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Basic data
| Standard ID | SN/T 5242-2020 (SN/T5242-2020) |
| Description (Translated English) | (Import and export textiles Determination of germanium content Inductively coupled plasma mass spectrometry) |
| Sector / Industry | Commodity Inspection Standard (Recommended) |
| Classification of Chinese Standard | W04 |
| Classification of International Standard | 59.010 |
| Word Count Estimation | 9,944 |
| Date of Issue | 2020-08-27 |
| Date of Implementation | 2021-03-01 |
| Regulation (derived from) | General Administration of Customs Announcement No. 98 [2020] |
| Issuing agency(ies) | General Administration of Customs |
SN/T 5242-2020: (Import and export textiles Determination of germanium content Inductively coupled plasma mass spectrometry)
---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Textiles for import and export Determination of germanium-
Inductively coupled plasma mass spectrometry method
The People's Republic of China Entry-Exit Inspection and Quarantine Industry Standards
2020-08-27 release
2021-03-01 implementation
Issued by the General Administration of Customs of the People's Republic of China
Foreword
This standard was drafted in accordance with the rules given in GB/T 1.1-2009.
This standard was proposed and managed by the General Administration of Customs of the People's Republic of China.
Drafting organizations of this standard. Shaoxing Customs of the People's Republic of China, the Patent Office of the State Intellectual Property Office, China Inspection and Control Technology Group Co., Ltd.
the company.
The main drafters of this standard. Yu Chunhua, Dong Wenhong, Qiao Pengjuan, Yu Haiyong.
Determination of germanium content in import and export textiles
Inductively coupled plasma mass spectrometry
Warning personnel who use this standard should have practical experience in formal laboratory work. This standard does not point out all possible safety issues. The user is responsible
Take appropriate safety and health measures and ensure compliance with the conditions stipulated by relevant national laws and regulations.
1 Scope
This standard specifies the inductively coupled plasma mass spectrometry (ICP-MS) method for the determination of germanium in textiles.
This standard applies to the determination of germanium content in textiles.
2 Normative references
The following documents are indispensable for the application of this document. For dated reference documents, only the dated version applies to this article
Pieces. For undated reference documents, the latest version (including all amendments) is applicable to this document.
GB/T 6682 Analytical laboratory water specifications and test methods
GB/T 8170 Numerical rounding rules and the expression and determination of limit values
3 Principle
After the sample is digested by microwave, the measured element in the sample solution undergoes a plasma process and enters the mass spectrometer through the nickel sampling cone.
The response value of the mass spectrum is directly proportional to the content of the element to be measured. Compared with the standard working curve, indium is used as the internal standard, and the internal standard method is used for quantification.
Calculate the content of germanium in the sample.
4 Reagents and materials
Unless otherwise specified, the reagents used are all premium grade pure, and the experimental water is the first grade water that meets the requirements in GB/T 6682.
4.1 Nitric acid (MOS grade, 65%).
4.2 Hydrogen peroxide (30% aqueous solution).
4.3 Nitric acid solution (2 98). Take 20 mL of nitric acid (4.1) and slowly add 980 mL of ultrapure water.
4.4 Germanium (Ge) standard stock solution (1000 μg/mL). the element standard solution within the validity period of the certificate of standard material can be used, and the concentration
It is 1000 μg/mL.
4.6 Germanium standard intermediate working solution (10 μg/mL). Pipette 1.0 mL of germanium standard stock solution (4.4), use nitric acid solution (4.3) to determine
Volume to 100 mL.
4.7 Germanium standard working solution (reference concentration range is 0.2 μg/L~40.0 μg/L). the germanium standard intermediate working solution (4.6) is gradually diluted
The medium is nitric acid solution (4.3).
4.8 Indium (In) standard stock solution (1000 μg/mL). as an internal standard in ICP-MS detection, a certificate of standard substance can be used
The element standard solution within the expiry date of, the concentration is 1000 μg/mL.
4.9 Indium standard intermediate solution (10 μg/mL). Pipette 1.0 mL of indium standard stock solution (4.8), and dilute to volume with nitric acid solution (4.3)
100 mL.
4.10 Indium standard working solution (1.0 μg/mL). diluted from indium standard intermediate solution (4.9) to 1.0 μg/L, the medium is nitric acid solution
(4.3).
4.11 Argon. The purity is greater than or equal to 99.999%.
Note. The prepared standard solution should be promptly transferred to the special plastic reagent bottle for standard solution storage, and stored in the refrigerator at 0 ℃ ~ 5 ℃. The storage period is generally 1 month.
5 Apparatus and equipment
5.1 Inductively coupled plasma mass spectrometer.
5.2 Analytical balance. Sensitivity 1.0 mg.
5.3 Microwave digestion system.
5.4 Volumetric flask. 50 mL.
5.5 Pipette. 0.5 mL, 1.0 mL, 2.0 mL, 5.0 mL.
5.6 Water phase filter membrane. 0.45 μm.
5.7 Electrothermal digestion device.
6 Sample preparation and storage
The sample should be representative as a whole, should contain various yarn and fiber components of the fabric, and the number of samples should be sufficient for testing. will
Cut the 10 g sample into pieces not larger than 5 mm × 5 mm, and mix them evenly. The sample is put into a clean container, sealed, and marked with a mark. test
The sample should be stored at room temperature.
7 Measurement procedure
7.1 Sample digestion
Weigh two 0.5 g samples (for parallel test) from the shredded mixed samples, accurate to 0.001 g, and place them in the microwave digestion inner tank.
Add 5.0 mL of nitric acid (4.1), and then add 3.0 mL of hydrogen peroxide (4.2) to fully infiltrate the sample, and preheat the sample in a 120 ℃ electrothermal digester.
After 30 minutes of digestion, place it in a microwave digestion system for digestion. Refer to Table A.1 in Appendix A for the digestion procedure. After digestion, take out the digestion tank
Cool to room temperature.
7.2 Constant volume of sample solution
Transfer the solution to a 50.0 mL volumetric flask, rinse the tank wall with water 3 times or more, combine the lotions and dilute to the mark, and mix. take
5mL water phase filter membrane (5.6), the filtrate should be used for instrument analysis and testing as soon as possible.
7.3 Instrument working conditions
It should be adjusted to the best condition according to the performance of the respective instruments. For working conditions, see Table B.1 in Appendix B.
7.4 Sample determination
The internal standard working solution (4.10) was added online in the analysis, and the internal standard calibration quantitative analysis method in the ICP-MS analysis method was used for determination.
7.5 Blank test
Except that the sample to be tested is not added, the others are operated according to the above steps.
8 Result calculation
The content of germanium in textiles is calculated according to formula (1).
X - Germanium content in textile samples, in milligrams per kilogram (mg/kg);
C - The concentration of the measured element in the sample solution, in micrograms per liter (μg/L);
0C-the concentration of the measured element in the blank solution, in micrograms per liter (μg/L);
V - The constant volume of the sample solution, the unit is milliliters (mL);
m - The mass of the sample, in grams (g).
The test result is the average of the two determinations, and the calculated result is expressed to two decimal places, and the data obtained is rounded to comply with GB/T 8170.
Value rounding rules.
9 Determination of the lower limit, recovery rate and relative standard deviation
9.1 Low limit of determination
The lower limit of determination of this standard method is 0.020 mg/kg.
9.2 Recovery rate and relative standard deviation
The recovery rate and relative standard deviation of this standard method (within the range of different additive concentrations) are shown in Table 1.
Appendix A
(Informative appendix)
Sample microwave digestion reference program
Appendix B
(Informative appendix)
Reference operating conditions for plasma mass spectrometry
The parameters listed in this table were completed on the Bruker M90 ICP-MS. The test instrument models listed here are for reference only and do not involve commercial purposes.
Yes, standard users are encouraged to try instruments of different manufacturers and models.
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