GB/T 40030-2021 English PDF (GBT40030-2021)

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.

GB/T 40030-2021
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 31.020
L 10
Determination of medium chain chlorinated paraffins
in electrical and electronic products
ISSUED ON: APRIL 30, 2021
IMPLEMENTED ON: NOVEMBER 01, 2021
Issued by: State Administration for Market Regulation;
Standardization Administration of the People's Republic of
China.
Table of Contents
Foreword ... 3
1 Scope ... 4
2 Normative references ... 4
3 Terms and definitions ... 4
4 Principle ... 5
5 Reagents and materials ... 5
6 Instruments ... 5
7 Samples ... 6
8 Test steps ... 6
9 Test data processing ... 9
10 Limit of detection ... 9
11 Precision ... 9
Annex A (informative) Total ion current chromatogram of medium chain
chlorinated paraffin ... 10
Annex B (normative) Total response factor correction method ... 11
Determination of medium chain chlorinated paraffins
in electrical and electronic products
WARNING -- PERSONNEL USING THIS STANDARD SHALL HAVE
PRACTICAL EXPERIENCE IN FORMAL LABORATORY WORK. THIS
STANDARD DOES NOT POINT OUT 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 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.
e) Establish the linear relationship between the total response factor Fa of the medium chain chlorinated paraffin of the standard solution and the
measured chlorine content D', see formula (B.5).
Where,
A - The peak area of CmH2m+2-nCln;
Aa - The overall peak area of medium chain chlorinated paraffin;
Fa - Total response factor, in per microgram (μg-1);
Cs - The mass concentration of medium chain chlorinated paraffin in standard solution, in micrograms per milliliter (μg/mL);
Vs - The injection volume of the instrument test standard solution, in milliliters (mL);
D - The theoretical chlorine content of CmH2m+2-nCln;
M - The relative molecular mass of CmH2m+2-nCln and Cl relative atomic mass; D’ - The measured chlorine content of medium chain chlorinated paraffins; a, b - The linear equation parameters of the total response factor Fa of medium chain chlorinated paraffins and the measured chlorine content D'. 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).