This standard is applicable to the determination of lead content in nickel-based alloy powder. Determination range: 0.010% to 1.00%. This standard complies with GB 1467-78 "General Principles and General Provisions for Chemical Analysis Methods of Metallurgical Products". GB/T 8638.8-1988 Chemical analysis method for nickel-based alloy powder - Determination of copper content by new cuproline-chloroform extraction spectrophotometry GB/T8638.8-1988 Standard download decompression password: www.bzxz.net

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Chemical analysis method for nickel base alloy powder
Determination of copper content Neocuproine-chloroform extraction spectrophotometric method Nickel base alloy powder -. Determination of copper content Neocuproine-chloroform extraction spectrophotometric method This standard is applicable to the determination of copper content in nickel base alloy powder. Determination range: 0.010%~1.00%. UDC 669.245-492-2
GB8638.8:88
This standard complies with GB1467-78 "General Principles and General Provisions of Standards for Chemical Analysis Methods for Metallurgical Products". 1 Method Summary
The sample is dissolved in acid, and copper is reduced to valence with hydroxylamine hydrochloride in the presence of citric acid. In the pH range of 5-6, neocuproine and copper form an insoluble complex, which is extracted with chloroform and its absorbance is measured at a wavelength of 456nm on a spectrophotometer. 2 Reagents
2.1 Hydrochloric acid (p1.19 g/mL).
2.2 Nitric acid (g1.42 g/mL).
2.3 Perchloric acid (p1.67 g/mL).
2.4 Hydrofluoric acid (p1.15 g/mL).
2.5 Anhydrous ethanol.
2.6 Chloroform.
Hydrochloric acid (1+1).
2.8 Sodium citrate solution (30%).
2.9 Hydroxylamine hydrochloride solution (10%).
2.102.9-Dimethyl-1,10-phenanthene (neucuprol) ethanol solution (0.1%): Weigh 1g of neucuprol and dissolve it in 000)ml of anhydrous ethanol (2.5), and store it in a brown bottle. 2.11 Copper standard stock solution: weigh 0.1000g pure copper and place it in a 250mL beaker, add 20mL water and 10mL nitric acid (2.2). Place on a watch glass, heat slightly to dissolve, add 5mL perchloric acid (2.3), continue heating and evaporating until perchloric acid smoke appears, cool slightly, add water to dissolve the salt, transfer to a 1000mL volumetric flask, dilute to the mark with water, and mix. This solution contains 100 μg copper in 1mL. 2.12 Copper standard solution: transfer 50.00mL copper standard stock solution (2.11) to a 500mL volumetric flask, dilute to the mark with water, and mix. This solution contains 10% copper in mL.
3 Instrument
Spectrophotometer.
4 Analysis steps
4.1 Number of determinations
Measure twice in parallel and take the average value.
China Nonferrous Metals Industry Corporation approved 386 on January 11, 1988
Implementation on January 10, 1989
4.? Sample quantity
Weigh the sample according to Table 1:
Key, %
0.01--0. 10
≥0. 10~1. 00
4.3 Blank test
Carry out a blank test together with the sample.
4.4 Determination
GB 8638.8-88
Sample Mouse
4.4.1 Place the sample (4.2) in a 150mL beaker, add 15mL hydrochloric acid (2.1), cover with Table III, heat at low temperature to dissolve, when most of the sample is dissolved, add 5mL nitric acid (2.2) C for insoluble samples, add hydrofluoric acid (2.4) to assist dissolution, continue heating until the sample is completely dissolved, add 10mL perchloric acid (2.3), evaporate until perchloric acid smoke appears, when all chromium is oxidized to hexavalent, add hydrochloric acid (2.1) to evaporate and remove the chromium, and control the residual amount of perchloric acid to 1mL. Cool slightly, add 20mL water, heat to dissolve the salt, cool Cool to room temperature, transfer to a 100mL volumetric flask, dilute to the mark with water, and mix (if there is precipitation in the test solution, it must be clarified or dry filtered). 4.4.2 Transfer 10.00mL of the test solution (4.1.1). (When the copper content is more than 0.5%, transfer 5.00mL) into a 125mL separatory funnel and dilute to a volume of about 25mL with water.
4.4.3 Add 10mL of sodium citrate solution (2.8), 5mL of hydroxylamine hydrochloride solution (2.9), and 5mL of cuprous solution (2.10). Add any solution and mix. Add 15mL of trifluoromethane (2.6), shake for 1m in, after standing and stratifying, filter the organic phase through absorbent cotton and put it into a 25mL volumetric flask filled with 5mL anhydrous ethanol (2.5), add 5ml. chloroform (2.6) to the separating funnel and stir 30%. After standing and stratifying, filter the organic phase through absorbent cotton and combine it in a 25mL volumetric flask, dilute it to the scale with anhydrous ethanol (2.5), mix 4.4.4. Transfer the colorimetric solution into the colorimetric blood (use 1cm colorimetric III for copper 0.10%~1.00%, use %cm colorimetric III for copper 0.01%~010%), use the blank solution accompanying the sample as a reference, and measure the absorbance at a wavelength of 456nm on a spectrophotometer. Photometry. Find the corresponding copper content from the working curve.
4.5 Drawing of working curve
4.5.1 When the copper content of the sample is 0.01% to 0.10%, transfer 0, 0.50, 1.00, 2.00, 3.00, 4.00, 5.010mL of copper standard solution (2.12). When the copper content is between 0.10% and 1.00%, transfer 0.2.50, 5.00, 7.50, 10.00, 12.50mL of copper standard solution (2.12)3, respectively, into a 25mL separatory funnel, dilute with water to a volume of about 25mL, and proceed as in 4.4.3. 4.5.2 Transfer part of the colorimetric solution into a 1 or 3cm colorimetric tube, use the zero concentration solution in the standard series as a reference, and measure the absorbance at a wavelength of 456nm on a spectrophotometer. With the copper content as the horizontal axis and the absorbance as the vertical axis, draw a working curve. Calculation of analysis results
Calculate the percentage of copper according to formula (1):
Where: Volume of test solution taken, mL;
.Total volume of test solution. ml;
Cu(%) =- m. V.× 10-1
m-the amount of copper found from the working curve, ug; m. Sample weight, g.
6 Allowable difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table 2. X100
Additional Notes:
Copper Content
0.010~0.050
>0.050~0.10
>0.10~0.50
>0.50~1.00
GB8638, 8
This standard was drafted by the Central Iron and Steel Research Institute of the Ministry of Metallurgical Industry. This standard was drafted by the Central Iron and Steel Research Institute of the Ministry of Metallurgical Industry. The main drafter of this standard is Wang Zhichun.
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