 모세관 GC 법 (ES 09303.1) μ

악취공정시험기준트라이메틸아민 - SPME- 모세관 GC 법 (ES 09303.2) μ

악취공정시험기준트라이메틸아민 - SPME- 모세관 GC 법 (ES 09303.2)

악취공정시험기준트라이메틸아민 - 저온농축 GC 법 (ES 09303.3) μ

악취공정시험기준알데하이드 - DNPH-HPLC 법 (ES 09304.1)

악취공정시험기준알데하이드 - DNPH-GC 법 (ES 09304.2)

스타이렌 - 저온흡착농축 - GC 법 (ES 09305.1)

악취공정시험기준스타이렌-저온흡착농축- GC법 (ES 09305.1)

악취공정시험기준스타이렌-SPME-GC법 (ES 09305.2)

악취공정시험기준톨루엔외 7 종 - 저온농축 GC 법 (ES 09306) μ

1.3.1

악취공정시험기준지방산 - HS-GC 법 (ES 09307.1)

악취공정시험기준지방산 - SPME-GC법 (ES 09307.2) μ

악취공정시험기준지방산 - SPME-GC법 (ES 09307.2) μ μ

악취공정시험기준지방산 - SPME-GC법 (ES 09307.2)

악취공정시험기준전기냉각법을이용한황화합물연속측정방법 (ES 09900)

악취공정시험기준전기냉각법을이용한황화합물연속측정방법 (ES 09900) μ

악취공정시험기준전기냉각법을이용한황화합물연속측정방법 (ES 09900)

악취공정시험기준흡광차분석장치를이용한암모니아연속측정방법 (ES 09901)

악취공정시험기준흡광차분석장치를이용한스타이렌연속측정방법 (ES 09901)

악취공정시험기준고효율막채취장치를이용한트라이메틸아민과암모니아의연속측정방법 (ES 09903)

악취공정시험기준고효율막채취장치를이용한카르보닐류의연속측정방법 (ES 09905)

악취공정시험기준저온농축장치를이용한휘발성물질류의연속측정방법 (ES 09906)

악취공정시험기준고효율막채취장치를이용한유기산류의연속측정방법 (ES 09907)

제 3 장최신기법을도입한추가개정 ( 안 ) 마련 제 1 절서론

μ μ 제 2 절유기지방산공정시험방법연구

No. Group Full name Short name CAS No. Chemical formula Structure Molecular weight a] Threshold b Permissible concentration c] Industrial region Other region Refer ence d] 1 Acid Propionic acid PA 79-0 9-4 C 3H 6O 2 74.08 0.0057 0.07 0.03 2010 2 Butyric acid BA 107-92-6 C 4H 8O 2 88.11 0.00019 0.002 0.001 2010 3 Isovaleri c acid IA 503-74-2 C 5H 10O 2 102.1 0.000078 0.004 0.001 2010 4 Valeric acid VA 109-52-4 C 5H 10O 2 102.1 0.000037 0.002 0.0009 2010 Full Short No. Group name name 1 Aromatic Benzene B CAS No. 71-4 3-2 Permissible Chemical Molecular Structure Threshold b concentration c] Refer formula weight a] Industrial Other ence d] region region C 6H6 78.11 0.33 - - - 2 Toluene T 108-88-3 C 7H 8 92.14 0.33 30 10 2008 3 para-xy lene p-x 106-42-3 C 8H 10 106.2 0.058 2 1 2008 4 ortho-x ylene o-x 95-4 7-6 C 8H 10 106.2 0.38 2 1 2008 5 Styrene S 6 Ketone 7 8 Acetate 9 Alcohol Methyl ethyl ketone Methyl isobutyl ketone Butyl acetate Isobutyl alcohol MEK 100-42-5 78-9 3-3 MIBK 108-10-1 BuAc i-bu Al 123-86-4 78-8 3-1 C 8H 8 104.2 0.035 0.8 0.4 2005 C 4H 8O 72.11 0.44 35 13 2008 C 6H 12O 100.2 0.17 3 1 2008 C 6H 12O 2 116.2 0.016 4 1 2008 C 4H 10O 74.12 0.011 4 0.9 2010

μ μ μ μ μ

S T p-x o-x MEK MIBK BuAc i-bual PA BA IA VA (μg/ml) 59,994 59,945 59,573 59,667 61,100 60,800 60,984 60,872 62,073 60,192 61,050 61,380 S T p-x o-x MEK MIBK BuAc i-bual PA BA IA VA μg/l 60.0 59.9 59.6 59.7 61.1 60.8 61.0 60.9 62.1 60.2 61.1 61.4 (ppm) 14.1 15.9 13.7 13.7 20.7 14.8 12.8 20.1 20.5 16.7 14.62 14.70 Gaseous N 2 Dilution Concentration (ppb) STD ratio (ml) (ml) S T p-x o-x MEK MIBK BuAc i-bual PA BA IA VA 10 9990 0.001 14.1 15.9 13.7 13.7 20.7 14.8 12.8 20.1 20.5 16.7 14.6 14.7 25 9975 0.0025 35.2 39.8 34.3 34.4 51.8 37.1 32.1 50.2 51.2 41.8 36.5 36.7 50 9950 0.005 70.4 79.5 68.6 68.7 104 74.2 64.2 100 102 83.5 73.1 73.5 S T p-x o-x MEK MIBK BuAc i-bual PA BA IA VA (μg/ml) 59,994 59,945 59,573 59,667 61,100 60,800 60,984 60,872 62,073 60,192 61,050 61,380 S T p-x o-x MEK MIBK BuAc i-bua l PA BA IA VA

μg/l 60.0 59.9 59.6 59.7 61.1 60.8 61.0 60.9 62.1 60.2 61.1 61.4 (ppm) 14.1 15.9 13.7 13.7 20.7 14.8 12.8 20.1 20.5 16.7 14.62 14.70 Gaseous STD N 2 Dilution Concentration (ppb) ratio (ml) (ml) S T p-x o-x MEK MIBK BuAc i-bual PA BA IA VA 200 99800 0.002 28.2 31.8 27.4 27.5 41.4 29.7 25.7 40.2 41.0 33.4 29.2 29.4 Order Tube code Absorbent type 1 TA Tenax TA 300 mg 2 CX Carbopack X 300 mg 3 CB Carbopack B 300 mg 4 TA-CB-CX Tenax TA 100 mg + Carbopack B 100 mg + Carbopack X 100 mg 5 TA-CB Tenax TA 200 mg + Carbopack B 100 mg

μ μ μ Order VOC Ketone Acetate Alcohol S T m-x p-x o-x MEK MIBK BuAc i-bual 1 9.90 10.0 10.0 10.0 10.0 10.0 9.85 10.0 9.92 2 19.8 20.0 20.0 20.0 20.0 19.9 19.7 20.0 19.8 3 39.6 40.0 40.0 40.0 40.0 39.8 39.4 40.1 39.7 4 99.0 100 100 100 100 100 98.5 100 99.2 5 198 200 200 200 200 199 197 200 198 Order Acid PA BA IA VA 1 9.80 9.50 9.16 9.21 2 19.6 19.0 18.3 18.4 3 39.2 38.0 36.6 36.8 4 98.0 95.0 91.6 92.1 5 196 190 183 184

Column WAX(Length: 60 m, ID: 0.25 mm, Film thickness: 0.25 μm, Chrompack) GC-FID system a] Initial oven temp 50 Initial hold time 5 min Rate 6 min -1 Final oven temp 230 Final hold time 5 min Total time 40 min Detector temp 240 Thermal desorber b] Carrier gas(n 2) 1.5 ml min -1 Split ratio 5:1 Sampling tube desorption temp. 300 Sampling tube holding time 10 min Cold trap temp low 5 Cold trap temp high 300 Cold trap hold time 5 min Valve temp 120 Transfer line temp 120

Minimum pressure 10 psi Column WAX(Length: 60 m, ID: 0.25 mm, Film thickness: 0.25μm, Chrompack) GC-FID system a] Carrier gas(n 2) 1.5 ml min -1 Split ratio 10:1 Injector temp 250 Initial oven temp 50 Initial hold time 5 min Rate 6 min -1 Final oven temp 230 Final hold time 5 min Total time 40 min Detector temp 240 Solid phase Carboxen polidimethylsiloxane (PDMS) 75 μm microextraction Adsorption temp 90 Adsorption time 20 min

μ μ μ

460 440 TA CX CB TA-CB-CX TA-CB 420 400 380 360 340 320 S T p-x m-x o-x TA 400 350 300 CX CB TA-CB-CX TA-CB 250 200 150 100 50 0 MEK MIBK BuAc i-bual

250 200 TA CX CB TA-CB-CX TA-CB 150 100 50 0 PA BA IA VA Tube type S T p-x o-x MEK MIBK BuAc i-bu Al PA BA IA VA TA 1.25 1.45 1.22 3.00 0.68 0.80 0.96 1.45 9.05 10.6 9.36 15.4 CX 0.65 1.67 0.33 0.34 1.87 0.59 0.60 0.08 0.56 0.85 0.98 1.46 CB 1.25 1.70 1.41 5.09 1.31 1.27 1.27 1.00 0.30 2.27 3.08 2.59 TA-CB-CX 1.60 1.72 1.54 4.04 1.31 1.39 1.69 1.46 4.26 2.31 2.71 2.69 TA-CB 1.88 4.77 1.80 1.79 1.26 1.82 1.74 1.88 0.56 1.85 2.87 2.47 b. Method detection limit (ppb)** TA 0.01 0.01 0.01 0.01 0.04 0.02 0.02 0.02 0.07 0.04 0.03 0.04 CX 0.01 0.01 0.01 0.01 0.05 0.02 0.02 0.02 0.05 0.03 0.03 0.03 CB 0.01 0.01 0.01 0.01 0.05 0.02 0.02 0.02 0.06 0.03 0.03 0.02 TA-CB-CX 0.01 0.01 0.01 0.01 0.05 0.02 0.02 0.02 0.05 0.03 0.03 0.02 TA-CB 0.01 0.01 0.01 0.01 0.06 0.03 0.02 0.02 0.06 0.04 0.03 0.03

Date of analysis S T p-x o-x MEK MIBK BuAc i-bu Al PA BA IA VA Liquid phase STD* 22 Jun. 2010 Response factor r 219 236 213 225 71.3 131 115 143 76.8 97.3 114 111 0.99 0.99 0.99 0.99 95 92 95 95 0.98 0.999 0.99 0.99 0.99 78 1 94 94 95 0.99 0.99 0.99 94 93 92 Gaseous STD** 16 Jun. 2010 Response factor r 102 175 140 151 98.3 127 88.9 129 25.3 26.6 37.8 13.3 0.99 0.99 0.99 0.99 93 97 97 96 0.99 0.999 0.99 0.99 0.99 96 8 97 97 97 0.99 0.99 0.99 81 98 79 G/L ratio 0.47 0.74 0.66 0.67 1.38 0.97 0.77 0.90 0.33 0.27 0.33 0.12

1st bag 2nd bag 3rd bag Response factor r Response factor r Response factor r S T p-x o-x MEK MIBK BuAc i-bu Al PA BA IA VA 102 175 140 151 98.3 127 88.9 129 25.3 26.6 37.8 13.3 0.99 0.99 0.99 0.99 0.99 93 97 97 96 96 0.999 0.99 0.99 0.99 0.99 8 97 97 97 81 0.99 0.99 98 79 82.3 173 124 135 91.7 120 81.5 123 17.2 16.6 29.1 7.04 0.99 0.99 0.99 0.99 0.99 95 99 99 98 99 0.999 0.99 0.99 0.99 0.99 8 99 99 70 82 0.99 0.99 97 74 70.0 169 113 124 86.1 115 75.6 119 14.4 12.5 23.9 4.95 0.99 0.99 0.99 1.00 0.99 99 98 99 00 99 0.999 0.99 0.99 0.99 0.99 8 97 99 98 97 0.99 0.99 93 89 S T p-x o-x MEK MIBK BuAc i-bu PA BA IA VA

1st bag 2nd bag 3rd bag Response factor r Response factor r Response factor r Al 73.7 217 114 123 75.6 100 64.9 107 17.0 16.6 28.0 7.82 0.99 0.99 0.99 0.99 0.99 1.000 73 71 97 98 98 0.99 0.99 0.98 0.96 0.99 91 99 12 06 82 0.92 99 66.8 251 107 118 78.0 97.2 62.7 105 13.8 11.7 21.4 4.54 0.99 0.99 0.99 0.99 0.99 91 93 97 97 88 0.999 0.99 0.99 0.95 0.97 8 88 99 58 49 0.99 0.97 61 28 53.1 341 100 105 80.7 91.3 57.0 101 11.2 9.52 16.7 2.23 0.99 0.99 0.99 0.99 0.99 95 96 99 91 98 0.999 0.99 0.99 0.95 0.96 8 93 99 48 61 0.99 0.98 19 86 1st bag 2nd bag 3rd bag Response factor r Response factor r Response factor r S T p-x o-x MEK MIBK BuAc i-bu Al PA BA IA VA 61.2 136 105 113 77.3 102 66.0 108 10.9 11.7 24.5 4.69 0.99 1.00 0.99 0.99 1.00 98 00 99 99 00 0.999 0.99 1.00 0.99 0.99 9 99 00 83 91 0.99 0.99 96 56 48.9 133 95.1 103 73.8 99.4 61.5 107 7.78 7.56 18.1 2.65 1.00 0.99 1.00 1.00 0.99 00 99 00 00 97 0.999 0.99 0.99 0.99 0.99 9 98 99 92 99 0.99 0.99 87 97 41.6 129 86.5 94.7 70.0 95.8 57.4 104 7.03 6.21 15.3 2.16 0.99 0.99 0.99 0.99 0.99 93 98 95 93 97 0.999 0.99 0.99 0.98 0.99 8 98 98 72 58 0.99 0.98 89 28 1st bag 2nd bag 3rd bag Response factor r Response factor r Response factor r BuA i-bu S T p-x o-x MEK MIBK PA BA IA VA c Al 68.7 155 112 119 79.8 104 68.4 109 13.4 14.3 26.7 5.93 0.99 0.99 0.99 0.99 98 96 99 99 0.99 0.999 0.99 0.99 0.99 98 8 98 98 71 0.99 0.99 0.99 95 51 79 49.5 178 92.5 102 75.3 97.3 60.2 105 7.53 7.14 15.9 2.27 0.99 0.99 0.99 0.99 98 97 98 99 0.99 0.999 0.99 0.99 0.99 99 8 98 98 41 0.99 0.99 0.99 72 30 79 40.4 200 80.8 89.2 73.7 91.6 54.0 100 6.32 5.31 12.7 1.54 0.99 0.99 0.99 0.99 99 98 99 95 0.99 0.999 0.99 0.99 0.99 99 8 97 99 41 0.99 0.99 0.99 94 69 91

120 100 2nd bag 3rd bag 80 60 40 20 0 S T p-x o-x MEK MIBK BuAc i-bual PA BA IA VA 120 100 2nd bag 3rd bag 80 60 40 20 0 S T p-x o-x MEK MIBK BuAc i-bual PA BA IA VA 120 100 2nd bag 3rd bag 80 60 40 20 0 S T p-x o-x MEK MIBK BuAc i-bual PA BA IA VA

120 2nd bag 3rd bag 100 80 60 40 20 0 S T p-x o-x MEK MIBK BuAc i-bual PA BA IA VA

50000 40000 30000 20000 10000 PA BA IA VA y (PA) = 71.281x R 2 = 0.9963 y (IA) = 104.8x R 2 = 0.996 y (VA) = 97.887x R 2 = 0.9952 y (BA) = 94.331x R 2 = 0.996 0 0 100 200 300 400 500 (ng)

250 200 150 PA BA IA VA y (VA) = 0.5392x R 2 = 0.9748 y (IA) = 0.3671x R 2 = 0.9543 100 y (BA) = 0.1771x R 2 = 0.9811 50 y (PA) = 0.0644x R 2 = 0.9691 0 0 100 200 300 400 500 (ng)

S T p-x o-x MEK MIBK BuAc i-bual PA BA IA VA GC-TD (%) 2.94 2.43 3.81 2.74 6.59 3.39 3.13 2.99 2.88 4.20 1.17 1.69 GC-SPME (%) 1.05 11.3 5.23 6.49 4.58 5.21 29.3 6.50 4.06 1.72 0.85 3.17 S T p-x o-x MEK MIBK BuAc i-bual PA BA IA VA GC-TD (ng) 0.10 0.10 0.10 0.10 0.29 0.17 0.20 0.16 0.30 0.23 0.21 0.22 (ppb) 0.01 0.02 0.01 0.01 0.10 0.03 0.05 0.03 0.11 0.06 0.05 0.06 GC-SPME (ng) 0.09 0.07 0.10 0.08 1.58 0.28 3.87 3.11 14.9 5.43 2.62 1.78 (ppb) 0.01 0.01 0.01 0.01 0.32 0.04 0.49 0.62 2.96 0.91 0.38 0.26 Flow rate Loading time Volume Absorbed mass in tube (ng) (L/min) (min) (L) S T p-x o-x MEK MIBK BuAc i-bual PA BA IA VA 0.2 25 5 600 599 596 597 611 608 610 609 621 602 611 614 Flow rate Loading time Volume Absorbed mass in 5 ml 0.1 N NaOH (ng) (L/min) (min) (L) S T p-x o-x MEK MIBK BuAc i-bual PA BA IA VA 2 25 50 1000 999 993 994 1018 1013 1016 1015 1035 1003 1018 1023 Method Loading vol. (L) S T p-x o-x MEK MIBK BuAc i-bual PA BA IA VA GC-TD 5 (ppb) 11.3 21.9 16.5 17.0 50.1 27.4 17.2 34.3 8.73 6.27 9.93 2.64 GC-SPME 50 (ppb) 0.04 0.03 0.01 0.02 12.7 1.60 0.49 29.3 13.7 12.1 14.1 5.77 Ratio (GC-TD/GC-SPME) 278 739 119 4 817 3.95 17.1 35.2 1.17 0.64 0.52 0.71 0.46

제 3 절부지경계선에서의시료채취방법의최신기법검토

제 4 절공기희석관능법에대한수정안제시

β β

7.2.2 부지경계선시료관능시험절차 7.2.2.1 7.2.2.2 7.2.2.3 7.2.2.4 7.2.2.5 7.2.2.6 7.2.2.7

7.2.2.8 7.2.3 배출구시료관능시험절차 7.2.3.1 7.2.3.2 7.2.3.3 7.2.3.4 7.2.3.5 7.2.3.6 7.2.3.7

7.2.3.8 7.2.3.9 7.2.3.10 7.2.3.11 7.2.3.12 7.2.3.13

8.1 부지경계선시료희석배수산정 8.1.1 관능시험희석배수결정

8.1.2 희석배수산정방법 8.1.3 판정방법

8.1.4 결과표시 8.2 배출구시료희석배수산정 8.2.1 관능시험희석배수결정 8.2.2 희석배수산정방법 8.2.2.1

8.2.2.2 8.2.2.3

제 4 장악취배출시설측정법검토 제 1 절서론 제 2 절악취배출시설측정의외국사례

제 3 절악취측정방법의간이측정법, 검지관법등조사제시