GB/T 14949.6-1994 Chemical analysis methods for manganese ores - Determination of copper, lead and zinc content
Some standard content:
National Standard of the People's Republic of China
Chemical analysis method of manganese ore
Determination of copper, lead and zinc contents
Manganese ores--- Determination of copper, lead and zinc contents This standard is equivalent to the international standard ISC) 5889--1983 "Atomic absorption spectrometry for manganese ore and manganese concentrate".
Subject content and scope of application
This standard specifies the determination of copper, lead and zinc contents by flame atomic absorption spectrometry. GB/T14949-6--94
Determination of aluminum, copper, lead and zinc contents... Flame This standard is applicable to the determination of copper, lead and zinc contents in manganese ore and manganese concentrate. Determination range: copper 0.005%~~1.0%;
lead 0. 005%~~1.0%;
zinc 0.005%~0.25%.
2 Method Summary
The sample is decomposed with hydrochloric acid and nitric acid.
After the test solution evaporates, filter all insoluble residues and save the filtrate as the main solution. Ash the filter paper with residues, treat it with hydrofluoric acid and sulfuric acid, and then melt it with a mixed flux. The molten material is dissolved in hydrochloric acid, and the resulting solution is combined with the main solution. The test solution is sucked into an air-acetylene flame, and hollow cathode lamps of copper, lead and zinc are used as light sources, respectively. The absorbance of copper, lead and zinc is measured at the wavelength of 324.8nm (Cu), 283.3nm (Pb) and 213.8nm (Zn) of the atomic absorption spectrometer. 3 Reagents
All reagents used in this standard are of premium grade.
3.1 High-purity manganese (containing less than 0.0005% of copper, lead and zinc). 3.2 High-purity iron (containing less than 0.0005% of copper, lead and zinc). 3.3 Mixed flux: potassium carbonate and boric acid (3+1). 3.4 Nitric acid (pl.42g/ml).
Sulfuric acid (pl.84g/ml)
Hydrochloric acid (ml.19g/mL).
Hydrochloric acid (1+1).
Hydrochloric acid (1+50).
3.9 Hydrofluoric acid (pl.14g/ml).
Note: 1) GB/T 11919.6 94 replaces GB1520-79, GB 1521 -79. GB 1522 79. Approved by the State Administration of Technical Supervision on January 18, 1994 832
Implementation on October 1, 1994
3.10 Copper standard solution
GB/T 14949.6.--94
Weigh 0.1000g high-purity copper (99.99%), place it in a beaker, add 5mL nitric acid (3.4), heat and dissolve. Cool to room temperature, transfer to a 1000ml volumetric flask, dilute to scale with water, and mix well. This solution contains 100μg copper in 1ml. 3.11 Lead standard solution
3.11.1 Weigh 0.5000g high-purity lead (99.99%), place in a beaker, add 10mL nitric acid (3.4), dilute to 40mL with water, and heat to dissolve. Cool to room temperature, transfer to a 1000mL volumetric flask, dilute to scale with water, and mix. This solution contains 500μg lead in 1mL. 3.11.2 Transfer 50.00mL of lead standard solution (3.11.1) to a 500mL volumetric flask, dilute to scale with water, and mix. This solution contains 50μg lead in 1mL.
3.12 Zinc standard solution
Weigh 0.1000g high-purity zinc (99.99%), place in a beaker, add 10mL hydrochloric acid (3.7), and heat to dissolve. Cool to room temperature, transfer to a 1000mL volumetric flask, dilute to scale with water, and mix. 1 mL of this solution contains 100 μg of zinc. 3.13 Matrix solution
Weigh 12.50 g of high-purity manganese (3.1) and 1.25 g of high-purity iron (3.2) in a 1500 mL beaker, add 625 ml of hydrochloric acid (3.7) and 25 mL of nitric acid (3.4), and heat to dissolve. Cool the solution, slowly add 18.75 g of potassium carbonate and 6.25 g of boric acid, and heat to dissolve. Cool the solution to room temperature, transfer it to a 1000 mL volumetric flask, dilute to the mark with water, and mix. Note: This matrix solution should not contain copper, lead, and zinc. 4 Instruments and equipment
Common laboratory instruments and equipment and
4.1 Platinum crucible.
4.2 Atomic absorption spectrometer, equipped with air-acetylene burner, copper, lead, and zinc hollow cathode lamps. The original absorption spectrometer used should meet the following indicators: 4.2.1 Minimum sensitivity
The absorbance of the highest concentration calibration solution in the calibration curve should not be less than 0.3. 4.2.2 Linearity of the calibration curve
The ratio of the slope of the calibration curve in the upper 20% concentration range (expressed as the change in absorbance) to the slope of the curve in the lower 20% concentration range should not be less than 0.7.
4.2.3 Minimum stability
Measure the absorbance of the highest calibration solution 10 times and calculate the average value and standard deviation of the absorbance. Its standard deviation should not exceed 1.0% of the average absorbance of the highest calibration solution.
Measure the absorbance of the lowest calibration solution (not the "zero" calibration solution) 10 times and calculate its standard deviation. Its standard deviation should not exceed 0.5% of the average absorbance of the highest calibration solution. 5 Sample
The sample should pass through a 0.100mm sieve and air-dry under laboratory conditions. 6 Analysis steps
6.1 Sample quantity
Weigh about 2g of sample, accurate to 0.0001g. Weigh the sample at the same time as the determination to determine the mass percentage of wet water (A). When calculating the results of copper, lead and zinc, the obtained results (mass percentage) should be multiplied by the conversion factor (K), which is the mass percentage of copper, lead and zinc determined in the completely dry sample. Conversion factor (K) =
6.2 Blank test
Perform a blank test with the sample.
GB/T 14949.6-94
Preparation of blank solution: Weigh 1g of high-purity manganese (3.1) and 0.1g of high-purity iron (3.2) in a 200ml beaker. Add 40ml of hydrochloric acid (3.7) and heat to dissolve. All the following tests shall be carried out according to the analysis steps in Chapter 6. 6.3 Determination
6.3.1 Preparation of test solution
Place the sample (6.1) in a 200 mL beaker, moisten with water, add 40 mL of hydrochloric acid (3.7), heat to dissolve, and keep the volume constant with water. After the sample is decomposed, add 2 mL of nitric acid (3.4), heat the solution until the nitrogen oxide stops escaping, and then evaporate the solution to near dryness. Add 10 mL of hydrochloric acid (3.6) and 20 mL of hot water, heat to dissolve the salts, and cool the solution. Filter the insoluble residue with medium-speed filter paper containing a small amount of filter paper pulp, wipe off the precipitated particles on the wall of the beaker with a small piece of filter paper, and transfer all of them to the filter paper. Rinse the beaker with water, wash the filter paper with residue with hot hydrochloric acid (3.8), and then wash with hot water until the yellow color of the filter paper disappears. Save the filtrate as the main solution. 6.3.2 Transfer the filter paper and the residue into a platinum crucible (4.1), burn at a temperature below 600°C until the filter paper is completely ashed, cool the crucible, moisten it with water, add 1mL sulfuric acid (3.5) and 5~10mL hydrofluoric acid (3.9), slowly evaporate to remove silicon, then emit white smoke and burn at nearly 600°C. Cool the crucible, add 2g mixed flux (3.3), melt in a muffle furnace at 1.000°C for 5min, and cool. Place the crucible with the melt in the original 200mL beaker, add 10mL hydrochloric acid (3.7) and a small amount of water, heat to dissolve the melt, and wash out the crucible. Combine this solution with the main solution (6.3.1) (filter if necessary). Note: After inspection, if the residue does not contain lead or zinc, the main solution can be used for determination directly (pay attention to keep the matrix consistent). 6.3.3 Transfer the solution (6.3.2) into a 200mL volumetric flask, dilute to the mark with water, and mix. 6.3.3.1 For copper content less than or equal to 0.1%, lead content 0.5% and zinc content 0.025%, use the test solution (6.3.3) to measure according to 6.3.4.
6.3.3.2 For copper content greater than 0.1%, lead content 0.5% and zinc content 0.025%, take the test solution according to Table 1, add the matrix solution (3.13), add it to a 100mL volumetric flask, dilute it to the scale with water, and mix it. Measure according to 6.3.4. 6.3.4 Atomic absorption spectrum measurement
Adjust the atomic absorption spectrometer to the best working state and zero it with water. Inhale the test solution into the air-acetylene flame, use a hollow cathode lamp as the light source, and measure the absorbance of lead and zinc at wavelengths of 324.8nm (Cu), 283.3nm (Pb) and 213.8nm (Zn), respectively. Subtract the absorbance of the blank solution from the absorbance of the test solution to get the net absorbance of the test solution. bZxz.net
Determination of elements
Content of elements in the test solution
0.005~~0.1
0. 1~1. 0
0. 005~～0. 5
0. 005~0. 025
0. 025 ~~ 0. 05
0. 05~0. 1
0. 1 ～0. 25
6.4 Drawing of calibration curve
Add aliquots of test solution
to matrix solution (3.13)
volume, mL
6.4.1 Prepare calibration solution with copper (3.10), lead (3.11.1 and 3.11.2) and zinc (3.12) standard solutions and determine the content of elements in the solution
1. 25 ~ 2. 5
1. 0~2. 5
According to Table 2, transfer a certain amount of copper (3.10), lead (3.11.1 and 3.11.2) and zinc (3.12) standard solutions into a series of 100ml volumetric flasks, add 40mL of matrix solution (3.13), dilute to scale with water, and mix. 834
GB/T 14949.6-94
6.4.2 Measure the calibration solution (6.4.1) according to 6.3.4. The absorbance of each solution in each calibration curve series minus the absorbance of the zero concentration solution is the net absorbance of the copper, lead and zinc calibration curve series solutions.
Standard solution||tt| ... Calculation of results
The mass percentage of copper, lead and zinc is calculated as follows: Cu(Ph,Zn)(%) -
Wherein: (-
(c2 -- c,)V
m × 10°
.100?K
The concentration of copper, lead and zinc in the blank solution accompanying the sample obtained from the calibration curve, ug/mL; The concentration of copper, lead and zinc in the test solution obtained from the calibration curve, ug/mL; C
8 Allowable difference
The volume of the tested solution, ml;
The mass of the sample in g;
The conversion factor of the amount of copper, lead and zinc in the completely dried sample. The difference in the analysis results between laboratories should not be greater than the allowable difference listed in Tables 3 and 4. Table 3
The amount of copper and lead
0. 005~0. 01
>0. 01～0. 02
>0. 02~0. 05
>0. 05-~0. 10
>0.10~0.20
>0.20～0.50
>0. 50~~1. 00 | | tt | 25
GB/T14949.6--94
This standard is proposed by the Ministry of Metallurgical Industry of the People's Republic of China. Allowable difference
This standard is drafted by the Mineral Geology Research Institute of China Nonferrous Metals Industry Corporation and the Changsha Mining and Metallurgical Research Institute of the Metallurgical Industry. This standard is drafted by the Mineral Geology Research Institute of China Nonferrous Metals Industry Corporation. The main drafters of this standard are Zhang Peiyu and Shu Baichong. 836
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