GB/T 8638.5-1988 Chemical analysis methods for nickel-based alloy powders - Sodium (potassium) periodate oxidation spectrophotometric method for the determination of manganese content

This standard is applicable to the determination of manganese content in nickel-based alloy powder. Determination range: 0.01% to 2.00%. This standard complies with GB 1467-78 "General Principles and General Provisions for Chemical Analysis Methods for Metallurgical Products". GB/T 8638.5-1988 Chemical analysis method for nickel-based alloy powder - Determination of manganese content by sodium (potassium) periodate oxidation spectrophotometry GB/T8638.5-1988 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Chemical analysis method of nickel-base alloy powder
Determination of manganese content by sodium (potassium) periodate oxidation spectrophotometryNickel base alioy powder--- Determination manganese confent Sodium (patassium periodate spectrophotomeiric met'odThis standard is applicable to the determination of manganese content in nickel-base alloy powder. Determination range: 0.01%~~2.00%U: 668. 235-452 2
GB 8538.523
This standard complies with GB1467-78 "General Principles and General Provisions of Chemical Analysis Methods for Metallurgical Products". 1 Method Summary
After the sample is dissolved in acid, manganese is oxidized to seven valences with sodium (potassium) periodate in sulfuric acid and phosphoric acid medium, and its absorbance is measured at 530nm on a spectrophotometer.
2 Reagents
2.1 Hydrochloric acid (pl.19 g/mL).
2.2 Nitric acid (p1.42 g/mL).
2.3 Hydrofluoric acid (p1.15 g/mL).
2.4 Sulfuric acid (1+1).
2.5 Sodium nitrite solution (1%).
2.6 Phosphoric acid-perchloric acid mixed acid: Mix three parts of phosphoric acid (p1.69 g/mL) and one part of perchloric acid (1.67/ml). 2.7 Sodium (potassium) periodate solution (5%): Weigh 5g of sodium (potassium) periodate and place it in a 250ml beaker, add 60ml of water and 20ml of nitric acid (2.2), dissolve in warm water, and cool Cool, dilute to 100mL with water. 2.8 Manganese standard solution: weigh 0.5000g electrolytic manganese (99.9%) [Electrolytic manganese treatment method: put electrolytic manganese in sulfuric acid-9) # to clean, take out after the surface oxidized manganese is washed, immediately wash repeatedly with distilled water, and then wash with anhydrous ethanol 4~5 times, take out, put in a dryer: dry and set aside) Place in a 250mL beaker, add 20mL nitric acid (1 + 3), heat to dissolve, boil to drive out all cyanide oxides, remove, cool to room temperature, transfer to a 1000mL volumetric flask, dilute to scale with water, and mix well. This solution contains 500μg manganese in 1mL, 2.9 Manganese standard solution: transfer 20mL manganese standard solution (2.8) to a 100mL volumetric flask, dilute to scale with water, and 1mL of this solution contains 100g manganese.
2.10 Water without reducing substances: Heat deionized water (or distilled water) to boil, acidify with 10mL sulfuric acid (1+3) per liter, add sodium (potassium) periodate, continue to heat and boil for a few minutes, cool and set aside. 3 Instruments
Spectrophotometer.
4 Analysis stepsbzxZ.net
4.1 Number of determinations
Measure twice in parallel and take the average value.
China Nonferrous Metals Industry Corporation 1988-01~11 approved 378
1989-3#-01 implementation
4.2 Sample quantity
Weigh 0.10000.5000g sample.
4.3 Determination
GB 8638.5-88
4.3.1 Place the sample (4.2) in a 150mL conical flask, add 15mL hydrochloric acid (2.1) and 2mL nitric acid (2.2), and heat at low temperature to dissolve (for insoluble samples, hydrofluoric acid (2.3) can be added dropwise to assist dissolution]. 4.3.2 Add 10mL phosphoric acid-perchloric acid mixture (2.6), heat and evaporate until perchloric acid smoke appears (chromium-containing samples need to oxidize chromium), cool slightly, and add 10mL sulfuric acid (2.4). Dilute with water to about 40ml, add 10mL sodium (potassium) periodate solution (2.7), heat to boil and keep for 2~3min (to prevent the test solution from splashing), cool to room temperature, transfer to a 100mL volumetric flask, dilute to scale with water (2.10) that does not contain reducing substances, and mix.
4.3.3 Transfer part of the color development solution (4.3.2) to a 1~3cm colorimetric nozzle, and add sodium nitrite solution (2 ,5) until the purple color just fades away, transfer the solution to another colorimetric III as a reference. 4.3.4 Measure the absorbance at a wavelength of 530nm on a spectrophotometer, and find the corresponding manganese content from the working curve. 4.4 Drawing of the working curve
Transfer 0, 0.50, 2.00, 4.00, 6.00, 8.00, 10.00mL of manganese standard solution (2.9). When the manganese content is greater than 0.5%, transfer 0, 2.00, 2. 50, 3.00, 3.50, 4.00mL manganese standard solution (2.8) are placed in a group of 150mL conical flasks respectively, and the following is carried out according to 4.3.2~~1.3.3. Measure its absorbance at a wavelength of 530nm on a spectrophotometer, and draw a working curve with the amount of manganese as the horizontal axis and the absorbance as the vertical axis.
5 Calculation of analysis results
Calculate the percentage of manganese according to formula (1):
Mn(%) m×10
Where: m: - the amount of manganese found from the working curve, ug, - the amount of sample weighed;
6 Allowable difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table 1. Table 1
0. 010~0. 050
>0. 050~0. 100
>0. 10 ~0. 50
>0. 50~1. 00
1. 00 ~2. 00
Additional instructions:
This standard was drafted by the Iron and Steel Research Institute of the Ministry of Metallurgical Industry. This standard was drafted by the Iron and Steel Research Institute of the Ministry of Metallurgical Industry. The main drafters of this standard are Yang Qiuping and Hu Xiaoyan. Allowable difference
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