GB/T 8220.12-1998 Chemical analysis of bismuth - Determination of nickel content by electrothermal atomic absorption spectrometry

This standard specifies the determination method of nickel content in bismuth. This standard is applicable to the determination of nickel content in bismuth. Determination range: 0.0003%~0.001%. GB/T 8220.12-1998 Chemical analysis method for bismuth Determination of nickel content by electrothermal atomic absorption spectrometry GB/T8220.12-1998 Standard download decompression password: www.bzxz.net

GB/T 8220. 12-1998
This standard is a revision of Appendix H of GB/T915-1995 "Bismuth". This standard complies with:
Guidelines for Standardization Work Provisions for the Preparation of Chemical Analysis Methods GB/T 1. 4-1988
GB/T1467-1978 General Principles and General Provisions for Chemical Analysis Methods for Metallurgical Products GB/T7729-1987 General Rules for Spectrophotometric Methods for Chemical Analysis of Metallurgical Products This standard is a supporting standard for GB/T915-1995 "Bismuth". The preparation method of this standard complies with the provisions of GB/T1.1-1993 "Guidelines for Standardization Work Unit 1: Rules for Drafting and Presentation of Standards Part 1: Basic Provisions for the Preparation of Standards". From the date of implementation, this standard will also replace Appendix H of GB/T915-1995 "Bismuth". Appendix A of this standard is a prompt appendix.
This standard is proposed by China National Nonferrous Metals Industry Corporation. This standard is under the jurisdiction of the Standard and Metrology Institute of China National Nonferrous Metals Industry Corporation. This standard was drafted by Zhuzhou Refinery. The main drafters of this standard are Zhu Lijuan and Zhang Dongfeng. 358
1 Scope
National Standard of the People's Republic of China
Chemical analysis method of bismuth
Determination of nickel content by electrothermal atomic absorption spectrometric method
Methods for chemical analysis of bismuth--Determination of nickel rontent-Electrothermal atomic absorption spectrometric method This standard specifies the determination method of nickel content in bismuth. This standard is applicable to the determination of nickel content in bismuth. Determination range: 0.0003%~0.001%. 2 Method Summary
GB/T8220. 12-. 998
The sample was dissolved in nitric acid, and the appropriate solution was introduced into the electrothermal atomizer. The absorbance of the base nickel was measured at a wavelength of 232.0nm using an absorption spectrometer. The working curve was drawn using the matrix addition method to obtain the nickel content in the sample. 3 Reagents
The water used for preparing the solution and the analysis was double distilled water. The utensils used in the experiment were soaked in dilute nitric acid and then thoroughly cleaned with double distilled water. 3.1 Nitric acid (1+1), high-grade purity.
3.2 Nitric acid (2+98), high-grade purity.
3.3 Nickel standard stock solution: Weigh 1.0000g of nickel metal (≥99.99%) into a 100ml beaker, add 20ml of nitric acid (3.1) and cover with Table III, heat at low temperature until completely dissolved, remove, cool, transfer the solution into a 1000ml volumetric flask, dilute to scale with water, and mix. This solution contains mg nickel per ml.
3.4 ​​Nickel standard solution: Transfer 1.00mL of nickel standard stock solution (3.3) into a 100ml volumetric flask, dilute to scale with nitric acid (3.2) and mix. This solution contains 10g nickel per ml.
3.5 Nickel standard solution: Transfer 10.00mL of nickel standard solution (3.4) into a 100mL volumetric flask, dilute to scale with nitric acid (3.2), and mix. This solution contains 1μg nickel per ml.
3.6 Bismuth solution (100 mg/ml): Weigh 10.00 g of high-purity bismuth (≥99.999%) in a 250 mL tall beaker, add 40 ml of nitric acid (3.1), heat and dissolve completely, remove, cool, transfer to a 100 ml volumetric flask, rinse the beaker with 5 ml of nitric acid (3.1), add to the volumetric flask, dilute to scale with nitric acid (3.2), and mix. 4 Instruments
Graphite furnace atomic absorption spectrometer (with buckle background device), with automatic sampler and nickel hollow cathode lamp. Instrument working conditions are shown in Appendix A (suggested appendix). 5 Analysis steps
5.1 Sample
Approved by the State Administration of Quality and Technical Supervision from 1998 to 08-19 and implemented on 1999-03-01
Weigh 0.5000 g of sample.
5.2 Blank test
Carry out a blank test with the sample.
5.3 Determination
GB/T 8220. 12-1998
5.3.1 Place the sample (5.1) in a 25mL beaker, add 4.0mL nitric acid (3.1), cover with blood, heat at low temperature until completely dissolved, remove, cool, transfer to a 50mL volumetric flask, dilute to the scale with nitric acid (3.2), and mix well. 5.3.2 Adjust the instrument parameters to the optimal state according to Appendix A, and adjust the electric heating atomizer according to the selected conditions. Use the selected heating program to burn the graphite tube twice.
5.3.3 Inject the test solution into the atomizer and atomize according to the atomization program. Measure the absorbance of nickel at a wavelength of 232.0nm. Measure each test solution twice, take the average value, subtract the average value of the absorbance of the blank solution of the sample, and find the corresponding nickel concentration on the working curve. 5.4 Drawing of working curve
5.4.1 Transfer 0, 1.00, 2.00, 3.00, 4.00.5.00mL of nickel standard solution (3.5) to a set of 50mL volumetric flasks, add 5.0mL of bismuth solution (3.6) respectively, dilute to the scale with nitric acid (3.2), and mix. 5.4.2 Under the same conditions as the test sample, measure the absorbance of the standard solution. Measure each solution twice, take the average value, subtract the average value of the absorbance of the "zero" concentration solution in the standard series, and draw the working curve with nickel concentration as the horizontal axis and the average absorbance as the vertical axis. 6 Calculation and expression of analysis results
Calculate the percentage of nickel according to the following formula:
Ni(%) E:V× 10-6
Wherein: c-Ni concentration obtained from the working curve, ug/mL; V-total volume of test solution, mL;
m-mass of a test material, g.
Analysis results should retain 2 significant figures.
7 Allowable difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in the following table: Nickel content
0. 000 3 ~~ 0. 000 6
>0. 000 6-~0. 001 0
Allowance difference
GB/T8220.121998
Appendix A
(Suggestive appendix)
Instrument working conditions
Reference working conditions for determination by PE3030B atomic absorption spectrometer and HGA-600 graphite furnace atomizer. See Table A1: Table Al
Wavelength, nm
Slit, nmwww.bzxz.net
Lamp current, mA
Graphite tube
Injection stack + μl
Pyrolytic coating plus platform
Atomization
Temperature, C
Hold, s
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