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GB/T 5009.152-2003 English PDF (GBT5009.152-2003)
GB/T 5009.152-2003 English PDF (GBT5009.152-2003)
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GB/T 5009.152-2003: Determination of residual acrylonitrile monomer in styrene-acrylonitrile copolymers and rubber-modified acrylonitrile-butadiene-styrene resins and their products used for food packaging
GB/T 5009.152-2003
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 67.040
C 53
Replacing GB/T 17338-1998
Determination of residual acrylonitrile monomer in
styrene-acrylonitrile copolymers and rubber-modified
acrylonitrile-butadiene-styrene resins and their
products used for food packaging
ISSUED ON. AUGUST 11, 2003
IMPLEMENTED ON. JANUARY 1, 2004
Issued by. Ministry of Health of the People's Republic of China;
Standardization Administration Committee.
Table of Contents
Foreword ... 3
Introduction ... 4
1 Scope ... 5
2 Principle... 5
3 Reagents ... 6
4 Apparatus ... 6
5 Analysis steps ... 6
6 Principle... 10
7 Regents ... 11
8 Apparatus ... 11
9 Analysis steps ... 11
Foreword
This Standard replaces GB/T 17338-1998 “Determination of residual
acrylonitrile monomer in styrene-acrylonitrile copolymers and rubber-modified
acrylonitrile-butadiene-styrene resins and their products used for food
packaging”.
This Standard modifies the previous standard structure based on GB/T
20001.4-2001 “Rules for drafting STANDARDs - Part 4. Methods of chemical
analysis”.
This Standard was proposed by and shall be under the jurisdiction of Ministry
of Health of the People's Republic of China.
Drafting organizations of the first method of this Standard. Shanghai Gaoqiao
Petrochemical Co. Chemical Factory, and Shanghai Health and Epidemic
Prevention Station.
Drafting organizations of the second method of this Standard. Shanghai Health
and Epidemic Prevention Station, Guangxi Zhuang Autonomous Region Food
Hygiene Supervision and Inspection, and Shanghai Luwan District Health and
Epidemic Prevention Station.
Main drafters of the first method of this Standard. Wu Keqin, Wang Junfu, Dong
Jianfang and Pan Xihe.
Main drafters of the second method of this Standard. Zhu Yingmin, Shen Wen,
Ye Bisha and Lao Baofa.
The previous standard was issued in 1998 for the first time. This Standard is
the first revision.
Determination of residual acrylonitrile monomer in
styrene-acrylonitrile copolymers and rubber-modified
acrylonitrile-butadiene-styrene resins and their
products used for food packaging
1 Scope
This Standard specifies the method for determination of residual acrylonitrile
monomer in acrylonitrile - styrene copolymers (AS) and acrylonitrile-butadiene-
styrene copolymers (ABS) by headspace gas chromatography (HP-GC).
This Standard is applicable to the determination of residual acrylonitrile
monomer in acrylonitrile-styrene, acrylonitrile-butadiene-styrene resins and
their products, and the determination of residual acrylonitrile monomer in
rubber-modified acrylonitrile-butadiene-styrene resins and their products.
The detection limits of this method. Nitrogen-Phosphorus Detector method
(NPD) is 0.5 mg/kg; Flame Ionization Detector method (FID) is 2.0 mg/kg.
The First Method. Gas Chromatography Nitrogen-
Phosphorus Detector method (NPD)
2 Principle
Place the sample in a headspace bottle. Add acetonitrile solvent that contains
the known amount of internal standard substance. Immediately seal it. After it
is completely dissolved, heat the headspace bottle to make vapor-liquid
equilibrium, and draw headspace in quantification to conduct NPD
determination. Quantify it based on the response value of internal standard
substance.
3 Reagents
3.1 Reagent purity. it shall use analytical reagent. If other grades of reagents
are used, they must have a sufficiently high purity so as not to reduce the
accuracy of determination.
3.2 Solvents. N,N-dimethylformamide or N,N-Dimethylacetamide (DMA). When
conducting chromatography of solvent headspace, there must be no interfering
peaks at retention time of acrylonitrile (AN) and propionitrile (PN).
3.3 Propionitrile. chromatographic grade.
3.4 Acrylonitrile. chromatographic grade.
4 Apparatus
4.1 Gas chromatograph
It shall be equipped with nitrogen-phosphorus detector.
It is better to use the device that can automatically collect and analyze the
headspace, for example, manual collection and analysis of headspace shall be
attached with the following equipment.
4.1.1 Thermostatic bath that can be maintained at 90°C±1°C.
4.1.2 Gas tight syringe used for headspace collection and injection.
4.2 Headspace bottle sealer.
4.3 5.0 mL headspace sampling bottle.
4.4 Aluminum sealing bottle cap.
4.5 Silicone rubber or butyl rubber with good gas tightness of which inner
surface is covered with polytetrafluoroethylene membrane.
5 Analysis steps
5.1 Internal standard calibration
5.1.1 Prepare polymer solvent that contains the known amount of internal
standard substance (PN).
5.1.2 Fill certain amount of the solvent (3.2) in advance into a 100 mL flask.
gasket and aluminum cap, fully shake it to make the polymer in the bottle
completely dissolved or dispersed.
5.3 Gas chromatographic conditions
5.3.1 Chromatographic column. Φ 3mm×4m stainless steel column.
Fill in 101 white test acidic carrier body (60~80 mesh) painted with 15% of
polyethylene glycol-20M.
5.3.2 Temperature
Column temperature. 130°C;
Vaporization temperature. 180°C;
Detector temperature. 200°C.
5.3.3 Gas speed
Carrier gas nitrogen (N2) flow rate. 25 mL/min ~ 30 mL/min.
5.3.4 Other conditions
Nitrogen of 99.95% or greater purity.
Hydrogen shall be dried and purified.
Air shall be dried and purified.
5.4 Determination
Place headspace bottle in a 90°C bath for thermal equilibrium for 50 min. Use
a heated gas syringe to extract 2.0 mL of headspace that has reached to vapor-
liquid equilibrium from the bottle. Immediately inject gas chromatograph to
determine. Operation conditions of gas chromatograph shall be set according
to 5.3. If it uses commodity instrument of automated headspace analysis, it shall
adjust according to the instructions for use of this instrument.
5.5 Result calculation
Calculate the content of residual acrylonitrile in sample (c, mg/kg) according to
equation (5).
7 Regents
7.1 N,N-dimethylformamide (DMF). analytical reagent. There must be no
interfering peaks at retention time of acrylonitrile.
7.2 Acrylonitrile (AN). analytical reagent.
7.3 GDX-102 (60~80 mesh).
7.4 Acrylonitrile standard stock solution. weigh 0.0500 g of acrylonitrile; add
N,N-dimethylformamide to dilute constant volume to 50 mL. Per milliliter of this
storage solution equals to 1.0 mg of acrylonitrile. Store it in the refrigerator.
7.5 Acrylonitrile standard solution. draw 0.2 mL, 0.4 mL, 0.6 mL, 0.8 mL and 1.6
mL of stock solution. Respectively move them to 10 mL flasks. Separately add
N,N-dimethylformamide to dilute constant volume to scale. Well mix it (each
milliliter equals 20 µg, 40 µg, 60 µg, 80 µg and 160 µg of acrylonitrile
respectively).
8 Apparatus
8.1 Gas chromatograph (with flame ionization detector).
8.2 1 mL centered type glass syringe.
8.3 12 mL headspace determination bottle with rubber cover that is coated with
polyvinyl fluoride silicon and aluminum cap.
8.4 Electric heated water bath.
9 Analysis steps
All samples shall be stored in sealing bottle. The prepared sample solution shall
be analyzed within 24h. If it exceeds 24h, it shall report the storage time of
solution.
9.1 Sample processing
Weigh 0.5g~1g (accurate to 0.001 g) of homogeneous sample in headspace
determination bottle. Add 3 mL of N,N-dimethylformamide. Immediately sea...
Get QUOTATION in 1-minute: Click GB/T 5009.152-2003
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GB/T 5009.152-2003: Determination of residual acrylonitrile monomer in styrene-acrylonitrile copolymers and rubber-modified acrylonitrile-butadiene-styrene resins and their products used for food packaging
GB/T 5009.152-2003
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 67.040
C 53
Replacing GB/T 17338-1998
Determination of residual acrylonitrile monomer in
styrene-acrylonitrile copolymers and rubber-modified
acrylonitrile-butadiene-styrene resins and their
products used for food packaging
ISSUED ON. AUGUST 11, 2003
IMPLEMENTED ON. JANUARY 1, 2004
Issued by. Ministry of Health of the People's Republic of China;
Standardization Administration Committee.
Table of Contents
Foreword ... 3
Introduction ... 4
1 Scope ... 5
2 Principle... 5
3 Reagents ... 6
4 Apparatus ... 6
5 Analysis steps ... 6
6 Principle... 10
7 Regents ... 11
8 Apparatus ... 11
9 Analysis steps ... 11
Foreword
This Standard replaces GB/T 17338-1998 “Determination of residual
acrylonitrile monomer in styrene-acrylonitrile copolymers and rubber-modified
acrylonitrile-butadiene-styrene resins and their products used for food
packaging”.
This Standard modifies the previous standard structure based on GB/T
20001.4-2001 “Rules for drafting STANDARDs - Part 4. Methods of chemical
analysis”.
This Standard was proposed by and shall be under the jurisdiction of Ministry
of Health of the People's Republic of China.
Drafting organizations of the first method of this Standard. Shanghai Gaoqiao
Petrochemical Co. Chemical Factory, and Shanghai Health and Epidemic
Prevention Station.
Drafting organizations of the second method of this Standard. Shanghai Health
and Epidemic Prevention Station, Guangxi Zhuang Autonomous Region Food
Hygiene Supervision and Inspection, and Shanghai Luwan District Health and
Epidemic Prevention Station.
Main drafters of the first method of this Standard. Wu Keqin, Wang Junfu, Dong
Jianfang and Pan Xihe.
Main drafters of the second method of this Standard. Zhu Yingmin, Shen Wen,
Ye Bisha and Lao Baofa.
The previous standard was issued in 1998 for the first time. This Standard is
the first revision.
Determination of residual acrylonitrile monomer in
styrene-acrylonitrile copolymers and rubber-modified
acrylonitrile-butadiene-styrene resins and their
products used for food packaging
1 Scope
This Standard specifies the method for determination of residual acrylonitrile
monomer in acrylonitrile - styrene copolymers (AS) and acrylonitrile-butadiene-
styrene copolymers (ABS) by headspace gas chromatography (HP-GC).
This Standard is applicable to the determination of residual acrylonitrile
monomer in acrylonitrile-styrene, acrylonitrile-butadiene-styrene resins and
their products, and the determination of residual acrylonitrile monomer in
rubber-modified acrylonitrile-butadiene-styrene resins and their products.
The detection limits of this method. Nitrogen-Phosphorus Detector method
(NPD) is 0.5 mg/kg; Flame Ionization Detector method (FID) is 2.0 mg/kg.
The First Method. Gas Chromatography Nitrogen-
Phosphorus Detector method (NPD)
2 Principle
Place the sample in a headspace bottle. Add acetonitrile solvent that contains
the known amount of internal standard substance. Immediately seal it. After it
is completely dissolved, heat the headspace bottle to make vapor-liquid
equilibrium, and draw headspace in quantification to conduct NPD
determination. Quantify it based on the response value of internal standard
substance.
3 Reagents
3.1 Reagent purity. it shall use analytical reagent. If other grades of reagents
are used, they must have a sufficiently high purity so as not to reduce the
accuracy of determination.
3.2 Solvents. N,N-dimethylformamide or N,N-Dimethylacetamide (DMA). When
conducting chromatography of solvent headspace, there must be no interfering
peaks at retention time of acrylonitrile (AN) and propionitrile (PN).
3.3 Propionitrile. chromatographic grade.
3.4 Acrylonitrile. chromatographic grade.
4 Apparatus
4.1 Gas chromatograph
It shall be equipped with nitrogen-phosphorus detector.
It is better to use the device that can automatically collect and analyze the
headspace, for example, manual collection and analysis of headspace shall be
attached with the following equipment.
4.1.1 Thermostatic bath that can be maintained at 90°C±1°C.
4.1.2 Gas tight syringe used for headspace collection and injection.
4.2 Headspace bottle sealer.
4.3 5.0 mL headspace sampling bottle.
4.4 Aluminum sealing bottle cap.
4.5 Silicone rubber or butyl rubber with good gas tightness of which inner
surface is covered with polytetrafluoroethylene membrane.
5 Analysis steps
5.1 Internal standard calibration
5.1.1 Prepare polymer solvent that contains the known amount of internal
standard substance (PN).
5.1.2 Fill certain amount of the solvent (3.2) in advance into a 100 mL flask.
gasket and aluminum cap, fully shake it to make the polymer in the bottle
completely dissolved or dispersed.
5.3 Gas chromatographic conditions
5.3.1 Chromatographic column. Φ 3mm×4m stainless steel column.
Fill in 101 white test acidic carrier body (60~80 mesh) painted with 15% of
polyethylene glycol-20M.
5.3.2 Temperature
Column temperature. 130°C;
Vaporization temperature. 180°C;
Detector temperature. 200°C.
5.3.3 Gas speed
Carrier gas nitrogen (N2) flow rate. 25 mL/min ~ 30 mL/min.
5.3.4 Other conditions
Nitrogen of 99.95% or greater purity.
Hydrogen shall be dried and purified.
Air shall be dried and purified.
5.4 Determination
Place headspace bottle in a 90°C bath for thermal equilibrium for 50 min. Use
a heated gas syringe to extract 2.0 mL of headspace that has reached to vapor-
liquid equilibrium from the bottle. Immediately inject gas chromatograph to
determine. Operation conditions of gas chromatograph shall be set according
to 5.3. If it uses commodity instrument of automated headspace analysis, it shall
adjust according to the instructions for use of this instrument.
5.5 Result calculation
Calculate the content of residual acrylonitrile in sample (c, mg/kg) according to
equation (5).
7 Regents
7.1 N,N-dimethylformamide (DMF). analytical reagent. There must be no
interfering peaks at retention time of acrylonitrile.
7.2 Acrylonitrile (AN). analytical reagent.
7.3 GDX-102 (60~80 mesh).
7.4 Acrylonitrile standard stock solution. weigh 0.0500 g of acrylonitrile; add
N,N-dimethylformamide to dilute constant volume to 50 mL. Per milliliter of this
storage solution equals to 1.0 mg of acrylonitrile. Store it in the refrigerator.
7.5 Acrylonitrile standard solution. draw 0.2 mL, 0.4 mL, 0.6 mL, 0.8 mL and 1.6
mL of stock solution. Respectively move them to 10 mL flasks. Separately add
N,N-dimethylformamide to dilute constant volume to scale. Well mix it (each
milliliter equals 20 µg, 40 µg, 60 µg, 80 µg and 160 µg of acrylonitrile
respectively).
8 Apparatus
8.1 Gas chromatograph (with flame ionization detector).
8.2 1 mL centered type glass syringe.
8.3 12 mL headspace determination bottle with rubber cover that is coated with
polyvinyl fluoride silicon and aluminum cap.
8.4 Electric heated water bath.
9 Analysis steps
All samples shall be stored in sealing bottle. The prepared sample solution shall
be analyzed within 24h. If it exceeds 24h, it shall report the storage time of
solution.
9.1 Sample processing
Weigh 0.5g~1g (accurate to 0.001 g) of homogeneous sample in headspace
determination bottle. Add 3 mL of N,N-dimethylformamide. Immediately sea...
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