GB/T 3254.4-1998 Chemical analysis method for antimony trioxide - Determination of copper content

This standard specifies the determination method of copper content in antimony trioxide. This standard is applicable to the determination of copper content in antimony trioxide. Determination range: 0.000 20% to 0.005 0%. GB/T 3254.4-1998 Chemical analysis method for antimony trioxide Determination of copper content GB/T3254.4-1998 Standard download decompression password: www.bzxz.net

1 Scope
National Standard of the People's Republic of China
Chemical analysis method of antimony trioxide
Determination of copper content
Antimony trioxide--Determination of copper contentThis standard specifies the method for determining the copper content in antimony trioxide. GB/T3254.41998
This standard applies to the determination of copper content in antimony trioxide: Determination range: 0.00020%~0.0050%. 2 Reference standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be revised, and parties using this standard should explore the possibility of using the latest versions of the following standards. GB1.488 Guidelines for standardization work Provisions for the preparation of chemical analysis methods GB146778 General principles and general provisions for chemical analysis methods for metallurgical products GB7729--87 General principles for spectrophotometric methods for chemical analysis of metallurgical products 3 Method summary
The sample is dissolved in hydrobromic acid and hydrochloric acid, evaporated to dryness, and most of the antimony is removed by volatilization. In an ammonia medium with a pH of 8-10, potassium sodium tartrate is used to mask the interfering elements, and diacetaldehyde oxalyl dichloride reacts with copper to form a stable purple compound, and its absorbance is measured at a wavelength of 540nm on a spectrophotometer
4 Reagents
4.1 Acetaldehyde (40%).
4.2 Hydrochloric acid (pl.19 g/ml).
4.3 Nitric acid (pl.42 g/ml.).
4.4 Hydrogen iodide (pl.48g/ml.)
4.5 Ammonia water (p0.90 g/ml)
4.6 Hydrochloric acid (1+1),
4.7 Nitric acid (1+1).
4.8 Potassium sodium tartrate solution (400g/L). 4.9 Bicyclohexanone oxalyl (BCO) solution (2g/i.): Weigh 1.0g BCO and place it in a 500mL beaker. Add 100ml Z alcohol and 200ml hot water (60-80℃), stir to dissolve (if there is undissolved residue, heat to dissolve), cool, transfer to a 500ml volumetric flask, dilute to scale with water, mix. 4.10 Copper standard pyrrolidone solution: Weigh 0.1000g pure copper and place it in a 100ml beaker. Add 10mL nitric acid (4.7), dissolve under low heat and boil for 0.5min to remove nitrogen oxides, cool, transfer to a 1000ml volumetric flask, dilute to scale with water, mix. This solution is 1m! Contains 1001g copper
Approved by the State Administration of Quality and Technical Supervision on July 15, 1998 40
Implemented on February 1, 1999 bZxz.net
GB/T3254.4--·1998
4.11 Copper standard solution: Pipette 5.00ml. Copper standard stock solution (4.10) into a 200ml. volumetric flask, dilute to full scale with water, and mix about 1ml. of this solution. Contains 2.5g copper.
4.12 Red ethanol solution (0.1g/1.). 5 Instruments
Spectrophotometer.
6 Analysis steps
6.1 Test sample
Weigh the sample according to Table 1, accurate to 0.0001g
Copper content, %
5:0.00050
0.000 50-0.001 2
Test sample amount·g
Add t.ml of hydrochloric acid
Carry out measurements repeatedly and take the average value. 6.2 Chamber test
Carry out a blank test with the sample.
6.3 Determination
Copper housing address, depth
20. 001 2- 0. 002
~0. 002 1~- 0. 003 0
Test volume·
Amount of hydrochloric acid added
6.3.1 Place the sample (6.1) in a 100ml beaker. Add 2ml of oxybromic acid and add hydrochloric acid (4.2) according to Table 1. Heat at low pressure to dissolve and evaporate for ten minutes. Remove and cool. Add 2ml of hydrobromic acid and heat to evaporate to dryness. Remove and cool slightly. Add 2mL hydrochloric acid (4.2). 1ml caustic soda (4.3) and evaporate to dryness. Cool slightly. 6.3.2 Add 3ml water. 2ml hydrochloric acid (1.6). 2ml potassium sodium tartrate along the beaker, heat to boiling, dissolve the residue and cool. 6.3.3 Transfer the test solution to 25ml colorimetric tube, add 1 drop of neutral red alcohol solution, adjust to red with ammonia water. Continue to add hydrogen water until the red color disappears, and add 1ml acetaldehyde. 4ml excess. 1.1 BCO solution, each time adding a reagent, must be mixed, heated in 60) (right) water for 8 minutes: take out, cool, dilute with water to the scale and mix well. 6.3.4 Transfer part of the solution into a 3cm absorption III, use the blank test solution accompanying the sample as a reference, measure its absorbance at a wavelength of 540mm on a spectrophotometer, and find the corresponding copper content from the working curve. 6.41 Draw the plot line
6.4.1 Transfer 0.1.00.2.00.3. 00.4.00.5.00.6.00ml. copper standard solution, respectively put 2ml. Add 1ml. hydrochloric acid (4.6) to the fish tube. Follow G.3.3. 6.4.2 Transfer part of the solution into 3cm absorption III. Take the reagent itself as reference, adjust its absorbance at the wavelength of 540nm on the spectrophotometer, and draw a working curve with copper content as the horizontal axis and absorbance as the vertical axis. 7 Expression of analysis results
Calculate the percentage of copper according to method (1): | |tt||u(%)
武中m““There is the amount of copper obtained on the working curve μg;.
.The mass of the sample.
The result is expressed to four decimal places. If the copper content is less than 0.0010%, it is expressed to five decimal places. Allowable difference
GB/T3254.41998
The difference in the analysis results between laboratories should not be greater than the allowable difference listed in Table 2 Table 2
Copper content
>0.000 50~0.001 0
≥0. 001 0~ 0. 002 0
Allowable difference
Copper content
≥0. 002 0~ 0. 003 0
>0.0030~0.0050
Allowable difference
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