GB/T 3884.6-2000 Chemical analysis methods for copper concentrates - Determination of lead, zinc, cadmium and nickel content
Some standard content:
GB/T3884.6—2000
This standard is a revision of GB/T3884.7-1983 "Chemical analysis method for copper concentrate - determination of lead content by atomic absorption spectrophotometry", GB/T3884.11-1983 "Chemical analysis method for copper concentrate - determination of sales volume by atomic absorption spectrophotometry", and GB/T3884.12-1983 "Chemical analysis method for copper concentrate - determination of zinc content by atomic absorption spectrophotometry", among which the "Chemical analysis method for copper concentrate - determination of nickel content" is a newly formulated standard.
This standard reorganizes the separate determination methods for lead, cadmium and zinc in GB/T3884.7-1983, GB/T3884.11-1983 and GB/T3884.12--1983 into a unified analysis method, and adds a new analysis method for nickel. The determination range of lead was adjusted from 0.10%~2.00% to 0.10%~5.00%; the determination range of zinc was adjusted from 0.10%~2.00% to 0.10%~1.00%. This standard complies with:
GB/T1.1-1993 Guidelines for Standardization Unit 1: Rules for Drafting and Presenting Standards Part 1: Basic Provisions for Standard Writing
GB/T1.4-1988, Guidelines for Standardization Provisions for the Writing of Chemical Analysis Methods GB/T1467-1978 General Principles and General Provisions for Chemical Analysis Methods for Metallurgical Products GB/T7728-1987 General Rules for Flame Atomic Absorption Spectrometry for Chemical Analysis of Metallurgical Products GB/T17433-1998 Basic Terminology for Chemical Analysis of Metallurgical Products This standard replaces GB/T3884.7-1983, GB/T3884.11-1983, and GB/T3884.12-1983 from the date of implementation. Appendix A of this standard is a reminder 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 was drafted by Daye Nonferrous Metals Company. This standard was drafted by Tongling Nonferrous Metals (Group) Company. The main drafters of this standard are Shao Conghe, Chen Xiaoyan and Cui Xianfu. 31
1 Scope
National Standard of the People's Republic of China
Chemical Analysis Methods of Copper Concentrates
Determination of Lead, Zinc, Cadmium and Nickel Contents
Methods for chemical analysis of copper concentrates-Determination of lead, zinc, cadmium and nickel contents This standard specifies the determination method of lead, zinc, cadmium and nickel contents in copper concentrates. This standard is applicable to the determination of lead, zinc, cadmium and nickel contents in copper concentrates. The determination range is shown in Table 1. Table 1
Measurement range, %
Method principle
0.10~5.00
0.10~1.00
GB/T 3884.6—2000
Replaces GB/T3884.7-—1983
GB/T3884.11—1983
GB/T3884.12—1983
0.010~0.50
0.010~1.00
The sample is decomposed with hydrochloric acid. In dilute nitric acid medium, the absorbance of each element is measured by air-acetylene flame method at the wavelength listed in Table 2 on an atomic absorption spectrometer, and the content of each element is calculated by standard curve method after deducting the background absorption. Table 2
Wavelength, nm
3 Reagents
3.1 Bromine.
3.2 Hydrochloric acid (p1.19 g/mL).
3.3 Nitric acid (pl.42 g/mL).
3.4 Perchloric acid (p1.67 g/mL).
3.5 Nitric acid (1+1).
3.6 Lead standard stock solution: Weigh 1.0000 g of golden fan lead (99.99%) in a 200 mL beaker, add 10 mL of nitric acid (3.5), cover with blood, place on a hot plate and heat at low temperature until completely dissolved, boil to drive off nitride, and cool to room temperature. Transfer to a 500 mL volumetric flask, add 20 mL of nitric acid (3.5), dilute to scale with water, and mix well. This solution contains 2 mg of lead in 1 mL. , 3.7 Zinc standard storage solution: weigh 0.5000g metallic zinc (99.99%) in a 200mL beaker, add 10mL nitric acid (3.5), cover the surface with blood, place on a hot plate and heat at low temperature until completely dissolved, boil to drive out nitrides, and cool to room temperature. Transfer to a 1000mL volumetric flask, add 20mL nitric acid (3.5), dilute to scale with water, and mix. This solution contains 0.5mg zinc in 1mL. 3.8 Standard storage solution: weigh 0.5000g metal pot (99.99%) in a 200mL beaker, add 10mL nitric acid (3.5), cover the surface with blood, place on a hot plate and heat at low temperature until completely dissolved, boil to drive out nitrides, and cool to room temperature. Transfer to a 1000mL volumetric flask, dilute to the mark with water, and mix well. This solution contains 0.5mg of nickel in 1mL. 3.9 Nickel standard stock solution: Weigh 0.5000g of metallic nickel (99.99%) in a 200mL beaker, add 10mL of nitric acid (3.5), cover with a watch glass, place on a hot plate and heat at low temperature until completely dissolved, boil to drive off nitrides, and cool to room temperature. Transfer to a 1000mL volumetric flask, dilute to the mark with water, and mix well. This solution contains 0.5mg of nickel in 1mL. 3.10 Mixed standard solution of lead, zinc, cadmium and nickel: Pipette 50.00mL of lead standard stock solution (3.6), 10.00mL of zinc and standard storage solution (3.7, 3.8) and 25.00mL of nickel standard storage solution (3.9) into a 500mL volumetric flask, add 10mL of nitric acid (3.5), dilute to the mark with water and mix. 1mL of this solution contains 200pg of lead, 10pg of zinc, 10μg of cadmium and 25pg of nickel respectively. 4 Instruments
Atomic absorption spectrometer, equipped with hollow cathode lamps for lead, zinc, tin and nickel. The instrument should be equipped with a background subtraction device. Under the best working conditions of the instrument, any instrument that meets the following indicators can be used. Sensitivity: In a solution consistent with the matrix of the test solution, the characteristic concentrations of lead, zinc, tin and nickel should not be greater than 0.048, 0.00270.0038 and 0.015μg/mL respectively.
Precision: When the absorbance is measured 10 times with the highest concentration standard solution, the standard deviation should not exceed 1.0% of the average absorbance; when the absorbance is measured 10 times with the lowest concentration standard solution (not the "zero" standard solution), the 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. The ratio of the absorbance difference of the highest section to the absorbance difference of the lowest section should not be less than 0.85 times the absorbance difference between the lowest concentration standard solution and the "zero" standard solution. See Appendix A (Suggested Appendix) for instrument working conditions. 5 Sample
5.1 The sample particle size should not be greater than 0.082mm. 5.2 The sample should be dried at 100-105C 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 determinations and take the average value. 6.2 Blank test
Perform a blank test with the sample.
6.3 Determination
6.3.1 Place the sample (6.1) in a 125mL conical beaker, moisten it with a small amount of water, add 10mL of hydrochloric acid, cover it with surface III, place it on a hot plate and heat it for several minutes, remove it and cool it slightly. Add 10mL of nitric acid (3.3) [If monomeric sulfur is precipitated, add 0.5mL of bromine. If the sample has a high carbon content, add 2~3mL of pernitrogen acid, place it on a hot plate and heat it to completely decompose the sample, continue heating and steaming until it is almost dry, remove it and cool it slightly. 6.3.2 Add 5mL of nitric acid (3.5), heat to a slight boil, blow the watch glass and the wall of the cup with a small amount of water, and cool it to room temperature. 6.3.3 Transfer the test solution (6.3.2) into a 100mL volumetric flask, dilute it to the mark with water, mix it well, and let it stand or dry filter it. 6.3.4 Take the test solution (6.3.3) according to Table 3 and add nitric acid (3.5) into a 100ml volumetric flask (if the content of lead, nickel is less than or equal to 0.50%, 0.020% and 0.10% respectively, directly operate according to 6.3.5). 33
Zn content, %
Cd>0.020~0.10
Pb>0.50~2.00
Zn>0.10~0.15
Cd>0.10~0.15
Ni>0.10~0.50
Pb>2.00~5.00
Zn>0.15~0.50
Cd>0.15~0.50
Ni>0.50~1.00
Zn>0.50~1.00
GB/T.3884.6-2000
Amount of filtrate, mL
Amount of nitric acid (3.5) added, mL
6.3.5 Use air-acetylene flame and water to zero the atomic absorption spectrometer at the wavelength listed in Table 2 to measure the absorbance of lead, zinc, pot and nickel test solutions respectively. Obtain the corresponding concentration of the element being measured from the working curve. 6.4 Drawing of working curves
6.4.1 Take 0, 2.00, 4.00, 6.00.8.00, 10.00mL of the mixed standard solutions of lead, zinc, cadmium and nickel, place them in a set of 100mL volumetric flasks, add 10mL of nitric acid (3.5), dilute to the mark with water and mix well. 6.4.2 Under the same conditions as the test solution, measure the absorbance of the standard solution. With the absorbance (minus the absorbance of the "zero" concentration solution) as the ordinate and the concentration of the element being measured as the abscissa, draw the working curves of lead, zinc, cadmium and nickel respectively. 7 Description of analytical results
Calculate the percentage of the element being measured according to formula (1): X(%) = (c - co)V. V, × 10-6m. .V
Wherein, X is the percentage of the measured element (lead, zinc, nickel), %; - the concentration of the measured element found on the working curve, μg/mL, X100
- the concentration of the blank test solution of the measured element found on the working curve, g/mL, - the total volume of the test solution, mL
V - the volume of the test solution taken, mL, www.bzxz.net
V - the dilution volume of the test solution after taking, mL, - the mass of the test material, &.
The result is expressed to two decimal places. If the content is less than 0.10%, it is expressed to three decimal places. 8 Allowable difference
The difference between the analysis results of laboratories should not be greater than the allowable difference listed in Table 4. 34
·(1)
Element containing disk
0.10~0.50
>0.50~1.00
>1.00~2.00
>2.00~3.00
>3.00~5.00||tt| |0.10~0.20
>0.20~0.50
>0.50~1.00
0.010~0.050
>0.050~0.10
>0.10~0.30
>0.30~0. 50
0.010~0.050
>0.050~0.10
>0.10~0.30
>0.30~0.60
>0.60~1.00
GB/T3884.6—2000
Tolerance
GB/T3884.6-2000
Appendix A
(Suggestive Appendix)
Instrument Working Conditions
The working conditions for measuring lead, zinc, cadmium and nickel using Hitachi Z--8200 atomic absorption spectrometer are shown in Table A1. Table AI
Wavelength, nm
Lamp current, mA
PMT voltage, V
Burner height, mm
Slit width, mm
Air flow, L/min
Acetylene flow, L/min
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