KS M 9245-2008 Determination of chlorophenols in industrial products as paint dye《油漆和颜料中氯酚分析方法》.pdf

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1、 KSKSKSKSKSKSKSK KSKSKS KSKSK KSKS KSK KS KS M 9245 KS M 9245:2008 2008 9 30 http:/www.kats.go.krKS M 9245:2008 : ( ) ( ) ()KCC () ( ) ( ( ) : (http:/www.standard.go.kr) ： ：2003 12 26 ：2008 9 30 2008-0616 ： ： ( 02-509-7301) (http:/www.kats.go.kr). 10 5 , . KS M 9245:2008 Determination of chloropheno

2、ls in industrial products as paint, dye , . 1 , , . 10 ppb . 2 . . ( ) . KS M 0001, KS M 0124, ( ) KS M 0126, ( ) KS M 0127, ( ) KS M 1671, (PCP)( ) KS M ISO 8165 1, 1 1： 3 (liquid liquid extraction), (soxhlet extraction), (sonic extraction), (solid phase extraction) (acetic anhydride) N,O-bis-(trim

3、ethylsilyl) acetamide . (ECD： electron capture detector) (GC) / (GC/MS) . mg/kg . (applier) . 4 KS M 9245:2008 2 . 4.1 4.1.1 1 000 g/mL PCP(pentachlorophenol) 10 mg 10 mL . 1 mg/mL 3 18 . 4.1.2 100 g/mL 5 g/mL 1 mL 10 mL (volumetric flask) . 4.1.3 10 g/mL 5 g/mL 1 mL 10 mL . 4.2 4.2.1 2,3,6- 1 000 g

4、/mL 2,3,6- (2,3,6-trichlorophenol) 10 mg 10 mL . 1 mg/mL 3 18 . 4.2.2 2,3,6- 100 g/mL 5 g/mL 1 mL 10 mL . 4.2.3 2,3,6- 10 g/mL 5 g/mL 1 mL 10 mL . 4.2.4 2,3,6- 2 g/mL 10 g/mL 2 mL 10 mL . 4.3 . 5 . KS M 9245:2008 3 1 . 4.4 (acetylation) 35 mL 0.1 M (K2CO3) 5 50 mL . 2 g/mL 5 200 L . 10 g/mL 10 ng/mL

5、, 40 ng/mL, 100 ng/mL, 400 ng/mL, 1 000 ng/mL 5 . 5 mL 1 mL ( 3 , ). . . 4.5 (silylation) 1 mL 10 ng/mL, 40 ng/mL, 100 ng/mL, 400 ng/mL, 1 000 ng/mL . N,O- N,O-bis-(trimethylsilyl)acetamide 200 L . . 5 (ultra sonic extraction) (ultra sonic bath) , . 5.1 5.1.1 0.001 g 5.1.2 40 5.1.3 5.1.4 5.1.5 50 mL

6、, 250 mL 5.1.6 25 L, 100 L, 500 L, 1 000 L 5.1.7 (PTFE： polytetrafluoroethylene) 100 mL 5.1.8 / 5.1.9 (DB 5, ： 2530 m, ： 0.20.32 mm, ： 0.250.33 m) 5.1.10 (glass filter) KS M 9245:2008 4 5.2 5.2.1 (acetic anhydride) 5.2.2 (acetone) 5.2.3 (n-Hexane) 5.2.4 (ultrapurified water) 5.2.5 0.1 M (sodium phos

7、phate 0.1 M solution) pH 9 10 5.2.6 (potassium carbonate) 0.1 M 5.2.7 (sodium sulphate, anhydrous) 5.2.8 (pentachlorophenol) 5.2.9 2,3,6- 2,3,6-trichlorophenol(TCP) 5.2.10 , 10 g 5.2.11 (celite) 5.2.12 1 M 5.3 10 g(0.1 g) . 1 ppm 1 mL 20 mL 24 . 5.4 100 mL 1： 1(v/v) 2 . 100 m . 10 g . 20 mL 2 . 0.1

8、M 50 mL 250 mL . n- 40 mL . 30 mL . 1 M 10 mL pH 1 2 . 50 mL n- . 50 mL . n- 5 mL . KS M 9245:2008 5 5.5 (acetylation) 50 mL 0.1 M 35 mL 3 . 1 mL ( ). 3 . . 24 . 6 (SPE： solid phase extraction) , PCP . 6.1 6.1.1 0.001 g . 6.1.2 6.1.3 5 % (phenyl column), 3 mL, 500 mg 6.1.4 6.1.5 6.1.6 6.1.7 6.1.8 25

9、 L, 100 L, 500 L, 1 000 L 6.1.9 (PTFE： polytetrafluoroethylene) 100 mL 6.1.10 / 6.1.11 (DB 5, ： 2530 m, ： 0.20.32 mm, 0.250.33 m) 6.1.12 6.1.13 KS M 9245:2008 6 1 6.2 6.2.1 (acetic anhydride) 6.2.2 N,O- N,O-bis-(trimethylsilyl) acetamide 6.2.3 (ultrapurified water) 6.2.4 (methanol) 6.2.5 (n-Hexane)

10、6.2.6 0.1 M (potassium carbonate) 6.2.7 (sodium sulphate, anhydrous) 6.2.8 (pentachlorophenol) 6.2.9 2,3,6- 2,3,6-trichlorophenol(TCP) 6.2.10 1 M 6.3 10 g 200 mL . 100 6 0.45 m . 10 g . 2 ppm 200 L . 1 M 10 mL . 6.4 6.4.1 (conditioning) KS M 9245:2008 7 2 mL 0.1 M . 6.4.2 (concentration) 10 15 in Hg

11、 23 mL/min . 5 mL ( 510 ). 6.4.3 (elution) 10 mL . 6.5 (acetylation) 50 mL 0.1 M 35 mL 3 . 1 mL ( ). 3 . . 24 . 6.6 (silylation) 5 mL 1 mL . 200 L N,O- N,O-bis-(trimethylsilyl)acetamide . 7 (soxhlet extraction) 7.1 7.1.1 7.1.2 7.1.3 (cellulose thimble) 7.1.4 7.1.5 7.1.6 7.1.7 25 L, 100 L, 500L 7.1.8

12、 polytetrafluoroethylene(PTFE) 100 mL 7.1.9 / (GC/MS) KS M 9245:2008 8 7.1.10 (DB 5, ： 2530 m, ： 0.20.32 mm, ： 0.250.33 m) 7.2 7.2.1 (n-Hexane) 7.2.2 (acetone) 7.2.3 N,O- (N,O-bis-(trimethylsilyl)acetamide) 7.2.4 7.2.5 7.2.6 2,3,6- 2,3,6-trichlorophenol(TCP) 7.2.7 , 7.3 , 10 g . 100 mL 6 . 5 mL 1 mL

13、 200 L N,O- . . 8 (liquid liquid extraction) . 8.1 (salt) . . / . mg/kg . 8.2 8.2.1 250 mL 8.2.2 8.2.3 8.2.4 KS M 9245:2008 9 8.2.5 8.2.6 / (GC/MS) 8.2.7 (DB 5, ： 25 30 m, ： 0.2 0.32 mm, ： 0.25 0.33 m) 8.2.8 0.001 g 8.2.9 8.3 8.3.1 (n-Hexane) 8.3.2 (sulphuric acid) 8.3.3 (acetic anhydride) 8.3.4 0.1

14、 M (potassium carbonate solution) 8.3.5 (vat dye) 8.3.6 2,3,6- (2,3,6-trichlorophenol) 8.4 10 g 50 mL . 30 mL . 30 mL 3 . 5 mL . 0.1 M 35 mL 200 L . 1 mL . . 9 PCP . PCP / . ppb GC/MS SIM . . 9.1 / (gas chromatograph/mass spectrometer) 1 L 250 350 KS M 9245:2008 10 1 mL/min 20 /min 50 180 2 2 /min 2

15、00 1 20 280 5 9.2 / (selected ion monitoring) (retention time) . 266, 308 323, 338 . 9.3 (pulsed discharge electron capture detector) 1 L 300 320 1 mL/min 20 /min 100 200 1 , 2 /min 300 10 . 9.4 . 9.5 . Ar Mr . istPCPristPCPrMMMAAA= APCP ： Aist ： MPCP ： (g) Mist ： (g) (f ) . . KS M 9245:2008 11 isti

16、stistPCPAMAMf= Aist ： MPCP ： (g) Mist ： (g) 9.6 APCP . Aist . . istsistPCPPCPAMMAfC= CPCP ： (mg/kg) f ： Mist ： (g) Ms ： (g)( 10 g) APCP ： Aist ： 9.7 . . . 10 % . . . . 9.8 ( ) . . ( , , , , ) . . . . . KS M 9245:2008 12 A ( ) . g/kg 1 2 3 KS M 9245:2008 13 B () Level Response Factor 1 2 3 4 5 12 20

17、62 240 589 1 4 12 54 149 0.01 0.04 0.10 0.40 1.00 0.00078762 0.00198150 0.00158996 0.00166446 0.00169728 0.000000 0.001692* R-square 0.999778 Average Response Factor 0.00078762 Response Factor /Absolute KS M 9245:2008 14 C ( ) C.1 C.2 KS M 9245:2008 15 D () 1 Soil quality Determination of selected p

18、henols and chlorophenols Gas chromatographic method, DRAFT INTERNATI ONAL STANDARD ISO/DIS 14154(2000) 2 Win, T., Determination of pentachlorophenol(PCP) in wood. Federal Institute for Mechanical and Chemical Testing(BAM), Berlin, Germany, pp. 46 47(2001) 3 Quantitative determination of pentachlorop

19、henol in wood, CEN/TC 38/WG 26 N 67A 4 Pulp, paper and board Determination of pentachlorophenol, DRAFT INTERNATIONAL STANDARD ISO/DIS 15320(2001) 5 L. J. Fitzpatrick et al., Pressurised liquid extraction of pentachlorophenol from dyestuffs and cotton, J. chromatogr. A, 873(2), 287 291(2000) 6 Hans E

20、. A. and M. van langeveld, Determination of pentachlorophenol in Toy Paints, J. AOAC, 58(1), 19 22(1975) 135513 7017 (02)60094114 (02)600948878 http:/ KS M 9245:2008 KSKSKS SKSKS KSKS SKS KS SKS KSKS SKSKS KSKSKS Determination of chlorophenols in industrial products as paint, dye ICS 71.080.90 Korean Agency for Technology and Standards http:/www.kats.go.kr