Some standard content:
Registration No.: 2780-1999
HG/T 3592-1999
This standard is not equivalent to the German national standard DIN50972Dez:1995 "Requirements and Inspection of Copper Sulfate for Electroplating Coating Copper Plating Bath". This standard divides copper sulfate for electroplating into two grades, of which the indicators of superior products are equivalent to the German national standard. The main technical differences between this standard and the German national standard are as follows; it is divided into two grades according to the actual situation in my country. The main content of the German national standard is specified in Cu; this standard is based on the habits of domestic users. The test methods of various indicators are not specified in the German national standard; this standard is mainly determined by referring to relevant domestic standard methods. Appendix A of this standard is a prompt appendix.
This standard was proposed by the Technical Supervision Department of the former Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Inorganic Chemical Branch of the National Technical Committee for Chemical Standardization. The drafting units of this standard are: Tianjin Chemical Research and Design Institute of the Ministry of Chemical Industry, Hubei Xiangfan Electrochemical Industry Research Institute, and Huaxin Metal Co., Ltd., Guixi Refinery of Jiangxi Copper Company. The main drafters of this standard are: Guo Fengxin, Zhao Chengxian, Wan Yinlan, and Yao Jinjuan. This standard is entrusted to the Inorganic Chemical Branch of the National Technical Committee for Chemical Standardization for interpretation. 1104
Chemical Industry Standard of the People's Republic of China
Copper sulfate for electroplating use
Copper sulfate for electroplating useHG/T 3592--1999
This standard specifies the requirements, test methods, inspection rules, and marking, labeling, packaging, transportation, and storage of copper sulfate for electroplating. This standard applies to copper sulfate for electroplating. This product is mainly used for electroplating copper, electroplating brass, and chemical copper plating. Molecular formula: CuSO·5H,0
Relative molecular mass: 249.68 (according to the 1995 international relative atomic mass)2
Cited 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 the parties using this standard should explore the possibility of using the latest versions of the following standards. GB 191-1990↑
Packaging, storage and transportation pictorial symbols
GB/T601-1988 Chemical reagents - Preparation of standard solutions for titration analysis (volume analysis) GB/T602--1988
Chemical reagents
Preparation of standard solutions for impurity determination (neqISO6353-1:1982) GB/T 6031988
GB/T 1250-1989
GB/T 3049--1986
Chemical reagents
Preparation of preparations and products used in test methods (neqISO6353-1:1982) Methods for expressing and determining limit values - General method for determination of iron content in chemical products (1982)
GB/T 6678—1986
General rules for sampling of chemical products
Phenanthroline spectrophotometry (eqvISO6685: GB/T 6682—1992
Specifications and test methods for water used in analytical laboratories (eqvISO3696: 1987) 3 Requirements
3.1 Appearance: blue crystals or powder.
Copper sulfate for electroplating shall comply with the requirements of Table 1.
Table 1 Requirements
Copper sulfate (as CuSO, -5H2O) Content/% Arsenic (As) Content/%
Lead (1Pb) Content/%
Calcium (Ca) Content/%
Chloride Content of iron (in terms of CI)/%
Iron (Fe) content/%
Approved as a superior product by the State Administration of Petroleum and Chemical Industry on April 20, 1999
Implemented on April 1, 2000
Cobalt (Co) content/%
Nickel (Ni) content/%
Zinc (7.n) content/%
Water-insoluble matter content/%
pH value (5%, 20℃)
4Test method
HG/T 3592--1999
Table 1 (end)
Superior quality
First-class quality
The reagents and water used in this standard, unless otherwise specified, refer to analytically pure reagents and grade 3 water specified in GB/T6682. The standard titration solutions, impurity standard solutions, preparations and products used in the test, unless otherwise specified, are prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603.
Safety Tips: This standard The strong acid and alkali used are corrosive. Users should be careful to avoid splashing on the skin. 4.1 Determination of copper sulfate content
4.1.1 Method summary
Under slightly acidic conditions, an appropriate amount of potassium iodide added to the sample reacts with divalent copper to precipitate an equivalent amount of iodine. The precipitated iodine is titrated with sodium thiosulfate standard titration solution, starch is used as an indicator, and the end point is determined by the color change. 4.1.2 Reagents and materials
4.1.2.1 Potassium iodide;
4. 1.2. 4
4. 1. 2. 6
4. 1. 2. 7
Sodium pyrophosphate;
Acetic acid solution: 4+1;
Ammonia solution: 1+4;
Potassium thiocyanate solution: 100g/1;
Standard sodium thiosulfate titration solution: c(NazS,O.) about 0.1mol/L; Starch indicator solution: 10g/L (useable period is 2 weeks). 4.1.3 Instruments and equipment
4. 1. 3. 1
4. 1. 3. 2
Glass sand crucible: pore size 5μm~15μm;
Constant temperature drying oven: control temperature 105℃110℃. 4.1.4 Analysis steps
4.1.4.1 Preparation of test solution
Weigh 10g of sample (accurate to 0.0002g), dissolve in a small amount of distilled water, and filter it after dissolution using a glass crucible that has been dried to constant weight at 105℃~110℃. Wash the filter residue with hot distilled water until the washing liquid is colorless and check with ammonia solution that there is no copper ion reaction. Cool the filtrate to room temperature, collect it in a 500mL volumetric flask, dilute it to the scale with water, and shake it well. Keep the glass crucible and filter residue for the determination of water-insoluble matter content.
4.1.4.2 Determination
Use a pipette to transfer 50 ml of the test solution into a 250 ml iodine volumetric flask, add 1 g of sodium pyrophosphate, 2 g of potassium iodide and 10 ml of acetic acid solution, shake well, place in a dark place for 10 min, titrate with sodium thiosulfate standard titration solution until the solution turns light yellow, add 2 ml of starch indicator solution, continue titrating until the solution turns light blue, add 10 ml of potassium thiocyanate solution, mix well and continue titrating until the blue disappears, which is the end point. Perform a blank test at the same time.
4.1.5 Expression of analysis results
HG/T3592—1999
The content of copper sulfate (CuSO·5H2O) expressed as mass fraction (X,) is calculated according to formula (1): c(V1 - V,) X 0. 249 7 × 100 =Xi =
Wherein:
m×500
actual concentration of sodium thiosulfate standard titration solution, mol/L; Vr
249. 7 c(V, - V.)
volume of sodium thiosulfate standard titration solution consumed by titration test solution, mL; Vvolume of sodium thiosulfate standard titration solution consumed by titration blank test solution, mLmass of sample, g;
..........( 1)
0.2497——The mass of copper sulfate (in terms of CuSO·5H2O) expressed in grams equivalent to 1.00mL of sodium thiosulfate standard titration solution Lc (NazS,O,) = 1.000mol/LJ. 4.1.6 Allowable difference
The arithmetic mean of the results of two parallel determinations is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.3%. 4.2 Determination of arsenic content
4.2.1 Method summary
In an acidic solution, potassium iodide and stannous chloride are used to reduce high-valent arsenic to trivalent arsenic. Trivalent arsenic reacts with new ecological hydrogen to generate arsenic hydrogen gas, forming a brown-yellow arsenic spot on the mercuric bromide test paper, which is compared with the standard arsenic spot. 4.2.2 Reagents and materials
4.2.2.1 Hydrochloric acid.
4.2.2.2 Acetic acid.
4.2.2.3 Ascorbic acid.
4.2.2.4 Metallic zinc.
4.2.2.5 Potassium iodide.
4.2.2.6 Stannous chloride solution: 400 g/L. 4.2.2.7 Arsenic standard solution: 1 mL of solution contains 0.001 mg As. Use a pipette to transfer 1 mL of the arsenic standard solution prepared according to GB/T 602 into a 100 mL volumetric flask, dilute to the mark with water, and shake well. Prepare this solution before use.
4.2.2.8 Lead acetate cotton.
4.2.2.9 Mercuric bromide test paper.
4.2.3 Instruments and equipment
Arsenic analyzer.
4.2.4 Analysis steps
Weigh (0.40 ± 0.01) g of sample, place it in a 100 mL beaker, add 5 mL of water to dissolve, add 3 mL of acetic acid and 2 g of potassium iodide, cover with a watch glass, leave it for 5 min, then add 0.2 g of ascorbic acid to dissolve it, as the test solution. Place the test solution in the arsenic analyzer, dilute to about 40 mL with water, add 6 mL of hydrochloric acid, and shake well. Add 1g potassium iodide, add stannous chloride solution dropwise until the solution is colorless, shake well, let stand for 10min, add 2.5g arsenic-free metal zinc, and immediately plug the test tube pre-filled with lead acetate cotton and mercuric bromide test paper. Place in a dark place at 25℃~40℃ for 1h~1.5h. The brown-yellow color of the mercuric bromide test paper shall not be deeper than the color produced by the standard colorimetric solution. Preparation of standard colorimetric solution: Use a pipette to transfer 2mL arsenic standard solution (superior product) or 4mL arsenic standard solution (first-class product), place in a fixed container, dilute with water to 40mL, add 6mL hydrochloric acid, and treat it in the same way as the test solution. 4.3 Determination of lead content
4.3.1 Summary of method
Dissolve the sample in water and determine it on an atomic absorption spectrophotometer at a wavelength of 283.3am using an air-acetylene flame using the standard addition method.
4.3.2 Reagents and materials
HG/T 3592—1999
Standard lead solution: 1ml. The solution contains 0.1mgPb. 4.3.3 Instruments and equipment
Atomic absorption spectrophotometer: equipped with a lead hollow cathode lamp. 4.3.4 Analysis steps
4.3.4.1 Preparation of test solution A
Weigh about 40g of the sample (accurate to 0.01g), place it in a beaker, add water to dissolve it, transfer it to a 500ml volumetric flask, dilute it with water to the scale, and shake it. This solution is test solution A, and this solution is reserved for the determination of calcium content, cobalt content, nickel content, and zinc content. 4.3.4.2 Determination
Use a pipette to take four portions of test solution A (4.3.4.1): 25 mL for each portion of superior product and 20 mL for each portion of first-class product, and place them in four 100 mL volumetric flasks, respectively, and add 0.00 mL, 1.50 mL, 3.00 mL, and 4.50 mL of lead standard solution, respectively, dilute to the scale with water, and shake the hook.
On an atomic absorption spectrophotometer, use air-acetylene flame, select the best conditions, adjust to zero with water at a wavelength of 283.3 nm, and measure the absorbance of the above solutions.
Use the concentration of the added standard solution as the horizontal axis and the corresponding absorbance as the vertical axis to draw a curve, and extend the curve in the opposite direction to intersect with the horizontal axis. The intersection is the concentration of the lead element to be measured. 4.3.5 Expression of analysis results
The lead (Pb) content (X,) expressed as mass fraction is calculated according to formula (2):\ X, = mi X10-3
× 100 m
m×500
Wherein: ml is the mass of lead in the test solution obtained by the graphic epitaxy method, mg; V—the volume of the test solution A (4.3.4.1) removed, mL; m is the mass of the sample in 4.3.4.1, g.
4.3.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.001%. 4.4 Determination of calcium content
4.4.1 Summary of method
The sample is dissolved in water and determined by the standard addition method at a wavelength of 422.7nm on an atomic absorption spectrophotometer with an air-acetylene flame.
4.4.2 Reagents and materials
4.4.2.1 Strontium chloride solution: 250g/L.
Preparation: Take 400mL of water, heat to about 70℃, add 1000g of strontium chloride (SrC12·6H,O) to dissolve and filter. Slowly add 400ml of anhydrous ethanol to the solution, stir well, place and filter, wash the crystals once with 1+1 ethanol, dry at 105℃～110℃ for use. Weigh 25g of recrystallized strontium chloride, dissolve in water, place in a 100mL volumetric flask, dilute with water to the scale, and shake well. 4.4.2.2 Calcium standard solution; 1mL of solution contains 0.1mgCa. 4.4.3 Instruments and equipment
Atomic absorption spectrophotometer: equipped with a calcium hollow cathode lamp. 4.4.4 Analysis steps
Use a pipette to transfer four 25 ml portions of test solution A (4.3.4.1) into four 100 ml volumetric flasks, add 0.00 ml, 1.00 ml, 2.00 ml, and 3.00 ml of calcium standard solution and 4 ml of strontium nitride solution, dilute to scale with water, and shake well. On an atomic absorption spectrophotometer, use an air-acetylene flame, select the best conditions, adjust to zero with water at a wavelength of 422.7 nm, and measure the absorbance of the above solutions.
Use the concentration of the added standard solution as the abscissa and the corresponding absorbance as the ordinate to draw a curve. Extend the curve in the opposite direction to intersect with the abscissa. The intersection is the concentration of the calcium element to be measured. 4.4.5 Expression of analysis results
HG/T 3592--1999
Calcium (Ca) content (X:) expressed as mass fraction is calculated according to formula (3): X = mi×10-3
× 100 =
m×500
wherein mi—
—the mass of calcium in the test solution obtained by the graphical epitaxy method, mg; m-the mass of the sample in 4.3.4.1, g.
4.4.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.0002%. 4.5 Determination of fluoride content
4.5.1 Summary of the method
The sample is dissolved in water, and silver nitrate solution is added to form silver chloride precipitation with chloride, and the turbidity is compared with that of the standard turbidity solution. 4.5.2 Reagents and materials
4.5.2.1 Nitric acid solution: 1+2.
4.5.2.2 Silver nitrate solution: 17g/L.
4.5.2.3 Chloride-free copper sulfate solution: 100g/L. (3)
Preparation: Weigh about 10g of copper sulfate, dissolve in an appropriate amount of water, add 8mL of nitric acid solution and 5mL of silver nitrate solution, dilute with water to 100ml, and shake well. After leaving in a dark place to clarify, filter with glass sand (pore size 5μm~~15μm), and collect the filtrate in a reagent bottle. 4.5.2.4 Chloride standard solution: 1mL of solution contains 0.1mgCl. 4.5.3 Analysis steps
Weigh (2.5±0.01)g of sample, place in a 50mL colorimetric tube, add 25mL water to dissolve, filter if necessary, add 2mL nitric acid solution and 1mL silver nitrate solution, dilute to scale with water, place for 10min and compare the turbidity. The turbidity produced shall not be deeper than the standard turbidity solution. The standard turbidity solution is 0.5mL chloride standard solution and 25mL chloride-free copper sulfate solution, which are treated in the same way as the test solution.
4.6 Determination of iron content
4.6.1 Summary of method
Use ammonia water to separate copper and iron, and then use ascorbic acid to reduce the trivalent iron in the test solution to divalent iron. The divalent iron and o-phenanthroline form an orange-red complex, and its absorbance is measured at a wavelength of 510nm on a spectrophotometer. 4.6.2 Reagents and materials
According to Chapter 3 of GB/T3049-1986 and
4.6.2.1 Ammonium chloride.
4.6.2.2 Nitric acid solution: 1+2.
4.6.2.3 Washing solution.
Preparation: Weigh 5g of ammonium chloride, dissolve it in an appropriate amount of water, add 5mL of ammonia water, and dilute it to 100mL with water. 4.6.3 Instruments and equipment
According to Chapter 4 of GB/T3049-1986.
4.6.4 Analysis steps
4.6.4.1 Drawing of standard curve
According to 5.3 of GB/T3049-1986, use a 3cm absorption cell and the corresponding iron standard solution to draw a standard curve. 4.6.4.2 Preparation of test solution
Weigh about 5g of sample (accurate to 0.01g), place in a 250ml beaker, dissolve in 50mL of water, transfer to a 250mL volumetric flask, dilute to scale with water, and shake well.
4.6.4.3 Preparation of blank test solution
HG/T 3592—1999
Except for not adding the sample, the amount of other reagents added is exactly the same as that of the test solution, and they are processed at the same time. 4.6.4.4 Determination
Use a pipette to take 25mL of the superior product, 5mL of the first-class product and the blank test solution, respectively, and place them in a 250mL beaker, add 0.5ml of nitric acid solution, add water to the second-class product to 25mL, boil for 2min, cool, add 1.5g of ammonium chloride, add 1+2 ammonia water dropwise until the generated precipitate dissolves, heat in a boiling water bath for 30min, filter with slow qualitative filter paper, wash the precipitate with washing liquid until the blue color on the filter paper disappears completely, and then wash with hot water for 3 times. Dissolve the precipitate with 3ml 1+1 hydrochloric acid solution, wash the filter paper with water, collect the filtrate and washing solution in a 100mL volumetric flask, control the solution volume to less than 50mL, neutralize with 1+2 ammonia water, and follow the provisions of 5.4 of GB/T3049-1986, starting from "If necessary, add water to 60 ml" to "Measure the absorbance of the test solution and the reagent blank solution". Use a 3cm absorption cell, measure the absorbance according to the provisions of 5.4 of GB/T3049--1986, and find out the mass of iron in the test solution and the blank test solution according to the standard curve.
4.6.5 Expression of analysis results
The iron (Fe) content (X) expressed as mass fraction is calculated according to formula (4): X, = (ml-mz)×10-6
0. 025(mi - mz)
X 100 =
m×250
Wherein: m1—-the mass of iron in the test solution found from the standard curve, μg; the mass of iron in the blank test solution found from the standard curve, g; m2
V—-the volume of the test solution transferred, mL; -the mass of the sample, g.
4.6.6 Allowable difference
(4)
The arithmetic mean of the results of the parallel determinations is taken as the determination result. The absolute difference of parallel determinations is not more than 0.002% for superior products and not more than 0.02% for first-class products.
4.7 Determination of cobalt content
4.7.1 Summary of method
Dissolve the sample in water and determine it on an atomic absorption spectrophotometer at a wavelength of 240.7nm with an air-acetylene flame using the standard addition method.
4.7.2 Reagents and materials
Cobalt standard solution: 1mL of solution contains 0.1mgCo. Use a pipette to transfer 10mL of cobalt standard solution prepared according to GB/T602 into a 100mL volumetric flask, dilute to the mark with water, and shake well. This solution is prepared before use.
4.7.3 Instruments and equipment
Atomic absorption spectrophotometer: equipped with a cobalt hollow cathode lamp. 4.7.4 Analysis steps
Use a pipette to transfer four 25mL portions of test solution A (4.3.4.1) and place them in four 100mL volumetric flasks. Add 0.00ml, 1.00ml, 2.00mL, and 3.00mL of cobalt standard solution, dilute to the mark with water, and shake. On an atomic absorption spectrophotometer, use an air-acetylene flame, select the best conditions, adjust to zero with water at a wavelength of 240.7nm, and measure the absorbance of the above solutions.
Use the concentration of the added standard solution as the horizontal axis and the corresponding absorbance as the vertical axis to draw a curve. Extend the curve in the opposite direction to intersect with the horizontal axis. The intersection is the concentration of the cobalt element to be measured. 4.7.5 Expression of analysis results
The cobalt (Co) content (X,) expressed as mass fraction is calculated according to formula (5): Xs = m; ×10-3
m×500
×100m
HG/T 3592-1999
wherein: m—the mass of cobalt in the test solution obtained by the graphic epitaxy method, mg; - the mass of the sample in 4.3.4.1, g.
4.7.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.0002%. 4.8 Determination of nickel content
4.8.1 Summary of method
Dissolve the sample in water and determine it on an atomic absorption spectrophotometer at a wavelength of 232.0nm using an air-acetylene flame and the standard addition method.
4.8.2 Reagents and Materials
Nickel standard solution: 1 ml. The solution contains 0.1 mg Ni. 4.8.3 Instruments and Equipment
Atomic Absorption Spectrophotometer: Equipped with a nickel hollow cathode lamp. 4.8.4 Analysis Procedure
Use a pipette to take four portions of test solution A (4.3.4.1): 25 ml for each portion of superior product and 2.5 ml for each portion of first-class product, and place them in four 100 ml volumetric flasks, respectively, and add 0.00 ml., 1.00 ml., 2.00 ml., and 3.00 ml of nickel standard solution, respectively, dilute to the mark with water, and shake well.
On the atomic absorption spectrophotometer, use an air-acetylene flame, select the best conditions, adjust to zero with water at a wavelength of 232.0 nm, and measure the absorbance of the above solutions.
Use the concentration of the added standard solution as the abscissa and the corresponding absorbance as the ordinate to draw a curve. Extend the curve in the opposite direction and intersect with the abscissa. The intersection is the concentration of the nickel element to be measured. 4.8.5 Expression of analysis results
The nickel (Ni) content (X.) expressed as mass fraction is calculated according to formula (6): X. = mi ×10~3
× 100
m×500
Where: m1\—the mass of nickel in the test solution obtained by the graphical epitaxy method, mg; V-—the volume of the test solution A (4.3.4.1) transferred, mL; m
-the mass of the sample in 4.3.4.1, g.
4.8.6 Allowable difference
·（6）
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference of the parallel determination results is not more than 0.0002% for superior products and not more than 0.01% for standard products.
4.9 Determination of zinc content
4.9.1 Summary of method
Dissolve the sample in water and determine it on an atomic absorption spectrophotometer at a wavelength of 213.8nm using an air-acetylene flame and the standard addition method.
Reagents and materials
Standard zinc solution: 1mL of solution contains 0.1mgZn. 4.9.3 Instruments and equipment
Atomic absorption spectrophotometer: equipped with a zinc hollow cathode lamp. 4.9.4 Analysis steps
Use a pipette to take four portions of test solution A (4.3.4.1): 25 mL of each portion of superior product and 1 mL of each portion of first-class product, and place them in four 100 mL volumetric flasks, respectively, and add 0.00 mL, 0.50 mL, 1.00 mL, and 1.50 mL of zinc standard solution, respectively, dilute to the scale with water, and shake well.
HG/T 3592—1999
On an atomic absorption spectrophotometer, use air-acetylene flame, select the best conditions, adjust to zero with water at a wavelength of 213.8 nm, and measure the absorbance of the above solutions
Use the concentration of the added standard solution as the abscissa and the corresponding absorbance as the ordinate to draw a curve, and extend the curve in the opposite direction to intersect with the abscissa. The intersection is the concentration of the zinc element to be measured. 4.9.5 Expression of analysis results
The zinc (Zn) content (X100) expressed as mass fraction is calculated according to formula (7): X100 = m×10-3
X100 =
m×500
Wherein: m1——the mass of zinc in the test solution obtained by the graphical epitaxy method, mg; V
the volume of the test solution A (4.3.4.1) removed, mL; the mass of the test material in 4.3.4.1, g.
4.9.6 Allowable difference
(7)
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.0005% for superior products and 0.01% for first-class products.
4.10 Determination of water-insoluble matter contentbZxz.net
4.10.1 Instruments and equipment
Constant temperature drying oven: control the temperature at 105℃~110℃. 4.10.2 Analysis steps
Put the glass sand crucible (4.1.4.1) containing the filter residue in a constant temperature drying oven at 105℃~~110℃ and dry it to constant weight. 4.10.3 Expression of analysis results
The water-insoluble matter content (Xg) expressed as mass fraction is calculated according to formula (8): Xg=
—-mass of residue and glass sand, g;
Where: mi-
mass of glass sand crucible, g;
-mass of the sample in 4.1.4.1, g.
4.10.4 Allowable difference
m1 - m2 × 100
（8）
Take the arithmetic mean of the results of two parallel determinations as the determination result. The absolute difference of the parallel determination results shall not exceed 0.001% for superior products and 0.005% for first-class products. 4.11 Determination of pH value
4.11.1 Instruments and equipment
Acidometer: The graduation value is 0.02 pH unit, equipped with saturated calomel electrode and glass electrode. 4.11.2 Analysis steps
Weigh (5 ± 0.01) g of sample, dissolve it in an appropriate amount of water, transfer it to a 100ml volumetric flask, dilute it with water to the scale, and shake it. Determine the pH value with an acidometer.
4.11.3 Allowable difference
Take the arithmetic mean of the results of two parallel determinations as the determination result. The absolute difference of the parallel determination results shall not exceed 0.1 pH. 5 Inspection rules
5.1 All items specified in this standard are factory inspection items. 5.2 Each batch of products shall not exceed 10t.
5.3 Determine the number of sampling units according to 6.6 of GB/T66781986. When sampling, insert the sampler obliquely from the top of the packaging bag to 3/4 of the depth of the material layer. After mixing the collected samples, reduce them to no less than 500g by quartering method, and pack them in two clean and dry plastic bottles and seal them. 1112
HG/T3592--1999
labels are attached to the bottles, indicating: manufacturer name, product name, grade, batch number, sampling date and name of the sampler. One bottle is used as a laboratory sample, and the other bottle is kept for three months for reference. 5.4 Copper sulfate for electroplating shall be inspected by the quality supervision and inspection department of the manufacturer in accordance with the provisions of this standard. The manufacturer shall ensure that each batch of products leaving the factory meets the requirements of this standard.
5.5 If one of the indicators in the test results does not meet the requirements of this standard, samples should be taken from twice the amount of packaging for re-testing. Even if only one indicator does not meet the requirements of this standard, the entire batch of products shall be unqualified. 5.6 Determine whether the test results meet the standard by the rounded value comparison method specified in 5.2 of GB/T1250-1989. 6 Marking and labeling
6.1 The packaging of copper sulfate for electroplating should have firm and clear markings, including: manufacturer name, factory address, product name, trademark, grade, net content, batch number or production date, this standard number and the "wet-afraid" mark specified in GB191. 6.2 Each batch of copper sulfate for electroplating shipped from the factory should be accompanied by a quality certificate. The contents include: manufacturer name, factory address, product name, trademark, grade, net content, batch number or production date, proof that the product quality meets this standard and this standard number. 7 Packaging, transportation, purchase and storage
7.1 Copper sulfate for electroplating is packaged in double layers. The inner packaging is made of polyethylene plastic film bags with a thickness of not less than 0.05mm; the outer packaging is made of plastic woven bags. The net content of each bag is 25kg, 50kg. 7.2 For the packaging of copper sulfate for electroplating, the inner bag is tied with vinyl rope or other ropes of equivalent quality, or sealed with other equivalent methods; the outer bag is folded at a distance of not less than 30mm from the bag edge, and the mouth is sewn with vinyl thread or other thread of equivalent quality at a distance of not less than 15.mm from the bag edge. The stitches are neat and the needle spacing is even. There is no leakage or skipping. 7.3 Copper sulfate for electroplating should be covered during transportation to prevent rain, moisture and sunlight. 7.4 Copper sulfate for electroplating should be stored in a cool and dry place to prevent rain, moisture and sunlight. 1113
HG/T3592—1999
Appendix A
(Suggestive Appendix)
Hull cell test method for copper sulfate for electroplating
If it is necessary to inspect the coating quality of copper sulfate products for electroplating after copper electroplating, the following method can be used: A1 Reagents and materials
A1.1 Copper sulfate;
A1.2 Sulfuric acid.
Instruments and equipment
A2.1 Hull cell: 250mL;
A2.2 Electroplating test power supply: single-phase half-wave 10A/12V;A2.3 Copper plate: (1~2)mm×70mm×100mm, degreased and derusted, with a smooth and flat surface;A2.4 Pure copper plate: (1~2)mm×70mm×63mm, degreased and derusted, with a smooth and flat surface;A2.5 Constant temperature water bath.
Test conditions
Temperature: (25±2)℃;
A4 Analysis steps
A4.1 Preparation of electroplating test solution
Weigh 62.5g of copper sulfate sample (accurate to 0.01g), dissolve it in water, add 12.5g of sulfuric acid to the solution, and then add water to 500ml.
A4.2 Determination
Put 250mL of the electroplating test solution in a Hull cell, which is placed in a constant temperature water bath and controlled at (25±2)°C. Use a copper plate as the cathode and a pure copper plate as the anode. Start electroplating with a current of 2A for 2 minutes. When the time is up, turn off the power, take out the cathode plate, wash it with pure water, and dry it. Measure the width of the poor coating (i.e., the distance from the point of maximum current density of the good coating to the edge of the anode) at half the height of the coating.
A4.3 Calculation formula
The current density Dk is calculated as follows:
Ds = I(5.10 - 5.24lgl)
Wherein: Dk--the maximum current density in the good coating area on the cathode plate in the Hull cell test, A/dm2; 1--the current intensity indicated by the ammeter in the test, A; L--the distance from the edge of the cathode plate near the anode end to the edge of the good coating in the Hull cell test, cm. A4.4 Judgment basis
When Dk ≥ 6A/dm2, the Hull cell test is qualified. 11143 Copper sulfate for electroplating should be covered during transportation to prevent rain, moisture and sunlight. 7.4 Copper sulfate for electroplating should be stored in a cool and dry place to prevent rain, moisture and sunlight. 1113
HG/T3592—1999
Appendix A
(Suggested Appendix)
Hull Cell Test Method for Copper Sulfate for Electroplating
If it is necessary to inspect the coating quality of copper sulfate products for electroplating after copper plating, the following method can be used: A1 Reagents and Materials
A1.1 Copper sulfate;
A1.2 Sulfuric acid.
Instruments and equipment
A2.1 Hull cell: 250mL;
A2.2 Electroplating test power supply: single-phase half-wave 10A/12V;A2.3 Copper plate: (1~2)mm×70mm×100mm, degreased and derusted, with a smooth and flat surface;A2.4 Pure copper plate: (1~2)mm×70mm×63mm, degreased and derusted, with a smooth and flat surface;A2.5 Constant temperature water bath.
Test conditions
Temperature: (25±2)℃;
A4 Analysis steps
A4.1 Preparation of electroplating test solution
Weigh 62.5g of copper sulfate sample (accurate to 0.01g), dissolve it in water, add 12.5g of sulfuric acid to the solution, and then add water to 500ml.
A4.2 Determination
Put 250mL of the electroplating test solution in a Hull cell, which is placed in a constant temperature water bath and controlled at (25±2)°C. Use a copper plate as the cathode and a pure copper plate as the anode. Start electroplating with a current of 2A for 2 minutes. When the time is up, turn off the power, take out the cathode plate, wash it with pure water, and dry it. Measure the width of the poor coating (i.e., the distance from the point of maximum current density of the good coating to the edge of the anode) at half the height of the coating.
A4.3 Calculation formula
The current density Dk is calculated as follows:
Ds = I(5.10 - 5.24lgl)
Wherein: Dk--the maximum current density in the good coating area on the cathode plate in the Hull cell test, A/dm2; 1--the current intensity indicated by the ammeter in the test, A; L--the distance from the edge of the cathode plate near the anode end to the edge of the good coating in the Hull cell test, cm. A4.4 Judgment basis
When Dk ≥ 6A/dm2, the Hull cell test is qualified. 11143 Copper sulfate for electroplating should be covered during transportation to prevent rain, moisture and sunlight. 7.4 Copper sulfate for electroplating should be stored in a cool and dry place to prevent rain, moisture and sunlight. 1113
HG/T3592—1999
Appendix A
(Suggested Appendix)
Hull Cell Test Method for Copper Sulfate for Electroplating
If it is necessary to inspect the coating quality of copper sulfate products for electroplating after copper plating, the following method can be used: A1 Reagents and Materials
A1.1 Copper sulfate;
A1.2 Sulfuric acid.
Instruments and equipment
A2.1 Hull cell: 250mL;
A2.2 Electroplating test power supply: single-phase half-wave 10A/12V;A2.3 Copper plate: (1~2)mm×70mm×100mm, degreased and derusted, with a smooth and flat surface;A2.4 Pure copper plate: (1~2)mm×70mm×63mm, degreased and derusted, with a smooth and flat surface;A2.5 Constant temperature water bath.
Test conditions
Temperature: (25±2)℃;
A4 Analysis steps
A4.1 Preparation of electroplating test solution
Weigh 62.5g of copper sulfate sample (accurate to 0.01g), dissolve it in water, add 12.5g of sulfuric acid to the solution, and then add water to 500ml.
A4.2 Determination
Put 250mL of the electroplating test solution in a Hull cell, which is placed in a constant temperature water bath and controlled at (25±2)°C. Use a copper plate as the cathode and a pure copper plate as the anode. Start electroplating with a current of 2A for 2 minutes. When the time is up, turn off the power, take out the cathode plate, wash it with pure water, and dry it. Measure the width of the poor coating (i.e., the distance from the point of maximum current density of the good coating to the edge of the anode) at half the height of the coating.
A4.3 Calculation formula
The current density Dk is calculated as follows:
Ds = I(5.10 - 5.24lgl)
Wherein: Dk--the maximum current density in the good coating area on the cathode plate in the Hull cell test, A/dm2; 1--the current intensity indicated by the ammeter in the test, A; L--the distance from the edge of the cathode plate near the anode end to the edge of the good coating in the Hull cell test, cm. A4.4 Judgment basis
When Dk ≥ 6A/dm2, the Hull cell test is qualified. 1114
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