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GB 31604.39-2016 English PDF (GB31604.39-2016)

GB 31604.39-2016 English PDF (GB31604.39-2016)

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GB 31604.39-2016: National Food Safety Standard -- Food Contact Materials and Articles -- Determination of Polychlorobiphenyls (PCBs) in Food Contact Paper

This Standard specifies using the gas chromatography and gas chromatography-mass spectrometry to determine the polychlorobiphenyls in food contact paper. This Standard first method is gas chromatography, the second method is gas chromatography-mass spectrometry; both of which are applicable to determine 8 polychlorobiphenyls in the various food contact papers.
GB 31604.39-2016
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
National Food Safety Standard - Food Contact Materials
and Articles - Determination of Polychlorobiphenyls
(PCBs) in Food Contact Paper
ISSUED ON. OCTOBER 19, 2016
IMPLEMENTED ON. APRIL 19, 2017
Issued by. National Health and Family Planning Commission of PRC
3. No action is required - Full-copy of this standard will be automatically & immediately delivered to your EMAIL address in 0~60 minutes.
Table of Contents
Foreword ... 3
1 Scope .. 4
2 Principle ... 4
3 Reagents and Materials .. 4
4 Instruments and Equipment .. 6
5 Analytical Procedures ... 6
6 Expression of Analytical Results ... 8
7 Precision ... 8
8 Others ... 8
9 Principle ... 9
10 Reagents and Materials ... 9
11 Instrument and Equipment ... 10
12 Analytical Procedures .. 10
13 Expression of Analytical Results ... 12
14 Precision ... 12
15 Others ... 12
Appendix A Relevant Information on 8 PCBs and Internal Standard Substance ... 13
Appendix B Gas Chromatogram of 8 PCBs and Internal Standard Substance
Standard Solution ... 14
Appendix C Characteristic Ions of 8 PCBs and Internal Standard Substance 15 Appendix D Gas Chromatography-Mass Spectrometry Total Ion
Chromatogram of 8 PCBs and Internal Standard Substance Standard Solution ... 16
Foreword
This Standard replaces SN/T 2200-2008 Food Contact Materials ?€? Pulp, Paper and Board ?€? Determination of 7 Specified Polychlorinated Biphenyls (PCBs).
Compared with SN/T 2200-2008, this Standard has the major changes as follows. --- Modify the standard name into ?€?National Food Safety Standard ?€? Food Contact Materials and Articles ?€? Determination of Polychlorobiphenyls (PCBs) in Food Contact Paper?€?.
--- Increase the determination types of polychlorobiphenyls (increase PCB 118). --- Modify the pre-treatment procedures.
National Food Safety Standard - Food Contact Materials
and Articles - Determination of Polychlorobiphenyls
(PCBs) in Food Contact Paper
1 Scope
This Standard specifies using the gas chromatography and gas chromatography-mass spectrometry to determine the polychlorobiphenyls in food contact paper. This Standard?€?s first method is gas chromatography, the second method is gas chromatography-mass spectrometry; both of which are applicable to determine 8 polychlorobiphenyls in the various food contact papers.
The First Method of Gas Chromatography
2 Principle
Polychlorobiphenyls (PCBs) in monolayer food contact paper are extracted through water-bath shaking of n-hexane-dichloromethane mixed solution or extracted by accelerated solvent extractor; polychlorobiphenyls (PCBs) in composite food contact papers are extracted by accelerated solvent extractor. After the extracting solution is concentrated, through the concentrated sulfuric acid solution treatment, it shall be detected by the gas chromatograph equipped with electronic capture detector; use internal standard method to quantify.
3 Reagents and Materials
Unless otherwise is specified, the reagents used in this method are analytically pure; while the water is Class-I water stipulated in GB/T 6682.
3.1 Reagents
3.1.1 N-hexane (C6H14). chromatographic pure.
3.1.2 Dichloromethane (CH2Cl2).
3.1.3 Acetonitrile (CH3CN). chromatographic pure.
3.1.4 Concentrated sulfuric acid (H2SO4). guarantee reagent.
3.2 Reagents preparation
3.2.1 N-hexane-dichloromethane mixed solution (1+1). weigh 100mL of n-hexane and 100mL of dichloromethane; mxi evenly.
3.3 Standard substance
2, 2?€?, 5-trichlorobiphenyl (PCB18); 2, 4, 4?€?- trichlorobiphenyl (PCB 28); 2, 2?€?, 5, 5?€?- tetrachlorobiphenyl (PCB 52); 2, 2?€?, 4, 5, 5?€?-pentachlorobiphenyl (PCB 101); 2, 3?€?, 4, 4?€?, 5- pentachlorobiphenyl (PCB 118); 2, 2?€?, 3, 4, 4?€?, 5?€?-hexachlorobiphenyl (PCB 138); 2, 2?€?, 4, 4?€?, 5, 5?€?- hexachlorobiphenyl (PCB 153); 2, 2?€?, 3, 4, 4?€?, 5, 5?€?-heptachlorobiphenyl (PCB 180); internal standard substance 2, 2?€?, 3, 3?€?, 4, 4?€?, 5, 5?€?, 6, 6?€?- decachlorobiphenyl (PCB 209). purity of all standard substances is ???98%; or the standard substances that are approved by the state or awarded standard substance certificate by the state. Relevant information on the 8 polychlorobiphenyls (PCBs) and internal standard substance can refer to Table A.1.
3.4 Preparation of standard solution
3.4.1 PCBs and internal standard substance standard stock solution. accurately weigh appropriate amount of PCBs standard substances; use n-hexane to prepare into the solution with concentration of 200mg/L, respectively; seal and store at -18??C; the shelf life is 12 months.
3.4.2 Mixed standard working solution. separately and accurately pipette 8 PCBs standard stock solutions; use n-hexane to gradually dilute into the 1.00mg/L mixed standard working solution; seal and store at -18??C; the shelf life is 3 months. 3.4.3 Internal standard substance working solution. accurately pipette appropriate amount of internal standard substance (PCB 209) standard stock solution; use n- hexane to prepare into the solution with concentration of 1.00mg/L; seal and store at - 18??C; the shelf life is 3 months.
3.4.4 Mixed standard series solution. pipette appropriate amount of mixed standard working solution and internal standard substance working solution; use n-hexane to prepare into the mixed standard series solutions (the concentration of internal standard substance is 0.050mg/L) with concentration of 0.0050mg/L, 0.010mg/L, 0.025mg/L, 0.050mg/L, 0.100mg/L and 0.200mg/L. It shall be prepared for current use. 3.5 Materials
3.5.1 Nylon filter. 0.22??m.
3.5.2 Diatomaceous earth carrier G. excellent grade; CAS No. of 68855-54-9; heat for 4h in the 400??C muffle furnace before use, then prepare for later-use. The Second Method of Gas Chromatography ?€? Mass Spectrometry
9 Principle
Polychlorobiphenyls (PCBs) in monolayer food contact paper are extracted through water-bath shaking by adopting the n-hexane-dichloromethane mixed solution or extracted by accelerated solvent extractor; polychlorobiphenyls (PCBs) in composite food contact papers are extracted by accelerated solvent extractor. After the extracting solution is concentrated, through the concentrated sulfuric acid solution treatment, it shall be detected by the gas chromatograph-mass spectrometry; use internal standard method to quantify.
10 Reagents and Materials
Unless otherwise is specified, the reagents used in this method shall be analytically pure; while the water is Class-I water stipulated in GB/T 6682.
10.1 Reagents
10.1.1 N-hexane (C6H14). chromatographic pure.
10.1.2 Dichloromethane (CH2Cl2).
10.1.3 Acetonitrile (C6H14) [here translator notes it shall be (CH3CN)]. chromatographic pure.
10.1.4 Concentrated sulfuric acid (H2SO4). guarantee reagent.
10.2 Preparation of specimen
10.2.1 N-hexane-dichloromethane mixed solution (1+1, volume ratio). weigh 100mL of n-hexane and 100mL of dichloromethane, mix evenly.
10.3 Standard substance
2, 2?€?, 5-trichlorobiphenyl (PCB 18); 2, 4, 4?€?-trichlorobiphenyl (PCB 28), 2, 2?€?, 5, 5?€?- tetrachlorobiphenyl (PCB52); 2, 2?€?, 4, 5, 5?€?-pentachlorobiphenyl (PCB 101); 2, 3?€?, 4, 4?€?, 5-pentachlorobiphenyl (PCB 118); 2, 2?€?, 3, 4, 4?€?, 5?€? -hexachlorobiphenyl (PCB 138); 2, 2?€?, 4, 4?€?, 5, 5?€?-hexachlorobiphenyl (PCB 153); 2, 2?€?, 3, 4, 4?€?, 5, 5?€?-heptachlorobiphenyl (PCB 180); internal standard substance (13C12-PCB 209). the purity of all standard substances is ???98%, or the standard substances approved by the state or awarded standard substance certificate by the state; relevant information on 8 PCBs and internal standard substance can refer to Table A.1.
10.4 Preparation of standard solution
The operation is the same as 5.1.
12.2 Preparation of specimen
The operation is the same as 5.2.
12.3 Extraction
12.3.1 Water bath oscillation extraction (applicable to the monolayer food contact paper)
Take about 2g (accurate to 0.01g) of sample into 50mL stopper glass centrifuge tube; after adding 100??L of 13C12-PCB209 internal standard substance working solution (1.00mg/L), the following operation is the same as 5.3.1.
12.3.2 Accelerated solvent extraction (applicable to the monolayer food contact paper and composite food contact paper)
Take about 2g (accurate to 0.01g) of sample; after adding 100??L of 13C12-PCB209 internal standard substance working solution (1.00mg/L), the following operation is the same as 5.3.2.
12.4 Purification
The operation is the same as 5.4.
12.5 Determination
12.5.1 Reference conditions of gas chromatography-mass spectrometry
a) Chromatographic column. 5% phenyl-methyl polysilane packing capillary column; column length is 30m, inner diameter is 0.25mm, film thickness is 0.25??m. b) Inlet temperature. 280??C.
c) Temperature-rise procedures. the starting temperature is 90??C; it rises to 200??C at 15??C/min, maintain for 5min; then rise to 250??C at 2.5??C/min, maintain for 2min; finally rise to 290??C at 20??C/min, maintain for 5min.
d) Ion source temperature. 230??C.
e) Ion source voltage. 70 eV.
f) Carrier gas. high-purity nitrogen (purity???99.999%), 1.0mL/min.
g) injecting volume. splitless mode, 1.0??L.
h) The characteristic ions of 8 PCBs and the internal standard substance (13C12- PCB209) can refer to Table C.1.

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