GB/T 15080.5-1994 Chemical analysis method for antimony concentrates Determination of zinc content GB/T15080.5-1994 standard download decompression password: www.bzxz.net

UDC669.754：543.06
National Standard of the People's Republic of China
GB/T 15080.1~15080.9--94
Methods for chemical analysis of antimony concentrates
Published on May 11, 1994
State Administration of Technical Supervision
Implementation on December 1, 1994
National Standard of the People's Republic of China
Methods for chemical analysis of antimony concentrates
Antimony concentrates-Determination of zinc content
1 Subject content and scope of application
This standard specifies the method for determining the zinc content in antimony concentrate. This standard is applicable to the determination of zinc content in antimony concentrate. Determination range: 0.001%~～1%. 2 Reference standards
GB1.4 Guidelines for standardization work Provisions for the preparation of chemical analysis methods GB1467 General principles and general provisions for chemical analysis methods for metallurgical products GB7728 General principles for flame atomic absorption spectrometry for chemical analysis of metallurgical products 3 Summary of methods
GB/T 15080.5-94
After the sample is dissolved in hydrochloric acid and nitric acid and evaporated to dryness, hydrofluoric acid is added to volatilize to remove silicon, and then hydrobromic acid is added to volatilize to remove antimony. In a dilute hydrochloric acid medium, use an air-acetylene flame at a wavelength of 213.8nm on an atomic absorption spectrometer to measure the absorbance, and use the working curve method to obtain the zinc content. 4 Reagents
The water used in this standard is double distilled water.
4.1 Hydrochloric acid (p1.19g/mL), high-grade purity. 4.2 Nitric acid (pl.42g/mL), high-grade purity. 4.3 Hydrofluoric acid (p1.13g/mL), high-grade purity. 4.4 Perchloric acid (p1.67g/mL).
4.5 Hydrobromic acid (p1.48g/mL), high purity. 4.6 Hydrochloric acid (1+1).
4.7 Zinc standard stock solution: Weigh 1.0000g of metallic zinc (99.99%), place in a 250mL beaker, add 20mL of hydrochloric acid (4.6), heat to boiling after a violent reaction, remove and cool, transfer to a 1000mL volumetric flask, dilute to scale with water, and mix. This solution contains 1 mg zinc per mL.
4.8 Zinc standard solution: Transfer 20.00mL of zinc standard stock solution (4.7) to a 1000mL volumetric flask, add 20mL of hydrochloric acid (4.6), dilute to scale with water, and mix. This solution contains 20μg zinc per mL. 5 Instruments
Atomic absorption spectrometer, with zinc hollow cathode lamp. Under the best working conditions of the instrument, any instrument that can meet the following indicators can be used. The minimum requirement for precision is to measure the absorbance of the highest standard solution 10 times, and the standard deviation should not exceed 1.5% of the average absorbance. Approved by the State Bureau of Technical Supervision on May 11, 1994 and implemented on December 1, 1994
GB/T 15080.5--94
Measure the absorbance of the lowest standard solution (not the "zero" standard solution) 10 times, and its standard deviation should not exceed 0.5% of the average absorbance of the highest standard solution.
Characteristic concentration: In a solution consistent with the matrix of the test sample solution, the characteristic concentration of zinc should not be greater than 0.01ug/mL. Working curve linearity: Divide the working curve into five equal segments according to concentration. The ratio of the absorbance difference of the highest segment to the absorbance difference of the lowest segment should not be less than 0.7 .
For instrument working conditions, see Appendix A (reference). 6 Test specimens
6.1 The particle size of the test specimen should be less than 0.100 mm.
6.2 The test specimen should be dried at 100-105°C for 1 hour and then placed in a desiccator to cool to room temperature. 7 Analysis steps
7.1 Test material
Weigh the test specimen according to Table 1, accurate to 0.0001 g. Table 1
Zinc content.%
0.0010~0.0050
>0. 005 0~0. 020
>0. 020~0. 10
>0. 10~0.50
>0. 50~1. 00
Sample amount g
Volume of volumetric flask, mL
Carry out two independent determinations and take the average value. 7.2 Blank test
Carry out a blank test with the sample.
7.3 Determination
Add hydrochloric acid (4.6) volume before dilution, mL
Pipette solution volume, mL
7.3.1 Place the sample (7.1) in a 100mL polytetrafluoroethylene crucible and Moisten with a small amount of water, add 5 mL of hydrochloric acid (4.1), heat to drive off hydrogen sulfide, add 20 mL of aqua regia, heat to dissolve, evaporate to dryness at low temperature, cool slightly, add 2 mL of perchloric acid (4.4) and 10 mL of hydrofluoric acid (4.3) and evaporate to dryness, continue to add about 5 mL of hydrofluoric acid (4.3) and evaporate to dryness to remove silicon, add 1 mL of perchloric acid (4.4) and evaporate to dryness, repeat 2~3 times, cool slightly, add 1 mL of hydrochloric acid (4.1) and 4 mL of hydrobromic acid (4.5) and evaporate to dryness, evaporate Remove antimony. Continue to add 3mL hydrobromic acid (4.5) and evaporate to dryness, add 2mL hydrochloric acid (4.1) and evaporate to dryness. Add 4mL hydrochloric acid (4.6) to dissolve the residue with slight heat, wash the cup wall with about 5mL water, heat to boil, and cool to room temperature. Transfer to a volumetric flask according to Table 1 and add hydrochloric acid (4.6) to dilute to scale with water, and mix well. [When the zinc content is greater than 0.02%, transfer the solution according to Table 1 to a 50mL volumetric flask, add 3.0mL hydrochloric acid (4.6) to Dilute with water to the scale and mix well]. 7.3.2 Use air-acetylene flame to zero the atomic absorption spectrometer at a wavelength of 213.8nm with water and measure the absorbance of the solution. 7.4 Drawing of working curve:
Pipette 0, 1.00, 2.00, 3.00, 4.00, 5.00mL of zinc standard solution (4.8) and place them in a 100mL volumetric flask, add 8mL of hydrochloric acid (4.6), dilute with water to the scale and mix well. Measure the absorbance of the standard solution under the same conditions as the sample determination. Draw the working curve with zinc concentration as the horizontal axis and absorbance (minus the absorbance of the zero concentration solution) as the vertical axis. 8 Expression of analysis results
Calculate the percentage of zinc by the following formula:
Wherein: Gi—
GB/T 15080.5—94
Zn(%) = (c1 = co) V. : V, × 10-sX100
Zinc concentration of the sample solution obtained from the working curve, ug/mL; Zinc concentration of the blank solution obtained from the working curve, μg/mL; Co
V. - total volume of solution, mL;
V--—volume of the solution transferred, mL;
V2—dilution volume after the solution was transferred, mL; m
Mass of the sample, g.
The result should be expressed to two decimal places. If it is less than 0.1%, it should be expressed to three decimal places. 9 Allowable Difference
The difference between the analysis results of laboratories shall not be greater than the allowable difference listed in Table 2. Table 2
Zinc Content
≤0. 005 0
>0. 005 0～0.010
>0.010～0.030www.bzxz.net
>0. 030~～0. 050
>0.050～0.100
>0. 01~0. 30
>0. 30 ~0. 50
>0. 50~1. 00
Allowable difference
GB/T15080.5—94
Appendix A
Instrument working conditions
(reference)
The working conditions of WFX-1B atomic absorption spectrometer are shown in Table A1: Table Al
Determination elements
Additional notes:
Wavelength, nm
Lamp current, mA
Spectral passband, nm
This standard is proposed by China Nonferrous Metals Industry Corporation. This standard is technically managed by Beijing Research Institute of Mining and Metallurgy. Observation height, mm
This standard is drafted by Xikuangshan Mining Bureau and Hunan Nonferrous Metals Research Institute. This standard is drafted by Hunan Nonferrous Metals Research Institute. The main drafters of this standard are Hu Youfang and Luo Bifang. 18
Air flow, L/min
Acetylene flow, L/min
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