This standard specifies the determination method of zirconium content in copper and copper alloys. This standard is applicable to the determination of zirconium content in copper and copper alloys. Determination range: 0.10% ~ 0.70%. GB/T 5121.20-1996 Chemical analysis method for copper and copper alloys Determination of zirconium content GB/T5121.20-1996 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Chemical analysis method for copper and copper alloys-Determination of zirconium content1 Scope
This standard specifies the method for determining zirconium content in copper and copper alloys. This standard is applicable to the determination of zirconium content in copper and copper alloys. Determination range: 0.10%~~0.70%. 2 Referenced standards
GB/T5121.20--1996
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. The versions shown are valid at the time of publication of this standard. All standards are subject to revision, and parties using this standard should explore the possibility of using the latest version of the following standards. GB1.4-88 Standardization Guidelines for the Preparation of Chemical Analysis Methods Standards G131467-78 General Principles and General Provisions for Chemical Analysis Methods of Metallurgical Products GB7729-87 General Principles for Spectrophotometric Methods for Chemical Analysis of Metallurgical Products 3 Method Summary
The sample is dissolved in hydrochloric acid and hydrogen peroxide, and the acidity is adjusted with perchloric acid. Cresol orange is used as a color developer. The sample solution is added with EDTA-masked zirconium solution as a reference, and its absorbance is measured at a wavelength of 540nm on a spectrophotometer. 4 Reagents
4.1 Hydrochloric acid (μl.19g/ml.)
4.2 Perchloric acid c (HClO,) = 5.0mol/L]: Pipette 278ml perchloric acid (pl.54g/mL) and dilute to 300ml with water. Mix 4.3 Hydrogen peroxide (30%).
4.4 Ethylaminetetraacetic acid sodium (CnHNONa2·2H0) solution (10g/L): Weigh 10g of ethylaminetetraacetic acid sodium (HNOgNa:·2H0), dissolve in 400mL warm water, cool to room temperature, dilute to 1000ml with water, mix. 4.5 Xylenol orange solution (1g/L), store in a brown bottle. 4.6 Zirconium standard stock solution: Weigh 0.1000g of pure zirconium in platinum III, add 10ml sulfuric acid (ml.84g/mlL), 1ml hydrochloric acid (pl.15g/ml), heat until completely dissolved, evaporate the solution until a small amount of sulfur trioxide smoke appears, cool, blow a small amount of water along the wall of the dish, shake the solution, and evaporate again until a small amount of sulfur trioxide smoke begins to appear. Cool to room temperature, slowly blow about 25mlL of water, mix and cool to room temperature, transfer to a 100ml plastic container, dilute to the scale with water, and mix well. 1 ml of this solution contains 1 mg of zirconium. 4.7 Lead standard solution: Pipette 10.00 ml of zirconium standard storage solution into a 500 ml volumetric flask, add 30 ml of lead acid (pl.19 g/ml), dilute to scale with water, and mix with a spoon. 1 ml of this solution contains 20 μg. 5 Instruments
Spectrophotometer.
Approved by the State Administration of Technical Supervision on November 4, 1996, and implemented on April 1, 1997
6 Analysis steps
6.1 Test materials
GB/T 5121.20-Www.bzxZ.net
- 1996
Weigh the sample according to Table 1, accurate to 0.0001 g. Table 1
Zirconium content, %
0.10~-0.35
0. 35 ~0. 55
>0. 55 ~0. 70
Carry out two independent determinations and take the average value. 6.2 Blank test
Carry out a blank test along with the sample.
6.3 Determination
Take the volume of the test solution, ml
6.3.1 Place the test material in a 100mL beaker, add 10mL hydrochloric acid, cover the surface, and at room temperature, drop 5~10mL hydrogen peroxide (about 45 drops each time) in several times. After the test material is completely dissolved, move it to an electric stove and heat it slowly until the solution volume is about 5mL. Wash the surface and the wall of the beaker with water to make the solution volume about 25mL, add 3mL hydrochloric acid, boil for 2~3min, cool to room temperature, transfer to a 100mL volumetric flask, and dilute to the scale with water (if there is a small amount of precipitate, filter it with dry filter paper). 6.3.2 According to Table 1, transfer two portions of the test solution to a 50mL volumetric flask, add 5mL of disodium ethylenediaminetetraacetic acid (CtH1aN.0Na2·2Hz0) solution to one portion, and then add 5mL of perchloric acid to both portions and mix. Add 2.5 ml of cresol orange solution, mix well, dilute to the mark with water, mix well, and let stand for 30 min.
6.3.3 Take a portion of solution with disodium ethylenediaminetetraacetic acid (CiH14N20.Na2·2H,0) as a reference, absorb with 1 cm, and measure its absorbance at a wavelength of 540 nm on a spectrophotometer. 6.3.4 Subtract the absorbance of the blank solution accompanying the sample and find the corresponding zirconium amount from the working curve. 6.4 Drawing of the working curve
Pipette 0.0.50, 1.00, 1.50.2.00, 2.50, 3.00 ml of zirconium standard solution into a set of 50 ml volumetric flasks, add 5 ml of perchloric acid, and mix well. Add 2.5 ml of cresol orange solution, mix well. Let stand for 30 min. Use 1cm absorption III, take reagent blank as reference, and measure its absorbance at 540nm wavelength on a spectrophotometer. Use zirconium content as horizontal axis and absorbance as vertical axis to draw a working curve. Expression of analysis results
Calculate the percentage of zirconium according to formula (1):
Wherein: m-
Zr(%) = m V. × 10-6
The amount of zirconium found from the working curve, ug; the total volume of the test solution, mL;
V1——-the volume of the test solution taken, mL;
mo-——the mass of the sample, g.
The result is expressed to two decimal places.
8Allowable difference
The difference between the analysis results of laboratories should not be greater than the allowable difference listed in Table 2. 290
0. 10~ 0. 35
0.35--0.55
0.55~0.70
GB/T 5121-20
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