GB/T 34436-2023_English: PDF (GB/T34436-2023)
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Determination of formamide in toy materials -- High performance liquid chromatography-mass spectrometry
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GB/T 34436-2023
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| GB/T 34436-2017 | English | 399 |
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Determination of formamide in toy materials -- Gas chromatography-mass spectrometry (GC-MS)
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| Standard ID | GB/T 34436-2023 (GB/T34436-2023) | | Description (Translated English) | Determination of formamide in toy materials -- High performance liquid chromatography-mass spectrometry | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | Y57 | | Classification of International Standard | 97.200.50 | | Word Count Estimation | 9,983 | | Date of Issue | 2023-03-17 | | Date of Implementation | 2023-10-01 | | Older Standard (superseded by this standard) | GB/T 34436-2017 | | Drafting Organization | Shenzhen Institute of Metrology and Quality Inspection, Yike Testing and Certification Co., Ltd., Baoju (China) Children's Products Co., Ltd., Shantou Quality Supervision and Inspection Institute of Guangdong Province, Jiaxing Xiaohuzi Vehicle Industry Co., Ltd., Beijing Zhongqinglian Certification Center Co., Ltd. company | | Administrative Organization | National Toy Standardization Technical Committee (SAC/TC 253) | | Issuing agency(ies) | China National Light Industry Council | | Standard ID | GB/T 34436-2017 (GB/T34436-2017) | | Description (Translated English) | Determination of formamide in toy materials -- Gas chromatography-mass spectrometry (GC-MS) | | Sector / Industry | National Standard (Recommended) | | Classification of Chinese Standard | Y57 | | Classification of International Standard | 97.200.50 | | Word Count Estimation | 10,147 | | Date of Issue | 2017-10-14 | | Date of Implementation | 2018-05-01 | | Drafting Organization | Shenzhen Institute of Metrology and Quality Inspection, Bureau Veritas US Product Testing (Shanghai) Co., Ltd., Goodbaby Children Products Co., Ltd., Jiangsu Yike Detection Technology Service Co., Ltd., Inspection and Quarantine Technology Center of Guangdong Entry-Exit Inspection and Quarantine Bureau Toys Baby Products Laboratory, Shanghai Institute of Quality Supervision, Inspection and the Shenzhen Entry-Exit Inspection and Quarantine Bureau Toy Testing Technology Center, Weikai Testing Technology Co., Ltd., Jiangsu Exit Inspection and Quarantine Light Industry Products and Children Products Testing Center, Fujian Province Product Quality Inspection Research Institute, China Import and Export Toys Testing Center in Shanghai, Zhejiang Province Quality Inspection Institute of Science and Technology, Beijing Light Alliance Certification Center | | Administrative Organization | National Toy Standardization Technical Committee (SAC/TC 253) | | Proposing organization | China National Light Industry Council | | Issuing agency(ies) | General Administration of Quality Supervision, Inspection and Quarantine of PRC; China National Standardization Administration |
GB/T 34436-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 97.200.50
CCS Y 57
Replacing GB/T 34436-2017
Determination of formamide in toy materials - High
performance liquid chromatography-mass spectrometry
ISSUED ON: MARCH 17, 2023
IMPLEMENTED ON: OCTOBER 1, 2023
Issued by: State Administration for Market Regulation;
Standardization Administration of the PRC.
Table of Contents
Foreword ... 3
1 Scope ... 5
2 Normative references ... 5
3 Terms and definitions ... 5
4 Principle ... 5
5 Reagents or materials ... 6
6 Apparatus ... 6
7 Sample preparation ... 6
8 Sample extraction ... 7
9 Determination ... 7
10 Result calculation ... 7
11 Method limit of quantitation ... 8
12 Precision ... 8
13 Test report ... 8
Appendix A (Informative) Reference working conditions of high performance
liquid chromatograph-mass spectrometer for the determination of formamide
... 10
Appendix B (Informative) Precision test results... 12
Determination of formamide in toy materials - High
performance liquid chromatography-mass spectrometry
IMPORTANT NOTE: The use of this document may involve certain hazardous
materials, procedures and equipment; but not all safety issues related thereto are
recommended. It is the user's responsibility to, before applying this document,
establish appropriate safety and protection measures AND determine the
applicability of relevant regulatory limitations.
1 Scope
This document describes a method for the determination of formamide in toy materials
using high performance liquid chromatograph-mass spectrometer.
This document is applicable to the determination of formamide in foam materials such
as ethylene-vinyl acetate copolymer (EVA), polyethylene (PE), chemically cross-linked
polyethylene (XPE), and polyvinyl chloride (PVC) in toy products. It is used as a
reference for the determination of formamide in other foam materials.
2 Normative references
The contents of the following documents, through normative references in this text,
constitute indispensable provisions of this document. Among them, for dated references,
only the edition corresponding to that date applies to this document. For undated
references, the latest edition (including all amendments) applies to this document.
GB/T 6682 Water for analytical laboratory use - Specification and test methods
3 Terms and definitions
There are no terms and definitions that need to be defined in this document.
4 Principle
Use water to ultrasonically extract the prepared samples. After filtering the extract, use
high performance liquid chromatograph-mass spectrometer to determine; use external
standard method to quantify.
8 Sample extraction
Weigh two specimens of about 0.1 g (accurate to 0.1 mg) into the glass sample vial
(6.4); accurately add 10 mL of water (5.1) and seal. After fully infiltrating the specimen,
place it in an ultrasonic generator (6.2) for ultrasonic extraction for 3.5 h; cool to room
temperature; use an organic microporous membrane (6.6) to filter it; wait for the
determination.
9 Determination
9.1 Reference working conditions for high performance liquid chromatograph-
mass spectrometer
Since the setting of working conditions depends on the instrument used, the set
parameters shall ensure the effective separation of formamide chromatographic peaks.
Appendix A gives the reference working conditions of high performance liquid
chromatograph-mass spectrometer for the determination of formamide.
9.2 Qualitative analysis
According to the above analysis conditions (9.1), analyze the standard working solution
(5.6) and the sample extract; use the retention time of characteristic ions and
chromatographic peaks (see Figure A.1 in Appendix A) for qualitative analysis. If the
selected ion proton number/charge number (m/z) is 46.0, the retention time of the
detected chromatographic peak is consistent with that of the standard solution; it can be
considered that the sample contains the target component.
9.3 Quantitative analysis
Use the external standard method for quantitative analysis. Use the mass concentration
of the standard working solution as the abscissa; use the quantitative ion peak area of
the compound as the ordinate; draw the standard working curve; obtain the regression
equation of the standard curve, to calculate the formamide content in the sample.
If the specimen response value exceeds the linear range, it is necessary to dilute the
specimen by an appropriate multiple AND re-inject the specimen for analysis.
9.4 Blank test
Except that no specimen is added, follow the above operation steps.
10 Result calculation
According to the formula (1), calculate the content of formamide in the specimen.
Where:
w - The content of formamide in the specimen, in milligrams per kilogram (mg/kg);
c - The mass concentration of formamide in the sample solution, in milligrams per liter
(mg/L);
c0 - The mass concentration of formamide in the blank test, in milligrams per liter
(mg/L);
V - The volume of the extract, in milliliters (mL);
D - The dilution factor of the extract;
m - The mass of specimen weighed, in grams (g).
The calculation result retains 3 significant figures.
11 Method limit of quantitation
When the sampling size is 0.1 g and the extraction solution volume is 10 mL, the
quantitation limit of this method is 10.0 mg/kg.
12 Precision
In the same laboratory, using the same equipment by the same operator, according to
the same test method, within a short period of time, by independently testing the same
measured object; the absolute difference between the two independent test results
obtained is not greater than 10% of the arithmetic mean of the two measured values;
provided that no more than 5% of the cases are greater than 10% of the arithmetic mean
of these two measured values.
See Appendix B for the precision test data of the method in this document.
13 Test report
The test report shall at least provide the following content:
a) Specimen description;
b) Number of this document;
......
GB/T 34436-2017
Determination of formamide in toy materials - Gas chromatography-mass spectrometry (GC-MS)
ICS 97.200.50
Y57
National Standards of People's Republic of China
Determination of formamide in toy materials
Gas chromatography - mass spectrometry
spectrometry (GC-MS)
2017-10-14 Published
2018-05-01 implementation
General Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
China National Standardization Administration released
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard proposed by the China Light Industry Federation.
This standard by the National Toy Standardization Technical Committee (SAC/TC253) centralized.
This standard was drafted unit Shenzhen Institute of Metrology and Quality Inspection, Bureau Veritas US Commodity Inspection (Shanghai) Co., Ltd., good children for children
Co., Ltd., Jiangsu billion Branch Detection Technology Services Ltd., Guangdong CIQ Inspection and Quarantine Technology Center toys baby products
Laboratory, Shanghai Institute of Quality Supervision, Inspection and Quarantine, Shenzhen CIQ Toy Testing Technology Center, Wei Kai testing technology
Limited, Exit Inspection and Quarantine of Jiangsu Light Industry Products and Children's Products Testing Center, Fujian Province Product Quality Inspection Institute, Shanghai, China
Import and Export Toys Testing Center, Zhejiang Province Quality Inspection Institute of Science and Technology, Beijing Light Alliance Certification Center.
The main drafters of this standard. Zhao Yan, Zhang Yao, Ke Dengming, Hu Aisheng, ants Le Chau, Sun Duoshi, Dong Fu silver, Xia Qingyun, Cheng Yulong, Chen Wei,
Yu Wenjia, Liao Shangfu, Xu Dongyu.
Determination of formamide in toy materials
Gas chromatography - mass spectrometry
1 Scope
This standard specifies the use of gas chromatography - mass spectrometry toys toys products ethylene - vinyl acetate (EVA) materials, formyl
Amine detection methods.
This standard applies to toys EVA material in the determination of formamide.
2 principle
The prepared sample was extracted with a certain volume of methanol by ultrasound and the solution was filtered and determined by gas chromatography-mass spectrometry (GC-MS)
Ding, external standard method.
3 Reagents and materials
Unless otherwise specified, only reagents identified as analytically pure are used in the analysis.
3.1 Formamide (CAS No. 75-12-7) standard substance mass fraction of not less than 99%.
3.2 methanol. Chromatographic purity and above.
4 instruments and equipment
4.1 Gas Chromatography-Mass Spectrometry (GC-MS) with Electron Impact Source (EI).
4.2 ultrasonic generator. Temperature accuracy of ± 5 ℃.
4.3 electronic balance. Accuracy 0.1mg.
4.4 Reagent bottle, equipped with a sealing cap, of suitable volume, such as a 20 mL headspace bottle.
4.5 organic phase filter membrane pore size 0.45μm.
5 Sample Preparation
Mechanical methods to obtain samples of EVA material from the toy samples, select the representative area of the sample, the sample is cut to no more than
5mm × 5mm × 5mm size particles.
6 sample
Weigh about 0.25g sample, accurate to 1mg. Quickly loaded into the reaction flask (4.4), accurately add 10mL of methanol (3.2), sealed
The sample is fully infiltrated and placed in an ultrasonic generator (4.2) for ultrasonic extraction. The temperature of the ultrasonic bath is maintained at (55 ± 5) ° C during the extraction process,
Total extraction time 3.5h; water bath liquid level should not be less than the reaction bottle liquid level. The reaction flask out every 0.5h, shaking, shake. In the room
The extract was filtered through a filter membrane (4.5) to a chromatographic flask under the temperature to be tested.
Note formaxamine samples (≥1000mg/kg) may be appropriate to reduce the sample size and increase the volume of the extraction solution.
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