犌犅 ! "#!

2015 09 21! 2016 03 21"#!

GB/T5009.17 2003 GB/T5009.17 2003!,"#$%&': ()* ; +,-./0!1, 1 234 ; 56-78 9 1 2:;; (LC AFS) Ⅰ

! 1 "# - <=. -78 >? 9 1 2:;; @< (LC AFS). <=78 >? $%&! $%' (' 2 ) ABCD6E,, D,AB FGH%IJGH%KL M 2N,O ( ) 2%, PQRSTU',8N 2FVWXY N, OY N 8N,W U Z[\ :;,]:;^_ >?M`!,abc9!? 3 *+,-. /:, <A, GB/T6682 3.1 *+ 3.1.1 D(HNO3) 3.1.2 %H(H2O2) 3.1.3 /D(H2SO4) 3.1.4 H %I(KOH) 3.1.5 GH%I(KBH4): 3.2 *+01 3.2.1 Dc9(1+9):?+50mL D, 6 450mL 3.2.2 Dc9(5+95):?+5mL D, 6 95mL 3.2.3 H %Ic9(5g/L): +5.0gH %I, c X1000mL, 3.2.4 GH%Ic9(5g/L): +5.0gGH%I,<5g/L H %Ic9c X1000mL, < 3.2.5 DI Dc9(0.5g/L): +0.05g DIc=100mL Dc9(5+95) 3.2.6 D Y D c9(5+1):?+500ml D,100mL Y D, 1

3.3 % (HgCl2): _ 99% 3.4 01 3.4.1 9(1.00mg/mL): +0.1354gC %,< DI Dc9 (0.5g/L)c X100mL?, X _, c9 _ 1.00mg/mL =4 ;, 2 J C)* c9 3.4.2 9(10μg/mL):3+1.00mL 9(1.00mg/mL)=100mL?,< DI Dc9(0.5g/L) X _,, c9 _ 10μg/mL =4 ;, 2 3.4.3 <9(50ng/mL):3+0.50mL 9(10μg/mL)=100mL?,< 0.5g/L DI Dc9 X _,, c9 _ 50ng/mL, < 4, /:, Dc9(1+4) 24h,<, < 2 4.1 2:;; 4.2 :? 0.1mg 1mg 4.3 [, a 4.4, 4.5 (50 ~300 ) 4.6 E (50 ~200 ) 4.7 5 (23 5.1 *456) 5.1.1 B, AB 5.1.2 B,, < 5.1.3! " #$%B, &,+ ',,,=4 < 5.2 *478 5.2.1 9:;78' + AB0.2g~1.0g( 0.001g),$%B0.5g~2.0gJ9 AB3+1mL~5mL?( 0.001g), =,,6 5mL D ( )* ),+,-./0,1,140 ~160 4h~5h, X, +2-./0,3, +,<4? ),1 E 5J,=80 J 6 2min~5min 7 81 +,,3,%9 X25mL?,<4? 39 :, :9 =? X _, <;; A 2

5.2.2 78' + AB0.2g~0.5g( 0.001g) $%B0.2g~0.8gJ9 AB1mL~3mL =,,6 5mL~8mL D,6)1 (,+, ), T [, <=>, (,?@ABCDEA A.1) +, ),<4? ),3, 1 E 5J,=80 6EJ 6 2min~5min,7 81,+,, 3,%9 X25mL?,<4? 39 :, :9 =? X _, <;; A 5.2.3 78' 5.2.3.1 +1.0g~4.0g( 0.001g)AB, =,% FG,6 HIJ,645mL D 10mL/D, KFG LMN'O% 5, 6 E, W P Q M 6 E,W Q M,6E R2h &6E c9$81,s65ml D,TU R2h,, BV(c, WXY 1J 1,1 5 P620mL,TU6E R10min1,<?, 9,%9,3,%9C =100mL?,< 4? : F G, :9?,6 X _, ; Z A 5.2.3.2 <= ><=? +1.0g~3.0g( 0.001g)AB, =,% FG,6 HIJ,6 7mL /D, P Xc9[1$ 81, 640mL D ' 5.2.3.1 5, 6E ; Z A < 5.2.3.3 @A B1 +1.0g~4.0g( 0.001g), =,% FG,6 HIJ 30mL D 5mL / D, KFG LMN' O % ' 5.2.3.1 5, 6 E ; Z A < 5.2.3.4 C DA +0.5g~2.0g( 0.001g), =,% FG,6 HIJ 30mL D 5mL / D KFG LMN' O % ' 5.2.3.1 5, 6 E ; Z A < 5.2.3.5 E E1 +1.0g~4.0g( 0.001g)\J\, =,% FG,6 HIJ 30mL D,\610mL /D,\ 65mL /D, KFG LMN'O% ' 5.2.3.1 5, 6E ; Z A < 5.3! 5.3.1 1 ]3+50ng/mL < 90.00mL 0.20mL 0.50mL 1.00mL 1.50mL 2.00mL 2.50mL=50mL?,< Dc9(1+9) X _, ^ _= _ 0.00ng/mL 3

0.20ng/mL 0.50ng/mL 1.00ng/mL 1.50ng/mL 2.00ng/mL 2.50ng/mL 5.3.2 *4! `* aab,bu< Dc9(1+9)=B, ci, ab?, AB?, < Dc9(1+9)=B, ci8,s ] AB AB,%9, ; AB =B AB (1) 5.4 F ; 5 Y :240V; P Q R S R:30 ma; 2 % _:300 ; R : 500mL/min; R :1000mL/min 6 (GHIJ AB >? (1) : : 犡 = ( 犮 - 犮 0) 犞 1000 犿 1000 1000 犡 AB >?, J (mg/kgj mg/l); 犮 B9 >?, (ng/ml); 犮 0 9 >?, (ng/ml); AB,%9, (ml); 犞 1000 ai; 犿 AB?, J (gj ml) I (1) 7 KLM AB' 9 20% 8 NO _B B? 0.5g, 25mL, 0.003mg/kg,? 0.010mg/kg $ ' ' 9 ) [\253.7nm ^ 34 < ABC D, J %D, 2 N, ^D % L M, 3,=> 234, _ ]34 >?M`!,/? 10 *+,-. /:, <A, GB/T6682 4

10.1 *+ 10.1.1 D(HNO3) 10.1.2 D(HCl) 10.1.3 %H(H2O2)(30%) 10.1.4 % (CaCl2): 10.1.5 Y DI(KMnO4): 10.1.6 DI(K2Cr2O7): 10.1.7 % (SnCl2 2H2O): 10.2 *+01 10.2.1 Y D I c 9(50g/L): +5.0g Y D I =100mL 8 1,< c X 100mL 10.2.2 Dc9(5+95):?+5mL D, 95mL, 10.2.3 DI Dc9(0.5g/L): +0.05g DIc=100mL Dc9(5+95) 10.2.4 % c9(100g/l): +10g % c=20ml D,90 6E,, % c M,, X100mL,6 J, Q ; CW $ 10.2.5 Dc9(1+9):?+50mL D, 6 450mL 10.3 % (HgCl2): _ 99% 10.4 01 10.4.1 9(1.00mg/mL): +0.1354g %,< DI Dc9 (0.5g/L)c X100mL?, c9 _ 1.00mg/mL =4 ;, J C)* c9 10.4.2 9(10μg/mL):3+1.00mL 9(1.00mg/mL)=100mL?, < DI Dc9(0.5g/L) c9 _ 10μg/mL =4 ;, 10.4.3 <9(50ng/mL):3+0.50mL 9(10μg/mL)=100mL?,< DI Dc9(0.5g/L) c9 _ 50ng/mL, < 11, /:, Dc9(1+4) 24h,<, < 2 11.1 (D W 34 ),J( K 11.2 :? 0.1mg 1mg 11.3 [, a 11.4, 11.5 (200 ~300 ) 11.6 E (50 ~200 ) 11.7 5

12 (23 12.1 *456) C5.1 12.2 *478 12.2.1 9:;78' C5.2.1 12.2.2 78' C5.2.2 12.2.3 78' C5.2.3 12.3 F, E1h, 3 X a N 12.4 1 ]3+ <9(50ng/mL)0.00mL 0.20mL 0.50mL 1.00mL 1.50mL 2.00mL 2.50mL=50mL?,< Dc9(1+9) X _, ^ _= _ 0.00ng/mL 0.20ng/mL 0.50ng/mL 1.00ng/mL 1.50ng/mL 2.00ng/mL 2.50ng/mL 3abc9 ] = W,b, 6 3.0mL L % (100g/L), ),,, P R 1.0L/min JC O, C % =, ci Y ]34, 34 5 3 34=Y DIc9(50g/L), 5 ci =>' 9 ; Z A 3;_? a 12.5 *4! ]3+B9 A 9^5.0mL = W L, ' T12.4 b ; Z A => 3 3;_, abc9 ABc9 >? 13 (GHIJ AB >? (2) : : 犡 = ( 犿 1- 犿 2) 犞 1 1000 犿 1 犞 2 1000 1000 犡 AB >?, J (mg/kgj mg/l); 犿 1 B9?, (ng); (2) 6

犿 2 9?, (ng); 犞 1 AB,%9, (ml); 1000 ai; AB?, J (gj ml); 犿犞 2 B9, (ml) I 14 KLM AB' 9 20% 15 NO _B B? 0.5g, 25 ml, 0.002 mg/kg,? 0.007mg/kg $ &! PQ RST' 16 ) 78 C [ 5mol/L Dc9+, <C18 1,1 R 9= /, a, /;TU'^ % /DI,78 $ D ', GH%I M,O 2:;; O,/? 17 *+,-. /:, <A, GB/T6682 17.1 *+ 17.1.1 7(CH3OH):1 17.1.2 H %K(NaOH) 17.1.3 H %I(KOH) 17.1.4 GH%I(KBH4): 17.1.5 /DI(K2S2O8): 17.1.6 D(CH3COONH4): 17.1.7 D(HCl) 17.1.8 (NH3 H2O) 17.1.9 L D(L HSCH2CH(NH2)COOH): 17.2 *+01 17.2.1 RK (5%7+0.06mol/L D+0.1%L D): +0.5gL D,2.2g D, =500mL?,< c,s6 25mL 7, < X500mL C0.45μm 7

a,= 6 30min < 17.2.2 Dc9(5mol/L):?+208mL D,c= X500mL 17.2.3 Dc910%(!):?+100mL D,c= X1000mL 17.2.4 H %Ic9(5g/L): +5.0g H %I,c= X1000mL 17.2.5 H %Kc9(6mol/L): +24g H %K,c= X100mL 17.2.6 GH%Ic9(2g/L): +2.0gGH%I,<H %Ic9(5g/L)c X1000mL < 17.2.7 /DIc9(2g/L): +1.0g /DI,<H %Ic9(5g/L)c X500mL < 17.2.8 L Dc9(10g/L): +0.1gL D,c=10mL < 17.2.9 7c9(1+1):?+7100mL,6 100mL, 17.3 17.3.1 % (HgCl2), _ 99% 17.3.2 %78 (HgCH3Cl), _ 99% 17.4 01 17.4.1 % 9(200μg/mL, Hg ): +0.0270g %,<0.5g/L DI Dc9c, X100mL =4 ;, J C)* c9 17.4.2 78 9(200μg/mL, Hg ): +0.0250g %78,64?7c, <7c9(1+1) X100mL =4 ;, J C)* c9 17.4.3 <9(1.00μg/mL, Hg ): +0.50mL 78 9 0.50mL % 9, =100mL?, RK _ 1.00μg/mL < X _, <9, % 18, /: Dc9(1+4) 24h,<, < 2 18.1 9 1 2:;; @< (LC AFS):O9 1 (9 1 K=B ) /, a 2:;;!M 18.2 :? 0.1mg 1.0mg 18.3!" 18.4 Y 18.5 # 18.6 P : $ 10000r/min 18.7 19 (23 19.1 *456) C5.1 8

19.2 *4UV +B0.50g~2.0g( X0.001g), =15mL P,6 10mL D c 9 (5mol/L),1 ( ' +60min,% I9 4 ' 8000r/min P 15min 3+2.0mL 5 9X5mL? J _A,&'6 H %Kc9(6mol/L), B9pH 2~7 6 0.1mL L Dc9(10g/L), < X _ 0.45μm a, ; Z A /:'6H %Kc9(6mol/L) &'6, D E?, _ ( Y,)* % +W,,M -. 19.3 F 19.3.1 PQ F 9 1?@AB&': 1 :C18 (\150mm, /4.6mm,J /5μm),C18 ( \10mm, / 4.6mm,J/5μm) R :1.0mL/min =B :100μL 19.3.2 W F 2:;?@AB&': Y :300V; S R:30mA; 2% : 2; 9:10% Dc9; 9R :4.0mL/min; L :2g/L GH%Ic9; L R 4.0mL/min; % :2g/L /DIc9, % R 1.6mL/min; R :500mL/min; R :600mL/min 19.4 1 +5 010 ml?, ] 6 < 9(1.00μg/mL)0.00 ml 0.010 ml 0.020mL 0.040mL 0.060mL 0.10mL,< R K X _ a b c 9 _ ] 0.0ng/mL 1.0ng/mL 2.0ng/mL 4.0ng/mL 6.0ng/mL 10.0ng/mL 3+abc9100μL =B, abc91% _, 1, ABc9 :3ABc9100μL 9 1 2:;; @<, 1, /? > 9I4= 9 c9 ABc9 1?CD EB 20 (GHIJ AB78 >? (3) : 9

犡 = 犳 ( 犮 - 犮 0) 犞 1000 犿 1000 1000 : 犡 AB78 >?, (mg/kg); 犳 2; 犮 C 978 _, (ng/ml); 犮 0 C c978 _, (ng/ml); 6 +A, (ml); 犞 1000 ai; 犿 AB B?, (g) I (3) 21 KLM AB' 9 20% 22 NO _B B? 1g, 10 ml, 0.008 mg/kg,? 0.025mg/kg 10

X Y 犃 78 F 犃.1!"AB [,?@ABC A.1 I 犃.1 CA*4 78 F < 2(1600W)$%/% _/ /min /min 1 50 80 30 5 2 80 120 30 7 3 100 160 30 5 犃.2 34 5AB [,?@ABC A.2 I 犃.2 =? A*4 78 F < 2(1600W)$%/% _/ /min /min 1 50 50 30 5 2 70 75 30 5 3 80 100 30 5 4 100 140 30 7 5 100 180 30 5 11

X Y 犅 犅.1 c91 C B.1 Q 犅.2 AB(6!")1 C B.2 犅.1 Q 犅.2 *4( C)Q 12