Standard provisions: Determination of nickel content by flame atomic absorption spectrometry. This standard is applicable to the determination of nickel content in manganese ore and manganese concentrate. The determination range is: 0.005%-1:00%. GB/T 14949.2-1994 Chemical analysis method for manganese ore. Determination of nickel content. GB/T14949.2-1994 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Chemical analysis method of manganese ore
Determination of nickel content
Manganesc ores-Determination of nickel contentGB/T 14949.2 --- 94
Replace GB1520-79
This standard is equivalent to the international standard 1ISO315-1984 "Manganese ore and manganese concentrate-Determination of nickel content-Flame atomic absorption spectrometry".
1 Subject content and scope of application
This standard specifies the determination of nickel content by flame atomic absorption spectrometry. This standard is applicable to the determination of nickel content in manganese ore and manganese concentrate, with a determination range of 0.005% to 1:0%. 2 Method summary
The sample is decomposed with hydrochloric acid and nitric acid. Filter the insoluble residue and retain the filtrate as the main solution. Burn the residue and filter paper together and treat with hydrofluoric acid and sulfuric acid. Sodium carbonate is melted, and the melt is dissolved in hydrochloric acid solution. The obtained solution is combined with the main solution and the test solution is sprayed into an air-acetylene flame. A nickel hollow cathode lamp is used as the light source. The absorbance is measured at a wavelength of 232.0nm on an original absorption spectrometer.
3 Reagents
3.1 Anhydrous sodium carbonate.
3.2 Hydrochloric acid (pl.19g/ml).
3.3 Hydrochloric acid (1+1).
3.4 ​​Hydrochloric acid (1+4).
3.5 Hydrochloric acid (1+50).
3.6 Nitric acid (pl.42g/ml.).
3.7 Nitric acid (1+1).
3.8 Sulfuric acid (1+1)
3.9 Hydrofluoric acid pl.14g/ml.).
3.10 Matrix solution
3.10.1 Place 20g of high-purity manganese metal in a 500mL beaker, add 150mL of hydrochloric acid (3.3) to dissolve. After cooling, transfer to a 1000mL volumetric flask, dilute to the mark with water, and mix. 3.10.2 Place 20g of high-purity manganese metal in a 500mL beaker, add 150mL of hydrochloric acid (3.3) to dissolve. After cooling slightly, add 40g of anhydrous sodium carbonate (3.1) pre-dissolved in water. Add more acid (3.3) until all the precipitate is dissolved. After cooling, transfer to a 1000mL volumetric flask. Dilute to the mark with water, and mix.
3.11 Nickel standard solution
3.11.1 Weigh 1.0000g of nickel metal (99.95% or more) and place it in a 250mL beaker. Add 50mL nitric acid (3.7) and heat to dissolve. After cooling to room temperature, transfer to a 1000ml volumetric flask, dilute to scale with water, and mix. This solution contains 1mg nickel in 1mL. 3.11.2 Transfer 10.00ml of nickel standard solution (3.11.1) and place it in a 200mL volumetric flask. Dilute to scale with water and mix. This solution contains 50μg nickel in 1ml.
4 Instruments and equipment
Common laboratory instruments, equipment and
4.1 Platinum crucible.
4.2 Atomic absorption spectrometer, equipped with air-acetylene burner and nickel hollow cathode lamp. The atomic 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 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 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. The standard deviation should not exceed 1.5% 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. The standard deviation should not exceed 0.5% of the average absorbance of the highest calibration solution. 5 Sample
The sample should pass through a 0.100 mm sieve and be air-dried under laboratory conditions. 6 Analysis steps
6.1 Sample quantity
Weigh 1 g of sample to the nearest 0.0001 gram. At the same time, weigh the sample to determine the mass percentage of wet water (A). When calculating the result for nickel, the result (mass fraction) should be multiplied by the conversion factor (K), which is the mass percentage of nickel determined in the completely dry sample. Conversion factor (K)-
6.2 Blank test
Perform a blank test with the solid sample.
6.3 Determination
100- A
6.3.1 Place the sample (6.1) in a 250 mL beaker, moisten with water, add 10 mL of hydrochloric acid (3.2), cover with Table III, and heat to dissolve. Add 1 mL of nitric acid (3.6).
6.3.2 Evaporate the solution to dryness. Cool. Add 10 mL of hydrochloric acid (3.2) and heat until the soluble salts are dissolved. Dilute with about 30 mL of hot water and mix well.
6.3.3 Filter the residue with medium-speed filter paper containing a small amount of filter paper pulp. Then wash the residue with hot hydrochloric acid (3.5) 5 to 6 times, and then wash it with hot water 7 to 8 times, and keep the filtrate as the main liquid.
6.3.4 Put the filter paper and the residue into platinum. Dry, ash, and burn at 500-600°C until the filter paper is completely ashed. Cool the crucible. Wet the residue with water, add 2 to 4 drops of sulfuric acid (3.8) and 5 to 7 mL of hydrofluoric acid (3.9), and heat and evaporate until all white smoke is emitted. Then burn at 500-600°C for 10 minutes. Cool and block the crucible. Add 1g sodium carbonate (3.1) to the crucible and melt at 900-1000°C for 15min. Cool the crucible. Place the ground snail in a beaker, add 20ml hydrochloric acid (3.4), and heat to dissolve the melt. Then wash the snail with water, and combine the resulting solution with the main solution (6.3.3).
GB/T14949.2—94
Note: After inspection, if the residue does not contain nickel, the main solution can be used for measurement directly. 6.3.5 Preparation of test solution
Place the test solution (6.3.4) into a 100mL volumetric flask, dilute to the mark with water, and mix. 6.3.5.1 When the nickel content is 0.005% to 0.1%, use the test solution (6.3.5) to measure according to 6.3.6. 6.3.5.2 When the nickel content is greater than 0.1%, take the test solution (6.3.5) according to Table 1 into a 100mL volumetric flask, add the base solution (3.10) and hydrochloric acid (3.2), dilute with water to the scale, mix well, and measure according to 6.3.6. Table 1
Nickel content in sample
0. 005~0. 1
>0.1～0.5
>0, 5~1. 0
6.3.6 Atomic absorption spectrum measurement
Solution aliquot
Measure the amount of nickel in the solution
μg/mL
>2～10
>5～10
Matrix solution (3.10)
Hydrochloric acid (3.2)
Place the test solution on an atomic absorption spectrometer at a wavelength of 232.0nm, with an air-acetylene flame and adjust to zero with water, and measure its absorbance. 6.3.7 Use the absorbance of the test solution and the absorbance of the accompanying blank solution to find the corresponding nickel concentration from the calibration curve, ug/ml. 6.4 Drawing of the calibration curve
6.4.1 Nickel content is less than 0.02%
Use a burette to add 0, 1.00, 2.00, 2.50, 3.00 and 4.00 ml of nickel standard solution (3.11.2) to 6 100 mL volumetric flasks in sequence, add 25 mL of matrix solution (3.10) and 10 mL of hydrochloric acid (3.2), dilute to the scale with water and mix well. 6.4.2 Nickel content greater than 0.02%
Use a burette to sequentially add 0, 4.00, 8.00, 12.00, 16.00 and 20.00 ml of nickel standard solution (3.11.2) to six 100 ml volumetric flasks, add 25 ml of matrix solution (3.10) and 10 ml of hydrochloric acid (3.2), dilute to scale with water and mix. 6.4.3 Measure the calibration solution (6.4.1 or 6.4.2) according to 6.3.6. The absorbance of each solution in the calibration curve series minus the absorbance of the zero concentration solution is the net absorbance of the nickel calibration curve series solution. Draw a calibration curve with nickel concentration as the horizontal axis and net absorbance as the vertical axis. 7 Calculation of results
The mass percentage of nickel is calculated as follows:
Ni(%) = (.- c) × V × 100
m × 10g
Wherein: c2-the nickel concentration in the test solution obtained from the calibration curve, μg/mL, Ci-——the nickel concentration in the blank solution with the sample obtained from the calibration curve, μg/ml; V-the volume of the test solution, mL;
m-the mass of the test solution sample, g;
the conversion factor of the nickel content in the completely dried sample. 8 Allowable difference
The difference in the analysis results between laboratories should not be greater than the allowable difference listed in Table 2. Additional remarks:Www.bzxZ.net
0. 005 --0. 01
>0. 01～0.02
0.02-0.05
>0.05~0.1
>0. 1~0. 2
0. 2 ~~0. 5
>0. 5~1. 0
GB/T 14949.2---94
This standard is proposed by the Ministry of Metallurgical Industry of the People's Republic of China.
This standard is drafted by the Mineral Geology Research Institute of China Nonferrous Metals Industry Corporation and Changsha Mining and Metallurgical Research Institute of Metallurgical Industry. This standard is drafted by Guangxi Metallurgical Research Institute. The main drafter of this standard is Huang Zuan.
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