GB 4374.1-1984 Chemical analysis methods for magnesium powder and aluminum-magnesium alloy powder - New copper reagent extraction photometric method for the determination of copper content

GB 4374.1-1984 Chemical analysis method for magnesium powder and aluminum-magnesium alloy powder - Determination of copper content by extraction photometry with new copper reagent GB4374.1-1984 standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Methods for chemical analysis of magnesium powders and aluminium -magnesium alloy powdersThe neocuproine -extraction photometric methodfor the determination of copper contentThis standard is applicable to the determination of copper content in aluminium -magnesium alloy powders. Determination range: 0.0050~0.050%. This standard complies with GB1467-78 "General Principles and General Provisions for Chemical Analysis Methods for Metallurgical Products". Method Summary
UDC 669.721 + 669
.715'721-492
GB 4374.1 --84
The sample is dissolved with hydrochloric acid and hydrogen peroxide, and copper is reduced with hydrochloric acid hydroxylamine. In an acidic solution of pH 3-4, copper (") reacts with the new copper reagent to form a yellow complex, which is extracted with chloroform and its absorbance is measured at a wavelength of 460 mm by a spectrophotometer. The test solution contains 5 mg iron, 1 mg zinc, 1 mg silicon, and 0.1 mg manganese, which do not interfere with the determination. 2
Reagents and materials
2.1 Chloroform.
2.2 Hydrochloric acid (1+1).
2.3 Hydrogen peroxide (commercially available 30%).
2.4 Hydrochloric acid hydroxylamine solution (10%).
2.5 Lemon Sodium hydroxide solution (50%).
Ammonium hydroxide (1+1).
Aluminum-magnesium matrix solution:
Weigh 223.8g of tin trichloride (AICl: ·6H,O), place it in a 500ml beaker, add 200ml of water, and stir to dissolve it. Weigh 25g of pure magnesium (99.99%), place it in a 500ml beaker, add 200ml of hydrochloric acid (2.2), dissolve it and boil it. b.
Filter the solutions in a. and b. above into the same 500ml volumetric flask, cool, dilute to the mark with water, and mix well. This solution contains 0.05g of aluminum and magnesium in 1ml.
2.8 2.9-Methyl-1,10-phenanthroline (neucopterin) solution (0.1%): Weigh 0.1gneucopterin, place in a 100ml beaker, add a small amount of alcohol to dissolve it. Transfer to a 100ml volumetric flask and dilute to scale with ethanol (valid for about a week). 2.9 Copper standard stock solution: Weigh 0.1000g pure copper (99.95% or more), place in a 150ml beaker, add 15ml water and 5ml nitric acid (specific gravity 1.42), wait until completely dissolved, boil to drive off nitrogen oxides. Cool, transfer to a 1000ml volumetric flask, dilute to scale with water. This solution contains 0.1mg copper.
2.10 Copper standard solution: Pipette 10.00 ml of copper standard storage solution (2.9) into a 100 ml volumetric flask, dilute to the mark with water, and mix. This solution contains 10 ug copper per ml.
2.11 Congo red test paper (cut into small pieces without rough edges). 3
Spectrophotometer.
National Bureau of Standards Issued on April 30, 1984
Implemented on April 1, 1985
Analysis steps
4.1 Quantity of determination
Measure two samples and take the average value. 4.2 Sample quantity
Weigh the sample according to Table 1.
0.005 ~ 0.015
0.015~0.05
GB4374.1--84
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4.3 Blank test
Weigh the sample (1.2) according to Table 1 and place it in a 100ml beaker. The following shall be carried out according to 4.4.2.4.4.3 (without adding new copper reagent solution) and 4. ... 4.4.3 Add 5 ml of hydroxylamine hydrochloride solution (2.4) and 15 ml of sodium citrate solution (2.5), and apply a small piece of Congo red test paper (2.11): Use ammonium oxide (2.6) to adjust the Congo red test paper to a slightly purple color. Add 5 ml of new copper reagent solution (2.8), mix well, and let stand for 5 minutes. 4.4.4 Transfer the solution (4.4.3) to a 100 ml separatory funnel (the volume of the solution is about 60 ml at this time), add 10.0 ml of methyl chloride (2.1), shake for 2 minutes, and let stand for separation. 4.4.5 Transfer the damp organic phase (4.4.4) to a dry 1 cm colorimetric III. Take the organic phase of the blank test (4.3) as a reference and measure its absorbance at a wavelength of 460 nm on a spectrophotometer. Draw a curve from 1 to derive the corresponding copper content. 4.5 Drawing of working curve
4.5.1 According to the sample (4.2), transfer an appropriate amount of aluminum-magnesium matrix solution (2.7) (the amount of aluminum and magnesium should be the same as that contained in the sample), place it in a 100ml beaker of group F, and add 0.001.00, 2.00.3.00, 4.00, 5.00, and 6.00ml of copper standard solution (2.10) respectively. The following is carried out according to 4.4.3 to 4.4.4. 4.5.2 Transfer part of the organic phase (4.5.1) into a dry 1cm colorimetric, use the compensation solution (the one that is not copper standard solution in 4.5.1) as a reference, and measure its absorbance at a wavelength of 460nm on the spectrophotometer. Draw an oil line with the amount of copper as the horizontal scale and the absorbance as the vertical scale. 5
Calculation of analysis results
Calculate the percentage of copper according to the following formula:
Cu(%):
Wu Zhong: m-Nan "The value obtained on the curve, g: m
Allowance
Wu Xiang's maximum g.
The difference between the analysis results of different laboratories should not exceed the allowable difference listed in Table 2. 146
× 100
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0.005~0.010
>0.010~0.020
>0.020~0.050
GB 4374.1—84
This standard was proposed by the Ministry of Metallurgical Industry of the People's Republic of China. This standard was drafted by the Northeast Light Alloy Processing Plant. This standard was drafted by the Northeast Light Alloy Processing Plant and the Northwest Aluminum Processing Plant. The main drafter of this standard is You Guifa.
Allowance
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