Some standard content:
Record number: 2779-1999
HG/T 3591-1999
This industry standard has one level and six indicators: potassium pyrophosphate content, iron content, water-insoluble content, pH value, lead content and Hull cell test.
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 Electrochemical Industry Research Institute of Xiangfan City, Hubei Province. The main drafters of this standard are: Su Peiji and Zhao Chengxian. This standard is entrusted to the Inorganic Chemical Branch of the National Technical Committee for Chemical Standardization for interpretation. 1097
Chemical Industry Standard of the People's Republic of China
Potassium pyrophosphate for electroplating use
Potassium pyrophosphate for electroplating useHG/T 3591—1999
This standard specifies the requirements, test methods, inspection rules, marking, labeling, packaging, transportation and storage of potassium pyrophosphate for electroplating use. This standard applies to potassium pyrophosphate for electroplating. It is mainly used for cyanide-free electroplating. Molecular formula: K, P2O
Relative molecular mass: 330.33 (according to the international relative atomic mass in 1995) 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. GB/T 601 —1988
GB/T 602—1988
GB/T 603---1988
Preparation of standard solutions for titration analysis (volumetric analysis) of chemical reagents Preparation of standard solutions for determination of impurities of chemical reagents (negISO6353-1:1982) Preparation of preparations and products used in test methods for chemical reagents (neqISO6353-1:1982) GB/T 1250--1989
Expression and determination methods of limit values GB/T3049—1986
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/T6682—1992
Specifications and test methods for water used in analytical laboratories (eqvISO3696: 1987) GB/T 9723-1988
3 Requirements
General rules for flame atomic absorption spectrometry of chemical reagents Appearance: white powder or block.
Potassium pyrophosphate for electroplating shall meet the requirements of Table 1. Table 1 Requirements
Potassium pyrophosphate (K.P2O,) content/%
Iron (Fe) content/%
Water insoluble matter content/%
pHI value (10g/L aqueous solution)
Lead (Pb) content/%
Hull cell test (electroplating under Dk≥10A/dm2) Item
Approved by the State Administration of Petroleum and Chemical Industry on April 20, 1999 1098
10.5±0.5
Implemented on April 1, 2000
4 Test method
HG/T 3591-1999
The reagents and water used in this standard, unless otherwise specified, refer to analytically pure reagents and grade 3 water specified in (GI3/T6682. The standard titration solutions, impurity standard solutions, preparations and products used in the test, unless otherwise specified, are prepared in accordance with (GI3/T601, GB/T602, GB/r603.
Safety Tips: The hydrochloric acid and sodium hydroxide used in the test are corrosives, so be careful when operating! 4.1 Determination of potassium pyrophosphate content
4.1.1 Summary of the method
Potassium pyrophosphate reacts with hydrochloric acid to form dipotassium dihydrogen pyrophosphate. Zinc sulfate is added to form zinc pyrophosphate precipitation and sulfuric acid. The generated sulfuric acid is titrated with sodium hydroxide standard titration solution. The reaction formula is as follows: K,P,O, +2HCI ---K2H2 P,O, +2KC1K, H2 P,O, +2ZnSO =--Zn2 P,O, +K2S0. +H2 S044.1.2 Reagents and materials
4.1.2.1 Hydrochloric acid solution: 1+20.
4.1.2.2 Hydrochloric acid solution: 1+100.
H, SO4 +2NaOH ---Na2 SO. +2H,04.1.2.3 Zinc sulfate solution: 125g/L.
Weigh 125g zinc sulfate, dissolve it in water and dilute to 1000ml, adjust the pH value of the solution to 3.8 on the acidometer with sulfuric acid solution (1+500) or sodium hydroxide standard drop solution (4.1.2.4).4.1.2.4 Sodium hydroxide standard titration solution. Preparation: Prepare according to GB/T601[c(NaOH) about 0.1mol/LJ. Calibration: Weigh about 0.5g of anhydrous sodium pyrophosphate (accurate to 0.0002g) dried to constant weight at 400℃ (sodium pyrophosphate is recrystallized three times in water and placed in a platinum dish to dry), place it in a 250mL beaker, and add 90mL of water to dissolve. On the acidometer, slowly add hydrochloric acid solution of appropriate concentration under 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 under stirring until the pH value of the solution is close to 3.6. Stop titration, stir for 2min to allow the solution to reach equilibrium, and continue titration until the pH value of the solution is 3.8. At this time, stir for 30s after each drop of solution is added. The number of grams of 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 titration, mL. 4.1.3 Instruments and equipment
4.1.3.1 Acidity meter: graduation value is 0.02pH, 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
Weigh about 5g of sample (accurate to 0.0002g), put it in a 250mL beaker, add 50ml of water to dissolve, transfer to a 500mL volumetric flask, dilute to the scale with water, and shake well.
4.1.4.2 Determination
Use a pipette to transfer 50 ml of the test solution (4.1.4.1) into a 250 ml beaker, add 40 ml of water, and proceed as per 4.1.2.3 from “slowly add hydrochloric acid solution of appropriate concentration under stirring until the pH value of the solution reaches 3.8…” to 4.1.2.3. At this time, stir for 305° after each drop of solution added.
4.1.5 Expression of analysis results
HG/T 3591—1999
The sodium pyrophosphate (KP,O,) content (X) expressed as mass percentage is calculated according to formula (2): Xi = TV×1. 242
×100=1242×TV
m× 500
Wherein: T—grams of anhydrous sodium pyrophosphate equivalent to each milliliter of sodium hydroxide standard titration solution; V—volume of sodium hydroxide standard titration solution consumed by the titration test solution, ml; m—mass of the sample, g;
1.242——-coefficient for converting anhydrous sodium pyrophosphate to potassium pyrophosphate. 4.1.6 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 0.3%. 4.2 Determination of iron content
4.2.1 Method summary
Same as Chapter 2 of GB/T3049-1986.
4.2.2 Reagents and materials
Same as Chapter 3 of GB/T3049-1986.
4.2.3 Instruments and equipment
Spectrophotometer: with an absorption cell with a thickness of 3 cm. 4.2.4 Analysis steps
4.2.4.1 Drawing of standard curve
According to the provisions of 5.3 of GB/T3049-1986, a 3 cm thick absorption cell and the corresponding amount of iron standard solution are selected to draw the standard curve.
4.2.4.2 Preparation of test solution
Weigh 10g of sample (accurate to 0.1g), place in a beaker, add 50mL of water to dissolve, add 10mL of (1+1) hydrochloric acid solution, heat and slightly boil for 2min, cool to room temperature, transfer to a 250mL volumetric flask, dilute to scale, and shake well. 4.2.4.3 Preparation of blank test solution
According to 4.2.4.2, except that no sample is added. 4.2.4.4 Determination
Use a pipette to transfer 20 mL of the test solution and blank test solution respectively, and place them in 100 mL volumetric flasks respectively. Add water to each flask to 40 mL. The following operations are carried out according to the provisions of 5.4 of GB/T3049-1986, starting from "adjusting the pH to 2 with ammonia water or hydrochloric acid solution,..." to "· measuring its absorbance". Subtract the absorbance of the blank test solution from the absorbance of the test solution, and find the corresponding iron content from the standard curve. 4.2.5 Expression of analysis results
The iron (Fe) content (X2) expressed as a mass percentage is calculated according to formula (3): X2
×100=
20×1000
m×250×
Wherein: m2-
——the mass of iron found on the standard curve, mg; m
——the mass of the sample, g.
4.2.6 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 0.003%. 4.3 Determination of water-insoluble matter content
4.3.1 Summary of method
The sample is dissolved in hot water, and the insoluble matter is filtered, washed, dried and weighed. 4.3.2 Instruments and equipment wwW.bzxz.Net
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Glass sand: pore size 5μm~15μm.
4.3.3 Analysis steps
HG/T 3591—1999
Weigh about 20g of sample (accurate to 0.1g), place it in a 500ml beaker, add 400ml hot water to dissolve it, filter it through a glass crucible kept at a constant weight at 105℃~~110℃, wash the residue with hot water until it is neutral (check with pH test paper), and place the glass crucible in a drying oven at 105℃~~110℃ to dry it until it is constant weight
4.3.4 Expression of analysis results
The water-insoluble matter content (X:) expressed as mass percentage is calculated according to formula (4): m2 -ml × 100
Wherein: m
Mass of glass crucible, g;
Mass of glass crucible and water-insoluble matter, g; Mass of sample, g.
4.3.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results is not greater than 0.02%. 4.4 Determination of pH value
4.4.1 Instruments and equipment
Acidometer: The graduation value is 0.02 pH unit, and it is equipped with a saturated calomel electrode and a glass electrode. 4.4.2 Analysis steps
Weigh (1.00 ± 0.01) g of sample, dissolve it in 100 mL of water, and use an acidometer to determine the pH value. 4.4.3 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results is not greater than 0.1 pH. 4.5 Determination of lead content
4.5.1 Summary of method
Same as Article 3 of GB/T9723--1988.
4.5.2 Reagents and materials
Lead standard solution: 1ml. The solution contains 0.1mgPb. 4.5.3 Instruments and equipment
4.5.3.1 Atomic absorption spectrophotometer;
4.5.3.2 Light source: lead hollow cathode lamp.
4.5.4 Analysis steps
Weigh 25g of sample (accurate to 0.01g), add water to dissolve the sample, transfer it to a 250mL volumetric flask, dilute to the mark, and shake well. Use a pipette to transfer 25mL of the test solution respectively, place it in 4 100mL volumetric flasks, and then use a pipette to add 0ml, 1ml., 2ml, 3ml. of lead standard solution respectively, dilute to the mark with water, and shake well. On the atomic absorption spectrophotometer, use air-acetylene flame, adjust to zero with water at a wavelength of 283.3nm, and measure the absorbance of the above solution. With the concentration of added standard lead as the horizontal axis and the corresponding absorbance as the vertical axis, draw a curve, extend the curve in the opposite direction to intersect with the horizontal axis, and the lead concentration at the intersection is the lead concentration in the test solution. 4.5.5 Expression of analysis results
The lead (Pb) content (X) expressed as mass percentage is calculated according to formula (5): X4 =
×100=
m×250
Where: c—\-the lead concentration of the test solution obtained from the curve, ug/mL; m-
mass of the sample, g.
4.5.6 Allowable difference
HG/T 3591--1999
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference of the parallel determination results shall not exceed 0.001%. 4.6 Hull cell test
4.6.1 Reagents and materials
4.6.1.1 Copper pyrophosphate;
4.6.1.2 Pyrophosphoric acid;
4.6.1.3 Potassium hydroxide solution: 6 g/L.
4.6.2 Instruments and equipment
4.6.2.1 Hull cell: 250ml., the Hull cell test device is shown in Figure 1; o
Figure 1 Hull cell test device diagram
4.6.2.2 Electroplating test power supply: single-phase half-wave 10A/12V; 4.6.2.3 Steel plate: (1~~2)mm×70mm×100mm, degreased and derusted, with a smooth and flat surface; 4.6.2.4. Pure copper plate: (1~2)mm×70mm×63mm, degreased and derusted, with a smooth and flat surface; 4.6.2.5 Constant temperature water bath.
4.6.3 Test conditions
4.6.3.1 Temperature: (48±2)℃;
4.6.3.2 pH value of electroplating solution: 8.8±0.2. 4.6.4 Analysis steps
4.6.4.1 Preparation of electroplating test solution
Weigh 400g potassium pyrophosphate sample (accurate to 0.1g), dissolve it in water, then add 100g copper pyrophosphate (accurate to 0.1g) to the solution, then add water to 1000mL, and adjust the pH of the solution to 8.8±0.2 with pyrophosphoric acid or potassium hydroxide solution (check with precision pH test paper or pH meter).
4.6.4.2 Determination
Take 500mL of the electroplating test solution, heat it to 50℃, take 250mL and place it in a Hull cell. Place the cell in a constant temperature water bath and control the temperature to (48±2)℃. Use a steel plate as the cathode and a pure copper plate as the anode. Start electroplating with a current of 2A and a time of 2min. After the time is up, turn off the power, take out the cathode plate, wash it with pure water, dry it, and 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.
The current density Dk is calculated according to formula (6):
D= I(5.10 —5.24 1gL)
k-—The maximum current density of the good coating area on the cathode plate in the Hull cell test, A/dm; where: Dk
1——The current intensity indicated by the ammeter in the test, A; L—The distance between the edge of the cathode plate near the anode end and the edge of the good coating in the Hull cell test, cm. If the current density Dk is 10A/dm2 and the coating is good, the product can be considered to meet the requirements of this standard. 1102
5 Inspection rules
HG/T 3591-1999
5.1 All items specified in this standard are routine test items. 5.2 Each batch of products shall not exceed 5t.
5.3 Determine the number of sampling units in accordance with 6.6 of GB/T6678-—1986. When sampling, insert the sampler obliquely from the top of the packaging bag to 3/4 of the depth of the material layer to take a sample. After mixing the sample, divide it into four parts to no less than 500g, and pack it in two clean and dry wide-mouth bottles with stoppers and seal them. Paste labels on the bottles, indicating: manufacturer name, product name, batch number, sampling date and name of the sampler. One bottle is used for inspection and the other bottle is kept for three months for reference. 5.4 Potassium pyrophosphate 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 all potassium pyrophosphate for electroplating shipped from the factory meets the requirements of this standard. 5.5 If one of the indicators in the inspection results does not meet the requirements of this standard, re-samples should be taken from twice the amount of packaging for re-inspection. If even one of the indicators in the re-inspection results does not meet the requirements of this standard, the entire batch of products will be unqualified. 5.6 The rounded value comparison method specified in 5.2 of GB/T1250-1989 is used to determine whether the test results meet the standards. 6 Marking and labeling
6.1 Potassium pyrophosphate for electroplating should be clearly marked on the packaging, including: manufacturer name, factory address, product name, trademark, net content, batch number or production date, shelf life, and this standard number. 6.2 Each batch of potassium pyrophosphate for electroplating products shipped out of the factory should be accompanied by a quality certificate, including: manufacturer name, factory address, product name, trademark, net content, batch number or production date, shelf life, proof that the product quality complies with this standard and the number of this standard. 7 Packaging, transportation and storage
7.1 The inner packaging of potassium pyrophosphate for electroplating uses polyethylene plastic film bags with a thickness of not less than 0.05mm. The outer packaging uses plastic woven bags, and its performance and inspection methods should comply with relevant regulations. The net content of each bag is 25kg. The inner bag is tied twice with nylon rope, or sealed with other equivalent methods; the outer bag is folded at a distance of not less than 30mm from the bag edge, and sewed with vinyl nylon thread or other threads of equivalent quality at a distance of not less than 15mm from the bag edge. The stitches are neat and the stitch length is uniform. There is no leakage or skipping.
7.2 Potassium pyrophosphate for electroplating should be covered during transportation to prevent rain and moisture. 7.3 Potassium pyrophosphate for electroplating should be stored in a cool and dry place, away from rain and moisture. 7.4 The product has a shelf life of six months from the date of production under the packaging, transportation and storage conditions of this standard. If the shelf life is exceeded, it should be re-inspected to see if it meets the requirements of this standard.
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