GB/T 4375.1-1984 Chemical analysis of gallium - Spectrophotometric determination of copper content using 2,9-dimethyl-4,7-diphenyl-1,10-phenanthroline GB/T4375.1-1984 standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Methods for chemical analysis of galliumThe 2,9 - dimethyl- 4,7 -diphenyl-1, 10phenanthroline photometric method forthe determinatlon of copper contentThis standard is applicable to the determination of copper in gallium. Determination range: 0.00050～0.040%. This standard complies with GB1467-78 "General Principles and General Provisions of Standards for Chemical Analysis Methods of Metallurgical Products". 1 Method SummarybZxz.net
UDC 669.871: 543
42:546.56
GB 4375.1--84
The sample is dissolved with nitric acid and hydrochloric acid. In the presence of ammonium citrate, copper is reduced with hydroxylamine hydrochloride. At pH 5, copper (1) forms a yellow complex with 2,9+ dimethyl-4,7-diyl-1,10-phenanthroline. After extraction with isoamyl alcohol, its absorbance is measured at a wavelength of 470 nm on a spectrophotometer.
2 Reagents and materials
2.1 Anhydrous ethanol, high-grade purity.
2.2 Isoamyl alcohol.
2.3 Nitric acid, high-grade purity (specific gravity 1.42). 2.4 Hydrochloric acid, high-grade purity (specific gravity 1.19). 25 Ammonium hydroxide (1+1).
2.6 Ammonium citrate solution (30%).
2.7 Hydroxylamine hydrochloride solution (10%).
2.82,9·Dimethyl-4,7-diphenyl-1,10-phenanthroline solution (0.1%): Weigh 0.1g 2.9~dimethyl-4,7-diphenyl-1,10-phenanthroline, dissolve in 100ml ethanol, mix well. 2.9 Copper standard stock solution: Weigh 1.000g pure copper (99.9% or more), place in 400ml beaker c, add 20ml nitric acid (1+1), heat to dissolve, evaporate to nearly dry, add 10ml sulfuric acid (specific gravity 1.84), evaporate carefully until white smoke appears, cool. Add water and boil to dissolve all salts. Cool, transfer to a 1000ml volumetric flask with water and dilute to scale, mix well. This solution contains 1.0mg copper per ml.
2.10 Copper standard solution: Pipette 25.00 ml copper standard storage solution (2.9) into a 250 ml volumetric flask, dilute to scale with water, and mix. This solution contains 100 μg copper per ml.
2.11 Copper standard solution: Pipette 25.00 ml copper standard solution (2.10) into a 250 ml volumetric flask, dilute to scale with water, and mix. This solution contains 10 μg copper per ml.
2.12 Precision pH test paper.
Issued by the National Bureau of Standards on April 30, 1984
Implemented on April 1, 1985
3 Instruments
Spectrophotometer.
4 Analysis steps
4.1 Determination quantity
GB 4375.1—84
Weigh two samples for determination and take the average value. 4.2 Sample quantity
Weigh the sample according to Table 1.
Quantity, %
0.00050 ~0.0050
-0.0050~0.015
0.015~0.040
4.3 Blank test
Carry out a blank test with the sample.
4.4 Determination
Sample maximum,
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4.4.1 Place the sample (4.2) in a 50ml beaker and add 1 drop of hydrochloric acid (2.4) and 8 drops of nitric acid (2.3) to disperse the sample. Slightly heat, add 10ml hydrochloric acid (2.4), cover with Table III, place on an electric stove to heat, add nitric acid (2.3) dropwise to dissolve the sample completely, continue heating and evaporation, vacuum to a volume of about 1m, and cool. 4.4.2 Add 15ml ammonium citrate solution (2.6) and 5ml hydroxylamine hydrochloride solution (2.7), adjust to pH 5 with ammonium hydroxide (2.5), transfer the solution to a 100ml separatory funnel, add 2ml 2.9-monomethyl~4.7-monophenyl 1.10-phenanthroline solution (2.8), and mix. Let stand for 10min, add 10ml isoamyl alcohol (2.2), shake for 2min, let stand for oscillation, remove the aqueous phase, add 5ml water, shake for 15s, and discard the aqueous phase. Transfer the organic phase to a 25ml colorimetric tube, dilute to 15ml with anhydrous ethanol (2.1), and mix. 4.4.3 Pipette part of the solution (4.4.2) into a 1cm (3cm when the sample is 0.5g) colorimetric III, and measure its absorbance at a wavelength of 470nm on a spectrophotometer, using the blank accompanying the sample as a reference. Find the corresponding amount of copper from the working curve. 4.5 Drawing of the working curve
4.5:1 Pipette 0, 0.50, 1.00, 2.00, 3.00, 4.00ml or 0, 0.20, 0.40, 0.60, 0.80ml of the copper standard solution (2.11), respectively, into two groups of 100ml separating funnels, and proceed as in 4.4.2. 4.5.2 Pipette part of the solution (4.5.1) into the corresponding 1cm or 3cm colorimetric III, and measure its absorbance at a wavelength of 470nm on a spectrophotometer, using the reagent blank as a reference. Draw a T curve with copper content as the horizontal axis and absorbance as the vertical axis. Calculation of analysis results
Calculate the copper content according to the following formula:
Where: m—the amount of copper found on the I curve, μg; mn
sample amount, g.
ma × 106
Allowable difference
GB 4375.184
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table 2. Table 2
Additional notes:
0,0005~0.0030
-0.0030 ~0.0050
0.005~0.010
0.010-0.020
>0.020~0.040
This standard was proposed by China National Nonferrous Metals Industry Corporation. This standard was drafted by the Nonferrous Metals Research Institute of China National Nonferrous Metals Industry Corporation. The main drafter of this standard is Wang Liding.
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