GB/T 4324.10-1984 Chemical analysis method of tungsten - Determination of copper content by new copper reagent photometric method GB/T4324.10-1984 standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Chemical analysis method of tungsten
The neocuproine photometric method for thedetermination of copper contentUDC 669.27 : 643
42:546.56
GB 4324.10--84
This standard is applicable to the determination of copper content in tungsten powder, tungsten bar, tungsten trioxide, tungstic acid and ammonium paratungstate. The determination range is 0.0003%~0.0030%. This standard complies with GB1467-78 "General Principles and General Provisions of Chemical Analysis Methods for Metallurgical Products". 1 Method Summary
The sample is decomposed by oxidation with oxygen or sodium hydroxide, and in a slightly ammoniacal medium, the main pigeon is complexed with potassium sodium tartrate, and hydroxylamine hydrochloride reduces copper (II) to copper (I). At pH 7-8, the new reagent complex of copper (I) is extracted with chlorine-containing alkane, and its absorbance is measured. 2 Reagents
Ammonium hydroxide (specific gravity 0.90).
Hydrogen peroxide (specific gravity 1.10).
Chloroform.
Hydrochloric acid (1+1).
Sodium hydroxide solution (20%).
Phenol red ethanol solution (0.1%).
2,9-Dimethyl-1,10-aza-non (new copper reagent) ethanol solution (0.15%). 2.8 Hydroxylamine hydrochloride solution (10%). The purification steps are as follows: weigh 10g of hydroxylamine hydrochloride, place it in a 250ml beaker, add 60-70ml of water to dissolve it, adjust the pH to 7-8 with ammonium hydroxide (2.1) (check with pH test paper), transfer it to a 125ml separatory funnel with water and control the volume to 100ml, add 5ml of new copper reagent ethanol solution (2.7), mix well, let it stand for 5min, and shake it several times with chloroform (2.3) (10ml each time, shaking for 1min) until the organic phase is no longer yellow. Discard the organic phase, filter the aqueous phase into a reagent bottle and set aside. 2.9 Potassium sodium tartrate solution (40%). The purification steps are as follows: weigh 40g of potassium sodium tartrate, place it in a 250ml beaker, add 60-70ml water to dissolve, adjust the pH to 7-8 with hydrochloric acid (2.4) (check with pH test paper), transfer it into a 125ml separatory funnel with water and control the volume to 100ml, add 10nl of hydroxylamine hydrochloride solution (2.8), add 5ml of new copper reagent ethanol solution (2.7), mix well, let it stand for 5min, and shake it several times with chloroform (2.3) (10ml each time, shake for 1min) until the organic phase is no longer yellow. Discard the organic phase, filter the aqueous phase into a reagent bottle and set aside.
2.10 Double distilled water (this method uses this water) 2.11 Copper standard solution
2.11.1 Weigh 0.1000g of metallic copper (99.90% or more), place in a 250ml beaker, add 10m nitric acid (1+1) to dissolve, add 10ml sulfuric acid (1+1), evaporate until white sulfuric acid smoke appears, remove and cool, add 30-40ml water, heat to dissolve the salts, remove and cool, transfer to a 1000ml volumetric flask with water, dilute to the mark, and mix. This solution contains 100μg copper in 1ml. 2.11.2 Transfer 25.00ml of copper standard solution (2.11.1), place in a 500ml volumetric flask, dilute to the mark with water, and mix. This solution contains 5/g copper in 1ml.
National Bureau of Standards Issued on April 12, 1984
Implementation on March 1, 1985
Test sample
Tungsten bars should be crushed and passed through a 120-mesh screen.
4 Analysis steps
Table 1 Determination quantity
GB 4824.10—$4
Three samples should be weighed for determination during analysis. The measured values ​​should be within the allowable indoor difference and the average value should be taken. 4. 2 Sample quantity
Weigh 0.5000~1.000g of sample.
4.8 Blank test
Carry out a blank test with the sample
4.4 Determination
4.4.1 Pigeon powder, tungsten bar
Put the sample (4.2) in a 250ml beaker, moisten it with 1-2ml water, slowly add 15ml hydrogen peroxide (2.2) twice, let it decompose, wait for the violent reaction to stop, then add 10ml hydrogen peroxide (2.2) twice, heat to dissolve the sample completely, blow the surface blood and the cup with water (no need to cover it), continue heating and evaporating to dryness, repeat once, remove and cool, add 5m sodium hydroxide solution (2.5), heat and dissolve until the solution is clear. Tungsten trioxide, pigeon acid, ammonium paratungstate
Put the sample (4.2) in a 250ml beaker, add 5ml sodium hydroxide solution (2.5), heat and dissolve until the solution is clear. 4.4.3 Add 10 ml of potassium sodium tartrate solution (2.9) to the solution (4.4.1 or 4.4.2), add 5 ml of hydrochloric acid (2.4) while shaking, heat and boil for 1-2 min, remove and cool. 4.4.4 Add 10 ml of hydroxylamine hydrochloride solution (2.8) and 1-2 drops of phenol red ethanol solution (2.6), and adjust with ammonium hydroxide (2.1) until the solution is orange-red (pH?~8).
4.4.5 Transfer the mixture into a 125ml separatory funnel with water, control the volume to about 50ml, add 5ml of new copper reagent ethanol solution (2.7), mix, place for 5min, add 10.00ml of chloroform (2.3), shake for 1min, let stand for stratification, filter the organic phase through absorbent cotton into a 2cm colorimetric III, use trioxane (2.3) as reference, and measure its absorbance at a wavelength of 450mm with a hand spectrophotometer. 4.4.6 Subtract the absorbance of the blank prepared with the sample. Find the corresponding copper amount from the working curve. 4.5 Drawing of working curve
Pipette 0.00, 0.50, 1.00, 2.00, 3.00, 4.00ml of copper standard solution (2.11.2) and place them in a group of 100ml beakers respectively. Follow the procedures in 4.4.3 to 4.4.6, measure the absorbance, and subtract the absorbance of the reagent blank. Draw a working curve with the copper content as the horizontal axis and the absorbance as the vertical axis.
5 Calculation of analysis results
Calculate the percentage of copper as follows:www.bzxz.net
Cu(%):
Where: mi is the copper found on the working curve, g - the sample amount, g.
. Allowable difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in the following table. 30
Additional Notes:
0.00030~0.00060
0.000600.00.080
>0.00080~0.00120
≥0.0012-0.0020
>0.0020 -0.0030
GB 4824,10--84
This standard is proposed by the Ministry of Metallurgical Industry of the People's Republic of China. This standard is drafted by Zhuzhou Cemented Carbide Factory. This standard is drafted by Zhuzhou Cemented Carbide Factory. The main drafters of this standard are Liu Tingzhu and Tan Aiyun. Allowable difference
0,00015
interest From the date of implementation of this standard, the former Ministry of Metallurgical Industry Standard YB895-77 "Chemical Analysis Method for Tungsten" will be invalid. 藕稚17bzw.cn脆黛簡种黛颜红痕旅科5翅湖
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