1、 KSKSKSKSKSKSKSK KSKSKS KSKSK KSKS KSK KS KS E ISO 13291 EDTA KS E ISO 13291: 2007 2007 10 31 http:/www.kats.go.krKS E ISO 13291: 2007 : ( ) ( ) () () ( ) : (http:/www.standard.go.kr) : :2002 12 10 :2007 10 31 2007-0955 : : ( 02-509-7274) (http:/www.kats.go.kr). 10 5 , . KS E ISO 13291: 2007 EDTA Zi
2、nc sulfide concentrates Determination of zinc content Solvent extraction and EDTA titrimetric method 2006 2 ISO 13291, Zinc sulfide concentrates Determination of zincSolvent extraction and EDTA titrimetric method , . 1 . 11 %(m/m)62 %(m/m) . 1 , . . 2 . ISO . 2 . . ( ) . KS A ISO GUIDE 35, KS E ISO
3、9599, , , KS L ISO 385 1, 1: KS L ISO 648, KS L ISO 1042, KS L ISO 4787, KS M ISO 3696, 3 KS E ISO 13291: 2007 2 , . MIBK . C . 0.05 % pH 5.5 EDTA . 4 KS M ISO 3696 2 . 4.1 , 99.99 % . (4.2) (1: 9) 1 50 . 4.2 ( 1.16 1.19 g/mL) 4.3 4.4 ( 1.42 g/mL) 4.5 ( 1.13 1.15 g/mL) 4.6 ( 1.16 1.19 g/mL, 1: 4) 80
4、0 mL (4.2) 200 mL . 4.7 (1 1) 500 mL ( 1.84 g/ml) 500 mL . 4.8 ( 0.89 g/mL) 4.9 4.10 , . 4.11 200 g 100 g, 60 g 1 L . . 4.12 (20 g/L) 20 g 1 L . 4.13 (100 g/L) 100 g 1 L . KS E ISO 13291: 2007 3 4.14 250 g 60 mL ( 1.05 g/L) 1 L . 4.15 EDTA (0.05 mol/L) EDTA(2-Na) 18.6 g 1 L . 4.16 (1 000 g/L) 100 g
5、100 mL . . 4.17 (1 % m/m) 99 g 1 g . 4.18 Fe(NO3)3 9H2O 45 g 1 L . 5 . 5.1 KS L ISO 4787 KS L ISO 385 1, KS L ISO 648, KS L ISO 1042 A KS L ISO 4787 . 5.2 , 25mL 5.3 , 0.1 mg . 5.4 , (1055) . 5.5 , 800 . 5.6 6 6.1 KS E ISO 9599 . ( A ). KS E ISO 13291: 2007 4 6.2 2.5 g 0.1 mg . KS E ISO 9599 . A . 7
6、 7.1 2 . . 7.2 . 2 . 5 mL(4.18) . EDTA Vb . 7.3 300 mL 20 mL 23 mL (4.3) . 5 . (4.4) 15 mL 15 (5.6) . 100 mL . 500 mL . 500 mL . (5.2) 800 (5.5) . (4.7), (4.4), (4.5) 2 mL . 25 mL . . , , . . , (5.5) 600 700 . . (4.7) 2 mL, (4.6) 2 mL (4.5) 2 mL . KS E ISO 13291: 2007 5 . , . 7.4 250 mL 7.3 50 mL .
7、(4.8) (4.6) 5 mL (4.11) 50 mL . (4.9) 80 mL 1 . . 20 mL (4.9) . 400 mL 2 . 2 (4.6) 1 mL (4.10) 70 mL 2 400 mL . 7.5 10 mL (4.12), 10 mL (4.13), 20 mL (4.14), 5 mL (4.16), 0.1 g (4.17) . EDTA (4.15) . Vt . 7.6 EDTA 0.1 % 0.2 % EDTA . . . 7.4 . EDTA . 0.25 g 1.625 g (4.1) 0.000 1 g 3 m1, m2, m3 . (4.1
8、8) 5 mL (4.4) 15 mL, 15 mL . 500 mL . . 7.4 7.5 EDTA V1, V2, V3 . fix . fix: mx/Vxx 13 (1a) fix: mx: (g) Vx: EDTA (mL) fi1, fi2, fi3 0.000 01 g/mL . KS E ISO 13291: 2007 6 . 33i2i1iffff (1b) 8 wZn . HmfVVw100100100)(btZn (2) f : 7.6 (g/mL) H : (m/m% H 0) m : (g) Vb: EDTA (4.15) (mL) Vt: EDTA (4.15)
9、(mL) 9 9.1 . sr 0.000 8 X 0.038 2 (3) sL 0.001 6 X 0.053 9 (4) X : (%m/m) sr: (%m/m) sL: (%m/m) D 9.2 X1, X2 B . 2 :2)(21XXX (5) ( ): sr 0.000 8 X 0.038 2 (3) : r 2.8sr (6) 9.3 2 . . KS E ISO 13291: 2007 7 :22112 (7) : sL 0.001 6 12 0.053 9 (8) : sr 0.000 8 12 0.038 2 (9) :28.22r2LssP (10) : E |1 2|
10、 (11) 1: 1 (m/m%) 2: 2 (m/m%) E P . 9.4 (CRM) . Ac 2 . |c Ac|C (12) . |c Ac| C (13) . c: (m/m%) Ac: (m/m%) C : 9.4.1 (m/m%) 9.4.1 KS A ISO GUIDE 35 . 9.4.1.1 C . 2c22r2LAsnssC (14) s2Ac : n : 9.4.1.2 C . KS E ISO 13291: 2007 8 nssC2r2L2 . 10 . a) b) ( , KS E ISO 13291 ) c) (m/m%) d) e) KS E ISO 1329
11、1: 2007 9 A ( ) A.1 0.05 % 2 % . A.2 (1055) , . A.3 A.3.1 , . A.4 . A.4.1 , 0.1 mg . A.4.2 , , 3 g (20 g ). A.4.3 , (1055) . A.5 A.5.1 (1055) (A.4.3) (A.4.2) 1 (A.3.1) . A.5.2 (A.4.2) . . A.5.3 , , (1055) 2 KS E ISO 13291: 2007 10 . 2 , . 0.1 mg (m4) (m5) 0.1 mg . (1055) 2 (m4) 0.1 mg . m4 m4 0.5 mg
12、 . A.6 m6(g) . m6 m4 m5 m4: (g) m5: (g) . KS E ISO 13291: 2007 11 B ( ) r 9.2 |x1 x2|r |x1 x2|1.2r x1, x2 x3, x4 x4 x3 x1, x2,x3 1.2r x1, x2,x3,x4 1.3r x x1, x2, x3, x4 221xxx3321xxxx44321xxxxxKS E ISO 13291: 2007 12 C ( ) C.1 . C.2 . 0.05 % EDTA . C.3 7 % . C.4 2 % . . C.5 5 % . 0.8 % . C.6 0.2 % .
13、 . C.7 . Al: 2 % Ba: 10 % Cu: 10 % Ni: 1 % As: 0.5 % Ca: 5 % Fe: 15 % Sr: 2 % KS E ISO 13291: 2007 13 D ( ) D.1 9 12 . 11 %(m/m) 62 %(m/m) 5 , KS A ISO 5725 2 . D.2 . 2 (2 ) 2 . D.3 5 , D.1 . D.4 D.1 , D.2 D.3 . (sr, sL, r, p) D.2 , D.2 . KS E ISO 13291: 2007 14 a . D.1 laboratorya a a KS E ISO 1329
14、1: 2007 15 D.1 a 901 902 903 919 9110 Zn %(m/m) 50 33 62 11 55 S %(m/m) 30 30 30 20 31 Fe %(m/m) 10 14 2 8 8 Pb %(m/m) 3 14 1 53 2 Si %(m/m) 2 2 2 1 AI %(m/m) 0.5 0.6 0.3 0.2 0.1 Cu %(m/m) 0.2 0.5 0.1 0.8 0.1 Ca %(m/m) 0.4 0.5 0.3 0.1 0.1 Mg %(m/m) 0.3 0.3 0.2 0.8 0.2 Cd %(m/m) 0.2 0.1 0.2 0.02 0.2
15、As g/t 300 550 250 100 Sb g/t 250 700 300 20 Ag g/t 125 400 60 380 160 Co g/t 40 90 1 60 20 Tl g/t 25 60 1 10 Ni g/t 2 8 2 8 Bi g/t 1 1 1 1 600 1 a90 1 MIM( ) 90 2 MIM( ) 90 3 Polaris( ) 91 9 Cobar( ) 91 10 Hilton( ) KS E ISO 13291: 2007 16 D.2 kok non X r P srsLsL/sr90 1 21 21 80 80 49.445 0.190 0.
16、357 0.067 0.117 1.74 90 2 21 20 80 76 32.812 0.161 0.306 0.057 0.101 1.77 90 3 21 20 80 76 62.105 0.251 0.489 0.089 0.161 1.82 91 9 21 20 80 76 10.845 0.150 0.241 0.053 0.076 1.45 91 10 21 21 80 80 55.435 0.282 0.450 0.100 0.143 1.43 r 0.002 3 X 0.108 0 0.839 0 P 0.004 7 X 0.170 4 0.951 9 sr 0.000 8 X 0.038 2 0.839 0 sL 0.001 6 X 0.053 9 0.958 5 k : ko: n : no: P : , % r : ( ), % sL: , % sr: , % X : , % D.3 Cochran Grubbs 1