KS M 0033-2008 General rules for analytical methods in high performance liquid chromatography《高速液体色谱分离法通则》.pdf

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1、 KSKSKSKSKSKSKSK KSKSKS KSKSK KSKS KSK KS KS M 0033 KS M 0033:2008 2008 12 19 http:/www.kats.go.krKS M 0033:2008 : ( ) ( ) ()MPT ( ) : (http:/www.standard.go.kr) : : 1989 12 23 : 2008 12 19 2008-0927 : : ( 025097301) (http:/www.kats.go.kr). 10 5 , . KS M 0033:2008 General rules for analytical method

2、s in high performance liquid chromatography 1 1) . 2 . . ( ) . KS M 0001, KS M 0031, KS M 8458, ( ) 3 3.1 1 . a a . 1 ( ) 3.2 . 1) , . KS M 0033:2008 2 a) . b) . 1) . 2) . 3) . 4) . 5) . 6) . c) , , . d) 5.1 . e) , ( 150 ) . 50 0.5 . 3.3 . a) . b) . , . . 1) 1 mV 10 mV 2) 99 % 2 3) 5 mm/min 4) 0.15

3、% 3.4 . . a) b) c) d) e) f) g) h) 4 2)2) . . KS M 0033:2008 3 , . 5 , 5.1 . a) 18 mm, 0.05 5 m . b) 1 mm , 0.05 5 m . 5.2 5.2.1 1 . 1 m m2/g 20 50 1 20 20 50 20 3 100 , 100 600 5 100 50 100 5 50 3 100 , 3 100 , 5.2.2 2 . 2 meq./g m SO3H NR32 5 5 30 SO3H NR3 NH20.001 0.02 20 50 SO3H NR30.01 0.1 20 50

4、 SO3H NR30.001 0.01 30 50 KS M 0033:2008 4 5.2.3 3 . 3 , , 5.2.4 KS M 8458 , , , , , . 6 6.1 . a) 10 25 , 30 85 % . b) . c) . d) , . e) , 10 % . 100 . 6.2 . a) , , , , . . b) . c) . KS M 0033:2008 5 3). d) , . e) , . . 6.3 . 6.4 6.4.1 . a) (gradient) , , b) c) d) e) 6.4.2 6.4.1 10 1 % . 6.4.3 . 6.4.

5、4 . . 6.4.5 . a) b) c) (L mL) d) e) , (mm) (mm) f) () (Pa) 3) , . KS M 0033:2008 6 g) (mL/min) h) i) j) , (mL/min), k) l) 7 4), 5), 6) . , . a) b) c) d) 8 8.1 , , . 8.2 , . 8.3 . a) 2 (h) , (w) , (A) . . A wh A : w : h : 4) , . 5) 3 % . 6) (S/N) . KS M 0033:2008 7 2 8.4 7) ( ) . , ( ) 3 . 3 ( ) . .

6、8.5 (X) (Mx) (S)8) (Ms) 9) . (Mx) (Ms) sxMM , X (Ax) S (As) sxAA 4 . 7) 3 , 1 , . . 8) , . 9) . h h 2 w ()x KS M 0033:2008 8 4 (m) (n) , . (Ax) (As) ysxAA , (M x) (M s) xsxMM C(%) . . 100=mnxC C : (%) x : m : n : 8.6 A B a1 b1 . W A WA10) , A B a2 b2 . 11baKWWBA= 22baKWWWBAA=+10) WA 12ba 1.2 2.0 . y

7、 xsxAAsxMMKS M 0033:2008 9 WA: A WB: B WA: A K : a1: A b1: B a2: A , A b2: A , B A C(%) . 10011122=WabbaWCA C : A (%) a1: A b1: B a2: A , A b2: A , B WA: A W : A 1 . 2 A WA A , A C(%) . 100112=WaaWCA C : A (%) WA: A a1: A a2: A , A W : A 8.7 8.4 8.6 . . 8.8 %( , , mol), ppm( , ), mg/L, g/m3 . KS M 0

8、033:2008 10 9 ( ) . 11) , . a) ( , , , ) . 1) . 2) . 3) , , Q ( ) , ( ) . (Mi) (Hi) (10). =iiiiiinMHHNNMM iiiiiiiwHMHNMNMM=2nwMMQ = nM : wM : Mi: Ni: Hi: Q : Q 4) , ( 12) . b) , a) 1), 2) (Hi) . 10 . 11) 1.1)()(nwMM . 12) . KS M 0033:2008 11 a) b) , c) 13)d) 1) 2) , 3) ( ) 4) , , , 5) 6) e) . , , .

9、f) 1) 2) 3) , ( , ), , g) 13) ( ) . KS M 0033:2008 12 KS M 0033:2008 . . . 1 . , . 3 3.2 c) . ( 1) 2.94 3.92 MPa . ( ) . ( 2) ( 3) . , , . 6 , . . . KS M 0033:2008 13 1 2 a) b) 3 ( ) ( ) 1 2 34 5 6 6543 21 KS M 0033:2008 14 3.3 a) , , , , , . 4 . a) . b) . c) . d) . e) . 0.45 m . e) . 1) “ ” ( 1 ).

10、KS M 0033:2008 15 1 doah0 a7.0 7.0 0 0 0 0.01 0.50 7.0 6.9 0.5 0.5 0 0.28 0.37 n 7.1 7.1 0 0 0 0.00 0.23 n 7.3 7.3 0 0 0 0.01 0.32 n 7.4 7.4 0 0 0 0.01 0.41 7.4 6.7 2 2 0 0.38 0.23 7.5 7.5 0 3.5 0 0.36 8.1 8.1 0 0 0 0.05 0.47 8.2 8.2 0 0 0 0.04 1.00 8.3 7.3 3 0 0 0.30 0.35 8.6 8.6 0 0.5 0 0.18 0.97

11、8.6 8.2 2 0.5 0 0.38 0.45 8.6 7.0 3 2 0 0.58 0.45 8.7 7.3 4 6.5 0.5 8.8 7.8 3 0 0 0.37 m 8.8 8.8 0 0.5 0 0.26 0.62 0.81 8.9 8.9 0 0.5 0 0.29 0.59 9.1 8.1 3 0.5 0 0.40 0.57 9.1 7.6 4 3 0 0.45 9.2 6.8 4.5 2 0 0.60 0.37 9.2 9.2 0 0.5 0 0.32 0.65 9.3 9.3 0 0.5 0 9.4 6.8 5 2.5 0 0.56 0.32 9.6 6.4 5.5 0.5

12、 0 0.42 0.44 9.6 9.2 2 0.5 0 0.30 0.80 9.7 9.1 2.5 2 1,2 9.7 8.2 4 0 0 0.49 0.79 9.8 9.2 2.5 1 0 9.8 7.8 4 3 0 0.56 1.54 9.9 9.3 2 0.5 0 9.9 9.6 1.5 0.5 0 10.0 10.0 0 0.5 0 0.15 0.37 10.2 7.2 2.5 4 4 0.82 2.3 10.4 9.0 4 5 0 0.71 0.94 10.7 9.2 3.5 1.5 0 11.0 7.3 8 1 0 0.64 0.67 11.1 9.5 4 0.5 0 11.2

13、6.8 4.0 5 5 0.88 1.20 11.4 9.5 11.5 7.9 11.8 6.5 8 2.5 0 0.65 0.37 11.9 11.3 1 0.5 0 12.8 8.4 7.5 5 0 0.6 2.22 12.9 6.2 5 7.5 7.5 0.95 0.60 KS M 0033:2008 16 1 ( ) doah0 1,3 13.0 8.0 8 3 0 13.3 13.5 8.3 14.7 8.0 1.11 19.9 17.9 8.3 21 6.3 : . , . d: S , Cl , Br, I ( , DDT, ) . d .o: ( ) ( , , ) . a:

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