This standard specifies the determination method of antimony content in copper concentrate. This standard is applicable to the determination of antimony content in copper concentrate. GB/T 3884.10-2000 Chemical analysis method for copper concentrate Determination of antimony content GB/T3884.10-2000 Standard download decompression password: www.bzxz.net

GB/T3884.10—2000
This standard is published for the first time.
This standard complies with:
GB/T1.1—1993
Guidelines for Standardization Work Unit 1: Basic Rules for Drafting and Expression of Standards
Rules for Writing Chemical Analysis Methods
GB/T1.4-1988
8Guidelines for Standardization Work
GB/T1467-1978 General Principles and General Provisions for Chemical Analysis Methods for Metallurgical Products GB/T17433—1998 Basic Terminology for Chemical Analysis of Metallurgical Products Appendix A in this standard is a prompt appendix.
This standard is proposed by the State Bureau of Nonferrous Metals Industry. This standard is under the jurisdiction of the China Nonferrous Metals Industry Standard Metrology and Quality Research Institute. This standard is drafted by Daye Nonferrous Metals Company. This standard is drafted by Jiangxi Copper Company.
The main drafters of this standard are Xiong Jianping, Zhan Guangxian and Xing Yingxiang. Part 1: Standard preparation
1 Scope
National Standard of the People's Republic of China
Chemical analysis methods of copper concentrates
Determination of antimony content
Methodsforchemical analysis of copper concentratesDetermination of antimony contentThis standard specifies the determination method of antimony content in copper concentrates. This standard is applicable to the determination of antimony content in copper concentrates. Determination range: 0.010%~0.20%. 2 Summary of the method
GB/T3884.10—2000
The sample is decomposed with sulfuric acid and potassium sulfate. Antimony is coprecipitated in a nitrogen medium using the iron contained in the sample and a certain amount of lanthanum added, and separated from copper. The precipitate is dissolved with hot hydrochloric acid, and part of the solution is taken, and ascorbic acid is added for pre-reduction, and sulfur glands mask the copper. Pipette a certain amount of the test solution into the hydride generator, antimony (II) is reduced to antimony hydride by potassium borohydride, and introduced into the quartz furnace atomizer with gas, and the antimony hollow cathode lamp is used as the light source to measure its fluorescence intensity on the atomic fluorescence spectrometer. 3 Reagents
3.1 Potassium sulfate.
3.2 Sodium hydroxide.
3.3 Sulfuric acid (pl.84g/mL).
3.4 ​​Nitric acid (pl.42g/mL).
3.5 Hydrochloric acid (p1.19g/mL).
3.6 Ammonia water (p0.90g/mL).
3.7 Nitric acid (1+1).
3.8 Hydrochloric acid (1+9).
3.9 Ammonia water (1+95).
3.10 Thiourea solution (100g/L).
3.11 Ascorbic acid solution (100 g/L).
3.12 Lanthanum nitrate solution (20 mgLa/mL): Weigh 11.73 g lanthanum oxide [La20,] into a 250 mL beaker, add 40 mL nitric acid (3.7) to dissolve at low temperature, heat to remove nitrogen oxides, cool, transfer to a 500 mL volumetric flask, dilute to scale with water, and mix. 3.13 Lanthanum nitrate solution (1 mgLa/mL): Transfer 10 mL nitric acid solution (3.12) into a 200 mL volumetric flask, dilute to scale with water, and mix.
3.14 Ferric nitrate solution (10 mgFe/mL): Weigh 73.40 g ferric nitrate [Fe(NO)·9HOJ into a 250 mL beaker, add 10 mL nitric acid (3.7), add appropriate amount of water to dissolve, transfer to a 1000 mL volumetric flask, dilute to scale with water, and mix. 3.15 Antimony standard stock solution: Weigh 0.5000g high purity antimony powder, add 25mL nitric acid (3.4), 3g tartaric acid, dissolve at low temperature, transfer to a 500mL volumetric flask after cooling, dilute to scale with water, and mix well. This solution contains 1mg antimony in 1mL. Approved by the State Administration of Quality Supervision, Inspection and Quarantine on February 16, 200056
2000-08-01 implementation
GB/T3884.10—2000
3.16 Standard solution: Transfer 10.00mL antimony standard stock solution (3.15) to a 100mL volumetric flask, add 10mL hydrochloric acid (3.5), dilute to scale with water, and mix well. This solution contains 0.1mg antimony in 1mL. 3.17 Antimony standard solution: Pipette 10.00mL antimony standard solution (3.16) into a 200mL volumetric flask, add 10mL hydrochloric acid (3.5), dilute to the mark with water, and mix. 1mL of this solution contains 5μg antimony. 3.18 Potassium borohydride solution (10g/L): Weigh 10g potassium borohydride and dissolve it in 1000mL sodium hydroxide solution (2g/L), and mix. Prepare before use.
4 Instruments
Atomic fluorescence spectrometer. Attached with shielded quartz furnace atomizer, glass hydride generator. Special antimony hollow cathode lamp or antimony high-intensity hollow cathode lamp. Argon: used as shielding gas and carrier gas. Under the best working conditions of the instrument, those that can meet the following indicators can be used. Detection limit: not more than 2×10-ug/mL.
Precision: The relative standard deviation of the fluorescence intensity measured 11 times with 0.02ug/mL antimony standard solution should not exceed 5%. For instrument working conditions, see Appendix A (suggested appendix). 5 Sample
5.1 The sample particle size should not be greater than 0.082mm. 5.2 The sample should be dried at 100~105℃ for 1h and then placed in a desiccator to cool to room temperature. 6 Analysis steps
6.1 Sample
Weigh 0.20g of sample to an accuracy of 0.0001g. Perform two independent measurements and take the average value. 6.2 Blank test
Perform a blank test along with the sample.
6.3 Determination
6.3.1 Place the sample (6.1) in a 400mL low-type beaker, add 2g potassium sulfate, moisten with water, add 10mL sulfuric acid [add a little nitric acid (3.4) if necessary], cover with a watch glass, place on an electric stove and heat to decompose until white sulfur trioxide smoke is emitted, add a small piece of filter paper (about 4cm) and continue to heat on a high-temperature electric stove until the black color is safely faded, remove and cool, rinse the cup wall and surface blood with water, boil to dissolve the salts, remove and cool. 6.3.2 Add 2.5mL of sodium nitrate solution (add 5mL of iron nitrate solution to the blank sample), dilute to about 150mL with water, place on a hot plate and heat until it is almost boiling, remove, add ammonia water while stirring until the generated copper hydroxide precipitate is dissolved (the solution is blue), then add 20mL in excess, slowly heat to a slight boil, move to a low temperature place (about 60℃), and keep warm for 30min. 6.3.3 Filter with rapid quantitative filter paper, wash the beaker and precipitate 4-5 times with hot ammonia (3.9), wash the beaker and precipitate 3-4 times with hot water, and discard the filtrate.
6.3.4 Remove the filter paper and precipitate from the funnel, spread them in the original beaker (placed on a glass rod), flush the precipitate into the beaker with a small amount of water, wash the filter paper with hydrochloric acid (3.9) until it is colorless, add 5mL of hydrochloric acid (3.5), place it on an electric stove to heat and dissolve the salts, remove it and cool it, transfer the solution to a 100mL volumetric flask with hydrochloric acid (3.9), dilute to the mark, and mix. 6.3.5 Take the test solution according to Table 1 and put it into a 50mL volumetric flask that has been added with 30mL of water and 5mL of hydrochloric acid (3.5), add 5mL of ascorbic acid solution and 5mL of thiophene solution, dilute to the mark with water, and mix for testing. 57
Antimony content, %
0.010~0.050
>0.050~0.10
>0.10~0.20
GB/T3884.10-2000
Volume of test solution, mL
6.3.6 Transfer 2 mL of the test solution (6.3.5) into the hydride generator, add potassium borohydride solution at a constant rate, and measure its fluorescence intensity on an atomic fluorescence spectrometer. Subtract the fluorescence intensity of the blank solution accompanying the sample and obtain the corresponding antimony concentration from the working curve. 6.4 Drawing of working curve
Pipette 0.50, 1.00, 1.50, 2.00, 2.50 mL of antimony standard solution into a 50 mL volumetric flask that has been added with 30 mL of water and 5 mL of hydrochloric acid (3.5), then add 0.25 mL of ferric nitrate solution, 2.5 mL of nitric acid solution, 5 mL of ascorbic acid solution, and 5 mL of sulfur solution, dilute with water to the scale, and mix. Under the same conditions as the test plate sample, measure the fluorescence intensity of the standard solution series (minus the fluorescence intensity of the "zero" concentration standard solution), and draw the working curve with antimony concentration as the horizontal axis and fluorescence intensity as the vertical axis. 7 Expression of analysis results bzxz.net
Calculate the percentage of antimony according to formula (1):
cV. .V.X10-*
Sb(%)=
the antimony concentration found from the working curve, ug/mL; the total volume of the test solution, mL;
the volume of the test solution taken, mL,
the volume of the diluted test solution taken, mL;
the mass of the test material·g.
The result is expressed to two decimal places. If the antimony content is less than 0.10%, it is expressed to three decimal places. 8 Allowable difference
The difference between the analysis results of laboratories shall not be greater than the allowable difference listed in Table 2. Table 2
0.010~0.050
>0.050~0.10
>0.10~0.20
（1）
GB/T3884.10—2000
Appendix A
(Suggested Appendix)
Instrument Working Conditions
Using XDY-3 dual-channel atomic fluorescence spectrometer and special antimony hollow cathode lamp, the working conditions for determining antimony content are shown in Table A1. Table A1
Lamp current
Liquid addition time
Negative high voltage
Delay time
Carrier gas flow
Sampling time
Screen knock gas flow
Quartz furnace height
Atomization temperature
Curve fitting
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