GB/T 39934-2021 PDF English
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Determination of volatile organic compounds from furniture products - Gas chromatography-mass spectrometry
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GB/T 39934-2021: Determination of volatile organic compounds from furniture products - Gas chromatography-mass spectrometry
---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT39934-2021
(Method for screening and detecting volatile organic compounds in furniture gas chromatography-mass spectrometry)
ICS 97.140
CCSY80
National Standards of People's Republic of China
Screening and detection methods of volatile organic compounds in furniture
Gas chromatography-mass spectrometry
Released on 2021-03-09
2021-10-01 implementation
State Administration of Market Supervision and Administration
Issued by the National Standardization Management Committee
Table of Contents
Foreword Ⅲ
1 Scope 1
2 Normative references 1
3 Terms and definitions 1
4 Principle 1
5 Reagents or materials 1
6 Equipment 2
7 Sample 2
8 Analysis step 3
9 Calculation of results 4
10 Method characteristics 5
Appendix A (informative) List of target volatile organic compounds in furniture 6
Appendix B (informative) Typical GC-MS chromatograms of volatile organic compounds in furniture 11
Appendix C (Informative) Detection Limits of Typical Volatile Organic Compounds 19
Preface
This document is in accordance with the provisions of GB/T 1.1-2020 "Guidelines for Standardization Work Part 1.Structure and Drafting Rules of Standardization Documents"
Drafting.
Please note that some of the contents of this document may involve patents. The issuing agency of this document is not responsible for identifying patents.
This document was proposed by the China National Light Industry Council.
This document is under the jurisdiction of the National Furniture Standardization Technical Committee (SAC/TC480).
Drafting organizations of this document. Shandong Institute of Product Quality Inspection, Shanghai Institute of Quality Supervision and Inspection Technology (National Furniture Quality Supervision
Inspection Center), Nanjing Customs Industrial Product Inspection Center, Xiamen Minghongtang Arts & Crafts Co., Ltd., Yucheng Furunde Wood Co., Ltd., Zhejiang
Jiangbaizhijia Furniture Co., Ltd., Shandong Jianzhu University, Deqing Dingsen Quality and Technical Testing Center, Shandong Guangming Yuandi Children's Furniture Technology Co., Ltd.
Company, Guangdong Federal Furniture Group Co., Ltd., Zhejiang Guanchen Furniture Manufacturing Co., Ltd., Foshan Weishang Furniture Manufacturing Co., Ltd., Shenzhen Yangtze River
Furniture Co., Ltd., Zhejiang Meisheng Cabinet Co., Ltd., Dongguan Jinhui Testing Equipment Manufacturing Co., Ltd., Xiamen Gold Kitchen Cabinet Co., Ltd.
Division, Shandong Wanjiayuan Wood Industry Co., Ltd., Hunan Provincial Product Quality Supervision and Inspection Institute, Chongqing Customs Technology Center.
The main drafters of this document. Gao Cuiling, Ji Fei, Zhu Haiou, Liu Mengmeng, Pei Yirong, Peng Lizheng, Peng You, Zhang Guiqin, Yu Guoping, Wang Xianyong,
Huang Can, Zhou Genfu, Zhou Shanlin, Li Suijun, Luo Yefu, Li Gan, Jiang Xueyuan, Tu Chunsheng, He Bing, Hao Defeng, Pan Xiaozhen, Zhang Gang, Shi Pengtu, Hu Yanjun,
Xi Cunxian, Li Xianliang.
Screening and detection methods of volatile organic compounds in furniture
Gas chromatography-mass spectrometry
1 Scope
This document specifies the terms and definitions for the screening and detection of volatile organic compounds in furniture products using gas chromatography-mass spectrometry.
Principles, reagents or materials, instruments and equipment, samples, analysis procedures, result calculations and method characteristics.
This document is applicable to the screening and testing of 106 volatile organic compounds in furniture products. Volatile organic compounds in furniture raw materials
The screening test can be performed with reference to this document.
2 Normative references
The contents of the following documents constitute the indispensable clauses of this document through normative references in the text. Among them, dated quotations
Only the version corresponding to the date is applicable to this document; for undated reference documents, the latest version (including all amendments) is applicable to
This document.
Preparation of preparations and products used in GB/T 603 chemical reagent test method
GB/T 31107 General technical conditions for climate chambers for testing volatile organic compounds in furniture
GB/T 35607-2017 Green Product Evaluation Furniture
3 Terms and definitions
The following terms and definitions apply to this document.
3.1
Volatile organic compounds volatileorganic compounds; VOCs
Organic compounds with a boiling point between 50°C and 260°C released from furniture or raw and auxiliary materials.
4 Principle
Collect the volatile organic compounds released by the furniture sample into the adsorption tube, use gas chromatography-mass spectrometry (GC-MS) and thermodynamics
The analysis principle is to transfer the volatile organic compounds adsorbed in the adsorption tube to the GC-MS system through the thermal analysis device for screening and
Detection, mass spectrometry ion qualitative, peak area or peak height quantification.
5 Reagents or materials
5.1 General
Unless otherwise specified, the purity of the reagents used should be chromatographically pure. If it is analytically pure, it should be purified to ensure no chromatographic analysis
Impurities. The preparation used should be prepared in accordance with the provisions of GB/T 603.
5.2 Volatile Organic Compound Standard Substances
See Appendix A for the types of volatile organic compound standard substances.
5.3 Methanol (CH3OH)
It should be chromatographically pure.
5.4 Standard solution
Prepare the standard material (5.2) by yourself, and use methanol (5.3) as the dilution solvent to prepare the standard solution of the target VOCs to make the mass concentration
They are.2000μg/mL, 500μg/mL, 100μg/mL, 20μg/mL, 5μg/mL and 2μg/mL respectively. For the reference material (5.2),
The mixed standard solutions of benzene series, alcohols, halogenated hydrocarbons, terpenes, alkanes, aldehydes and ketones, esters, etc. can be configured according to the classification in Appendix A.
Standard solution can be configured separately. The standard solution can be stored at (4±2)℃ for 1 month.
5.5 Inert gas
5.5.1 High purity nitrogen. the purity is not less than 99.999%.
5.5.2 High purity helium. the purity is not less than 99.999%.
6 Equipment
6.1 VOCs adsorption tube
Adopt the adsorption tube matched with the thermal analysis instrument. The adsorption tube should be marked to confirm the direction of the air inlet during sampling. Adsorption tube should be installed
There are at least.200mg graphitized carbon black and graphite molecular sieve composite (CarbopackB/CarbosieveTM) adsorbent, the particle size of the adsorbent can be
Use a screen that passes 0.25mm~0.18mm (60 mesh to 80 mesh), or use an adsorption tube that can meet the same adsorption efficiency.
6.2 Thermal Desorber
The adsorption tube can be subjected to secondary thermal analysis, and the desorbed gas can be brought into the gas chromatograph/mass spectrometer through the inert gas.
6.3 Gas Chromatography-Mass Spectrometer (GC-MS)
Equipped with quality selective detector (MSD).
6.4 Electronic balance
Sensitivity is 0.1mg.
6.5 Constant flow gas sampler
The flow range is 0L/min~2L/min. The flow is stable and adjustable. Use soap film flowmeter to calibrate the sampling flow before and after sampling, the error should be
Not more than 5%.
6.6 Climate cabin
It should meet the requirements of GB/T 31107.
7 samples
7.1 Selection of samples
You can choose the whole piece of furniture, a complete set of furniture or furniture parts as samples. The composition and status of the sample should be indicated in the test report.
7.2 Pretreatment of samples
The sample to be tested should be pretreated before the test. Upholstered furniture shall be carried out in accordance with B.2.1 of GB/T 35607-2017.Wood furniture etc.
Other furniture shall be carried out in accordance with D.3.1.2 of GB/T 35607-2017.
8 Analysis steps
8.1 Activation and storage of VOCs adsorption tube
The adsorption tube needs to be activated by inert gas at high temperature before use. Under the inert carrier gas flow of 50mL/min~100mL/min, the temperature
The activation time is at least 5min at 280℃~300℃ to remove the volatile organic compounds remaining in the adsorption tube as much as possible. After activation or make
Before use, check that there is no interfering chromatographic peak.
The activated adsorption tube should be sealed with a metal screw cap and a PTFE ferrule, or it can be sealed with the adsorption tube matching the thermal desorber
The components are sealed.
8.2 Release and collection of VOCs
After the sample is pretreated, it should be placed in the climate chamber within 1h for the release of VOCs. Climatic cabins for the release of VOCs from upholstered furniture
The parts shall be carried out in accordance with the regulations in B.2.2~B.2.4 of GB/T 35607-2017.The climatic chamber conditions for the release of VOCs from wood furniture and other furniture are as follows
GB/T 35607-2017 stipulates D.3.1.3~D.3.1.5.
Connect the adsorption tube to the constant flow gas sampler, install the adsorption tube to the gas outlet of the climate chamber for VOCs collection, and adjust the sampler
Flow rate, sampling 1L~10L gas in the flow range of 50mL/min~200mL/min (according to the sample volatile organic compound
The amount of material released determines the sampling volume). During the test, record the sampling flow, sampling time, temperature and atmospheric pressure.
The release and collection conditions of the blank sample are the same as the release and collection conditions of the sample.
8.3 Analysis and test conditions
8.3.1 Thermal analysis conditions
Since the requirements for achieving thermal analysis efficiency are related to the instrument used, only the basic parameters of the second thermal analysis can be given, and the remaining parameters are set
Please refer to the instruction manual of the thermal desorber. The parameters given below are basic parameters.
a) Thermal analysis temperature. 260℃~280℃;
b) Thermal analysis time. 5min~15min;
c) Thermal analysis gas flow rate. 50mL/min;
d) Cold trap trap temperature. -20℃~-10℃;
e) Transmission line temperature. 220℃~250℃;
f) Split ratio. Choose according to the quality of volatile organic compounds in the adsorption tube.
8.3.2 Gas chromatography-mass spectrometry analysis conditions
Because the test results are related to the instrument used, it is impossible to give general parameters for gas chromatography-mass spectrometry. Parameterized
The principle is to obtain the best separation effect in the shortest time. The parameters given below have been tested and proved to be feasible.
a) Quartz capillary column. Polarity index is less than 10, column length is 50m~60m, inner diameter is 0.25mm, film thickness is 0.25μm, or phase
Principal
b) Heating program. 40℃, hold for 1min, then increase to 100℃ at a rate of 3℃/min, and then increase at a rate of 10℃/min
Warm to 250°C, keep for 10min;
c) Carrier gas. high-purity helium, purity ≥99.999%, flow rate 1.2mL/min;
d) Chromatography-mass spectrometry interface temperature. 260℃;
e) Ion source. electron ionization source EI, ion source temperature 230℃;
f) Ionization energy. 70eV;
g) Mass analyzer. quadrupole mass analyzer;
h) Quality scan range. 25amu~450amu;
i) Scan mode. select full scan mode.
8.4 Standard curve drawing
Use a syringe to accurately draw 1 μL of standard solutions (5.4) of different concentrations, and inject them into the activated adsorption tubes.
High-purity nitrogen purge at about 100mL/min for at least 5 minutes. Put the adsorption tube on the thermal desorber for gas chromatography mass spectrometry analysis,
Qualitative standard ion, quantification by peak area or peak height method. Take the peak area after deducting the blank as the ordinate and the mass of the target substance as the abscissa to draw
standard curve line. It is recommended to make a standard curve once a month, or make a standard adsorption tube of known concentration for each batch of samples, and use the standard curve to determine
The deviation of the measurement result is within 15%. For a list of target volatile organic compounds in furniture, see Appendix A, typical of volatile organic compounds in furniture
See Appendix B for the gas chromatography-mass spectrometry chromatogram.
8.5 Screening and analysis of samples
The analysis process of each sample adsorption tube is analyzed according to the operation steps of the standard curve.
Through the obtained full scan mass spectrum, the retention time of the target in the sample and the target in the standard series, the mass-to-charge ratio of fragment ions, and
Compare its abundance and other information, compare the gas chromatography-mass spectrometry chromatogram of the sample, observe whether the sample spectrum has the characteristic group peak of the target, and compare the sample
Qualitative screening and analysis of the types of volatile organic compounds.
9 Result calculation
9.1 Convert the sampling volume to the sampling volume in the standard volume state according to formula (1).
10 Method characteristics
10.1 Detection limit
The detection limit of volatile organic compounds in furniture in this method is shown in Appendix C.
10.2 Precision
In the same laboratory, the same operator uses the same equipment, according to the same test method, and compares the same test object in a short period of time.
The absolute difference between the two independent test results obtained in mutually independent tests is not more than 10% of the arithmetic mean of the two measured values, and
If it is greater than 10% of the arithmetic mean of these two measured values, it is assumed that it does not exceed 5%.
10.3 Repeatability
The relative deviation of the repeatability determination of the same sample is less than 10%.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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