GB/T 40030-2021Determination of medium chain chlorinated paraffins in electrical and electronic products (English PDF)
电子电气产品中中链氯化石蜡的检测方法
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Issued by
SAMR; SAC
Level / Type
National · Recommended
Issue date
April 30, 2021
Implementation date
November 1, 2021
Scope
GB/T 40030-2021 is the English-translated version of 电子电气产品中中链氯化石蜡的检测方法.
GB/T 40030-2021 is a laboratory method for determining medium chain chlorinated paraffins (MCCPs), mixtures of chlorinated alkanes with 14 to 17 carbon atoms, in electrical and electronic products.
It uses gas chromatography with electron capture negative chemical ionization mass spectrometry for both identification and quantification, and applies to MCCPs with five or more chlorine atoms.
The product is split according to SJ/T 11692, crushed to below 1 mm, extracted ultrasonically with n-hexane, concentrated under nitrogen and analysed under stated chromatographic conditions.
The content is calculated with a total response factor corrected for the measured chlorine content, as set out in Annex B. The limit of detection is 100 µg/g, and two results from the same laboratory may differ by no more than 30% of their mean. It was issued on 30 April 2021 and has applied since 1 November 2021.
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Document preview — GB/T 40030-2021
National Standard of the People's Republic of China
- ICS
- 31.020
- Classification
- L 10
Issued by: State Administration for Market Regulation; Standardization Administration of the PRC
Contents
- Foreword3
- 1 Scope4
- 2 Normative references4
- 3 Terms and definitions4
- 4 Principle5
- 5 Reagents and materials5
- 6 Instruments5
- 7 Samples6
- 8 Test steps6
- 9 Test data processing9
- 10 Limit of detection9
- 11 Precision9
- Annex A (informative) Total ion current chromatogram of medium chain chlorinated paraffin10
- Annex B (normative) Total response factor correction method11
1 Scope
This Standard specifies the qualitative and quantitative methods for the determination of medium chain chlorinated paraffins in electronic and electrical products by gas chromatography-electron capture negative chemical ionization source mass spectrometry.
This Standard applies to the determination of medium chain chlorinated paraffins with chlorine atoms greater than or equal to 5 in electronic and electrical products.
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.
SJ/T 11692, Guideline of sample disjointment for testing certain restricted substances in electrical and electronic products
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1 Medium chain chlorinated paraffins; MCCPs
a mixture of chlorinated alkanes with 14 to 17 carbon atoms
NOTE: The general chemical formula is CmH2m +2-nCln (m =14~17), and the CAS number […]
7 Samples
Split the electronic and electrical products according to SJ/T 11692 to obtain testing samples.
Crush the testing sample to a particle size of less than 1cm. Then use a freeze crusher or equivalent equipment (see 6.3) to crush to a particle size of less than 1mm.
8 Test steps
8.1 Extraction
Accurately weigh 1.0g of sample (to the nearest of 0.001g) into a glass sample bottle. Add 10mL of n-hexane (see 5.1), cap and seal. Put it in a water bath ultrasound system. Set the ultrasonic frequency to 40kHz±2kHz, the ultrasonic power greater than or equal to 600W, and the ultrasonic bath temperature at 70°C±5°C. Perform ultrasonic vibration extraction for 1.5h. Cool to room temperature. Then filter the extract and transfer it to a graduated glassware.
Use 3mL~5mL of n-hexane (see 5.1) to clean the sample bottle twice. Filter the cleaning fluid into the graduated glassware. Use the nitrogen blow dryer (see 6.6) to blow and concentrate all the collected filtered liquid nitrogen to near dryness. Use n-hexane to set volume to 1.0mL. Use the filter membrane to filter it to obtain the testing sample.
8.2 Determination
8.2.1 Description of test instrument parameters
Depending on the instrument used, the optimal analysis conditions may also be different. It is impossible to give general parameters for gas chromatography-mass spectrometry analysis. The set parameters shall ensure the effective separation and determination of the tested components. The parameters given below have proven to be feasible.
8.2.2 Chromatographic conditions
The chromatographic conditions are as follows:
a) Chromatographic column: 30m (column length) × 0.25mm (inner diameter) × 0.25µm (film thickness); the stationary phase is 5% phenyl; 95% dimethyl polysiloxane quartz capillary column or equivalent;
b) Inlet temperature: 280°C; […]
9 Test data processing
Calculate the content of medium chain chlorinated paraffin in the sample according to formula (1):
Where,
C - The content of medium chain chlorinated paraffin in the sample, in micrograms per gram (µg/g);
Aa - The overall peak area of medium chain chlorinated paraffin in the sample;
V - The constant volume of sample, in milliliters (mL);
Fa - The total response factor of medium chain chlorinated paraffin in the sample, in per microgram (µg-1);
Vs - The injection volume of medium chain chlorinated paraffin to be tested, in milliliters (mL);
m - The sample mass, in grams (g).
10 Limit of detection
The limit of detection of medium chain chlorinated paraffin in this method is 100µg/g.
11 Precision
In the same laboratory, the absolute difference between the two test results obtained by the same operator using the same equipment, using the same test method to perform independent tests on the same testing object at the same time is not greater than 30% of the arithmetic mean of these two measured values.
Annex B (normative) Total response factor correction method
B.2 Calculate the content of medium chain chlorinated paraffin in the sample
Calculate the content of medium chain chlorinated paraffin in the sample according to the following steps:
a) Calculate the overall peak area Aa of medium chain chlorinated paraffin in the sample according to formula (B.1);
b) Calculate the measured chlorine content D' of medium chain chlorinated paraffin in the sample according to formula (B.4);
c) According to the relationship between the total response factor derived from the standard sample and the measured chlorine content, calculate the total response factor Fa of medium chain chlorinated paraffin in the sample according to formula (B.5);
d) Calculate the content of medium chain chlorinated paraffin in the sample according to formula (1). […]
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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 15 pages — is available in the English PDF.
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