GB/T 5059.3-1985 Chemical analysis of ferromolybdenum - Determination of copper content by atomic absorption spectrophotometry

This standard is applicable to the determination of copper content in ferromolybdenum. Determination range: 0.10-1.20%. This standard complies with GB 1467-78 "General Principles and General Provisions of Chemical Analysis Methods for Metallurgical Products". GB/T 5059.3-1985 Chemical analysis method for ferromolybdenum - Determination of copper content by atomic absorption spectrophotometry GB/T5059.3-1985 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Methods for chemical analysis of ferromolybdenum
Atomic absorption spectrophotometric method for the determination of copper content
Methods for chemical analysis of ferromolybdenumThe atomic absorption spectrophotometric method forthe determination of copper contentThis standard is applicable to the determination of copper content in platinum iron towels. Determination range: 0.10～1.20%. This standard complies with GB1467-78 "General Principles and General Provisions of Standards for Chemical Analysis Methods of Metallurgical Products". 1 Method Summary
UDC 669.15'28
GB5059.3--85
The sample is decomposed with sulfuric acid and nitric acid, and the sample is treated with sulfuric acid to produce a white simmer. Soluble salts are dissolved with hydrochloric acid, a certain volume is diluted with water, and its absorbance is measured on an atomic absorption spectrophotometer using air-acetylene flame spray. 2 Reagents
2.1 Nitric acid (1 +1).
2.2 Hydrochloric acid (1 + 1).
2.3 Hydrochloric acid (1 + 50).
2.4 Sulfuric acid (1 + 1).
2.5 Iron solution
Purify as follows: Weigh 5 portions of 1g pure iron, place each in a 300ml beaker, add 10ml hydrochloric acid (specific gravity 1.19), cover with Table III, and heat at low temperature to dissolve. Add 5m2l hydrogen peroxide (specific gravity 1.11) to oxidize the iron, heat and evaporate to 1, and be careful to prevent burning. Cool, add 10ml hydrochloric acid (10 + 6), heat to dissolve the salts, remove, cool to room temperature, transfer the solution to a 200ml separatory funnel with 20ml hydrochloric acid (10 + 6), add 30ml methyl isobutyl ketone (MIBK), shake vigorously for 1min, let stand and separate, and discard the lower aqueous phase. Add 20 ml of hydrochloric acid (10+6) to the organic phase, shake vigorously for 1 min, let stand and separate, and discard the lower aqueous phase. Add 20 ml of water to the organic phase, shake vigorously for 1 min, let stand and separate. Put the lower aqueous phase into the original beaker. Add 10 ml of water to a separatory funnel, shake vigorously for about 1 min, let stand and separate, and put the lower aqueous phase into the original beaker. Discard the organic phase. Boil the aqueous solution for about 5 min to volatilize most of the MIBK, add 5 ml of nitric acid (specific gravity 1.42), heat and evaporate to, cool, add 20 ml of hydrochloric acid (2.2), heat at low temperature to dissolve the soluble salts. Cool to room temperature, transfer 5 portions of the solution into a 250 ml volumetric flask, dilute to scale with water, and mix. This solution contains 20 mg of iron in 1 ml.
2.6 Copper standard solution: Weigh 0.5000g pure copper, place in a 300ml beaker, cover with table III, add 10ml sulfuric acid (2.4) and 20ml nitric acid (2.1), heat at low temperature to dissolve, remove table III, continue to add heat to produce smoke, cool, rinse the inner wall of the beaker with a small amount of water, reheat and cool. Add about 50ml water to dissolve soluble salts, transfer to a 1000ml volumetric flask, dilute to scale with water, and mix. This solution contains 0.5mg copper in 1ml.
3 Instruments
Original absorption spectrophotometer. Equipped with a copper hollow cathode lamp. The best operating conditions of the instrument are shown in Appendix A (reference). Issued by the National Bureau of Standards on April 15, 1985
Implemented on January 1, 1986
4 Sample
The sample should pass through a 0.125mm sieve.
5 Analysis steps
5.1 Sample quantity
Weigh the sample according to Table 1.
Copper, %
0.10~0.50
2-0.50~1.20
5.2 Air self-test
Carry out air self-test with the sample.
5.3 Determination
GB5059.3--85
Sample quantity, g
5.3.1 Place the sample (5.1) in a 200ml beaker and cover with a beaker. Add 10 ml sulfuric acid (2.4) and 10 ml nitric acid (2.1). Heat to dissolve, rinse Table III with water and remove, and evaporate until all sulfuric acid smoke is removed. Cool, add 20 ml hydrochloric acid (2.2), heat to dissolve soluble salts, filter, and wash thoroughly with hydrochloric acid (2.3). Collect the filtrate and washing liquid in a 100 ml volumetric flask. Cool to room temperature, dilute to scale with water, and mix. Discard the residue.
5.3.2 Spray part of the solution (5.3.1) on the original absorption spectrophotometer in an air-acetylene flame, and measure its absorbance at 324.7 nm.
5.3.3 Subtract the absorbance of the blanking test performed with the sample. Calculate the corresponding copper amount from the curve 1. 5.41. Plotting the curve
Pipette 0.00, 1.00, 2.00, 3.00, 4.00, 5.00 ml of copper standard solution (2.6) and place them in 100 ml volumetric flasks respectively. Add 10 ml of iron solution (2.5) (add 4 ml when the sample volume is 0.2000 g) and 20 ml of hydrochloric acid (2.2), dilute to the scale with water and mix well. The following is carried out according to 5.3.2, minus the absorbance of the compensation solution (zero concentration copper standard solution). With copper as the horizontal axis and absorbance as the vertical axis, plot a curve.
6Calculation
Calculate the percentage of copper according to the following formula:
Where: m, - the copper content obtained from the plotted curve, g: sample volume, g.
The analysis result is accurate to the 1 decimal place. 7 Allowable Difference
The difference between the analysis results of laboratories should not be too small. The allowable difference is listed in Table 2. 283
0.10~0.25
0.25~0.50bzxz.net
>0.50~1.20
GB 5059.3—85
Allowable Voucher
GB5059.3—85
Appendix A
Optimal Working Conditions of Instrument
(Reference)
The working conditions of the domestically produced WYX-401 atomic absorption spectrophotometer are as shown in the following table. Item
Additional Notes:
Copper Hollow Cathode Lamp
Lamp Current
This standard was proposed by the Ministry of Metallurgical Industry of the People's Republic of China. This standard was drafted by the person in charge of Jilin Ferroalloy Factory of the Ministry of Metallurgical Industry. Air flow
Acetylene flow
Burner height
From the date of implementation of this standard, the original metallurgical industry standard YB580--65 "Silver and Iron Chemical Analysis Method" will be invalid. Slit width
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