GB/T 5120.4-1995 Chemical analysis methods for crude copper - Determination of lead, bismuth and antimony content
Some standard content:
National Standard of the People's Republic of China
Methods for chemical analysis of blister copperDetermination of Lead.Bismuth and Antimony contents1Subject content and scope of application
This standard extends the method for determination of lead, bismuth and antimony in blister copper. GB/T 5120.4-1995
Replaces GB5120.4~5126.68
This standard applies to the determination of lead, bismuth and antimony in blister copper. Determination range: Ph 0.05% ~ 0.60%; Bi 0.008% 0.15%; Sb 0. 05% -~ 0. 60%
2 Reference standards
GB1.4 Standardization work guidelines Chemical analysis method standard compilation regulations GB1467 General principles and general regulations for chemical analysis methods of metallurgical products GB7728 General principles for chemical analysis methods of metallurgical products Flame atomic absorption spectrometry 3 Method summary
The sample is dissolved in nitric acid, and lead, bismuth and antimony are enriched in an ammonia solution with iron hydroxide and lanthanum hydroxide as carriers, and separated from copper. In a dilute hydrochloric acid medium, use an air-acetylene flame on an atomic absorption spectrometer to measure the absorbance of each element at the wavelength listed in Table 1 Table 1
Wavelength, mm
4 Reagents
4.1 Nitric acid (pl.42 g/mL).
Hydrochloric acid (pl.19 g/mL).
4.3 Ammonia water (p1.90 g/mL).
4.4 Hydrochloric acid (1+1).
4.5 Hydrochloric acid (1+25).
4.6 Hydrochloric acid (1+50).
4.7 Hydrogen water (1+40).
4.8 Nitric acid solution: Weigh 5.87g La2O: add 20mL nitric acid (1+1) to a 250ml beaker to dissolve, slightly boil to drive off nitrogen oxides, remove, cool to room temperature, transfer to a 200ml volumetric flask, dilute to scale with water, and mix well. This solution contains 25ml of lanthanum in 1ml. 4.9 Ferric nitrate solution: Weigh 73.40g ferric nitrate [Fe(NO),·9Hz0 in a 400mL beaker. Dissolve in water, add 10ml nitric acid, transfer to a 1000ml volumetric flask, dilute to the mark with water, and mix. This solution contains 10mg iron in 1ml. 4.10 Lead standard solution: Weigh 0.2500g lead (99.99%) in a 250ml beaker, add 50ml nitric acid (1+1). Table IIIL: Approved by the State Administration of Technical Supervision on October 17, 1995 188
199603-01 Implementation
GB/T 5120.4 - 1995
Heat to completely dissolve, slightly boil to drive off nitrogen oxides, remove, cool to room temperature, wash the surface blood and the wall of the cup with water, transfer to a 500ml volumetric flask. Dilute to the mark with water, and mix. 1 ml of this solution contains 500 pg of lead. 4.11 Bismuth standard solution: Weigh 0.4000 g of bismuth (99.99%) into a 250 ml beaker, add 50 ml of nitric acid (1+1), cover with a long III and heat until completely dissolved, and drive off nitrogen oxides with a slight boil. Remove and cool to room temperature. Wash the watch glass and the wall of the beaker with nitric acid (1+25), then transfer to a 1000 ml volumetric flask with nitric acid (1+25), dilute to the mark, and mix well. 1ml of this solution contains 400μg bismuth, 4, 12 antimony standard solution: weigh 0.4788g antimony trioxide (spectrally pure) into a 250ml beaker 41, add 50ml acid (1.2) and cover 1 beaker III, heat at low temperature until completely dissolved, remove, cool to room temperature, wash the surface blood and the wall of the beaker with hydrochloric acid (4.6), then transfer the hydrochloric acid (4.6) into a 500mL volumetric flask containing 200mL hydrochloric acid (4.2), dilute to the mark, and mix well. 1ml of this solution contains 800μg antimony. 5 Instruments
Atomic absorption spectrometer, with lead, antimony, and bismuth hollow cathode lamps. Under the best working conditions of the instrument, those that can meet the following indicators can be used. Characteristic concentration: In a solution consistent with the matrix of the sample solution, the characteristic concentrations of lead, bismuth and antimony should not exceed 0.39 μg/mL, 0.27 μg/mL and 0.58 μg/mL, respectively. Precision: The absorbance of the highest concentration standard solution is measured 10 times, and its standard deviation should not exceed 1% of the half-mean absorbance: The absorbance of the low concentration standard solution (not the "Cen" standard solution) is measured 10 times, and its standard deviation should not exceed 0.5% of the average absorbance of the highest concentration standard solution.
Linearity of working curve: 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 0.8.
For the working conditions of the instrument, see Appendix B (reference). 6 Analysis steps
6.1 Sample
Weigh the sample according to 2, accurate to 0.0001g. Table 2
Content range
0.05~~0.15
>0. 15~0.25
>0.25～~0.60
0. 008 ~0.03
>0. 03~0. 15
0. 02~ 0. 06
>0.06~0.25
>0.25~0.60
Sample amount, g
Dilution volume
Carry out two tests independently and take the average value. 6.2 Blank test
Carry out a blank test along with the sample.
6.3 Determination
Add hydrochloric acid
(4.4), ml.
Add lanthanum nitrate solutionAdd ferric nitrate solutionTake the test solution volume mt.
GB/T 5120.41995
6.3.1Put the sample (6.1) in a 400mL beaker, add a small amount of water, cover with table III, slowly add 40mL nitric acid, after the violent reaction stops, heat on a low temperature electric hot plate until the sample is completely dissolved, drive off nitrogen oxides, remove, wash the table blood and the wall of the cup with water, and heat the water rate solution volume to about 150ml.
6.3.2Add 8ml. ferric nitrate solution and 2mL lanthanum nitrate solution, add ammonia water (4.3) while stirring until the generated copper hydroxide precipitates and dissolves (the solution becomes dark blue), then add 20mL in excess, heat to a slight boil, move to a low temperature and keep warm for 1h. 6.3.3 Filter with medium-speed quantitative filter paper, wash the beaker and the precipitate three times with warm ammonia water (4.7), transfer the precipitate to the original beaker with a small amount of hydrochloric acid (4.6), drip 15mL of hydrochloric acid (4.2) onto the filter paper and the wall of the cup, and then wash the filter paper 45 times with hot hydrochloric acid (4.5) (the whole filter paper is yellow with invaluable iron ions). Add the washing liquid to the original beaker. 6.3.4 Cover the test solution on the hot plate at a low temperature, heat it slightly (if the volume of the test solution is too large, the concentration rate is about 50mI at the lowest possible temperature), remove it, cool it to room temperature, transfer the solution to a 100mL volumetric flask with hydrochloric acid (1.6) and dilute to the scale. Mix well (if the content of the element is too high, take appropriate fractions according to Table 2).
6.3.5 Using air-acetylene flame, measure the absorbance of the test solution on the atomic absorption spectrometer at the wavelength shown in Table 1, adjust the zero with the sample blank solution, and find the concentration of the corresponding element from the working curve. 6.4 Drawing of working curve
6.4.1 Transfer 0, 1.00, 2.00, 3.00, 4.00, 5.00mL of lead, bismuth and antimony standard solutions to their respective 100mL volumetric flasks, add 8mL of ferric nitrate solution and 2mL of lanthanum nitrate solution, and then add 30mL of hydrochloric acid (4.4), dilute to the scale with water, and mix. 6.4.2 Under the same conditions as the measurement of the sample solution, adjust the zero with the "Cen" standard solution, and measure the absorbance of the lead, bismuth and antimony standard solutions at the wavelength shown in Table 1, and draw the working curve with the concentration of the element to be measured as the horizontal axis and the corresponding absorbance as the vertical axis. 7 Expression of analysis results
Calculate the percentage of the measured element according to the following formula: X(%) = : V.: V,X 10-
mn· V,
Formula: X—-the measured element (lead, bismuth, antimony); the concentration of the measured element found from the working curve, g/mL; V.-the total volume of the test solution, ml.
V. The volume of the tested solution, mL;
V,—the volume of the test solution taken, mL;;
the mass of the sample.
The obtained result is expressed to two decimal places. If the content is less than 0.1%, it is expressed to three decimal places; less than 0.01%, express to four decimal places.
8 Allowable difference
The difference between the analysis results of laboratories shall not be greater than the allowable difference listed in Table 3. 190
GB/T 5120. 4-1995wwW.bzxz.Net
0. 05 -~ 0. 15
>0.15~0.25
>0.25~0.50
>0. 50~0.60
0.008 0~0.015
0.015~0.030
>0.030~0.050
>0.050~~0.080
>0. 080~0. 15
0. 05~~0. 15
>0. 15~~0.25
>0. 25-~0. 40
>0. 40~0. 60
GB/T 5120.41995
Appendix A
Instrument working conditions
(reference)
The working conditions for determining the amount of lead, bismuth and antimony using PE-1100B atomic absorption spectrometer are shown in Table A1: Table A1
Additional notes:
Wavelength, nm
Lamp current, mA
This standard was proposed by China Nonferrous Metals Industry Corporation. This standard was revised by Daye Nonferrous Metals Corporation. This standard was revised by Daye Nonferrous Metals Corporation. The main editors of this standard were Liu Zhendong, Peng Jianjun and Li Yuqin. 192
Spectral passband, nm
Observation height, mm
Air streamline: Flow ground
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