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SN/T 5248-2020: (Method for determination of gold content in imported gold-loaded resin materials-flame atomic absorption spectrometry)
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(Method for determination of gold content in imported gold-loaded resin materials-flame atomic absorption spectrometry)
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Basic data | Standard ID | SN/T 5248-2020 (SN/T5248-2020) | | Description (Translated English) | (Method for determination of gold content in imported gold-loaded resin materials-flame atomic absorption spectrometry) | | Sector / Industry | Commodity Inspection Standard (Recommended) | | Classification of Chinese Standard | G31 | | Classification of International Standard | 83.020 | | Word Count Estimation | 7,762 | | 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 5248-2020: (Method for determination of gold content in imported gold-loaded resin materials-flame atomic absorption spectrometry)
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Determination of gold in imported gold loaded resin materials-
Flame atomic absorption spectrometry
The People's Republic of China Entry-Exit Inspection and Quarantine Industry Standards
Replace SN/T 0654-1997
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. Urumqi Customs of the People’s Republic of China, Shanghai Tuomi Testing Technology Service Co., Ltd., Xinjiang Agriculture
University College of Chemical Engineering, Beilun Customs of the People’s Republic of China, Xinjiang Shuiqingqing Environmental Monitoring Technology Service Co., Ltd., Xinjiang Uyghur
Autonomous Region Analysis and Testing Research Institute, Tianjin Customs of the People's Republic of China, Xinjiang University.
The main drafters of this standard. Liu Jun, Yang Zhong, Zhou Jun, Su Youzhi, Chen Guotong, Du Guangming, Yu Qing, Wang Liang, Zhao Lintong, Hu
Dexin, Liu Weiguo, Wang Cheng, Wang Chong.
Method for determination of gold content in imported gold-loaded resin materials
Flame atomic absorption spectrometry
1 Scope
This standard specifies the atomic absorption spectrometry method for the determination of gold content in gold-loaded resin materials.
This standard applies to the determination of gold content in gold-loaded resin materials.
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 602 Preparation of standard solutions for impurity determination of chemical reagents
GB/T 6682 Analytical laboratory water specifications and test methods
3 Method summary
After the sample is roasted to remove sulfur and organic matter, it is dissolved with hydrochloric acid and nitric acid, and the gold, the adsorbed gold chloride complex or the
After the gold bromine complex is dissolved and liberated with thiourea, its gold content is measured with a flame atomic absorption spectrometer.
4 Reagents and materials
Unless otherwise specified, only reagents confirmed to be analytically pure are used in the analysis, and the experimental water meets the first-grade water specified in GB/T 6682.
4.1 Hydrochloric acid (ρ=1.19 g/mL).
4.2 Nitric acid (ρ=1.42 g/mL).
4.3 Thiourea.
4.4 Bromine.
4.5 Dilute hydrochloric acid (1.9).
4.6 Gold standard stock solution (1 000 μg/mL). Prepare according to GB/T 602 method or directly use certified national standard materials.
4.7 Gold standard working solution (100 μg/mL). Pipette 10 mL of gold standard stock solution (4.6) into a 100 mL volumetric flask, and use dilute hydrochloric acid
(4.5) Dilute to the mark and mix well.
4.8 Aqua regia. mix 3 parts of hydrochloric acid (4.1) and 1 part of nitric acid (4.2), and prepare when used.
4.9 Aqua regia (1.1). Mix 1 part of aqua regia (4.8) and 1 part of water, and prepare when used.
4.10 Saturated bromine water. Dissolve a certain amount of bromine (4.4) in water, partially dissolve bromine (4.4), and take the supernatant to obtain saturated bromine (4.4).
And bromine water.
4.11 Thiourea solution (10 g/L). Weigh 1 g of thiourea (4.3) and dissolve it in 100 mL of water.
4.12 Sodium hydroxide solution (10 g/L). Weigh 10 g of sodium hydroxide and dissolve it in 1 L of water.
4.13 Plastic foam. polyurethane type or polyether type, cut into blocks of 3 cm×3 cm×1 cm, rinse with water before use,
Boil in sodium solution (4.12) for 15 minutes, wash with water until neutral, dry, and set aside.
5 Apparatus and equipment
5.1 Atomic absorption spectrophotometer. equipped with a gold element hollow cathode lamp.
5.2 Analytical balance. Sensitivity is 0.0001 g.
5.3 High-temperature furnace. The temperature can be controlled between 500 ℃ and 1 000 ℃.
5.4 Electric heating plate. can be heated to.200 ℃.
5.5 Oscillator.
5.6 Porcelain crucible. 30 mL.
5.7 Colorimetric tube. 25 mL.
5.8 Volumetric flask. 50 mL.
6 Sample
The particle size of the gold-loaded resin material analysis sample should be less than 0.096 mm, and it should be baked at 105 ℃ ± 5 ℃ for 2 h, and then cooled to room temperature in a desiccator for later use.
7 Analysis steps
7.1 Sample processing
Weigh 10.0 g (accurate to 0.0001 g) of the sample and place it in a 30 mL porcelain crucible (5.6), and place it in a high-temperature furnace (5.3) at 650 ℃
Burn for 2 h, after cooling, transfer to a 250 mL Erlenmeyer flask, add 25 mL of aqua regia (4.9), heat and boil on the electric hot plate (5.4) for 1 h,
Dilute with water to 70 mL, add 3.0 mL saturated bromine water (4.10), and shake quickly. After cooling to room temperature, put in 0.2 g~0.4 g plastic bubble
Foam (4.13), cover the stopper, shake on the shaker (5.5) for 30 minutes, take out the foam with a glass rod, and wash with water to remove foam
The residue and acid on the plastic squeeze out the water. Put the foam plastic into a 25 mL colorimetric tube pre-filled with 15.0 mL thiourea solution (4.11)
In (5.7), put it in a boiling water bath to release for 30 minutes, and take out the colorimetric tube (5.7). Move the foam plastic up to the upper part of the colorimetric tube (5.7) and squeeze it dry
Then take it out, cool the solution to room temperature, dry filter, and take the clear solution for measurement.
7.2 Blank test
Do a blank test with the sample.
7.3 Production of working curve
Pipette 0 mL, 0.20 mL, 0.24 mL, 0.48 mL, 0.68 mL, 0.90 mL gold standard working solution (4.7) into 6 250 mL
In the Erlenmeyer flask, follow the steps in (7.1). The concentrations of gold are 1.33 μg/mL, 1.60 μg/mL, 3.20 μg/mL, 4.53 μg/mL,
6.00 μg/mL, with the concentration of gold (μg/mL) as the abscissa and the absorbance value as the ordinate, draw a standard working curve.
7.4 Determination
Adjust the working conditions of the instrument to make the instrument to the best condition, and perform the standard working solution, sample blank solution and sample solution in sequence.
Determination. If the content of the gold element in the sample solution exceeds the content range of the standard curve, the sample solution can be diluted and re-measured. Instrument work
See Appendix A for conditions.
8 Result calculation
Calculate the content of gold in the sample according to formula (1).
ωi-the content of each gold element, in micrograms per gram (μg/g);
cx-the concentration of gold in the sample solution obtained from the working curve, in micrograms per milliliter (μg/mL);
c0-the concentration of gold in the blank solution obtained from the working curve, in micrograms per milliliter (μg/mL);
V-the volume of the sample solution, the unit is milliliters (mL);
m-the mass of the sample, the unit is grams (g);
k - Dilution factor.
Note. The result is the arithmetic average of two parallel determination results, expressed to two decimal places.
9 Precision
Under repeatability conditions, the absolute difference between the two independent determination results is not more than 20% of the arithmetic mean. Under repeatability conditions, two
The absolute value of a laboratory measurement result is not more than 30% of the arithmetic mean.
Appendix A
(Informative appendix)
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