KS I ISO 11885-2008 Water quality－Determination of selected elements by inductively coupled plasma optical emission spectrometry(ICP-OES)《水质 感应耦合等离子体光学发射光谱法(ICP-OES)测定选取的元素》.pdf

1、 KSKSKSKSKSKSKSK KSKSKS KSKSK KSKS KSK KS KS I ISO 11885 (ICP-OES) KS I ISO 11885:2008 2008 11 24 http:/www.kats.go.krKS I ISO 11885:2008 : ( ) ( ) ( ) : (http:/www.standard.go.kr) ： ： 1998 12 24 ： 2008 11 24 2008-0794 ： ： ( 025097266) (http:/www.kats.go.kr). 10 5 , . KS I ISO 11885:2008 (ICP-OES) W

2、ater quality Determination of selected elements by inductively coupled plasma optical emission spectrometry(ICP-OES) 2007 2 ISO 11885, Water quality Determination of selected elements by inductively coupled plasma optical emission spectrometry(ICP OES) , . . . . . 1 ( , , , , ) , , , , , , , , , , ,

3、 , , , , , , , , , , , , , , , , , , , , , , , , . , , ( , KS M ISO 15587 1 KS M ISO 15587 2 ). 2 g/L . , . . 1 . 2 . . ( ) . KS I ISO 11885:2008 2 KS A ISO Guide 30： 2005, KS M ISO 3696, KS M ISO 5667 1, ( ) KS M ISO 5667 3, 3： KS M ISO 7027, KS M ISO 15587 1, 1： KS M ISO 15587 2, 2： 3 . 3.1 (accur

4、acy) . . 3.2 (analyte) 3.3 (Background Equivalent Concentration： BEC) 3.4 (calibration blank solution) 3.5 (calibration solution) 3.6 (calibration check solution) , 3.7 (determination) , 3.8 (instrument performance check solution) KS I ISO 11885:2008 3 3.9 (linearity) ( ) ( ) ( ) 3.10 (limit of dete

5、ction), XLD 0 . XLD 3s0 XLD： s0： (3.14) 3 KS M ISO 13530 3.11 , (limit of quantification), XLQ srel 33.3 % XLQ 3XLD 9s0 KS M ISO 13530 3.12 (mean result) n , ( ) () . (mg/L) . 3.13 (precision) , . 3.14 (regent blank solution) ( .) 3.15 (reproducibility) KS A ISO 3534 2： 2008, 3.3.10 KS I ISO 11885:2

6、008 4 3.16 (reproducibility conditions) KS A ISO 3534 2： 2008, 3.3.11 3.17 (reproducibility standard deviation) KS A ISO 3534 2： 2008, 3.3.12 3.18 (reproducibility limit), R 95 % KS A ISO 3534 2： 2008, 3.3.14 3.19 (repeatability) KS A ISO 3534 2： 2008, 3.3.5 3.20 (repeatability acondition) KS A ISO

7、3534 2： 2008, 3.3.6 3.21 (repeatability standard deviation) KS A ISO 3534 2： 2008, 3.3.7 3.22 (repeatability limit), r 95 % KS A ISO 3534 2： 2008, 3.3.9 3.23 (stock solution) . . KS A ISO Guide 30 . KS I ISO 11885:2008 5 3.24 (test sample) ( , ) 3.25 (test sample solution) , . 3.26 (total element co

8、ncentration) (9.5.2) (9.5.1) 3.27 , (trueness, bias) . 4 . (aerosol) , . (ICP) . , . . . 5 , ( B ) (LOQ) 1 . , . . , 1 . KS I ISO 11885:2008 6 1 a, (XLQb) XLQ nm g/L g/L Ag 328.068 338.289 (20) (20) (4) (10) Fe, Mn, Zr Cr, Fe, Zr, Mn Al 167.079 308.215 396.152 1 100 10 2 17 6 Fe, Pb Fe, Mn, OH, V Cu

9、, Fe, Mo, Zr As 188.979 193.696 197.197 18 5 (100) 14 14 31 Al, Cr, Fe, Ti Al, Co, Fe, W, V Al, Co, Fe, Pb, Ti B 182.528 208.957 249.677 249.772 (6) (5) 10 4 (7) 5 24 S Al, Mo Co, Cr, Fe Co, Fe Ba 230.425 233.527 455.403 493.408 2 6 (3) 3 0.5 0.7 0.4 Fe, V Zr Be 313.042 313.107 234.861 (2) (5) (0.1)

10、 (0.3) (0.1) Fe V Bi 223.060 306.770 (40) (80) (17) (165) Co, Cu, Ti, V Fe, Mo, V Ca 315.887 317.933 393.366 422.673 100 26 0.4 13 4 25 Co, Mo Fe, V V, Zr V, Mo, Zr Cd 214.441 226.502 228.802 1 4 2 0.9 0.2 0.5 As, Cr, Fe, Sc, Sb As, Co, Fe, Ni As, Co, Sc Co 228.616 238.892 6 10 1 3 Ti Fe Cr 205.229

11、267.719 238.563 284.324 1 4 (10) (10) 5 2 (2) Be, Fe, Mo, Ni, Ti Mn, P, V Fe, Mo, V, W Fe Cu 324.754 327.396 9 4 2 3 Cr, Fe, Mo, Ti Co, Ti Fe 238.204 259.940 271.441 14 6 (3) 2 Co Co Ga 287.424 294.364 417.204 Cr Fe, Ti Fe, V KS I ISO 11885:2008 7 1 a, (XLQb) ( ) XLQ nm g/L g/L In 230.605 325.609 41

12、0.175 Fe Mn Ce K 766.490 769.896 66 20 (230) Ar, Ba, Mg Ba Li 460.290 670.778 900 6 (700) 10 Ar, Fe Ar Mg 279.078 279.553 285.213 33 1 4 19 7 14 Fe Fe Cr Mn 257.610 293.305 1 (20) 0.4 (8) Cr, Fe, Mo, W Al, Cr, Fe, Ti Mo 202.031 204.597 (30) (50) (2) (6) Al, Fe, Ni Co, Cr Na 330.237 588.995 589.592 (

13、20) 20 93 300 200 20 Zn Ar, V Ba Ni 221.648 231.604 10 15 2 2 Si Co, Sb P 177.434 178.221 213.618 214.915 500 25 500 330 (16) 13 50 9 Cu Fe, I Co, Cu, Fe, Mo, ZnAl, Co, Cu, Mg Pb 220.353 283.305 14 (70) 5 (20) Al, Co, Fe, Ti Cr, Fe S 180.669 181.975 13 39 33 17 As, Ca Cr, Mo Sb 206.834 217.582 (100)

14、 (100) (4) (18) Co, Cr, Fe, Mg, MnPb, Fe Se 196.089 203.984 (100) (100) (7) (7) Cr, Sb Si 212.412 251.611 288.158 3 20 (30) (13) 10 24 Mo Cr Sn 189.988 235.485 283.998 (100) (100) (60) (200) (120) Cr, Ti Cd, Mo Sr 407.771 421.552 460.733 2.6 0.1 (10) 0.6 0.1 (3) Cr Ti 334.941 336.123 337.280 368.521

15、 (5) (10) (10) (10) (2) (1) Cr Co, Cr KS I ISO 11885:2008 8 1 a, (XLQb) ( ) XLQ nm g/L g/L V 290.881 292.402 310.229 311.071 (10) (10) (10) (10) (3) (0.7) (1) Fe, Mo Cr, Fe, Mo, V Cr, Mg Cr, Fe, Mn, Ti W 202.998 207.912 209.860 222.589 239.711 (60) (30) (60) (60) (60) (10) (20) (30) Ni, Zn Ni, Mo, V

16、 Cr, Cu, Ni Zn 202.548 206.200 213.857 13 3.3 (3) 5 1 Cr, Cu, Co, Ni Cr Cu, Fe, Ni Zr 339.197 343.823 354.262 (10) (50) (2) (0.3) (1) Mo 1 XLQ： 3.11 (XLQ) 2 XLQ ( B ). 3.11 XLQ . 1 . . a 1 NIST . (http:/physics.nist.qov/PhysRefData/Handbook/) b , . . . 6 6.1 . . , , . , . , ICP MS . . 6.2 6.2.1 KS I

17、 ISO 11885:2008 9 . . . . 1 . 6.2.2 6.2.2.1 , . , . 6.2.2.2 , . , . 6.2.3 . 1) 2) . 6.2.4 , . , . . 6.3 6.3.1 . , / . / . ( , ), (excitation interference) , / . 6.3.2 (excitation interferences) ( ) , . , . (Li, K, Na) , KS I ISO 11885:2008 10 . 6.3.3 , . . , . , . , . 6.3.4 , . a) ( , 10 ), 10 % ( )

18、. b) ( ) 10 ( 100 ) 80 % 120 % . , . , . 6.4 . . , ( ) . . . , . , . , , ( ) . , . . , . . 7 7.1 KS I ISO 11885:2008 11 , . . , 105 1 . . . 7.2 KS M ISO 3696 1 , . 7.3 (HNO3) 1.4 g/mL (HNO3) 1.40 g/mLw(HNO3) 650 g/kg (HNO3) 1.42 g/mLw(HNO3) 690 g/kg . 2 . 7.4 w(H2O2) 30 % , . 7.5 (H2SO4) 1.84 g/mL 7

19、.6 (HCl) 1.16 g/mL 7.7 (HCl) 0.2 mol/L 7.8 (NH4)2SO4 7.9 1 000 mg/L Ag, Al, As, B, Ba, Be, Bi, Ca, Cd, Co, Cr, Cu, Fe, Ga, In, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, S, Sb, Se, Si, Sn, Sr, Ti, V, W, Zn, Zr KS A ISO Guide 30 . . KS I ISO 11885:2008 12 (： 100 mg/L) . , . 7.10 7.10.1 . , . (： ). . . . . . ,

20、 . , (： , , ) . 7.10.2 A (Al, Cd, Co, Cr, Cu, Ga, Fe, In, Pb, Li, Mn, Mo, Ni, V, Zn, Bi, Si, W, Zr) 1 mg/L 1 000 mL 250 mL (7.2) . 5 mL (7.3) . 1 000 mL (10.01) mL (Al, Cd, Co, Cr, Cu, Fe, Pb, Li, Mn, Mo, Ni, V, Zn, Bi, Si, W, Zr)(7.9) . (7.2) , . 7.10.3 B (Sn, Ti, As, Se, Sb) 10 mg/L 1 000 mL 250 m

21、L (7.2) . 5 mL (7.6) . 1 000 mL (100.1) mL (Sn, Ti, As, Se, Sb)(7.9) . (7.2) , . KS I ISO 11885:2008 13 7.10.4 C (Ba, Be, Sr) 0.1 mg/L 1 000 mL 250 mL (7.2) . 5 mL (7.3) . 1 000 mL (0.10.002) mL (Ba, Be ,Sr)(7.9) . (7.2) , . 7.10.5 D (Ag) 1 mg/L 1 000 mL 250 mL (7.2) . 5 mL (7.3) . AgCl2 10 mL (7.6) . 1 000 mL (1.00.01) mL (7.9) . (7.2) , . 7.10.6 E (B) 10 mg/L 1 000 mL 250 mL (7.2) . 5 mL (7.