GB/T 15080.3-1994 Chemical analysis methods for antimony concentrates - Determination of lead content
Some standard content:
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
Implemented on December 1, 1994
Published by the State Administration of Technical Supervision
National Standard of the People's Republic of China
Methods for chemical analysis of antimony concentrates
Antimony concentrates--Determination of lead content
Method 1: Flame atomic absorption spectrometry
1 Subject content and scope of application
This standard specifies the method for the determination of lead content in antimony concentrate. This standard is applicable to the determination of lead content in antimony concentrate. Determination range: 0.004% to 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 chemical analysis of metallurgical products by flame atomic absorption spectrometry 3 Summary of methods
GB/T 15080.3-94
After the sample is dissolved in hydrochloric acid and nitric acid, hydrobromic acid is added to volatilize and remove antimony. In a dilute hydrochloric acid medium, the absorbance is measured at a wavelength of 283.3nm using an air-acetylene flame on an atomic absorption spectrometer. The lead content is obtained by the working curve method. 4 Reagents
4.1 Hydrochloric acid (pl.19 g/mL).
4.2 Nitric acid (pl.42g/mL).
4.3 Hydrobromic acid (p1.48g/mL).
4.4 Hydrochloric acid (1+1).
4.5 Nitric acid (1+1).
4.6 Lead standard stock solution: Weigh 0.5000g of metallic lead (99.99%) into a 250mL beaker, add 20mL of nitric acid (4.5), dissolve with slight heat until clear, boil for 2-3min to drive off nitrogen oxides, remove and cool, transfer to a 500mL volumetric flask, dilute to scale with water, and mix. This solution contains 1mg lead per mL.
4.7 Lead standard solution: Transfer 50.00mL of lead standard stock solution (4.6) into a 500mL volumetric flask, add 10mL of hydrochloric acid (4.4), dilute to scale with water, and mix. This solution contains 100μg lead per mL. 5 Instruments
Atomic absorption spectrometer with lead hollow cathode lamp. Under the working conditions of the instrument, any instrument that can meet the following indicators can be used. Approved by the State Administration of Technical Supervision on May 11, 1994, and implemented on December 1, 1994
GB/T15080.394
Minimum precision requirement: measure the absorbance of the highest standard solution 10 times, and its standard deviation should not exceed 1.5% of the average absorbance. 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 that is consistent with the matrix of the sample solution, the characteristic concentration of lead should not be greater than 0.2μg/mL. Working curve linearity: Divide the working curve into five sections according to concentration, and the ratio of the absorbance difference of the highest section to the absorbance difference of the lowest section should not be less than 0.7.
See Appendix A (reference) for instrument working conditions. 6 Sample
6.1 The particle size of the sample should be less than 0.100mm.
6.2 The sample should be dried at 100105℃ for 1h, and then placed in a desiccator to cool to room temperature. 7 Analysis steps
7.1 Sample
Weigh the sample according to Table 1, accurate to 0.0001g. Table 1
Lead content.%
0. 004 0~~0. 010
>0.010~0. 050
>0. 050~-0. 25
>0. 25~~1. 00
Carry out two independent determinations and take the average value. 7.2 Blank test
Carry out a blank test along with the sample.
7.3 Determination
Sample quantity·name
7.3.1 Place the sample (7.1) in a 100mL beaker, moisten with a small amount of water, add 5mL hydrochloric acid (4.1), drive off hydrogen sulfide on a hot plate, add 20mL aqua regia, heat to dissolve, evaporate to dryness at low temperature, cool slightly, add 1mL hydrochloric acid (4.1) and 4mL hydrobromic acid (4.3) to evaporate to dryness, volatilize to remove antimony. Continue to add 3mL hydrobromic acid (4.3) to evaporate to dryness, add 2mL hydrochloric acid (4.1) and evaporate to dryness again, add 2mL hydrochloric acid (4.4) to dissolve the residue with slight heat, wash the wall of the cup with about 5mL water, heat to boil, and cool to room temperature. Transfer to a 25mL volumetric flask, dilute to scale with water, and mix [when the lead content is 0.25%, transfer to a 50mL volumetric flask, add 2mL hydrochloric acid (4.4), dilute to scale with water, and mix]. 7.3.2 Use air-acetylene flame to zero the atomic absorption spectrometer at a wavelength of 283.3 nm with water and measure the absorbance of the solution. Find the corresponding lead concentration from the working curve.
7.4 Working curve drawing
Put 0, 2.50, 5.00, 10.00, 15.0020.00, 25.00mL of lead standard solution (4.7) into a group of 100mL volumetric flasks, add 8mL of hydrochloric acid (4.4), dilute to the scale with water, mix well, and measure the absorbance of the standard solution under the same conditions as the test sample. With lead concentration as the abscissa and absorbance (minus the absorbance of the zero-concentration solution) as the ordinate, draw the working curve. 8 Expression of analysis results
Calculate the percentage of lead according to formula 1):
(c= co)V× 10- × 100
Pb(%) =
GB/T 15080.3-94
Wherein: c—lead concentration of the sample solution obtained from the working curve, /nL; Co--lead concentration of the blank solution obtained from the working curve, μg/mL; V-volume of test solution, mL;
-mass of the sample, g.
The result should be expressed to two decimal places. When it is less than 0.1%, it should be expressed to three decimal places. 9 Allowable difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table 2. Table 2
Lead content
>0.010～0. 030
>0.030~0.080
>0. 080~0. 120
>0.12~0.18
>0. 18~0. 25
>0. 25~0. 50
>0.50～1.00
Method 2: Oscillographic polarography
10 Subject content and scope of application
This standard specifies the method for determining the lead content in antimony concentrate. This standard is applicable to the determination of lead content in antimony concentrate. Determination range: 0.004%～1%. This standard is not used as an arbitration analysis method.
11 Reference standardsbzxz.net
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 Method summary
Allowance
After the sample is dissolved in hydrochloric acid and nitric acid and evaporated to dryness, hydrobromic acid is added to volatilize and remove antimony. The residue is dissolved in hydrochloric acid base solution, and iron powder is used to reduce interfering ions. The lead content is determined on an oscillographic polarograph.
13 Reagents
13.1 Reduced iron powder.
13.2 Hydrochloric acid (p1.19 g/mL).
13.3 Nitric acid (p1.42g/mL).
13.4 Hydrobromic acid (pl.48g/mL).
13.5 Hydrochloric acid base solution: Weigh 40g sodium chloride and place it in a 500mL beaker, dissolve it in water and transfer it to a 1000mL volumetric flask, add 9
GB/T15080.3-94
250mL hydrochloric acid (13.2), 10mL animal glue solution (10g/L), dilute to scale with water, and mix well. 13.6 Lead standard solution.
13.6.1 Weigh 1.0000g metallic lead (99.99%) in a 300mL beaker, add 20mL nitric acid (1+1), heat and dissolve until clear, boil for about 1min to drive off nitrogen oxides, remove and cool, transfer to a 1000mL volumetric flask, dilute to scale with water, and mix well. This solution contains 1mg lead in 1mL.
13.6.2 Transfer 20.00mL of lead standard solution (13.6.1) is placed in a 200mL volumetric flask, diluted to the mark with water, and mixed. This solution contains 0.1 mg lead in 1mL.
14 Instrument
Oscillographic polarograph.
15 Sample
15.1 The sample particle size should be less than 0.100rmm. 15.2 The sample should be dried at 100~105℃ for 1h and placed in a desiccator to cool to room temperature. 16 Analysis steps
16.1 Sample
Weigh the sample according to Table 3, accurate to 0.0001g. Table 3
Lead content.%
>0. 20~0.50
>0. 50～~1. 00
Carry out two independent determinations and take the average value. 16.2 Blank test
Carry out a blank test with the sample.
16.3 Determination
Sample quantity
16.3.1 Place the sample (16.1) in a 100mL beaker and moisten it with water. Add 10mL hydrochloric acid (13.2), shake, and heat to remove all hydrogen sulfide. Remove and cool slightly, add 3mL nitric acid (13.3), heat on a hot plate to dissolve and evaporate to dryness. Remove and cool slightly. Add 3mL hydrochloric acid (13.2) and 3mL hydrobromic acid (13.4), and evaporate until white smoke is emitted. Repeat this operation 1 to 3 times. Cool. Add 2mL hydrochloric acid (13.2) and evaporate to dryness, remove and cool. 16.3.2 Add 15mL hydrochloric acid base solution (13.5), heat slightly to dissolve soluble salts, and cool to room temperature. Wash with hydrochloric acid base solution (13.5) into a 25mL volumetric flask, dilute to the mark, and mix. 16.3.3 Take part of the solution (16.3.2) and place it in a 100mL beaker, add 0.1~0.3g reduced iron powder (13.1). Leave for 15min and shake occasionally. Pour an appropriate amount of clear solution into a 10mL electrolytic cup, start scanning at -0.38V (for saturated calomel electrode) on the oscillographic polarograph, and measure the peak current.
16.3.4 Accurately transfer three different amounts of lead standard solution with a lead content close to that of the sample into a 100mL beaker, add 2mL of hydrochloric acid (13.2), heat and evaporate to dryness, remove and cool slightly. The following is carried out according to 16.3.2 and 16.3.3. Measure the peak current simultaneously with the test solution and calculate the result by comparison method.
17 Expression of analysis results
Calculate the percentage of lead according to formula 2):
Wherein: hx--peak current of the sample solution, uA; GB/T15080.3-94
Pb(%) =
S——Sensitivity used to measure the peak current of the sample solution; m-mass of the sample, g;
-Comparison value calculated from the peak current of the standard solution, uA/g. F
h标1·S标1+h标2·S标2
h标3·S标3]
The analysis results are expressed to two decimal places; when less than 0.1%, they are expressed to three decimal places. Allowable difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table 4. Table 4
>0.010~0.030
>0. 030~0. 080
>0. 080~0. 120
>0. 12~0. 18
>0. 18~0. 25
>0. 25~0. 50
>0. 50~~1. 00
·（2）
GB/T15080.3—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 was drafted by Xikuangshan Mining Bureau and Hunan Nonferrous Metals Research Institute. This standard was drafted by Hunan Nonferrous Metals Research Institute. The drafters of this standard are Hu Youfang, Luo Bifang and Tang Jinglan. 12
Air flow, L/min|B flow, L/min8.3
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