Some standard content:
Record number: 2782-1999
HG/T3594-1999
This standard sets a grade and specifies five indicators: pyrophosphate (H4P.(),) content, phosphorus pentoxide (P2O) content, iron content, lead content and density (25℃).
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, and Hubei Xiangfan Electrochemical Industry Research Institute. The main drafters of this standard are: Guo Fengxin, Zhao Chengxian, and Yao Jinjuan. This standard is entrusted to the Inorganic Chemical Branch of the National Technical Committee for Chemical Standardization for interpretation. 1122
Chemical Industry Standard of the People's Republic of China
Pyrophosphoric acid for electroplating use
Pyrophosphoric acid for electroplating useHG/T 3594--1999
This standard specifies the requirements, test methods, inspection rules, and marking, labeling, packaging, transportation and storage of pyrophosphoric acid for electroplating use. This standard applies to pyrophosphoric acid for electroplating. This product is mainly used to adjust the pH value of the electroplating solution in the copper electroplating process. It can also be used for other electroplating.
Molecular formula: HP, O7
Relative molecular mass: 177.97 (according to the 1995 international relative atomic mass) 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 version of the following standards. GB190—1990 Dangerous Goods Packaging Marking
GB/T 601 —1988
Preparation of Standard Solutions for Titration Analysis (Volumetric Analysis) of Chemical ReagentsGB/T 602-1988
GB/T 603—1988
GB/T 611—1988
GB/T 1250—1989
GB/T 3049—1986
Preparation of standard solutions for determination of impurities in chemical reagents (neqISO6353-1:1982) Preparation of preparations and products used in test methods for chemical reagents (neqISO6353-1:1982) General method for determination of density of chemical reagents (neqISO6353-1:1982GM24) Expression and determination of limit values General method for determination of iron content in chemical products (1982)
GB/T 6678-—1986
General rules for sampling of chemical products
O-phenanthroline spectrophotometric method (eqvISO6685:GB/T 6682—1992
Specifications and test methods for analytical laboratory water (eqvISO3696:1987) Requirements
3.1 Appearance: colorless or light yellow viscous liquid or crystal. 3.2 Pyrophosphoric acid for electroplating shall meet the requirements of Table 1. Table 1 Requirements
Pyrophosphoric acid (H, P, O,) content/%
Phosphorus pentoxide (P.Os) content/%
Iron (Fe) content/%
Lead (Pb) content/%
Density (25℃))/(g/mL)
Approved by the State Administration of Petroleum and Chemical Industry on April 20, 1999
Implementation on April 1, 2000
Test method
HG/T 3594—1999
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 CB/T601, GB/T602 and GB/T603.
4.1 Determination of pyrophosphoric acid content
4.1.1 Summary of the method
After pyrophosphoric acid is diluted with water, it is neutralized with sodium hydroxide solution and converted into sodium pyrophosphate. Sodium pyrophosphate reacts with hydrochloric acid to form disodium dihydrogen pyrophosphate. Zinc sulfate is added to form zinc pyrophosphate precipitate and sulfuric acid, and the generated sulfuric acid is titrated with sodium hydroxide standard titration solution. The reaction is as follows:
Na P,O, +2HC1 --Naz H, P, O, +2NaClNa2 H, P,O, +2ZnSO =-Zn2 P,O,+Naz SO4 +Hz SOH, SO. +2NaOH -Na SO4 +2H,0
4.1.2 Reagents and materials
4.1.2.1 Hydrochloric acid solution: 1+20 and 1+100. 4.1.2.2 Zinc sulfate solution: 125g/I.
Weigh 125g zinc sulfate, dissolve it in water and dilute to 1000ml. Use sulfuric acid solution (1+500) or sodium hydroxide solution [c(NaOH) is about 0.1 mol/L] on the acidometer to adjust the pH value of the solution to 3.8. 4.1.2.3 Sodium hydroxide standard titration solution. Preparation: Prepare according to GB/T601 [c(NaOH) about 0.1mol/1.]. Calibration: Weigh about 0.5g (accurate to 0.0002g) of anhydrous sodium pyrophosphate dried to constant weight at 400℃ (recrystallize the sodium pyrophosphate three times in water, dry it in platinum blood, place it in a 250mL beaker, and add 90mL water to dissolve. On the acidometer, slowly add hydrochloric acid solution (1+20 and 1+100) while stirring until the pH value of the solution is 3.8. Add 50mL of zinc sulfate solution and stir for 5min. Titrate with sodium hydroxide standard titration solution until the pH value of the solution is close to 3.6 while stirring. Stop titration, stir for 2 minutes to allow the solution to reach equilibrium, and continue titrating until the pH value of the solution is 3.8. At this time, stir for 30 seconds after adding each drop of solution. The number of grams of anhydrous sodium pyrophosphate equivalent to each milliliter of sodium hydroxide standard titration solution (T) is calculated according to formula (1): T-
Where: m——the mass of anhydrous sodium pyrophosphate weighed.g; V-—the volume of sodium hydroxide standard titration solution consumed in the titration, mL. 4.1.3 Instruments and equipment
4.1.3.1 Acidity meter: The graduation value is 0.0 2pH, equipped with saturated calomel electrode and glass electrode; 4.1.3.2 Magnetic stirrer.
4.1.4 Analysis steps
4.1.4.1 Preparation of test solution AwwW.bzxz.Net
Weigh about 10g of sample (accurate to 0.0002g), place in a 250mL beaker, add 50mL of water, use sodium hydroxide solution [c (NaOH) about 0.1mol/L to adjust the pH of the solution to 10 (check with pH test paper), transfer to a 250mL volumetric flask, dilute with water Dilute to the mark and shake well. This solution is test solution A. This solution is reserved for the determination of phosphorus pentoxide and iron content. 4.1.4.2 Determination
Use a pipette to transfer 10 ml of test solution A (4.1.4.1) into a 250 mL beaker, add 40 mL of water, and proceed as in 4.1.2.3 starting from "In the acidometer, slowly add hydrochloric acid solution (1+20 and 1+100) under stirring until the pH value of the solution reaches 3.8..." to "At this time, stir for 30 s after each drop of solution is added." 4.1.5 Expression of analysis results
HG/T 3594—1999
The pyrophosphate (HP,O,) content (X1) expressed as mass fraction is calculated according to formula (2): Xi = TV × 0. 669 3 × 100 = 1 673. 25 × TVm×250
-Number of grams of anhydrous sodium pyrophosphate equivalent to each liter of sodium hydroxide standard titration solution; where: T—
V.-Volume of sodium hydroxide standard titration solution consumed by titrating the test solution, ml; m---mass of the sample, g;
0.6693——…The coefficient for converting anhydrous sodium pyrophosphate into pyrophosphoric acid. 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 0.2%. 4.2 Determination of phosphorus pentoxide content
4.2.1 Method summary
The sample is completely hydrolyzed into orthophosphate in an acidic solution. After adding quinoline phosphomolybdic acid solution, a precipitate of quinoline phosphomolybdic acid is generated. After filtering, washing and weighing, the phosphorus pentoxide content is calculated. 4.2.2 Reagents and materials
4.2.2.1 Hydrochloric acid solution: 1+3.
4.2.2.2 Quinoline molybdate solution.
Preparation method:
Weigh 70g sodium molybdate and dissolve it in 100mL water; a
bWeigh 60g citric acid and dissolve it in a mixture of 85mL nitric acid and 150mL water; cPour solution a into solution b under stirring; dAdd 35mL nitric acid and 5mL quinoline to 100mL water; ePour solution d into solution c, let it stand for 12h, filter it with a glass crucible, add 280mL acetone, dilute it to 1000mL with water, mix well, and store it in a polyethylene bottle. 4.2.3 Instruments and equipment
4.2.3.1 Glass crucible: filter plate pore size 5μm~~15μm; 4.2.3.2 Electric constant temperature drying oven: can control the temperature at (180±5)℃. 4.2.4 Analysis steps
Use a pipette to transfer 25mL of test solution A4.1.4.1), add 25mL of hydrochloric acid solution, heat and slightly boil for 2min, cool to room temperature, place in a 100mL volumetric flask, and dilute to the mark with water. Use a pipette to transfer 5mL of the above solution, place in a 400mL tall beaker, add water to a total volume of about 100mL, add 50mL of quinoline molybdate solution, cover with a watch glass, heat in a water bath until the content in the beaker reaches (75±5)℃, keep warm for 30s (during the addition of reagents and heating, do not use open flames, do not stir, so as not to coagulate into blocks). Cool, and stir 3 to 4 times during the cooling process. Use a glass sand crucible that has been dried to constant weight at (180±5)℃ to filter. First filter the upper clear liquid, wash the precipitate with water 6 times by pouring method, using about 30mL of water each time, and finally transfer the precipitate to a glass sand crucible and continue to wash with water 4 times. Place the glass crucible with the precipitate in an electric thermostat in a drying oven, dry at (180±5)℃ for 45min, cool to room temperature in a desiccator, and weigh. Perform a blank test at the same time. 4.2.5 Expression of analysis results
The content of phosphorus pentoxide (P2O) expressed as mass fraction (X,) is calculated according to formula (3): Xz = (ml -mz) × 0. 032 07)25 × 5
m××100
wherein: m.-
641. 4(m - m2)
×100 =
-mass of quinoline phosphomolybdic acid precipitate generated in the test solution, g:-mass of quinoline phosphomolybdic acid precipitate generated in the blank test, g;-mass of the test material in 4.1.4.1, g;
HG/T 3594-1999
0.03207-coefficient for converting quinoline phosphomolybdic acid into phosphorus pentoxide. 4.2.6 Allowable difference
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference between two parallel determinations shall not exceed 0.2%. 4.3 Determination of iron content
4.3.1 Summary of method
In an acidic medium, heat to hydrolyze pyrophosphate into orthophosphate, eliminate the interference of pyrophosphate, use ascorbic acid to reduce the trivalent iron in the test solution to divalent iron, and the divalent iron and o-phenanthroline form an orange-red complex, and measure its absorbance at a wavelength of 510nm on a spectrophotometer. 4.3.2 Reagents and materials
According to Chapter 3 of GB/T3049--1986
4.3.3 Instruments and equipment
According to Chapter 4 of GB/T3049-1986.
4.3.4 Analysis steps
4.3.4.1 Drawing of working curve
According to 5.3 of GB/T3049-1986, use a 3cm absorption cell and the corresponding iron standard solution to draw the working curve. 4.3.4.2 Determination
Use a pipette to transfer 10ml of test solution A (4.1.4.1) into a 100mL beaker, add 30mL of water, add 10mL of 1+3 hydrochloric acid solution, heat and slightly boil for 2min, cool to room temperature, transfer all the solution into a 100mL volumetric flask, and follow the provisions of 5.4 of GB/T3049-1986, starting from "add water to 60mL when necessary" to "measure the absorbance of the test solution and reagent blank solution". Select a 3cm absorption cell and measure the absorbance according to 5.4 of GB/T30491986. Find out the mass of iron in the test solution and blank test solution according to the working curve.
4.3.5 Expression of analysis results
The iron (Fe) content (X:) expressed as mass fraction is calculated according to formula (4): X = (ml=m)×10- ×100 = 9
m×250
Find out the mass of iron in the test solution from the working curve, ug; where: m-
m2————Find out the mass of iron in the blank test from the working curve, μg;-4.1.4.1 The mass of the test material, g.
4.3.6 Allowable difference
0. 002 5(m - mz)
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference of the parallel determination shall not exceed 0.002%. 4.4 Determination of lead content
4.4.1 Summary of method
Dissolve the sample in water and determine it on an atomic absorption spectrophotometer using a wavelength of 283.3nm and an air-acetylene flame using the standard addition method. 4.4.2 Reagents and materials
Lead standard solution: 1 mL of solution contains 0.1 mgPb. 4.4.3 Instruments and equipment
Atomic absorption spectrophotometer: equipped with a lead hollow cathode lamp. 4.4.4 Analysis steps
4.4.4.1 Preparation of test solution
Weigh 10g of sample (accurate to 0.01g), add water to dissolve the sample, transfer to a 250mL volumetric flask, dilute to the mark with water, and shake well. 4.4.4.2 Determination
Use a pipette to transfer 50mL of the test solution and place it in four 100mL volumetric flasks. Add 0mL, 1.00ml., 2.00mL, and 3.00mL of the lead standard solution respectively, dilute to the mark with water, and shake well. 1126
HG/T3594—1999
On an atomic absorption spectrophotometer, use an air-acetylene flame, select the best conditions, adjust to zero with water at a wavelength of 283.3nm, and measure the absorbance of the above solution.
Draw a curve with the concentration of the added standard solution as the horizontal axis and the corresponding absorbance as the vertical axis. 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. 4.4.5 Expression of analysis results
The lead (Pb) content (X,) expressed as mass fraction is calculated according to formula (5): X. = mX10-3
×100=0.5ml
m×250
Where: ml is the mass of lead in the test solution obtained by the graphical extension method, mg; m
The mass of the sample, g.
4.4.6 Allowable error
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%. 4.5 Determination of density
The determination shall be carried out in accordance with 5.1 of GB/T611-1988. 5 Inspection rules
5.1 All items specified in this standard are factory inspection items. 5.2 Each batch of products shall not exceed 5t.
5.3 Determine the number of sampling units according to 6.6 of GB/T6678--1986. When sampling, first mix the product in the barrel, insert the sampling tube into 3/4 of the barrel, and seal the upper end after the sample is full, and take it out. The sample must not be less than 500g; when the sample crystallizes into a solid, put the packaging barrel into 90-95℃ hot water and soak it. After the sample becomes liquid, sample it according to the above method. Mix the collected samples and divide them into two clean and dry plastic bottles and seal them. Stick labels on the bottles, indicating: manufacturer name, product name, 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 Pyrophosphoric acid for electroplating should be inspected by the quality supervision and inspection department of the manufacturer in accordance with the provisions of this standard. The manufacturer should ensure that each batch of products shipped from the factory meets the requirements of this standard.
5.5 If one of 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 of the re-test results does not meet the requirements of this standard, the entire batch of products shall be deemed unqualified. 5.6 Determine whether the test results meet the standards by the rounded value comparison method specified in 5.2 of GB/T1250--1989. 6 Markings and labels
6.1 The packaging of pyrophosphoric acid for electroplating should have firm and clear markings, including: manufacturer name, factory address, product name, trademark, net content, batch number or production date, this standard number and the "corrosive product" mark specified in GB190. 6.2 Each batch of pyrophosphoric acid for electroplating shipped out of the factory should be accompanied by a quality certificate, which includes: manufacturer name, factory address, product name, trademark, net content, batch number or production date, proof that the product quality complies with this standard and the number of this standard. 7 Packaging, transportation and storage
7.1 Pyrophosphoric acid for electroplating is packaged in plastic barrels, with a net content of 5kg per barrel. 7.2 The inner cover of the pyrophosphoric acid for electroplating barrel is tightly closed and the outer cover is tightened. 7.3 Pyrophosphoric acid for electroplating should be lifted and placed gently during transportation, and there should be a cover to prevent rain, sun and impact; it should not be mixed with alkaline substances, toxic substances and other easily corrosive substances. 7.4 Pyrophosphoric acid for electroplating should be stored in a cool and dry place to prevent rain and sun; it should not be mixed with alkaline substances, toxic substances and other easily corrosive substances.
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