This standard specifies the method for determining the manganese content in nickel-chromium and nickel-chromium-iron alloys by sodium periodate photometry. This standard is applicable to the determination of manganese content in nickel-chromium and nickel-chromium-iron alloys. Determination range: 0.10% to 2.00%. JB/T 6326.6-1992 Chemical analysis method for nickel-chromium and nickel-chromium-iron alloys Determination of manganese content by sodium periodate photometry JB/T6326.6-1992 Standard download decompression password: www.bzxz.net

Mechanical Industry Standard of the People's Republic of China
JB/T6326.6-1992
Chemical analysis method for nickel-chromium and nickel-chromium-iron alloys - determination of manganese content by sodium periodate photometry
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 - determination of manganese content by sodium periodate photometry
Subject content and scope of application
This standard specifies the method for determining the content of nickel-chromium and nickel-chromium-iron alloys by sodium periodate photometry. JB/T6326.61992
This standard is applicable to the determination of manganese content in nickel-chromium and nickel-chromium-iron alloys, with a determination range of 0.10% to 2.00%. Reference Standards
GB1467 General Principles and General Provisions for Chemical Analysis Methods of Metallurgical Products 3 Method Summary
The sample is dissolved in acid, perchloric acid smokes, manganese is oxidized to permanganic acid with sodium periodate, and its absorbance is measured. 4 Reagents
4.1 Sodium periodate
4.2 Hydrochloric acid (density pl.19g/ml),
Nitric acid (density pl.42g/ml).
4.4 Hydrofluoric acid (density pl.15g/ml).
Perfluoric acid (density pl.67g/ml).
Sulfuric acid (density pl.84g/ml).
Phosphoric acid (density pl.69g/ml). bzxz.net
Nitric acid (1+1).
Nitric acid (1+3).
Hydrochloric acid-nitric acid mixture: hydrochloric acid (4.2) + nitric acid (4.3) (1 + 1). Sulfuric acid (1 + 3).
Sulfuric acid-phosphoric acid mixture: slowly add 150ml sulfuric acid (4.6) to 500ml water. After cooling slightly, add 350ml phosphoric acid (4.7) and mix.
Sodium periodate solution (50g/L): weigh 50g sodium periodate (4.1) and place it in a 1000ml beaker. Add 500ml water and dissolve it in warm water. 4.13
Add 200ml nitric acid (4.8), cool, dilute to 1000ml with water, and mix. 4.14 Sodium nitrite solution (5g/L).
4.15 Water without reducing substances: heat 1000ml deionized water (or distilled water) to boil, and acidify with 10ml sulfuric acid (4.11). Add a few grains of sodium periodate (4.1) and continue boiling for 5 minutes. Use after cooling. 4.16 Manganese standard solution.
Weigh 0.5000g. electrolytic manganese (more than 99.9%) (\) and place it in a 250ml conical beaker, add 20ml nitric acid (4.9), heat 4.16.1
to dissolve, boil to drive out nitrogen oxides, remove and cool, transfer to a 500ml volumetric flask, dilute to scale with water, and mix well. This solution contains 1.00mg manganese in 1ml.
Approved by the Ministry of Machinery and Electronics Industry on June 26, 1992, and implemented on January 1, 1993
JB/T 6326.61992
Note: 1) If there is an oxide layer on the surface, it needs to be washed with 5+95% sulfuric acid. After the surface manganese oxide is washed away, take it out and immediately wash it repeatedly with distilled water, then wash it with anhydrous acetic acid for 4 to 5 times, and dry it in a desiccator for use. 4.16.2 Transfer 25.00ml of manganese standard solution (4.16.1) into a 500ml volumetric flask, dilute it to the mark with water, and mix it well. This solution contains 50% manganese in 1ml.
5 Analysis steps
5.1 Sample amount
Weigh the sample amount according to Table 1
Total manganese content
0.10~0.50
>0.50~1.00
>1. 00~2. 00
5.2 Blank test
Carry out a blank test together with the sample
5.3 Determination
5.3.1 Place the sample in a 125ml conical beaker, add 10~15ml of hydrochloric acid and nitric acid mixture (4.10) and heat at low temperature to dissolve. For the high-silicon sample, add 2~5 drops of hydrofluoric acid (4.4), add 5ml of perchloric acid (4.5) and continue heating to evaporate until the perchloric acid smoke reaches the bottle mouth. After the chromium fluoridation is complete and salts begin to precipitate, remove and cool slightly, add 20ml water to dissolve the salts, transfer to a 100ml volumetric flask after cooling, dilute to scale with water, and mix.
5.3.2 Color development solution: Transfer 20.00ml of the test solution to a 125ml conical beaker, add 10ml of sulfuric acid-phosphoric acid mixed acid (4.12), mix, add 10ml of sodium periodate solution (4.13), mix. Heat and boil for 2min, continue to keep it slightly boiling for 3min (to prevent the test solution from precipitating), cool to room temperature, transfer to a 50ml volumetric flask, dilute to scale with water (4.15) that does not contain reducing substances, and mix. This is the color development solution. Pour the color development solution into a 1cm or 2cm colorimetric blood. 5.3.3 Reference solution: Add sodium nitrite solution (4.14) to the remaining color development solution while shaking to make the color of high-valent manganese disappear. Pour this solution into another 1cm or 2cm colorimetric band. 5.3.4 Measure the absorbance of the reference solution at a wavelength of 540nm on the spectrophotometer, subtract the absorbance of the reagent blank, and find the corresponding manganese content on the working curve.
5.4 Drawing of working curve
Pipette 0.00, 1.00, 2.00, 4.00, 6.00, and 8.00ml of manganese standard solution (4.16.2) and place them in 6 125ml conical beakers respectively, adjust the volume to about 20ml with water, and proceed as in 5.3.2 to 5.3.3, using the color developing solution without manganese standard solution as the reference solution, measure its absorbance, and draw the working curve. 6
Calculation of analysis results
Calculate the percentage of manganese according to the following formula:
Mn (%)
Wherein;, the amount of manganese found from the working curve, g: V—total volume of test solution, ml;
V, volume of test solution taken, ml;
amount of sample, g.
Allowable difference
JB/T6326.6-1992
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table 2. Table 2
0.100~0.500
>0.500~1.000
>1.00~2.00
Additional instructions:
This standard is proposed and managed by the Shanghai Electric Science Research Institute of the Ministry of Machinery and Electronics Industry. This standard was drafted by the Shanghai Alloy Factory of the Ministry of Machinery and Electronics Industry. The main drafter of this standard is Li Peili.
Allowable difference
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