QC/T 944-2013 PDF English
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| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivery | Name of Chinese Standard | Status |
| QC/T 944-2013 | English | 125 |
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The methods of polybrominated biphenyls and polybrominated diphenyl ethers in automotive materials
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QC/T 944-2013: The methods of polybrominated biphenyls and polybrominated diphenyl ethers in automotive materials
---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/QCT944-2013
QC
AUTOMOTIVE INDUSTRY STANDARD OF
THE PEOPLE’S REPUBLIC OF CHINA
ICS 43.020
T 05
The methods of polybrominated biphenyls and
polybrominated diphenyl ethers in automotive
materials
Issued on. OCTOBER 17, 2013
Implemented on. MARCH 1, 2014
Issued by. Ministry of Industry and Information Technology of PRC
1 Scope
This Standard specifies the detection methods for PBBs and PBDEs in
automotive materials.
"X-ray fluorescence spectrometry" is for X-ray fluorescence spectroscopy
screening and rapid determination of bromine content in automotive materials.
The GC-MS method is applicable for the determination of PBBs and PBDEs in
automotive materials by gas chromatography-mass spectrometry.
2 Normative references
The following referenced documents are indispensable for the application of
this document. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any
amendments) applies.
GB/T 8170, Rules of rounding off for numerical values & expression and
judgement of limiting values
GB/T 30512-2014, Requirements for Prohibited Substances on Automobiles
GB/Z 21276-2007, Determination of restricted substances - Polybrominated
biphenyls and polybrominated diphenyl ethers in electrical and electronic
equipment
3 X-ray fluorescence spectrometry
3.1 Principle
Place the prepared sample in a sample chamber of an X-ray fluorescence
spectrometer. Analyze the sample according to the selected test mode.
Determine whether the content of bromine in the sample is qualified according
to the screening limits of different samples, and whether it is necessary to carry
out accurate determination.
3.2 Reagents and materials
3.3.4 Grinding machine. with tungsten carbide (WC) abrasives
3.3.5 Tableting machine. working pressure of not less than 20 MPa
3.3.6 Melting machine. working temperature of not less than 1150°C
3.4 Sample preparation
3.4.1 Sample preparation principle
3.4.1.1 The sample used for the test must cover the measurement window of
the spectrometer.
3.4.1.2 The irradiated surface of the sample should be representative of the
sample as a whole.
3.4.1.3 Pay attention to pollution prevention during sample preparation
process.
3.4.2 Sample preparation method
3.6.2 Screening of bromine
In accordance with Requirements for Prohibited Substances on Automobiles of
which the mass fractions of the limits of polybrominated biphenyls (PBBs) and
polybrominated diphenyl ethers (PBDEs) are 0.1% (1000 mg/kg), the screening
limits for bromine in automotive materials are shown in Table 1.Screen the
bromine in automotive materials based on screening limits. There are two cases
in results. Pass (P) - if the test results are less than the set minimum, the result
shall be acceptable; Uncertain (X) - if the test results are greater than the set
minimum, the result shall be uncertain and a further test shall be carried out in
accordance with Method 2.
3.6.3 Report of test results
Take the arithmetic mean of the test results as report results, in
milligrams/kilograms (mg/kg).
4 Gas chromatography-mass spectrometry (GC-MS)
4.1 Principle
Samples are extracted with toluene as solvent. After the extracted volume to
the appropriate volume, use Gas Chromatography-Mass Spectrometry (GC-
MS) Full Scan Mode (SCAN) and select Ion monitoring mode (SIM) to
qualitatively and quantitatively determine the polybrominated biphenyls and
polybrominated diphenyl ethers in extracts. Then calculate their content in
automotive materials.
4.2 Reagents and materials
4.2.1 Solvents. toluene, chromatography pure; or acetone, cyclohexane, n-
hexane, methanol, dichloromethane, isooctane, nonane, etc.
4.2.3 Standard stock solution.
Respectively take the right amount of polybrominated biphenyls and
polybrominated diphenyl ether standard sample (4.2.2). Use toluene (4.2.1) to
prepare 1 µg/mL mixed standard stock solution.
4.2.9 Glass wool
4.2.10 Micro-liter syringe or automatic pipette
4.2.11 Liquid nitrogen. industrial grade
4.3 Apparatus and equipment
4.3.1 Gas chromatography - mass spectrometry. equipped with mass
selective detector (MSD), of mass range (100-1000) amu.
4.3.2 Soxhlet extractor with condenser
4.3.3 Rotary evaporator
4.3.4 Grinding device. including cutting machine or scissors, grinder, grinding
machine and other devices, mainly for sample crushing
4.3.5 Balance. a sense of 0.0001 g
4.5 Analysis steps
4.5.1 Soxhlet extraction
4.5.1.1 Add 70 mL of toluene (4.2.1) into the Soxhlet extractor. Extract 2h to
clean the Soxhlet extractor, discard the extract.
4.5.2 Determination
4.5.2.1 Refer to gas chromatography - mass spectrometry conditions.
Gas chromatography-mass spectrometry parameters should be set to ensure
that chromatographic determination of the measured components and other
components can be effectively separated.
4.5.2.2 Calibration curve plotting. Different concentrations of calibrated
standard solution (4.2.5) are injected into the gas chromatography-mass
spectrometer in turn. Take calibrated standard solution concentration as
abscissa, calibrated standard solution of the peak area as the vertical
coordinate to build up the calibration curve.
4.7.2 Recovery rate
The recovery rate of polybrominated biphenyls (PBBs) and polybrominated
diphenyl ethers (PBDEs) in automotive materials is between 70% and 130%.
4.7.3 Precision
Under repeatability conditions, the absolute difference between the two
independent test results obtained is not more than 20% of the arithmetic mean
of the two measured values. It is premised that the ratio is not more than 5% of
the case of 20% of the arithmetic mean of the two measured values.
5 Test report
The test report should include the following content.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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