This standard specifies the method for determining the nickel content of chromium and nickel-chromium-iron alloys by dimethylglyoxime gravimetric method. This standard is applicable to the determination of nickel in nickel-chromium and nickel-chromium-iron alloys, with a determination range of 50.00% to 80.00. JB/T 6326.1-1992 Chemical analysis method for nickel-chromium and nickel-chromium-iron alloys Dimethylglyoxime gravimetric method for determination of nickel content JB/T6326.1-1992 Standard download decompression password: www.bzxz.net

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JB/T6326.1-1992
Chemical analysis method for nickel-chromium and nickel-chromium-iron alloys: diacetyl gravimetric method for determining nickel content
Published on June 26, 1992
Implementation by the Ministry of Machinery and Electronics Industry of the People's Republic of China on January 1, 1993
Mechanical Industry Standard of the People's Republic of China
Chemical analysis method for nickel-chromium and nickel-chromium-iron alloys: diacetyl gravimetric method for determining nickel content
Subject content and scope of application
This standard specifies the method for determining nickel content in nickel-chromium and nickel-chromium-iron alloys using the diacetyl gravimetric method. JB/T6326.1-1992
This standard is applicable to the determination of nickel content in nickel-chromium and nickel-chromium-iron alloys. Determination range: 50.00% to 80.00%. 2 Reference Standards
GB1467 General Principles and General Provisions for Chemical Analysis Methods of Metallurgical Products 3 Method Summary
In ammonium ester buffer solution, tartaric acid is used as a complexing agent. At pH 6.0-6.5, nickel and diacetyl are completely precipitated and separated from elements such as iron, chromium, cobalt, manganese, aluminum, titanium, molybdenum, vanadium, saw, copper and rare earth. Diacetyl nickel is dried at 140℃ to a constant weight. 4 Reagents
Hydrochloric acid (density p1.19g/ml).
Nitric acid (density pl.42g/ml).
4.3 Perchloric acid (density pl.67g/ml), 4. 4
Ammonium hydroxide (density p0.90g/ml).
Hydrochloric acid (1+1).
Hydrochloric acid (5+95).
Nitric acid (1+1),
Ammonium hydroxide (1+1).
Tartaric acid solution (200g/L): Use after filtration. Ammonium ester solution (500g/L): Use after filtration. Butanedione ethanol solution (10g/L): Use after filtration. Analysis steps
5.1 Sample amount
Weigh 0.1000g of sample.
5.2 Determination
5.2.1 Place the sample in a 250ml beaker, add 5ml hydrochloric acid (4.1), 5ml nitric acid (4.2), cover with surface III, and slowly heat until dissolved. After the dissolution is complete, add 5ml of perchloric acid (4.3), heat and evaporate until smoke appears, move to a low temperature place and continue to reflux for 10~15min while emitting perchloric acid smoke, until all the chromium oxide scales are high, remove and cool slightly, add 10ml of hydrochloric acid (4.5), 50ml of water, and heat to dissolve the salts. 5.2.2 Filter the solution with quantitative filter paper, place the filtrate in a 500ml beaker, wash the beaker with dilute hydrochloric acid (4.6), and wash the filter paper and precipitate 78 times, so that the total volume of the solution is controlled at 300ml. Approved by the Ministry of Machinery and Electronics Industry on June 26, 1992, implemented on January 1, 1993
JB/T6326.11992
5.2.3 Add 10ml of tartaric acid solution (4.9), 20ml of ammonium acetate solution (4.10), add ammonium hydroxide (4.8) dropwise while stirring, and adjust the solution to pH 6.0~6.5.
5.2.4 Heat the solution to 6070℃, add diacetyl alcohol solution (4.11) (calculated as 0.6ml diacetyl alcohol solution for every 1mg nickel, cobalt and copper) under constant stirring, and cool to room temperature. 5.2.5 Use constant volume F3-3 crucible filter (Gooch) to filter under negative pressure (the speed should not be too fast, and the precipitate must not be sucked dry), wash the beaker and precipitate with a small amount of water for multiple times. The amount of water used is generally about 200ml. 5.2.6 Place the glass cocoon in an oven and bake at 140℃ to a constant volume. Calculation of analysis results
Calculate the percentage of nickel according to the following formula.
Ni(%)=（(mlm)×0.2032×100
Wherein: 0,-
Mass of glass crucible and nickel diacetate precipitate, g: m2—Mass of glass crucible, g;
m—Test weight, g;
0.2032--—Coefficient for converting nickel diacetate to nickel. Allowable difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in the following table. Table
50.00~60.00
>60.00~80.00
Additional instructions:
This standard was proposed and managed by Shanghai Electric Science Research Institute of the Ministry of Machinery and Electronics Industry. This standard was drafted by Tianjin Electrical Alloy Factory. The main drafters of this standard were Zhao Shiyu and Liu Qinghai. 2
Allowable difference
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