w y wz 8«( 3y 143~153, 005 J. of the Korean Socety for Envronmental nalyss x yá Á Áyk Áy Á wá½ *Á ** y œ, *w x, **w t w Preparaton of Fly sh for Profcency Testng of Doxn nalyss Dongho Moon, Sangwon Lee, hangn Ihm, Taewoong Hwang, Yongyoul Hwang, Jongsang Km*, and Jnchun Woo ** Envronmental Management o. Kyungseo-dong, Seo-gu, Incheon, 404-708, Korea *Korea Insttute of onstructon Materals, Seoul 137-707, Korea **Korea Research Insttute of Standards and Scence, Daejeon 305-600, Korea Fly ash sample collected from muncpal waste ncnerator was prepared for profcency testng of doxn analyss. The collected sample was carred out several steps for homogenzng and then analyzed for evaluatng homogenety and stablty. One way NOV was used for the evaluaton. The uncertanty of each target somer from whole doxn analyss procedure was also evaluated and combned. Next, the uncertantes form repeatng analyss and analytcal procedure were combned. Fnally, the assgned value of the profcency testng sample was suggested. Key words : Doxn, Profcency testng, Uncertanty 1. w y j z j ƒ ³ ƒ w š.,» w» w š. y w» w»» v w sƒƒ v 1. x y w ISO/IE 1705 w x swwš x w ƒwš. ù x w ³ sƒƒ w w y sww p wì ùkü w w. ƒ w x w. ³ sƒwš3,4 EURHEM IT l w 5 Gude w y sƒw 6...1. x w ƒ w. yr w ƒ w screw conveyor l p w w z w 10 kg w... EP 1613(USEP, 1994 ü d ( y w, 00 w wš SP-331f w HRG/HRMS (VG Ultma, mcromass, UK w. t Wellngton t w, m To whom correspondence should be addressed.
144 yá Á Áyk Áy Á wá½ Á w œ m v Kess w. 3. š 3.1. x 3.1.1. ³ y ³ y w» w w w. w z z q ƒ yw» 4 yww z 00 mesh(75 um w w. w z w. 3.1.. ³ y 00 mesh w w, 00 mesh ƒ wš, ³ sƒ» w 00 mesh w s sƒw. j» 00 mesh j 100 mesh 00 mesh 30 mesh, 35 mesh w. ³ y 3 w s sƒ w w. ƒ w y e w, j»ƒ 4 j»ƒ. 100 mesh e w š w. 30 ³ w w š, ƒ e w., 3 00 mesh wƒ w ùkû, 00 mesh ƒ ƒ 89% q Fg. 1. The result of partcle sze analyss. ³ y 00 mesh w» q. Fg. 1 ùkü. mw l r z matrx ³ w š q 90 w. 3.1.3. (between-bottle ³ sƒ x 90 5 w w ³ sƒw. ³ sƒ Table 1 ùkü. ³ sƒ t 95% 30.357Û4.80 ng-teq/g ³ w s ƒ. 3.1.4. ü(wthn-bottle ³ sƒ x 90 kw ƒ 3 v, 6 m w ³ sƒw.» m w sƒw. ü ³ sƒ Table ùkü. ü ³ sƒ t 95% 30.744 Û 3.033 ng-teq/g Table 1. Homogenety between-bottle (unt : ng-teq/g 3-BB 6-BB F3-BB F6-BB J4-BB,3,7,8-TDF 0.156 0.19 0.157 0.181 0.139 1,,3,7,8-PeDF 0.185 0.04 0.160 0.185 0.155,3,4,7,8-PeDF.771 3.115.591.990.43 1,,3,4,7,8-HxDF 0.731 0.758 0.607 0.665 0.610 1,,3,6,7,8-HxDF 1.716 1.81 1.559 1.59 1.443,3,4,6,7,8-HxDF.630.737.00.413.00 1,,3,7,8,9-HxDF 0.151 0.183 0.13 0.158 0.13 1,,3,4,6,7,8-HpDF 1.069 1.118 0.903 1.000 0.844 1,,3,4,7,8,9-HpDF 0.53 0.45 0.11 0.06 0.184 ODF 0.195 0.188 0.144 0.165 0.144,3,7,8-TDD 3.348 3.99 3.046 3.88.975 1,,3,7,8-PeDD 6.318 6.831 5.94 6.083 5.05 1,,3,4,7,8-HxDD 1.664 1.78 1.369 1.545 1.319 1,,3,6,7,8-HxDD.433.605.105.69.049 1,,3,7,8,9-HxDD.494.60.01.7 1.986 1,,3,4,6,7,8-HpDD 4.84 4.93 3.915 4.195 3.806 ODD 1.456 1.43 1.066 1.197 1.019 PDFs 9.857 10.55 8.664 9.555 8.085 PDDs.537 4.068 18.816 1.443 18.06 (PDDs+PDFs 3.394 34.60 7.480 30.998 6.91
x 145 Table. Homogenety Wthn-bottle (unt : ng-teq/g I3-1-WB I3--WB I3-3-WB I6-1-WB I6--WB I6-3-WB,3,7,8-TDF 0.154 0.163 0.183 0.16 0.166 0.161 1,,3,7,8-PeDF 0.16 0.178 0.198 0.148 0.167 0.179,3,4,7,8-PeDF.53.769 3.08.485.770.83 1,,3,4,7,8-HxDF 0.610 0.694 0.77 0.637 0.67 0.730 1,,3,6,7,8-HxDF 1.455 1.699 1.781 1.495 1.485 1.75,3,4,6,7,8-HxDF.16.440.590.05.69.500 1,,3,7,8,9-HxDF 0.13 0.155 0.144 0.110 0.143 0.168 1,,3,4,6,7,8-HpDF 0.865 1.06 1.137 0.916 0.893 1.118 1,,3,4,7,8,9-HpDF 0.195 0.34 0.46 0.14 0.10 0.6 ODF 0.134 0.177 0.179 0.155 0.156 0.170,3,7,8-TDD 3.3 3.66 3.853.715 3.50 3.430 1,,3,7,8-PeDD 5.443 6.003 6.717 5.34 5.739 6.704 1,,3,4,7,8-HxDD 1.377 1.779 1.785 1.470 1.57 1.734 1,,3,6,7,8-HxDD.107.539.53.1.186.569 1,,3,7,8,9-HxDD.093.649.691.158.137.564 1,,3,4,6,7,8-HpDD 3.875 4.780 4.947 4.4 4.169 4.904 ODD 1.05 1.385 1.445 1.174 1.08 1.441 PDFs 8.356 9.535 10.31 8.491 8.931 9.87 PDDs 19.15.761 3.961 19.95 0.486 3.346 (PDDs+PDFs 7.508 3.96 34.73 7.786 9.417 33.173 ³ w sƒ. 3.1.5. (analyss of varance ³ y w ƒ w w e (one way NOV w. ü w p 0.8448 w Fg. w. ü ƒ w d d w ƒ w. 95% 30.567Û.01 ng-teq/g Fg.. The result of varance analyss. ³ w sƒ. ƒ w Table 3 ùkü. Table 3. onfdence nterval (unt:ng-teq/g mean SD nterval confdence nterval,3,7,8-tdf 0.16 0.019 0.013 0.16Û0.013 1,,3,7,8-PeDF 0.175 0.018 0.01 0.175Û0.01,3,4,7,8-PeDF.759 0.36 0.158.759Û0.158 1,,3,4,7,8-HxDF 0.681 0.061 0.041 0.681Û0.041 1,,3,6,7,8-HxDF 1.617 0.139 0.093 1.617Û0.093,3,4,6,7,8-HxDF.374 0.31 0.155.374Û0.155 1,,3,7,8,9-HxDF 0.146 0.00 0.013 0.146Û0.013 1,,3,4,6,7,8-HpDF 0.990 0.110 0.074 0.990Û0.074 1,,3,4,7,8,9-HpDF 0.0 0.0 0.015 0.0Û0.015 ODF 0.164 0.00 0.013 0.164Û0.013,3,7,8-TDD 3.414 0.398 0.68 3.414Û0.68 1,,3,7,8-PeDD 5.957 0.63 0.45 5.957Û0.45 1,,3,4,7,8-HxDD 1.57 0.174 0.117 1.57Û0.117 1,,3,6,7,8-HxDD.37 0.10 0.141.37Û0.141 1,,3,7,8,9-HxDD.335 0.7 0.18.335Û0.18 1,,3,4,6,7,8-HpDD 4.415 0.46 0.311 4.415Û0.311 ODD 1.59 0.178 0.119 1.59Û0.119 PDFs 9.88 0.88 0.556 9.88Û0.556 PDDs 1.79.183 1.466 1.79Û1.466 (PDDs+PDFs 30.567.995.01 30.567Û.01
146 yá Á Áyk Áy Á wá½ Á Table 3 xw yw y tx ùkü d ƒ y q wš x d y w w txw w. 3.. y sƒ y sƒ GUM(Gude 7 to the Expresson of Uncertanty n Measurement» w EURHEM IT l w Gude. r, d, d y w., y ƒ w ƒ w w., y yw., w y y y w., d w q wš w w, y wš m t y w ƒ y w y wš w y š w y y w y w. 3..1. 3 g w w w z ƒ w w z t ƒw z w HRG/HRMS w. x r. 3 g e z t 8 ng wš w. t z m wš - w we z mw w w. t 1 ng w š y, e f, ù f, y k f e z z z d t wš 0 µl w š w» w w. w Fg. 3 ùkü. 3... ùký ƒ ùkú y t w. 17 = d : ƒ k (ng/g : (ng-teq/g : ƒ TEF factor f TEQ f d TEQ d d w = ------- M 1 -- f d : M : (g f : w : (ng d : y (ng/g ----- w = ----------- x : w k v j l : ƒ ü t k v j l : ƒ ü t (ng RRF : : ƒ (ng w x l l RRF = l IS Fg. 3. Flow chart for doxn analyss. : ü t mcro
x 147 ppette (µl IS : ü t (ng/ml w. 17 ------------------- ( χ f IS f TEQ d = E M x» χ = ------------------ l RRF 17 ƒƒ wš ƒ y ƒƒ w w w tx. d = ---------------- M f l RRF x --------------- IS f TEQ w x w w. Table 4. The Example of calculatng doxn concentraton value unt calculaton d 100-10 µl M 3.1461 g f 0.9981 - x 6.9 10 5 - l 1.6 10 7 - RRF 0.986 - IS 100 pg/µl f TEQ 0.1 - x d = ---------------- --------------- M f l RRF IS f TEQ 100 10 = ------------------------------------- 3.1461 0.9981 6.9 10 5 ----------------------------------------- 1.6 10 7 100 0.1 0.986 = 139.7674 pg/g = 0.140 ng/g 3... y w w y Fg. w. y ƒ y p w š w y w. 1 x y 0 o k ƒ w w vq y w. t ƒw ü t y š w. t ƒw z ü t d w ù kü v w y š w. 3 G/MS d ü t d w ùkü y š w. 4 RRFƒ w y t RRF y w. 5 d y ƒ 1 mg yw e w w e» w d y w. š w w y Table 5 ùkü. 3..3. y y w š 3..3.1. w y [u(d] w» w volumetrc flask Fg. 4. Fshborn dagram of the uncertanty factors n doxn analyss.
148 yá Á Áyk Áy Á wá½ Á Table 5. Uncertanty factors n doxn analyss step uncertanty factor evaluaton method type sample dvde u(d Standard spke u( l mean RRF u(g volumetrc flask u(f calbraton certfcate B ppet u(p calbraton certfcate B concentraton of standard soluton u( IS certfcate from maker B dsposable mcroppet u( calbraton certfcate B ablty of analyst u(w repetton albraton standard u( VS certfcate from maker B mean rrf u(rrf SD of RRF volumetrc ppette w y d š w w B Type w t y w. v j vr f 1, p 1, f, p w w t y w. ud d ( --------- = up 1 ( uf ( 1 up ( uf ( ------------ + ---------- + ------------ + ---------- p 1 f 1 p f z Welch-Satterthwate w. u c y ( ν eff = ----------------------------- N [ c ux ( ] 4 --------------------- ν = 1 3..3.. ü t w y u( l l = IS ƒƒ y w z w w. ü t w y [u( IS ] q t w y wš, t B x y w. j vr y [u( ] vr y w y š w w j vr v w y w w Bx t y w. x w y x mw x sƒ ww. 3ƒ w w w t y w. u l ( ------------ = l u ( IS uv ( mp -------------- + ---------------- + IS uw ( ----------- V W 3..3.3.»» w y [u(g]»» ùkù y t y s³ RRF w RRF y ù. t w y u( VS q t w y wš t Bx y wš, RRF y u(rrf 5 t w 5 RRF w z s³ RRF w w RRF t r w t w z y w. ƒ w w w w t y w. 17 w RRF ƒƒ w»» w y ƒƒ w. ug G ( --------------- = u ( VS --------------- VS 3..3.4 w y y y w w y w w d w t y w w. u ( ---------- = ud d ( --------- uc l ƒ w t y ƒ w w t y wš» sw w y y wš, w y t w. doxn = 17 ( 95%, k= urrf RRF ( + ------------------ ( + ---------- + l 17 u ± k ug G ( --------------- ( ------------ ng-teq/g
x 149 3..4. y y 3..4.1. w y [u(d] 100 w» w» 10 ml volumetrc flask wš 1 ml ppette w w v j v j ƒƒ f 1, f š wš vr ƒƒ p 1, p š w w d. d f 1 f = ---- ---- p 1 p y 100 w 1/10 w w. v j, vr y w B Type w t y w. - 1 ml volumetrc ppette y u(p 1 w vr ³ 10.005 ml. ƒ k= w t y w. up 1 ( 0.005 ------------ = ------------ = 0.005 p 1-10ml volumetrc flask y u(f 1 10 ml volumetrc flask w ³ 100.0 ml š k=, t y, 0.0 --------- uf ( ---------- = --------- = 0.001 f 10 - vr 1/10 y u(p, ³ vr w, up ( 0.005 ------------ = ------------ = 0.005 p - v j y u(f, ³ v j w, 0.0 --------- uf ( 3 ---------- = --------- = 0.001 f 10 3 y q w w t y ud d ( --------- = = up 1 ( uf ( 1 up ( uf ( ------------ + ---------- + ------------ + ---------- p 1 f 1 p f [ 0.005] + [ 0.001] + [ 0.005] +[ 0.001] = 0.003808 z ν eff Welch-Satterthwate w ù» Bx sƒ ƒƒ y w m w š z w j ƒ z w 3..4.. ü t w y u(l (5 w l = IS ƒƒ y w z w w. -ü t w y [u( IS ] ü t q t w y w. t t š Bx y w. t ³ 100 ng/ml ± 5% ƒx s ƒ w u ( IS 0.05 -------------- = --------- = 0.08868 IS 3 š w. - j vr y [u( ] vr w y vr y w y š w. j v r v w y w w 10Û0.3 µl k= Bx t y w. 0.3 ------ uv ( mp ---------------- = ------ = 0.015 10 w. x w y w (10 µl 10z w w z x sƒ w. j vr d w Table 6 ùkü. u(w = 0.16499 š t y u(w/v W 0.016499. 3ƒ w w
150 yá Á Áyk Áy Á wá½ Á Table 6. The result of analyst ablty u l ( ------------ = l = 1st 9.9 nd 10.1 3rd 10. 4th 10.1 5th 10.0 6th 9.7 7th 9.7 8th 10.0 9th 9.9 10th 9.9 mean 9.95 SD 0.164991 standard uncertanty 0.05175 degree of freedom 9 u ( IS uv ( mp -------------- + ---------------- + IS uw ( ----------- V W [ 0.08868] + [ 0.015] +[ 0.016499] = 0.036477 z ν eff Welch-Satterthwate l w 15 3..4.3.»» w y [u(g]»» ùkù y t y s³ RRF w RRF y ù - t w y u( VS t q t w y w. t t š Bx y w. t ³ y 5% t wš ƒx s ƒ w u ( VS 0.05 --------------- = --------- = 0.08868 VS 3 š w. -RRF y u(rrf 5 t w 5 RRF w z s³ RRF w w RRF t r w t w z y w. RRF 1 RRF RRF 3 RRF 4 RRF 5 0.95 0.97 0.98 1.00 1.0 s³ RRF : 0.986(»» t r : 0.04(»» t : 0.0107 = u(rrf = t r / 5 : 4 ƒ s³ y u(rrf/rrf = 0.01093.» RRF ƒ ƒƒ w w. ƒ w w ug G ( --------------- = = u ( VS --------------- VS urrf RRF ( + ------------------ [ 0.08868] + [ 0.01093] = 0.030865 z Welch-Satterthwate w 55ƒ. w w y Table 7 w. Table 7. The result of uncertanty factors for doxn analyss step sample dvde u(d Standard spke u( l mean RRF u(g uncertanty factor evaluaton method type Relatve standard uncertanty volumetrc flask u(f calbraton certfcate B 0.001 ppet u(p calbraton certfcate B 0.005 concentraton of standard soluton u( IS certfcate from maker B 0.08868 dsposable mcro ppet u( calbraton certfcate B 0.015 ablty of analyst u(w repetton 0.016499 albraton standard u( VS certfcate from maker B 0.08868 mean rrf u(rrf SD of RRF 0.01093 ombnded standard uncertanty degree of freedom 0.003808 nfnte 0.036477 15 0.030865 55
x 151 Table 8. The uncertanty of nstrument analyss for Doxn u(d u( l / l u(g/g u(/ Furan Doxn,3,7,8-TDF 0.0038 0.0365 0.0309 0.0479 1,,3,7,8-PeDF 0.0038 0.0365 0.098 0.0473,3,4,7,8-PeDF 0.0038 0.0365 0.030 0.0487 1,,3,4,7,8-HxDF 0.0038 0.0365 0.0304 0.0477 1,,3,6,7,8-HxDF 0.0038 0.0365 0.0318 0.0485,3,4,6,7,8-HxDF 0.0038 0.0365 0.0303 0.0476 1,,3,7,8,9-HxDF 0.0038 0.0365 0.0306 0.0478 1,,3,4,6,7,8-HpDF 0.0038 0.0365 0.0308 0.0479 1,,3,4,7,8,9-HpDF 0.0038 0.0365 0.0308 0.0479 ODF 0.0038 0.0365 0.0451 0.0581,3,7,8-TDD 0.0038 0.0365 0.039 0.0493 1,,3,7,8-PeDD 0.0038 0.0365 0.0304 0.0476 1,,3,4,7,8-HxDD 0.0038 0.0365 0.0313 0.048 1,,3,6,7,8-HxDD 0.0038 0.0365 0.0305 0.0477 1,,3,7,8,9-HxDD 0.0038 0.0365 0.0314 0.0483 1,,3,4,6,7,8-HpDD 0.0038 0.0365 0.0314 0.0483 ODD 0.0038 0.0365 0.030 0.0475 3..4.4. w y y y w w y w w d w t y w w Table 8 ùkü. u ( ---------- = ud d ( --------- u l ƒ w t y ƒ w w t y wš» w y y wš, w y t w doxn = 17 ( 95%, k= ( + ------------ + l 17 u ± k ug G ( --------------- ( ------------ ng-teq/g, d Table 9 w t w. = (30.567Û 0.958 ng-teq/g( 95%, k= 3.3. x y tx x w d w y w w x p w. 3.4. sƒ» sƒ w 4 7 30 o ƒƒ z w š w 7 30 ƒƒ z w. Table 11 1 ùkþ. s³ 8.665 ng-teq/g, 9.079 ng-teq/g w wù q wš», ü» w sƒw. Table 13 ùkü. p 0.059 y. 4. w x w. ³ y w z,, ü ³ sƒ w w p w» w y q wš w. x p ³ w sƒ w w w š w.
15 yá Á Áyk Áy Á wá½ Á Table 9. Expresson of fly-ash concentratons wth uncertanty Furan Doxn concentraton (ng-teq/g u(/ standard uncertanty u( expanded uncertanty k=,3,7,8-tdf 0.1616 0.0479 0.0077 0.0155 1,,3,7,8-PeDF 0.1746 0.0473 0.0083 0.0165,3,4,7,8-PeDF.759 0.0487 0.1343 0.686 1,,3,4,7,8-HxDF 0.6805 0.0477 0.034 0.0649 1,,3,6,7,8-HxDF 1.617 0.0485 0.0785 0.1570,3,4,6,7,8-HxDF.3738 0.0476 0.1130 0.59 1,,3,7,8,9-HxDF 0.146 0.0478 0.0070 0.0140 1,,3,4,6,7,8-HpDF 0.9899 0.0479 0.0474 0.0948 1,,3,4,7,8,9-HpDF 0.04 0.0479 0.0106 0.011 ODF 0.1643 0.0581 0.0095 0.0191,3,7,8-TDD 3.414 0.0493 0.1683 0.3366 1,,3,7,8-PeDD 5.9569 0.0476 0.837 0.5674 1,,3,4,7,8-HxDD 1.575 0.048 0.0758 0.1516 1,,3,6,7,8-HxDD.370 0.0477 0.1110 0.0 1,,3,7,8,9-HxDD.3350 0.0483 0.117 0.54 1,,3,4,6,7,8-HpDD 4.4147 0.0483 0.13 0.464 ODD 1.589 0.0475 0.0598 0.1196 PDFs 9.877 0.016 0.403 PDDs 1.79 0.4343 0.8686 (PDDs+PDFs 30.5669 0.4788 0.9576 Table 10. The concentraton of profcency testng sample wth uncertanty expresson (ng-teq/g relatve standard uncertanty by repetton relatve standard uncertanty by evaluaton combned relatve standard uncertanty standard uncertanty expresson wth uncertanty (k=,3,7,8-tdf 0.03573 0.04793 0.05978 0.010 0.16Û0.019 1,,3,7,8-PeDF 0.03079 0.04457 0.05417 0.009 0.175Û0.019,3,4,7,8-PeDF 0.0574 0.04607 0.0577 0.146.759Û0.91 1,,3,4,7,8-HxDF 0.0699 0.04499 0.0547 0.036 0.681Û0.071 1,,3,6,7,8-HxDF 0.0587 0.04591 0.0570 0.085 1.617Û0.170,3,4,6,7,8-HxDF 0.0939 0.0449 0.05368 0.17.374Û0.55 1,,3,7,8,9-HxDF 0.0415 0.0451 0.06113 0.009 0.146Û0.018 1,,3,4,6,7,8-HpDF 0.03356 0.0455 0.05634 0.056 0.990Û0.11 1,,3,4,7,8,9-HpDF 0.03046 0.0456 0.05455 0.01 0.0Û0.04 ODF 0.03584 0.05597 0.06646 0.011 0.164Û0.0,3,7,8-TDD 0.03519 0.0467 0.05849 0.00 3.414Û0.399 1,,3,7,8-PeDD 0.0300 0.04496 0.05518 0.39 5.957Û0.657 1,,3,4,7,8-HxDD 0.03341 0.04558 0.05651 0.089 1.57Û0.178 1,,3,6,7,8-HxDD 0.074 0.04504 0.0563 0.1.37Û0.45 1,,3,7,8,9-HxDD 0.03507 0.04564 0.05756 0.134.335Û0.69 1,,3,4,6,7,8-HpDD 0.03158 0.04566 0.0555 0.45 4.415Û0.490 ODD 0.0455 0.04483 0.06181 0.078 1.59Û0.156 PDFs 0.3 9.88Û0.445 PDDs 0.505 1.79Û1.010 w (PDDs+PDFs 0.55 30.567Û1.104
x 153 Table 11. The evaluaton of stablty after 7 s Table 1. The evaluaton of stablty after 30 s B7-7 B-7 E-7 E7-7 B7-7 H7-30 K-30 K7-30,3,7,8-TDF 0.197 0.157 0.176 0.165 1,,3,7,8-PeDF 0.177 0.154 0.01 0.170,3,4,7,8-PeDF.784.577 3.457.65 1,,3,4,7,8-HxDF 0.595 0.581 0.730 0.615 1,,3,6,7,8-HxDF 1.506 1.40 1.709 1.496,3,4,6,7,8-HxDF.1.11.554.114 1,,3,7,8,9-HxDF 0.140 0.136 0.174 0.138 1,,3,4,6,7,8-HpDF 0.76 0.791 0.970 0.804 1,,3,4,7,8,9-HpDF 0.14 0.189 0.6 0.187 ODF 0.134 0.135 0.160 0.158,3,7,8-TDD 3.318.83 3.877 3.04 1,,3,7,8-PeDD 5.705 4.989 6.349 5.51 1,,3,4,7,8-HxDD 1.38 1.54 1.604 1.369 1,,3,6,7,8-HxDD.146.08.50.61 1,,3,7,8,9-HxDD.031 1.944.463.075 1,,3,4,6,7,8-HpDD 3.99 3.774 4.409 3.877 ODD 0.957 0.970 1.158 0.993 PDFs 8.71 8.61 10.357 8.47 PDDs 19.531 17.845.36 19.111 w (PDDs+PDFs 8.5 6.106 3.719 7.583,3,7,8-TDF 0.197 0.00 0.157 0.191 1,,3,7,8-PeDF 0.177 0.09 0.167 0.03,3,4,7,8-PeDF.784 3.31.903 3.44 1,,3,4,7,8-HxDF 0.595 0.669 0.580 0.691 1,,3,6,7,8-HxDF 1.506 1.644 1.408 1.69,3,4,6,7,8-HxDF.1.417.63.71 1,,3,7,8,9-HxDF 0.140 0.69 0.160 0.36 1,,3,4,6,7,8-HpDF 0.76 0.807 0.764 0.895 1,,3,4,7,8,9-HpDF 0.14 0.04 0.19 0.31 ODF 0.134 0.10 0.139 0.165,3,7,8-TDD 3.318 3.739 3.37 3.835 1,,3,7,8-PeDD 5.705 6.081 5.048 6.99 1,,3,4,7,8-HxDD 1.38 1.459 1.99 1.566 1,,3,6,7,8-HxDD.146.78.038.455 1,,3,7,8,9-HxDD.031.115 1.94.39 1,,3,4,6,7,8-HpDD 3.99 3.51 3.675 4.115 ODD 0.957 0.780 0.948 1.097 PDFs 8.71 9.851 8.733 10.440 PDDs 19.531 19.964 18.187 1.606 w (PDDs+PDFs 8.5 9.815 6.90 3.046 Table 13. The result of NOV for stablty evaluaton n mean SD SS MS F-value p-value reference 11 30.5669.9949 13.305 13.305 1.799 0.059 sample 8 8.870.418 130.7508 7.691 total 144.056 y yw» w y jš w sww. y s ƒ w m, w sww w. ù y q w ƒ w w. sƒ y %(y y 4% sƒ. ù sƒ yƒ g z sww y ƒw q. z 98% sƒw y 3% ƒw.» t w. š x 1. Yosho Ida, Hroyuk Ifak, etc., The japan Socety for nalytcal hemstry, 001, 50, 571-576.. x», 004. w x» 3. Xuel ao, Xaoba Xu, Wenxuan u, Zhqun X, Fresenus J nal hem., 001, 370, 1035-1040. 4. R.Van leuvenbereen, G.N. Kramer, E.. Maer, hemosphere, 1998, 37, 45-438. 5. S. L. R. Ellson, M. Roslen,. Wllams, Quantfyng Uncertanty n nalytcal Measurement nd ed., 000, EURHEM/IT workng group 6. Katsunor Motohash, k, 003, 30, 56-67. 7., d y tx e, 1998, w t w