GB/T 40971-2021 PDF English
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Methods for the determination of prohibited substance in furniture products and related materials -- Polycyclic aromatic hydrocarbons
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GB/T 40971-2021: PDF in English (GBT 40971-2021) GB/T 40971-2021
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 97.140
CCS Y 80
Method for the determination of prohibited substances in
furniture products and related materials - Polycyclic
aromatic hydrocarbons
多环芳烃
ISSUED ON: OCTOBER 11, 2021
IMPLEMENTED ON: MAY 1, 2022
Issued by: State Administration for Market Regulation;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Terms and definitions ... 4
4 Principles ... 4
5 Reagents or materials ... 5
6 Instruments and equipment ... 5
7 Samples ... 6
8 Test steps ... 6
9 Processing of test data ... 8
10 Precision ... 10
Appendix A (Informative) Molecular formulas, CAS numbers, and characteristic
fragment ions of 18 kinds of PAHs ... 11
Appendix B (Informative) Typical GC-MS selected ion chromatograms of 18 kinds of
PAHs ... 12
Method for the determination of prohibited substances in
furniture products and related materials - Polycyclic
aromatic hydrocarbons
Warning -- The personnel using this document shall have practical experience in
formal laboratory work. This document does not indicate all possible safety
issues. The user is responsible for taking appropriate safety and health measures
and ensuring compliance with the conditions stipulated by relevant national laws
and regulations.
1 Scope
This document describes a gas chromatography-mass spectrometry method for the
determination of 18 polycyclic aromatic hydrocarbons in furniture products and their
materials.
This document applies to the determination of 18 polycyclic aromatic hydrocarbons in
furniture products and their materials.
2 Normative references
There are no normative references in this document.
3 Terms and definitions
The following terms and definitions apply to this document.
3.1 Polycyclic aromatic hydrocarbons; PAHs
A series of hydrocarbon compounds and their derivatives in which two or more benzene
rings are fused together, and the rings may also have short alkyl or cycloalkyl
substituents.
Note: 18 kinds of polycyclic aromatic hydrocarbons are shown in Table A.1 of Appendix A.
4 Principles
By ultrasonic wave, extract polycyclic aromatic hydrocarbons from the sample with
toluene; purify the extract by silica gel solid-phase extraction cartridge, and concentrate
it to a constant volume; then, determine it by gas chromatography-mass spectrometry
(GC-MS) method, and use selected ion monitoring mode and external standard method
for quantification.
5 Reagents or materials
5.1 N-hexane: chromatographically pure.
5.2 Petroleum ether: chromatographically pure.
5.3 Toluene: chromatographically pure.
5.4 Nitrogen: purity ≥99.99%.
5.5 Helium: purity ≥99.999%.
5.6 18 kinds of polycyclic aromatic hydrocarbon reference materials: purity ≥98%; or
18 kinds of certified mixed standard solutions with known concentrations.
5.7 18 kinds of polycyclic aromatic hydrocarbon mixed standard working solutions:
there shall be at least 5 calibration points, which can cover samples with concentrations
ranging from 0.2 mg/kg~10 mg/kg. That is, the range of the standard solution is 10
ng/mL~500 ng/mL. The mixed standard working solution of polycyclic aromatic
hydrocarbons was stored at 0 °C~4 °C in the dark and airtight.
5.8 Silica gel solid-phase extraction cartridge: 2 g/10mL or equivalent; before using,
rinse it with n-hexane to keep it wet.
5.9 Centrifuge tubes.
5.10 Sample bottle: it shall be about 50 mL, with a sealable cap.
5.11 Filter membrane: organic phase syringe filter membrane with a pore size of 0.45
µm.
6 Instruments and equipment
6.1 Gas chromatograph-mass spectrometer (GC-MS): it shall be equipped with an EI
source.
6.2 Ultrasonic generator: it shall be equipped with a temperature controller; when the
basket does not be placed in it, the power per unit water bath area shall reach at least
0.28 W/cm2.
Accurately weigh 0.5 g of the sample, and the weight shall be accurate to 0.1 mg; put
it into the sample bottle (5.10), add 10 mL of the toluene (5.3) solution, and seal the
bottle; after the sample is fully soaked, place the bottle in the frameless ultrasonic
generator (6.2) and hang it at the temperature of (60±5) °C, then, carry out the ultrasonic
extraction for 60 min. After the extraction is complete, take out the sample bottle, cool
it to room temperature, and shake it well; then, transfer the extract to the centrifuge tube
(5.9), and place the tube in the centrifuge (6.5) for centrifugation (if the solution after
ultrasonic extraction can be stratification through standing, then the centrifugation is
unnecessary). The supernatant is to be purified.
8.3 Purification
It can be selective to purify the samples with interfering substances. Before purification,
rinse the silica gel solid-phase extraction cartridge (5.8) with 5 mL of n-hexane (5.1) to
keep it wet; take 2 mL of the supernatant after extraction (8.2) and transfer it to the
silica gel solid-phase extraction cartridge (5.8); elute with 5 mL of n-hexane (5.1),
control the flow rate to be 0.5 drops/s, and discard the above passing-through-column
liquid. Then, elute with 10 mL of petroleum ether (5.2), collect the petroleum ether
eluent, and add 1 mL of toluene (5.3) to the collected petroleum ether eluent; slowly
blow the liquid to about 1 mL with a nitrogen concentrator (6.6), and finally, make up
to 2 mL with toluene (5.3).
8.4 Filtration
Filter the liquid after constant volume processing with an organic microporous
membrane (5.11) and analyze it by a gas chromatography-mass spectrometer (6.1).
8.5 Determination
8.5.1 Gas chromatography and mass spectrometry reference conditions
Ensure the set parameters of the used instrument to be able to separate the tested
component and other components effectively during the chromatographic
determination. Since the test results depend on the used instrument, it is impossible to
give the general parameters of the instrumental analysis. The following parameters have
been proven to be suitable for the testing:
a) Chromatographic column: DB-EUPAH or equivalent, 20 m (column length) ×
0.18 mm (inner diameter) × 0.14 µm (film thickness);
b) Temperature of injection port: 290 °C;
c) Chromatographic column heating program: initial column temperature shall be
50 °C and held for 1 min; heat up to 200 °C at a rate of 20 °C/min and hold for 0.5
min; then, raise the temperature to 310 °C at a rate of 8 °C/min and hold for 5 min;
d) Temperature of transmitter interface: 280 °C;
e) The temperature of the ion source shall be 230 °C, the ionization method shall be
EI, and the ionization energy shall be 70 eV;
f) Temperature of quadrupole rod: 150 °C;
g) Determination method: Selected ion monitoring (SIM);
h) Sample injection method: splitless injection;
i) The carrier gas shall be the helium, and the purity shall be ≥99.999%; the carrier
gas flow rate shall be 1.0 mL/min;
j) Injection volume: 1 µL;
k) Solvent delay time: 4.0 min.
8.5.2 Qualitative and quantitative analysis by the GC-MS method
According to the analysis conditions of 8.5.1, determine 18 kinds of PAHs mixed
standard working solution (5.7) and the filtered solution (8.4). Integrate the peak area
of the quantitative ion (see Appendix A); take the peak area as the ordinate and the
corresponding standard solution concentration as the abscissa, to draw a standard
working curve, and the correlation coefficient shall be ≥0.995; use the external standard
method for quantification. If the retention time of the chromatographic peak in the
solution to be tested is similar to that of the standard working solution (5.7), and the
type and abundance ratio of the selected ions (see Appendix A) of the target compound
in the solution to be tested are consistent with those of the standard working solution,
it can be determined that the target compound exists in the solution to be tested. Typical
GC-MS selected ion chromatograms of 18 PAHs are shown in Appendix B.
8.5.3 Blank test
Carry out the blank test according to the above steps, except that no sample is added.
9 Processing of test data
9.1 Calculation of PAH content
Calculate the content of each PAH in the sample according to formula (1):
...... Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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