KS I ISO 11262-2009 Soil quality－Determination of cyanide《土质 总氰化物的测定》.pdf

1、 KSKSKSKS KSKSKSK KSKSKS KSKSK KSKS KSK KS KS I ISO 11262 KS I ISO 11262 :2009 2009 12 18 http:/www.kats.go.krKS I ISO 11262:2009 : ( ) ( ) ( ) : (ISO/TC190) () ( ) ( ) : (http:/www.standard.go.kr) ： ：2004 8 31 ：2009 12 18 2009-0830 ： ：(ISO/TC190) ( 02-509-7266) (http:/www.kats.go.kr). 10 5 , . KS I

2、 ISO 11262:2009 Soil qualityDetermination of cyanide 2003 1 ISO 11262, Soil qualityDetermination of cyanide , . . ( ) . 7. . (fume hood) , . . “ ” “ ” . , . 1 . . , . 0.5 mg/kg 10 000 mg/kg . . a) ： 0.5 mg/kg 50 mg/kg . b) ： 50 mg/kg . 2 . . ( ) . KS I ISO 9297, () KS I ISO 11465, () KS I ISO 14507,

3、 KS M ISO 3696, ISO 4793, Laboratory sintered(fritted) filtersPorosity grading, classification and designation KS I ISO 11262:2009 2 3 . 3.1 pH 4 7.4.2 (free cyanide method) (significantly) . 7.4.3 . . . 3.2 7.4.3 (HCN ) 3.3 . 4 pH 4 . . . . (II) (II) . . T (8. ). -4- 1,3- , 600 nm . (9. ). Ag(CN) 2

4、 5 -() rhodanine . Ag CN AgCN AgCNCN Ag(CN) 2 Ag Ag(CN) 2 AgAg(CN) 2 AgAg(CN) 2 rhodanine 5 , KS M ISO 3696 2 . 3 . KS I ISO 11262:2009 3 5.1 5.1.1 (orthophosphoric acid), -(H 3 PO 4 ) w85 %(), 1.69 g/mL 5.1.2 (sodium hydroxide solution), c(NaOH)1 mol/L NaOH 40 g 1 000 mL . . 5.1.3 (hydrochloric aci

5、d solution), c(HCl)1 mol/L 83 mL w37 %(), 1.18 g/mL 1 000 mL . 5.1.4 zinc(II) sulfate solution, 7 (ZnSO 4 7H 2 O) 100 g 1 000 mL . 5.1.5 (buffer solution), pH 4.00.2 C 8 H 5 KO 410.2 g 1 000 mL . 10 . 5.1.6 (phenolphthalein solution) 0.03 g 100 mL . 5.1.7 Tin(II) chloride solution (II)(SnCl 2 2H 2 O

6、) 5 g 5.1.3 100 mL . . 5.1.8 copper(II) sulfate solution (CuSO 4 5H 2 O) 200 g 1 000 mL . 5.2 5.2.1 , c(NaOH)0.8 mol/L NaOH 32 g 1 000 mL . . 5.2.2 (glacial acetic acid), 20 %() ( 1.049 g/mL) 100 mL 500 mL . 100 % ( 1.049 g/mL), 96 % ( 1.06 g/mL) . 5.2.3 T(N-chloro-4-methylbenzenesulfonamide sodium

7、salt solution) T(C 7 H 7 ClNNaO 2 S3H 2 O) 0.5 g 50 mL . . 5.2.4 (colour reagent) KS I ISO 11262:2009 4 7.0 g 500 mL . 1,3-dimethylbarbituric acid(C 6 H 8 O 3 N 2 ) 16.8 g, 4-pyridine carboxylic acid isonicotinic acid(C 6 H 5 NO 2 ) 13.6 g 1 000 mL . 30 8 m . 10 1 , ( 8 m) . 5.2.5 (potassium cyanide

8、 standard solution), 100 mg/L . (KCN) 250 mg 0.8 mol/L (5.2.1) , 1 000 mL . 0.01 mol/L (5.3.1) , (9. ). 10 . 5.2.6 , 10 mg/L . 10 mL (5.2.5) 100 mL , 0.8 mol/L (5.2.1) . . 5.2.7 p-(p-nitrophenol), 0.1 %() 0.1 g p- 100 mL . 5.3 5.3.1 (silver nitrate solution), c(AgNO 3 )0.01 mol/L 1.689 7 g 400 mL ,

9、1 000 mL . 2 KS I ISO 9297 0.01 mol/L . . 5.3.2 , c(AgNO 3 )0.001 mol/L 0.01 mol/L (5.3.1) . 250 mL 0.01 mol/L 25 mL , 250 mL . . 5.3.3 (indicator solution) 5 -(4-dimethylaminobenzylidene) rhodanine 0.02 g , 100 mL . , . 6 . 6.1 1 . (9) , KS I ISO 11262:2009 5 500 mL ( 29/32 , 19/24 ). (Liebig) (3)(

10、 16 cm, 30 mm), 50 mL (5), (7) . (2)( 20 cm, 2.5 cm) (1) . (2) . ( 15 cm, 1.3 cm) , HCN ( ) ISO 4793 P 160 No. 2 (4) . (f r ) , (total cyanide) . (8.4 9.3 ) . 6.2 1 30 L . . (Drechsel) ( 1 6) ( 1 13) . HCN . (flowmeter, 1 12) 10 L/h 20 L/h (flow rate) . . . . 1 8 2 9 500 mL 3 3 10 4 (glass frit sint

11、er) 11 5 12 6 13 7 a 1 KS I ISO 11262:2009 6 6.3 , 600 nm (optical path length) 10 mm 6.4 6.5 , 10 mL 6.6 7 7.1 pH 4 . C . . / / . (, ) . . D . 7.2 . 10 , . 48 . 3 , 4 . 7.3 7.3.1 (field-moist sample) . , 2 . 7.3.2 KS I ISO 14507 . KS I ISO 14507 8.2 . 7.3.3 . . , . KS I ISO 11464 KS I ISO 14507 . 7

12、.3.4 KS I ISO 11262:2009 7 KS I ISO 11465 . (8.4 9.3 ). 7.4 7.4.4 . 7.4.1 pH (7.3) 10 g (200 mL) , 100 mL 1 . (5.1.6) 0.5 mL . (5.1.3) (5.1.2) pH 8.00.2 . . (hood) . pH pH . 7.4.2 (5.1.5) pH 4.00.2 . . C . (5.1.2) 40 mL ( 1 2) . ( 1 6) (5.1.2) 100 mL . (7.3) 10 g 100 mL . 1 . . . 7.4.1 . ( 1 5) (5.1

13、.4) 10 mL pH 4.00.2 (5.1.5) 50 mL . 2 mL 3 mL . 1 . (HCN) ( 1 2) ( 1 13) 15 L/h (6.2 ). (605) ( 1 5) ( 1 9) (partial vacuum) . ( 1 2 6) ( 1 9) . ( ) , 5 mL . , 50 mL . 10 . . KS I ISO 11262:2009 8 7.4.3 40 mL (5.1.2) ( 1 2) . , (II) (5.1.8) 10 mL 2 mL (II)(5.1.7) . . . ( 1 2) ( 1 13) 15 L/h (6.2 ).

14、(5.1.1) 20 mL , 6 mL . 2 mL 3 mL . , (12010) . ( 5 mL ). 2 7.4.2 ( .) ( ) , 5 mL . , 50 mL . 10 . 7.4.4 (distillation of total cyanide) 40 mL (5.1.2) ( 1 2) (7.3) 10.0 g , 160 mL 7.4.3 “ , ” . 7.5 7.4 . 10 mL . 8 8.1 0.002 mg 0.020 mg 20 mL . 0.8 mol/L NaOH(5.2.1) 20 mL . 10 mL 0.8 mol/L NaOH(5.2.1)

15、 10 mL 20 mL . 8.2 7.4.2 7.4.3, 7.4.4 . 20 mL 50 mL p-(5.2.7) 2 . (mixing) 20 %() (5.2.2) p- . -T (5.2.3) 2 mL . (51) . (5.2.4) 6 mL . KS I ISO 11262:2009 9 . 10 mm 606 nm . 50 mL , 0.8 mol/L (5.2.1) 20 mL . . (205) ( ). (7.5) . 8.3 10 mg/L (5.2.6) 0 mL, 2.5 mL, 5 mL, 10 mL, 20 mL, 25 mL 250 mL 6 .

16、0.8 mol/L (5.2.1) . 8.2 . (mg) . . . 8.4 (7.3 ) . , (stone) . (mass fraction) (1) mg/kg . r 2 c 1 b a CN 000 1 ) ( f m V f V m m w (1) w CN ：(105 ) , KS I ISO 11465 (mg/kg) m a ： (mg), m b ： (mg) V 1 ： (mL)( 50 mL) V 2 ： (mL)( 20 mL) m ： (g)( 10 g) f c ： f c (100 %)/100 f r ： found known r m m f KS

17、I ISO 11465( 1 ) kg mg . KS I ISO 11262:2009 10 1 , w CN mg/kg 0.5 w CN 10 0.5 mg/kg 10 w CN 100 1.0 mg/kg 100 w CN 1 000 10 mg/kg 1 000 w CN 10 000 100 mg/kg KS I ISO 11464 . 9 9.1 0.05 mg 5 mg , . 9.2 7.4.2, 7.4.3 7.4.4 . 50 mL 20 mL (V 2 ) 0.1 mL (5.3.3) . (5.3.2) . . 0.001 mol/L 10 mL 0.01 mol/L (5.3.1) . 10 mL . (7.5) 20 mL . 0.001 mol/L (5.3.2) 0.16 mL, 0.4 mL . 10 g 2 mg/kg 5 mg/kg . 9.3 (7.3 ) . , . (2) mg/kg . r 2 c 1 b a CN ) ( f m V f V f V V w