KS D ISO 7523-2012 Nickel-Determination of silver arsenic bismuth cadmium lead antimony selenium tin tellurium and thallium contents-Electrothermal atomic absorption spectrometric .pdf

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1、 KSKSKSKSKSKSKSK KSKSKS KSKSK KSKS KSK KS KS D ISO 7523 , , , , , , , , KS D ISO 7523： 2012 2012 9 3 http:/www.kats.go.krKS D ISO 7523:2012 : ( ) ( ) () () ( ) : (http:/www.standard.go.kr) ： ：2002 5 1 ：2012 9 3 2012-0408 ： ： ( 02-509-7274) (http:/www.kats.go.kr). 10 5 , . KS D ISO 7523:2012 i ii 1 1

2、 2 1 3 2 4 2 5 .4 6 .4 7 4 7.1 .4 7.2 5 7.3 .5 7.4 6 8 .7 8.1 .7 8.2 .8 9 .8 10 8 11 .8 A( ) .9 B( ) .11 KS D ISO 7523:2012 ii 1985 1 ISO 7523, Nickel Determination of silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin, tellurium and thallium contents Electrothermal atomic absorption s

3、pectrometric method , . KS D ISO 7523:2012 , , , , , , , , Nickel Determination of silver, arsenic, bismuth, cadmium, lead, antimony, selenium, tin, tellurium and thallium contentsElectrothermal atomic absorption spectrometric method 1 1 , , , , , , , , , , . . 1 a(mg/kg)bAg As Bi Cd Pb Sb Se Sn Te

4、Tl 0.110.50.10.11110.20.510 20 15 2 10 10 10 5 10 10 a , KS D ISO 6283 b 1 mg/kg = 1 g/t 9. . 2 . . ( ) . KS D ISO 7523:2012 2 KS A ISO 5725 2, ( ) 2： KS D ISO 6283, KS L ISO 385 1, 1： KS L ISO 648, KS L ISO 1042, 3 , . . , (background correction) . 4 , . 4.1 (20= 1.41 g/mL) . . 4.2 (1 19) . 4.3 4.3

5、.1 (Ag, As, Bi, Cd, Pb, Sb, Se, Te Tl 1.000 g/L) . 4.3.1.1 , , , , , ( 99.9 % ) 0.100 g 0. 000 1 g 100 mL , 10 mL (1 1) . . 10 mL (1 1) 100 mL . . . 4.3.1.2 K(SbO)C4H4O6 1/2H2O 0.274 g 100 mL , . KS D ISO 7523:2012 3 . . 4.3.1.3 0.112 g ( ) (Tl2O3) 100 mL 10 mL (4.1) . 100 mL , . 4.3.1.4 ( 99.9 % )

6、0.250 g 0.001 g 100 mL , 48 % (20= 1.13 g/mL) (4.1) 7.5 mL . . 250 mL . . 4.3.2 A As, Bi, Pb, Sb, Se, Sn, Te Tl 1.0 mg/L 4.3.2.1 1.000 g/L As, Bi, Pb, Sb, Se, Sn, Te Tl (4.3.1.1) 10.0 mL 100 mL (1 1) 1 000 mL . (5.6) . 4.3.2.2 (4.3.2.1) 10.0 mL 10 mL (1 1) 100 mL . (5.6) . 4.3.3 B(Ag Cd 0.1 mg /L )

7、4.3.3.1 1.000 g/L (4.3.1.1) 10 mL 100 mL (1 1) 1 000 mL . . (5.6) . 4.3.3.2 (4.3.3.1) 10.0 mL (1 1) 100 mL 1 000 mL . . , . 4.4 (Ni 40 g/L ) 4.4.1 (5 mg/kg Fe, 1 mg/kg , , , , , , , , ) 4.00 g 0.001 g 400 mL . 50 mL 28 mL (4.1) . . . 4.4.2 (1 1) . . 100 mL . . 0.8 mol/L (5 %) (free HNO3) . A KS D IS

8、O 7523:2012 4 5 5.1 5.1.1 , . 5.1.2 . 5.2 KS L ISO 385 1, A 0.01 mL 5 mL 10 mL 5.3 KS L ISO 648, A 10 mL 25 mL 5.4 KS L ISO 1042, A 10 mL, 100 mL, 200 mL, 250 mL 1 000 mL 5.5 5 L 25 L 5.6 (4.2) , . 6 6.1 , . 6.2 , . 6.3 . 6.4 (riffling) . 7 7.1 KS D ISO 7523:2012 5 0.9 1.1 g 0.01 g 100 mL . 30 mL 12

9、 mL (4.1) . , 100 mL . . 12 mL 5 mL . 7.2 (7.3) (zero member) . . . 7.3 7.3.1 A 7.3.1.1 0 mg, 0.005 mg, 0.010 mg, 0.02 mg, 0.05 mg, 0.07 mg, 0.1 mg, 0.15 mg, 0.20 mg, 0.25 mg 0.30 mg As, Bi, Pb, Sb, Se, Sn, Te Tl( 2 ) , 0.5 mg/kg 30 mg/kg . 10 g . 2 A A(4.3.2) mL (As, Bi, Pb, Sb, Se, Sn, Te, Tl) mg/

10、L 0 0.05 0.1 0.2 0.5 0.7 1.0 1.5 2.0 2.5 3.0 0.005 0.010 0.02 0.05 0.07 0.1 0.15 0.20 0.25 0.30 7.3.1.2 (4.4) 2.50 mL 11 10 mL . A(4.3.2) 0 mL, 0.05 mL, 0.1 mL, 0.2 mL, 0.5 mL, 0.7 mL, 1.0 mL, 1.5 mL, 2.0 mL, 2.5 mL 3.0 mL . (1 19)(4.2) . 7.3.2 B 7.3.2.1 0 mg/L, 0.0 005 mg/L, 0.001 mg/L, 0.002 mg/L,

11、 0.005 mg/L, 0.010 mg/L, 0.02 mg/L 0.05 mg/L Ag Cd ( 3 ) , 0.01 mg/kg KS D ISO 7523:2012 6 5.0 mg/kg . 10 g . 7.3.2.2 (4.4) 2.50 mL 8 10 mL . B(4.3.3) 0 mg/L, 0.05 mg/L, 0.1 mg/L, 0.2 mg/L, 0.5 mg/L, 1.0 mg/L, 2.0 mg/L 5.0 mL . (1 19)(4.2) . 3 B B(4.3.3) mL (Ag Cd) mg/L 0 0.05 0.1 0.2 0.5 1.0 2.0 5.

12、0 0.000 5 0.001 0.002 0.005 0.010 0.02 0.05 7.4 7.4.1 7.4.1.1 4 . 4 Ag As BiaCd Pb nm 328.1 193.7 223.1 228.8 283.3 Sb Se Sn Te Tl nm 217.6 196.0 286.3 214.3 276.8 a 306.8 nm .7.4.1.2 . . . . 2 6002 700 . 7.4.1.3 (5 25 L) . 7.4.1.4 (7.1) (7.3) 1 . 7.4.1.5 (0) , . KS D ISO 7523:2012 7 7.4.1.6 . . 7.4

13、.1.7 (7.1) (5 L 25 L) . . 3 4 . 7.4.1.8 , (bracketing) . 7.4.1.9 . 3 , . , (blank firing) . . 7.4.1.10 7.4.2 . 7.4.2 7.4.2.1 3 . 7.4.2.2 . . ( A ) . , . . . 8 8.1 8.1.1 3 (7.4.2) . 8.1.2 . mV ： (mg/L) V ： (mL) m ： (g) KS D ISO 7523:2012 8 8.2 6 11 . 6 . 4 , 2 . KS A ISO 5725 2 . B . . 9 9.1 . 9.2 .

14、9.3 . 9.4 . 9.5 . , . 10 . 10 g 1 000 mL . . . 10 g/L . 11 . a) b) c) d) e) . KS D ISO 7523:2012 9 A ( ) A.0 , . . . . . . . A.1 5 % (100 g/L) . . , . , . . . A.2 A.2.1 (C30H28N2S4Zn) 0.50 g/L 200 mL 100 mg . . . . A.2.2 (20= 1.41 g/mL, 1 19) A.2.3 , 100 g/L 495 g 6 Ni(NO3)2 6H2O (A.2.2) , 100 mL .

15、KS D ISO 7523:2012 10 A.3 A.3.1 (A.2.3) 100 mL (A.2.1) . 10 . , 100 mL . 10 (A.2.2) . A.3.2 283.3 nm 5 25 L . 0.010 . 3 . 3 . A.3.3 250 mL (4.4) . KS D ISO 7523:2012 11 B ( ) B.0 6 11 . 6 . 4 . KS A ISO 5725 2 . B.1 KS A ISO 5725 2, ( ) 2： KS Q ISO 3534 4, 4： B.2 KS Q ISO 3534 4 . B.3 B.3.1 3 , 3 .

16、B.3.2 3 (7.4.1.9) . B.4 B.4.1 4 , . . 28 65 (Tyler screen)( 0.60 mm 0.21 mm) . B.4.2 2 . . B.5 B.5.1 KS A ISO 5725 2 . , , KS D ISO 7523:2012 12 . . B.5.2 Cochran Dixon KS A ISO 5725 2 95 % . Cochran . Dixon . B.5.3 KS A ISO 5725 2 . . . sw2 sb2 r , 2w83.2 sr = R , 2b2w83.2 ssR += B.6 B.6.1 B.1 . B.

17、6.2 . B.6.3 . KS D ISO 7523:2012 13 B.1 % g/t sw sb r R H79 P45 P44 P45 P44 P46 H79 P45 P46 P44 P44 P45 P46 P42 S65 P45 P46 P44 P46 S65 H79 P46 P45 H79 H79 P44 P46 S65 P44 P46 9 10 11 6 7 7 6 10 11 11 10 9 10 11 10 10 11 7 10 9 6 8 7 8 7 9 9 8 10 10 100 90 100 100 86 100 100 90 100 91 90 89 90 82 90 90 100 71 100 78 100 88 100 100 86 100 100 75 100 80 0.204.4 7.6 3.1 6.8 8.2 16.4 8.0 8.6 11.5 0.581.4 1.8 0.261.5 3.9 8.5 2.8 8.5 12.0 1.3 6.3 8.3 2.5 0.482.0 8.4 0.652.0 8.6 0.04 0.13 0.21 0.18 0.18 0.58 0.54 0.39 0.41