1、 KSKSKSKSKSKSKSK KSKSKS KSKSK KSKS KSK KS KS I ISO 5666 KS I ISO 5666:2011 2011 9 2 http:/www.kats.go.krKS I ISO 5666:2011 : ( ) ( ) ( ) : (ISO/TC147) () ( ) () : (http:/www.standard.go.kr) ： ：2011 9 2 2011-0308 ： ：(ISO/TC147) ( 02-509-7270) (http:/www.kats.go.kr). 10 5 , . KS I ISO 5666:2011 i ii i
2、ii 1 1 2 1 3 1 4 (II) 2 4.1 .2 4.2 2 4.3 .2 4.4 4 4.5 6 4.6 / .6 4.7 .6 4.8 .7 4.9 8 4.10 8 5 8 5.1 .8 5.2 9 5.3 .9 5.4 9 5.5 10 5.6 .10 5.7 .11 5.8 .11 5.9 11 5.10 11 6 .11 A( ) .13 A.1 13 A.2 .13 B( ) .14 B.1 14 B.2 .14 C( ) 15 C.1 15 C.2 15 C.3 15 C.4 15 KS I ISO 5666:2011 ii (0.1 g/L ) , . . . (
3、digestion procedure) , , . , , (mercury-free) . . . KS I ISO 5666:2011 iii 1999 1 ISO 5666, Water quality Determination of mercury , . KS I ISO 5666:2011 Water quality Determination of mercury 1 ( , ) . 4. (II) . 5. . (3. ). 0.1 g/L 10 g/L . . 2 . . ( ) . KS I ISO 5667 1, 1 ： KS I ISO 5667 2, 2 ： KS
4、 I ISO 5667 3, 3 ： 3 , ( , ) (4.4 ). , . , (- ) FEP , . , , , 10 . (background compensation) . 25 . (cuvette) . . 1 KS I ISO 5666:2011 2 , . (II) (sodium tetrahydroborate, NaBH4) . (flow system) , 1 . 1 , mg/L ( ) NaBH4NaBH4SnCl2 0.5 mol/L HCl 5 mol/L HCl + 0.2 g/L Fe(III) 0.5 mol/L HCl Cu(II) Ni(II
5、) Ag(I) IAs(V) Bi(III) Sb(III) Se(IV) 10 1 0.1 100 0.5 0.05 0.5 0.005 10 500 10 10 0.5 0.5 0.5 0.005 500 500 1 0.1 0.5 0.5 0.5 0.005 (II) , . , . 4 () 4.1 1 2 (II) . . 253.7 nm . 4.2 3. . 0.1 mg/L . (5. ) . (II) - , . 4.3 4.3.1 KS I ISO 5666:2011 3 “ ” . 2 . . 4.3.2 , (NHO3) 1.40 g/mL 4.3.3 , (H2SO4
6、) 1.84 g/mL 4.3.4 , (HCl) 1.16 g/mL 4.3.5 50 g (KMnO4) 1 000 mL . 4.3.6 5 g (K2Cr2O7) 500 mL (4.3.2) , 1 000 mL . . 4.3.7 40 g (potassium peroxodisulfate, K2S2O8) 1 000 mL . 4.3.8 10 g (hydroxylammonium chloride, NH4OCl) 100 mL . 4.3.9 (II) 5 g (II) 2 tin(II)chloride dihydrate, SnCl2 2H2O 30 mL (4.3
7、.4) 100 mL . (flow system) ( , 100 mL 0.5 g ) , . (4.6) , 30 . 4.3.10 I, (Hg) 100 mg/L 108.0 mg mercury(II) oxide, HgO (4.3.6) 10 mL , 1 000 mL ( 1 mL 0.1 mg ). I , 1 . 4.3.11 II, (Hg) 1 mg/L (4.3.6) 10 mL I(4.3.10) 10 mL , 1 000 mL KS I ISO 5666:2011 4 ( 1 mL 1 g ). 1 . 4.3.12 (1), (Hg) 100 g/L (4.
8、3.6) 10 mL II(4.3.11) 100 mL , 1 000 mL ( 1 mL 100 ng ). . 4.3.13 (2), (Hg) 50 g/L (4.3.6) 10 mL II(4.3.11) 50 mL , 1 000 mL ( 1 mL 50 ng ). . 4.3.14 . 0.5 g/L 5 g/L 100 mL 6 (2)(4.3.13) 1 mL, 2 mL, 4 mL, 6 mL, 8 mL 10 mL . (4.3.6) 1 mL . . 0.5 g/L, 1 g/L, 2 g/L, 3 g/L, 4 g/L, 5 g/L , , . 4.3.15 1 0
9、00 mL (4.3.6) 10 mL . (batch) , (4.6) . 4.3.16 500 mL 150 mL (4.3.2) , 1 000 mL . 4.4 4.4.1 , (4.3.16) (4.3.1) . 4.4.2 (AAS) , . KS I ISO 5666:2011 5 4.4.3 , . 4.4.4 ( 1 ) 2 cm, 15 cm (borosilicate glass) ( .) ( ) ( ) , 1 L/min2 L/min ( , , ) ( , 3. ) . 100 mL, 250 mL 1 000 mL , , . 1 . 1 , 2 cm, 15
10、 cm 4 , 100 mL, 250 mL 1 000 mL 2 , (1 2) L/min 5 (frit) 3 , 29/32 1 (3. ). 2 , . 1 (II) ( ) 4.4.5 100 mL, 200 mL, 1 000 mL 4.4.6 1 mL, 5 mL, 10 mL KS I ISO 5666:2011 6 , . 4.5 KS I ISO 5667 1, KS I ISO 5667 2 KS I ISO 5667 3 . , , (PSU) - (FEP) . . (4.3.6) 10 mL , 1 000 mL . , pH 1 - . , . 4.6 / .
11、, A, B, C . . (4.5 ) 100 mL ( 1 000 mL) 4.5 . 15 mL (4.3.5) , (4.3.2) 1 mL (4.3.3) 1 mL . 15 , (4.3.7) 10 mL . 95 2 . , , . . . , . (4.3.1) (4.3.6) . (permanganate) , . 4.7 4.7.1 , (4.4.2) . KS I ISO 5666:2011 7 4.6 , (4.3.8) 5 mL( ) . 5 mL . 30 , . , ( , 200 mL) . ( ) . 100 mL 2 mL (II) (4.3.9) . ,
12、 (II) , . ( 1 000 mL) , 5 mL . 1 L/min 2 L/min . . . (4.3.14) (4.3.15) . 4.7.2 . a) 4.3.14 . b) 4.7.1 . c) . 4.7.3 (matrix effect) . . , 1 g/L 50 mL . a) 4 100 mL 50 mL (4.7.1). b) 3 (1)(4.3.12) 0.5 mL, 1.0 mL 1.5 mL ( 1 g/L, 2 g/L 3 g/L). c) 4.7.1 4 . d) (4.3.15) . 4.8 KS I ISO 5666:2011 8 4.8.1 .
13、pMs)(VbVAA-= ： (g/L) A ： As ： b ： (L/g) Vp ： (mL) VM ： (mL) 4.8.2 (4.7.3) . . A=0 . . , . . 4.9 g/L . (Hg) 0.7 g/L (Hg) 2.0 g/L 4.10 . a) b) 4.9 c) d) 5 5.1 1 2 . , . 253.7 nm , KS I ISO 5666:2011 9 . 5.2 3. . , 1 mg/L 0.1 mg/L . 1： 1 (III) , 500 mg/L , 10 mg/L . 5.3 4.3 (II) , . 5.3.1 (NaBH4) 3 g (
14、NaOH) 1 g , 100 mL . . (flow system) , (NaBH4) 0.02 g (NaOH) 0.03 g , 100 mL . . 5.3.2 14 g (III) 9 iron(III) nitrate nonahydrate(Fe(NO)3 9H2O) 100 mL . . 5.4 5.4.1 . 5.4.2 (AAS) , . 5.4.3 , . 5.4.4 2 cm, 15 cm ( .) KS I ISO 5666:2011 10 ( ) ( , 3. ) 100 mL 250 mL (double-necked) , , . 2 . 1 (3. ).
15、2 , . 1 , 2 cm, 15 cm 4 2 5 (100 mL 200 mL 3 ) 2 ( ) 5.5 4.5 . 5.6 4.6 . KS I ISO 5666:2011 11 5.7 5.7.1 a) , (5.4.1 ) . b) 4.6 , (4.3.8) 5 mL( ) . 5 mL . 30 , . c) , ( , 200 mL) . d) 10 mL 0.5 mL (4.3.4) . e) ( ) ( 2 ). f) 10 mL 2.5 mL (5.3.1) , 50 mL 7.5 mL . g) . . h) ( 1 ), 25 mL 25 mL (4.3.4) 0
16、.5 mL (5.3.2) . , 25 mL . i) (4.3.14) (4.3.15) . 5.7.2 4.7.2 . 5.7.3 4.7.3 . 5.8 4.8 . 5.9 4.9 . 5.10 4.10 . 6 1996 1 2 . KS I ISO 5666:2011 12 2 L n NAP % g/L x g/L R g/L VCR% r g/L VCr% % A 21 62 9 0.819 0.831 0.250 0 30.1 0.131 0 15.8 101.5 B 20 59 13 1.474 1.459 0.391 8 26.9 0.185 5 12.7 99.0 C
17、21 68 0 5.732 5.799 1.374 5 23.7 0.574 6 9.9 101.2 () L n NAP % g/L x g/L R g/L VCR% r g/L VCr% % A 13 37 14 0.819 0.737 0.216 5 29.4 0.072 9 9.9 90.0 B 13 36 14 1.474 1.335 0.380 0 28.5 0.194 9 14.6 90.6 C 13 37 14 5.732 5.588 0.835 9 15.0 0.235 9 4.2 97.5 L n NAP % g/L x g/L R g/L VCR% r g/L VCr% % A 8 22 0 0.819 0.991 0.242 4 24.5 0.193 2 19.5 121.0 B 7 21 13 1.474 1.68 0.333 9 19.9 0.169 1 10.1 114.0 C 8 23 0 5.732 6.51 1.304 7 20.0 0.281 1 4.3 113.6 A B C L n NAP (%) x R VCR r VCr KS I ISO 5666:2011 13 A ( )
