GB/T 39181-2020 English PDF (GB/T39181-2020)

GB/T 39181-2020: Consumer products - Polyester fiber and ABS material - Rapid determination method of fragrance allergens
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GB/T 39181-2020
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 13.120
Y 41
Consumer products - Polyester fiber and ABS material
- Rapid determination method of fragrance allergens
消费品 聚酯纤维及 ABS材质
ISSUED ON: OCTOBER 21, 2020
IMPLEMENTED ON: OCTOBER 21, 2020
Issued by: State Administration for Market Regulation;
Standardization Administration of the PRC.
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Principle ... 4 
3 Reagents or materials ... 4 
4 Apparatus ... 5 
5 Samples ... 5 
6 Analytical procedure ... 6 
7 Data processing ... 8 
8 Method quantification limit ... 9 
9 Recovery rate and precision ... 9 
10 Test report ... 10 
Appendix A (Normative) Analysis parameters of 54 fragrance materials ... 11 
Appendix B (Informative) Total ion chromatogram of 54 fragrance materials . 13 
Appendix C (Informative) Statistical data of precision test obtained from
laboratory ... 14 
Consumer products - Polyester fiber and ABS material
- Rapid determination method of fragrance allergens
1 Scope
This Standard specifies the determination method of headspace gas
chromatography-mass spectrometry for 54 kinds of fragrance allergens in
consumer product polyester fiber and acrylonitrile-butadiene-styrene (ABS)
material.
This Standard applies to the rapid determination of the content of 54 kinds of
fragrance allergens in consumer product polyester fiber and ABS material.
2 Principle
CUT the polyester fiber into a headspace bottle; ADD a small amount of organic
solvent. After crushing the ABS, use solvent dissolution-precipitation method to
extract; PLACE the extracted trace solution into the headspace bottle. SET the
headspace parameters. The fragrance in the sample volatilizes and quickly
forms a dynamic equilibrium in the bottle (polyester fiber sample); or all is
transferred to the headspace (ABS sample). At this time, the concentration of
the fragrance in the headspace gas is proportional to its initial content in the
sample. Introduce the headspace gas to the gas chromatograph-mass
spectrometer for determination. By measuring the concentration of fragrances
in the headspace gas, the content of fragrances in the sample can be obtained.
3 Reagents or materials
3.1 Acetone: Chromatographically pure.
3.2 Methanol: Chromatographically pure.
3.3 Fragrance reference materials: The purity is all greater than 90%. The
material types are shown in Appendix A.
3.4 Single standard stock solution: Respectively weigh the appropriate amount
of fragrance reference materials (3.3) accurately; USE acetone to prepare a
single standard solution of appropriate concentration; STORE it in a refrigerator
at 4 °C. The expiry date is 12 months.
FREEZE and crush the sample to a particle size of less than 1 mm; WEIGH 0.2
g (accurate to 0.1 mg) into a 20 mL glass bottle (4.6). ADD 5 mL of acetone to
dissolve; then slowly add 5 mL of methanol while shaking. After the polymer
precipitation is complete, take 40 μL of the supernatant and place it in a 20 mL
headspace bottle (4.5). Quickly seal the headspace bottle; PLACE it in the
headspace autosampler. Under the set headspace conditions, the fragrance is
transferred to the gas phase. At this time, the concentration of the fragrance
material in the headspace gas is proportional to its initial content in the sample.
Introduce the gas in the quantitative loop into a gas chromatograph-mass
spectrometer for analysis.
6 Analytical procedure
6.1 Headspace injection conditions
The test results depend on the apparatus used. General parameters for
headspace injection cannot be given. The following operating conditions have
been proven appropriate:
a) Equilibrium temperature: 180 °C~200 °C. High-temperature-resistant
headspace bottle sealing caps and gaskets shall be used; otherwise the
gasket may be damaged and leaking or even the bottle cap may burst.
b) Equilibrium time: 10 min (polyester fiber); 6 min (ABS).
c) Auxiliary gas pressurization pressure: 70 kPa (polyester fiber); 80 kPa
(ABS).
d) Auxiliary gas pressurization time: 10 s.
e) Quantitative loop temperature: 5 °C~10 °C higher than the equilibrium
temperature.
f) Transmission line temperature: 5 °C~10 °C higher than the quantitative
loop temperature.
g) Volume of quantitative loop: 1 mL.
h) Equilibrium time of quantitative loop: 10 s.
i) Injection time: 20 s.
6.2 Determination conditions of gas chromatography-mass spectrometry
The test results depend on the apparatus used. General parameters for gas
chromatography-mass spectrometry cannot be given. The set parameters shall
ensure that, during the determination, the measured component and other
components can be effectively separated. The following parameters are
available for reference:
a) Chromatographic column: Low-loss quartz capillary column (30 m×0.25
mm×0.25 μm) with a stationary phase of 35% phenyl and 65% dimethyl
polysiloxane; or equivalent;
b) Temperature programming: KEEP at 40 °C for 1 min; RAISE to 210 °C at
5 °C/min; then raise to 300 °C at 10 °C/min;
c) Temperature of injection port: 280 °C;
d) Ion source temperature: 230 °C;
e) Transmission line temperature: 280 °C;
f) Carrier gas: Helium (purity≥99.999%). Flow rate is 1.0 mL/min;
g) Ionization method: EI ionization;
h) Ionization energy: 70 eV;
i) Injection mode: Split injection. Split ratio is 10:1;
j) Data acquisition mode: Selected ion monitoring (SIM). The analysis
parameters of each material are shown in Appendix A;
k) Solvent delay: 2.5 min.
6.3 Drawing of standard curve
6.3.1 Polyester fiber
ADD 20 μL of standard working solution (3.6) to the headspace bottle (4.5)
containing the blank sample of polyester fiber. Quickly press the bottle cap to
prepare a series of standard samples with different fragrance content. Then,
the standard samples are determined in order from low to high concentration.
USE the peak area of the quantitative ion chromatographic peak as the ordinate;
USE the corresponding fragrance mass (in micrograms) as the abscissa;
DRAW the standard working curve. For the total ion chromatogram of 54
fragrance materials under the above analysis conditions, refer to Appendix B.
6.3.2 ABS
ADD 40 μL of standard working solution (3.6) to the headspace bottle (4.5).
Quickly press the bottle cap to prepare a series of standard samples with
GB/T 39181-2020
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 13.120
Y 41
Consumer products - Polyester fiber and ABS material
- Rapid determination method of fragrance allergens
消费品 聚酯纤维及 ABS材质
ISSUED ON: OCTOBER 21, 2020
IMPLEMENTED ON: OCTOBER 21, 2020
Issued by: State Administration for Market Regulation;
Standardization Administration of the PRC.
Table of Contents
Foreword ... 3 
1 Scope ... 4 
2 Principle ... 4 
3 Reagents or materials ... 4 
4 Apparatus ... 5 
5 Samples ... 5 
6 Analytical procedure ... 6 
7 Data processing ... 8 
8 Method quantification limit ... 9 
9 Recovery rate and precision ... 9 
10 Test report ... 10 
Appendix A (Normative) Analysis parameters of 54 fragrance materials ... 11 
Appendix B (Informative) Total ion chromatogram of 54 fragrance materials . 13 
Appendix C (Informative) Statistical data of precision test obtained from
laboratory ... 14 
Consumer products - Polyester fiber and ABS material
- Rapid determination method of fragrance allergens
1 Scope
This Standard specifies the determination method of headspace gas
chromatography-mass spectrometry for 54 kinds of fragrance allergens in
consumer product polyester fiber and acrylonitrile-butadiene-styrene (ABS)
material.
This Standard applies to the rapid determination of the content of 54 kinds of
fragrance allergens in consumer product polyester fiber and ABS material.
2 Principle
CUT the polyester fiber into a headspace bottle; ADD a small amount of organic
solvent. After crushing the ABS, use solvent dissolution-precipitation method to
extract; PLACE the extracted trace solution into the headspace bottle. SET the
headspace parameters. The fragrance in the sample volatilizes and quickly
forms a dynamic equilibrium in the bottle (polyester fiber sample); or all is
transferred to the headspace (ABS sample). At this time, the concentration of
the fragrance in the headspace gas is proportional to its initial content in the
sample. Introduce the headspace gas to the gas chromatograph-mass
spectrometer for determination. By measuring the concentration of fragrances
in the headspace gas, the content of fragrances in the sample can be obtained.
3 Reagents or materials
3.1 Acetone: Chromatographically pure.
3.2 Methanol: Chromatographically pure.
3.3 Fragrance reference materials: The purity is all greater than 90%. The
material types are shown in Appendix A.
3.4 Single standard stock solution: Respectively weigh the appropriate amount
of fragrance reference materials (3.3) accurately; USE acetone to prepare a
single standard solution of appropriate concentration; STORE it in a refrigerator
at 4 °C. The expiry date is 12 months.
FREEZE and crush the sample to a particle size of less than 1 mm; WEIGH 0.2
g (accurate to 0.1 mg) into a 20 mL glass bottle (4.6). ADD 5 mL of acetone to
dissolve; then slowly add 5 mL of methanol while shaking. After the polymer
precipitation is complete, take 40 μL of the supernatant and place it in a 20 mL
headspace bottle (4.5). Quickly seal the headspace bottle; PLACE it in the
headspace autosampler. Under the set headspace conditions, the fragrance is
transferred to the gas phase. At this time, the concentration of the fragrance
material in the headspace gas is proportional to its initial content in the sample.
Introduce the gas in the quantitative loop into a gas chromatograph-mass
spectrometer for analysis.
6 Analytical procedure
6.1 Headspace injection conditions
The test results depend on the apparatus used. General parameters for
headspace injection cannot be given. The following operating conditions have
been proven appropriate:
a) Equilibrium temperature: 180 °C~200 °C. High-temperature-resistant
headspace bottle sealing caps and gaskets shall be used; otherwise the
gasket may be damaged and leaking or even the bottle cap may burst.
b) Equilibrium time: 10 min (polyester fiber); 6 min (ABS).
c) Auxiliary gas pressurization pressure: 70 kPa (polyester fiber); 80 kPa
(ABS).
d) Auxiliary gas pressurization time: 10 s.
e) Quantitative loop temperature: 5 °C~10 °C higher than the equilibrium
temperature.
f) Transmission line temperature: 5 °C~10 °C higher than the quantitative
loop temperature.
g) Volume of quantitative loop: 1 mL.
h) Equilibrium time of quantitative loop: 10 s.
i) Injection time: 20 s.
6.2 Determination conditions of gas chromatography-mass spectrometry
The test results depend on the apparatus used. General parameters for gas
chromatography-mass spectrometry cannot be given. The set parameters shall
ensure that, during the determination, the measured component and other
components can be effectively separated. The following parameters are
available for reference:
a) Chromatographic column: Low-loss quartz capillary column (30 m×0.25
mm×0.25 μm) with a stationary phase of 35% phenyl and 65% dimethyl
polysiloxane; or equivalent;
b) Temperature programming: KEEP at 40 °C for 1 min; RAISE to 210 °C at
5 °C/min; then raise to 300 °C at 10 °C/min;
c) Temperature of injection port: 280 °C;
d) Ion source temperature: 230 °C;
e) Transmission line temperature: 280 °C;
f) Carrier gas: Helium (purity≥99.999%). Flow rate is 1.0 mL/min;
g) Ionization method: EI ionization;
h) Ionization energy: 70 eV;
i) Injection mode: Split injection. Split ratio is 10:1;
j) Data acquisition mode: Selected ion monitoring (SIM). The analysis
parameters of each material are shown in Appendix A;
k) Solvent delay: 2.5 min.
6.3 Drawing of standard curve
6.3.1 Polyester fiber
ADD 20 μL of standard working solution (3.6) to the headspace bottle (4.5)
containing the blank sample of polyester fiber. Quickly press the bottle cap to
prepare a series of standard samples with different fragrance content. Then,
the standard samples are determined in order from low to high concentration.
USE the peak area of the quantitative ion chromatographic peak as the ordinate;
USE the corresponding fragrance mass (in micrograms) as the abscissa;
DRAW the standard working curve. For the total ion chromatogram of 54
fragrance materials under the above analysis conditions, refer to Appendix B.
6.3.2 ABS
ADD 40 μL of standard working solution (3.6) to the headspace bottle (4.5).
Quickly press the bottle cap to prepare a series of standard samples with