GB/T 4324.11-1984 Chemical analysis of tungsten - The chrome azurol S photometric method for the determination of aluminum content

GB/T 4324.11-1984 Chemical analysis of tungsten - The chrome azurol S photometric method for the determination of aluminium content GB/T4324.11-1984 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Methods for chemical analysis of tungsten The chromazurol S photometric method for thedetermination of aluminium contentUdC 669.27*543wwW.bzxz.Net
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GB 4324.11—84
This standard is applicable to the determination of aluminium content in tungsten powder, strip, tungsten trioxide, tungstic acid and ammonium paratungstate. Determination range: 0.0005-0.025%. This standard complies with GB1467--78 "General Principles and General Provisions for Chemical Analysis Methods of Metallurgical Products". TMethod Summary
The sample is decomposed with hydrogen peroxide and sodium hydroxide, the residue is dissolved with potassium pyrosulfate, leached with water, and separated by extracting the aluminum-molybdenum reagent complex with ethyl acetate at pH 8.5-9.0. After back extraction with dilute hydrochloric acid, aluminum and chrome azuro S form a purple-red complex in a hexamethylenetetramine buffer solution, and its absorbance is measured.
2Reagents
Potassium pyrosulfate.
2.2Hydrogen peroxide (specific gravity 1.10).
Ethyl acetate.
Sodium hydroxide solution (10%), high-grade purity. 2.4
Hydrochloric acid (1+10), high-grade purity.
Hydrochloric acid (0.2N), high-grade purity.
Nitric acid (1+2).
Ammonium hydroxide (1+1).
2.9Hydroxide (1+10).
2.10 Ascorbic acid solution (1%), prepare when needed. Ammonium hydroxide-ammonium nitrate buffer solution (pH8.5), weigh 6.4g ammonium nitrate and dissolve in water, add 1.5ml ammonium hydroxide 2.11
(specific gravity 0.90), dilute with water to 1000ml, busy in a plastic bottle 2.12
N-benzoylphenylhydroxylamine (molybdenum reagent) ethanol solution (0.1%). Bromocresol green-methyl red solution: three parts of bromocresol green ethanol solution (1%) and one part of methyl red ethanol solution (0.2%) 2.13
Phenolyl ethanol solution (0.1%).
2.15 Ming Tianqing S ethanol solution (0.1%). 2.16 Methylenetetramine solution (20% pH about 6.5). 2.17 Calcium solution: Weigh 0.5g calcium carbonate, add 10ml hydrochloric acid (1+1) to dissolve, dilute with water to 1000ml, mix well. This solution contains 2.00mg calcium in 1ml.
2.18 Aluminum standard solution
2.8.1 Weigh 1.0000g metallic aluminum (99.90% or more), place in a 200ml beaker, add 10ml hydrochloric acid (1+1), heat at low temperature to dissolve, cool, transfer to a 1000ml volumetric flask 11, dilute with water to the mark, mix well. This solution contains 1.0mg aluminum in 1ml. National Bureau of Standards Issued on April 12, 1984
Implementation on March 1, 1985
G4324.11-
2.18.2 Take 10.00m aluminum standard solution (2.18.1), pour it into a 1000m bottle, dilute it with water, and mix it. This solution contains 10μg aluminum in 1ml.
a Sample
Tungsten bar should be powdered zinc and passed through a 120L sieve.
Analysis steps
41 Determination quantity
Three samples should be weighed for analysis, and the measured values ​​should be within the range of the test value. 42 Sample quantity
Weigh the sample quantity according to Table 1.
Aluminum, %
0.0005 --0.0020
0.0020 ~0.0040
>0.0040~0.010
0.0160.025
4.3 Blank test
Carry out a blank test together with the sample.
4.4 Determination
Crane powder, pigeon strips
4.4.11 Place the sample (4.2) in a 100ml beaker, add 5ml of water, heat to dissolve, remove and cool, add 10ml of sodium hydroxide solution (2.4), heat to decompose peroxide 4.4.12 Remove, filter the 100ml beaker, transfer all the drops in the original beaker to filter paper 15 times, retain the filtrate, put the filter paper and the residue into platinum, and dissolve. 4.4.1.3 Add 1g of potassium pyrosulfate (2.1), melt at 700~800℃ for 23min.10! Water, heat the melt and take it out and put it on the car, wash it with water, and use it for research. The liquid needs to be single. (2.), chemical solution (2.4) nitric acid (2.7) adjust the liquid to light red, add 10m ammonium chloride-magnetic buffer (211. Add 120ml separatory funnel, wash the beaker, and control the volume to about 70ml. 44.1.4 Add 4ml reagent ethanol solution (2.12), add 1mia, 3.3), shake for 1min, stand and separate, remove the water, and add 10m water in a peach machine. Shake, run (2.) back extraction twice, shake for 1min each time, stand and separate, remove the negative phase, and store the two processes in a 3-room cup, evaporate to a volume of about 2ml, remove and cool, transfer to a 10um container:, add water to about 70ml. 4.4.1.5 Add 1M calcium solution (2.17) and 1N anti-ascorbic acid solution (2.10), mix, add 1 ml cresol and methyl red solution (2.13), adjust the solution with hydrochloric acid (2.5) and ammonium hydroxide (2.9) to make the red turn green, add 5M hydrochloric acid (2.6), 3M chrome blue S (2.15), 5ml hexamethylenetetramine solution (2.1G): each reagent needs to be mixed. Dilute with water to the mark, mix, and put in the stomach. 10min.
4.4.1.6 Transfer part of the solution to a 1cm colorimetric colorimeter and measure its absorbance at 553m. Obtain the corresponding concentration from the 7-axis line. 4.4.2 Tungsten oxide, tungstic acid, ammonium paratungstate
Put the sample (4.2) in a 100ml beaker and add 10ml sodium hydroxide (2.1) and 5ml of water. Ionize 33
GB 4324.11—84
Hydrogen (2.2), heat and decompose hydrogen peroxide. The following is carried out according to 4.4.1.2-4.4,1.6. 4.5 Drawing of working curve
4.5.1 Transfer 0.00, 0.50, 1.00, 1.50, 2.00, 2.50, 3.00ml of aluminum standard solution (2.18.2) to a 100ml volumetric flask, and add about 7um! Water. The following is carried out according to 4.4.1.4~4.4.1.5. .5.2 Transfer part of the solution to 1 cm is smaller than l, and the absorbance is measured at a wavelength of 550nn on a spectrophotometer with the reagent air as a reference. A curve is drawn with the sales volume as the horizontal axis and the absorbance as the vertical axis. Calculation of analysis results
Calculate the aluminum content according to the following formula:
m, - aluminum content obtained from the curve, g1 sample, g.
6 Allowable error
The difference in the analysis results of the laboratory should not be greater than the allowable error listed in Table 2. Table 2
0.0005~0,0015
50 0015- 0. 0040
>0.0040~0.0080
0.0080 ~0.0120
>0.012 ~0.025
Additional Notes:
This standard was proposed by the Ministry of Metallurgical Industry of the People's Republic of China. This standard was drafted by Zhuzhou Hard Gold Factory. This standard was drafted by Baoji Nonferrous Metals Research Institute and Baoji Nonferrous Metals Processing Factory. The main drafter of this standard was Chen Jue.
From the implementation of this standard, the original Ministry of Metallurgical Industry Standard YB895-7 "Tungsten Content Analysis Method" will be invalid. 3i
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