Some standard content:
Chemical Industry Standard of the People's Republic of China
HG/T2771—1996
Nickel Chloride for Electroplating
Published on January 24, 1996
Ministry of Chemical Industry of the People's Republic of China
Implemented on January 1, 1997
WHG/T2771—1996
This standard is not equivalent to the German standard DIN50970Dez1984 "Requirements and Inspection of Nickel Salts for Electroplating Coating Nickel Plating Baths". This standard divides nickel chloride for electroplating into two grades, among which the indicators of superior products are equivalent to the German standard. The main technical differences between this standard and the German standard are as follows:
1 The main content index is not only specified in terms of Ni according to the German standard, but also specifies the indicators in terms of NiCl2·6H2O as is customary in China. 2This standard specifies the content index of water insoluble matter, while the German standard specifies the content index of insoluble matter in 0.1N sulfuric acid, which are essentially the same.
3This standard also specifies the content index of chromium and nitrate, which are very important in the electroplating industry. However, the German standard does not specify these two indicators.
4The German standard does not specify the specific test method, but only states that it is agreed upon by the supply and demand parties, while this standard is mainly determined by referring to relevant domestic standard methods.
This standard is proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Tianjin Chemical Research Institute of the Ministry of Chemical Industry. The drafting units of this standard are: Tianjin Chemical Research Institute of the Ministry of Chemical Industry, Electrochemical Industry Research Institute of Xiangfan City, Hubei Province, Huali Metal Smelting Company of Jiangdu City, Jiangsu Province, and Xiongxian Chemical General Plant of Sinochem Hebei Group. The main drafters of this standard are: Wang Qi, Zhao Chengxian, Li Youguang, and Wang Feitian. I
W.bzsosO.coI Scope
Chemical Industry Standard of the People's Republic of China
Nickel Chloride
For Electroplating
HG/T2771—1996
This standard specifies the requirements, sampling, test methods, marking, packaging, transportation and storage of nickel chloride for electroplating. This standard applies to nickel chloride for electroplating. This product is mainly used for nickel electroplating and as an anode activator in rapid nickel plating. Molecular formula: NiCl2·6H20
Relative molecular mass: 237.69 (according to the 1991 international relative atomic mass). 2 Referenced 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. GB191-90 Pictorial symbols for packaging, storage and transportation
GB/T601-88 Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB/T602-88 Preparation of standard solutions for determination of impurities in chemical reagents (negISO6353/1:1982) GB/T603-88 Preparation of preparations and products used in test methods for chemical reagents (neqISO6353/1:1982) GB/T610.1-88 General method for determination of arsenic in chemical reagents (spot method) GB/T1250-89
Representation of limit values Method and determination method GB/T3049—86
General method for determination of iron content in chemical products-Phenanthroline spectrophotometric method (neqISO6685:1982)
GB/T6678—86
General rules for sampling of chemical products
GB/T6682—92
Specifications and test methods for water used in analytical laboratories (eqvISO3696:1987)GB/T8946—88
Plastic woven bags
3 Requirements
3.1 Appearance: green crystals.
3.2 Nickel chloride for electroplating shall meet the requirements of Table 1: Table 1 Requirements
Main content
Calculated as NiC12·6H20
Calculated as Ni
Cobalt (Co) content
Approved by the Ministry of Chemical Industry of the People's Republic of China on January 24, 1996
Superior product
First-class product
Implemented on January 1, 1997||tt ||W. Zinc (Zn) content
Iron (Fe) content
Copper (Cu) content
Lead (Pb) content
Cadmium (Ca) content
Arsenic (As) content
Water-insoluble matter content
Chromium (Cr) content
Nitrate (as NOs) content
4 Sampling
4.1 Each batch of products shall not exceed 50t.
HG/T2771—1996
Table 1 (end)
Superior products
First-class products
4.2 Determine the number of sampling units in accordance with the provisions of GB/T66786.6. 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, 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. 4.3 If one of the indicators does not meet the requirements of this standard, re-sample from twice the amount of packaging for verification. If even one of the indicators does not meet the requirements of this standard, the entire batch of products will be unqualified. 5 Test method
5.1 All eleven indicator items specified in this standard are type test items, of which seven items, namely main content, zinc content, copper content, lead content, water-insoluble content, chromium content and nitrate content, are routine test items and should be tested batch by batch. Under normal production conditions, type tests should be carried out at least once every three months.
5.2 Use the rounded value comparison method specified in GB/T12505.2 to determine whether the test results meet the standard. 5.3 The reagents and water used in this standard, unless otherwise specified, refer to analytical pure reagents and grade 3 water specified in GB/T6682. The standard titration solution, impurity standard solution, 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. 5.4 Determination of main content
5.4.1 Method summary
In an ammonia solution, tartaric acid is added to form a soluble complex with impurities such as iron and aluminum to eliminate interference, and dimethylglyoxal and nickel are used to generate a red dimethylglyoxal nickel precipitate, which is filtered, washed and dried to constant weight, and the nickel content is calculated. 5.4.2 Reagents and materials
5.4.2.1 95% ethanol solution: 1+4;
W.bzsoso.coD5.4.2.2 Hydrochloric acid solution: 1+1;
5.4.2.3 Ammonia solution: 1+1;
5.4.2.4 Ammonium chloride solution: 200g/L,
5.4.2.5 Tartaric acid solution: 200g/L;
HG/T2771—1996
Dimethylglyoxal ethanol solution: 10g/L. 5.4.2.6
5.4.3 Instruments and equipment
Glass sand crucible: filter plate pore size 5~15μm.
5.4.4 Analysis steps
Weigh about 2g of sample (accurate to 0.0002g) and place it in a 250mL beaker. Add 2mL of hydrochloric acid solution and 50mL of water to dissolve. Cool to room temperature, transfer to a 100mL volumetric flask, dilute to scale with water, and shake well. Use a pipette to transfer 10mL of test solution and place it in a 400mL beaker. Add 150mL of water, 5mL of ammonium chloride solution, and 5mL of tartaric acid solution, cover with a watch glass, and heat to boiling. When cooled to 70-80℃, slowly add 30mL of dimethylglyoxal solution while stirring continuously, and add ammonia solution dropwise to adjust the pH value of the solution to 8-9 (check with precision pH test paper), and then add 12mL in excess. Keep warm at 70-80℃ for 30min, filter with a glass crucible that has been dried to constant weight at 105-110℃, wash with ethanol solution 4-5 times, and dry at 105-110℃ to constant weight.
5.4.5 Expression of analysis results
The main content expressed in mass percentage (calculated as NiClz·6HO) X is calculated according to formula (1): _(ml-mo)X0.8226)
822.6(mlmo)
The main content expressed in mass percentage (calculated as Ni) X2 is calculated according to formula (2): X2
Where: m1-
(mlm)X0.203 1
203.1 (ml-m)
-mass of precipitate and glass sand, g;
-mass of glass sand crucible, g;
coefficient of nickel dimethylglyoxal converted to nickel; 0.8226-
-coefficient of nickel dimethylglyoxal converted to nickel chloride hexahydrate. m——mass of sample, g.
5.4.6 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 0.2% (calculated as NiC126H20) and 0.05% (calculated as Ni).
5.5 Determination of cobalt content
5.5.1 Summary of method
In a hot solution of sodium acetate, sodium 1-nitroso-2-naphthol-3,6-disulfonate forms a stable complex with cobalt, and its absorbance is measured by a spectrophotometer at a wavelength of 550nm. 5.5.2 Reagents and materials
5.5.2.1 Sodium acetate solution: 300g/L;
5.5.2.2 Nitric acid solution: 1+1;
5.5.2.3 Hydrochloric acid solution: 1+1;
HG/T2771—1996
5.5.2.4 Cobalt standard solution: 1mL solution contains 0.01mgCo; Use a pipette to transfer 1mL of cobalt standard solution prepared according to GB/T602, place it in a 100mL volumetric flask, dilute with water to the mark, and shake well. This solution is prepared before use.
5.5.2.5 Nickel standard solution: 1mL solution contains 10mgNi; Weigh 6.730g of ammonium nickel sulfate, dissolve it in water, transfer it into a 100mL volumetric flask, dilute with water to the mark, and shake well. 5.5.2.6 1-nitroso-2-naphthol-3,6-disulfonic acid sodium salt (nitroso R salt) solution: 5g/L. 5.5.3 Instruments and equipment
Spectrophotometer: with 1cm absorption cell.
5.5.4 Analysis steps
5.5.4.1 Drawing of working curve
Accurately pipette 0, 5.00, 10.00, 15.00, 20.00, and 30.00mL of cobalt standard solution into six 250mL beakers containing 1.2mL of nickel standard solution, and add water to 40mL. Add 10mL of sodium acetate solution, heat to boiling, add 10mL of 1-nitroso-2-naphthol-3,6-disulfonic acid sodium salt solution, and boil for 2 to 3min. Add 10mL of nitric acid solution, and then boil slightly for 2min, and cool. Transfer to a 100mL volumetric flask, dilute to the mark with water, and shake well. Use a spectrophotometer at a wavelength of 550nm, use a 1cm absorption cell, and use water as a reference to measure its absorbance. Use the diamond content as the horizontal axis and the corresponding absorbance as the vertical axis to draw a working curve. 5.5.4.2 Preparation of test solution
Weigh about 1g of the sample (accurate to 0.0002g) and place it in a 250mL beaker. Add 2mL of hydrochloric acid solution and 50mL of water, dissolve, cool to room temperature, transfer to a 100mL volumetric flask, dilute to the mark with water, and shake well. 5.5.4.3 Preparation of blank test solution
Except for not adding the sample, the amount of other reagents added is exactly the same as the preparation of the test solution, and is treated in the same way as the sample. 5.5.4.4 Determination
Use a pipette to transfer 5mL of the test solution and blank test solution respectively, and place them in 250mL beakers respectively. The following operations are carried out according to 5.5.4.1 from "add water to 40mL..." to "., measure its absorbance.". According to the working curve, find out the mass of cobalt in the test solution and the blank test solution. 5.5.5 Expression of analysis results
Content X of cobalt (Co) expressed as mass percentage: calculated according to formula (3): (mi-m2)X10-8
_2 (ml-m2)
-mass of cobalt in the test solution, mg;
Where: m1-
mass of cobalt in the blank test solution, mg; m——mass of the sample, g.
5.5.6 Allowable difference
(3)
WHG/T2771—1996
Take the arithmetic mean of the parallel determination results as the determination result. The absolute difference of the parallel determination results shall not exceed 0.03%. 5.6 Determination of zinc content
5.6.1 Summary of method
Dissolve the sample in water and determine it on an atomic absorption spectrophotometer using a wavelength of 213.9nm and an air-acetylene flame by the standard addition method.
5.6.2 Reagents and materials
Zinc standard solution: 1mL of solution contains 0.1mgZn. 5.6.3 Instruments and equipment
Atomic absorption spectrophotometer: equipped with a zinc hollow cathode lamp. 5.6.4 Analysis steps
5.6.4.1 Preparation of test solution A
Weigh about 50g of the sample (accurate to 0.01g), place it in a 400mL beaker, add water to dissolve it, transfer it to a 500mL volumetric flask, add water to the scale, and shake well.
5.6.4.2 Determination
Use a pipette to transfer four 5mL portions of test solution A (5.6.4.1) into four 100mL volumetric flasks, add 0, 0.20, 0.40, and 0.60mL of zinc standard solution, dilute to the mark with water, and shake the hook. On an atomic absorption spectrophotometer, use an air-acetylene flame, adjust to zero with water at a wavelength of 213.9nm, and measure the absorbance of the above solution.
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 zinc in the tested solution. 5.6.5 Expression of analysis results
The zinc (Zn) content X expressed as mass percentage is calculated according to formula (4): X = miX10-a
Wherein: m1 is the mass of zinc in the test solution obtained by the graphical extension method, mg; m- is the mass of the sample in the test solution A, g. m-
5.6.6 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%. 5.7 Determination of iron contentbzxz.net
5.7.1 Summary of the method
According to Chapter 2 of GB/T3049.
5.7.2 Reagents and materials
According to Chapter 3 of GB/T3049 and
4-methylpentanone-(2).
5.7.3 Instruments and equipment
According to Chapter 4 of GB/T3049.
5.7.4 Analysis steps
5.7.4.1 Drawing of working curve
According to 5.3 of GB/T3049, use a 3cm absorption cell and the corresponding iron standard solution to draw the working curve. 5.7.4.2 Preparation of test solution
Weigh about 5g of sample (accurate to 0.01g), place it in a 250mL beaker, add 1~2mL of 1+3 hydrochloric acid solution, 50mL of water, heat and boil for 2~3min, transfer to a 100mL volumetric flask after cooling, dilute to the scale with water, and shake well. 5
ww.bzsoso：com5.7.4.3 Preparation of blank test solution
HG/T2771—1996
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 treated in the same way as the sample. 5.7.4.4 Determination
Use a pipette to transfer 10mL of the test solution and the blank test solution respectively, and place them in a 125mL separatory funnel, add 30mL of water, 40mL of concentrated hydrochloric acid, and 10mL of 4-methylpentanone-(2), shake for 1min, let stand and separate, and then discard the aqueous phase. Add 20mL of water to the separatory funnel, shake for 1min, and let stand and separate. Transfer the aqueous phase to a 100mL volumetric flask, add 5mL of water to the separatory funnel, shake for 30s, and let stand and separate. Transfer the aqueous phase to the same volumetric flask, add water to about 60 mL, and adjust the pH of the test solution to 2 with 1+8 ammonia solution (check with precision pH test paper). Add 2.5 mL of ascorbic acid solution, 10 mL of buffer solution, and 5 mL of o-phenanthroline solution, dilute to the scale with water, and shake well.
Use a 3 cm absorption cell, measure the absorbance according to 5.4 of GB/T3049, and find out the mass of iron in the test solution and blank test solution according to the working curve.
5.7.5 Expression of analysis results
The iron (Fe) content Xs expressed as mass percentage is calculated according to formula (5): Xx=(mm2) ×10-×100
(m1-m2)X10-8
Where: m1——the mass of iron in the test solution, ug; m2——the mass of iron in the blank test solution, ug; m-
——the mass of the sample, g.
5.7.6 Allowable difference
The arithmetic mean of the parallel determination results shall be taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.002%. 5.8 Determination of copper content
5.8.1 Summary of method
(5)
Dissolve the sample in water and determine it on an atomic absorption spectrophotometer using a wavelength of 324.8nm and an air-acetylene flame by the standard addition method.
5.8.2 Reagents and materials
Copper standard solution: 1mL of solution contains 0.1mgCu. 5.8.3 Instruments and equipment
Atomic absorption spectrophotometer: equipped with a copper hollow cathode lamp. 5.8.4 Analysis steps
Use a pipette to transfer four 40mL portions of test solution A (5.6.4.1) into four 100mL volumetric flasks, add 0, 1.00, 2.00, 3.00mL of copper standard solution, dilute to scale with water, and shake well. On an atomic absorption spectrophotometer, use an air-acetylene flame, adjust to zero with water at a wavelength of 324.8nm, and measure the absorbance of the above solution.
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 copper in the tested solution. 5.8.5 Expression of analysis results
The copper (Cu) content X expressed as mass percentage. Calculate according to formula (6): 6
HG/T2771--1996
XgmX10-8
Wherein: m1 is the mass of copper in the test solution obtained by the graphic epitaxy method, mg; m
is the mass of the sample contained in the test solution A (5.6.4.1), g. 5.8.6 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%. 5.9 Determination of lead content
5.9.1 Summary of method
(6)
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.
5.9.2 Reagents and materials
Lead standard solution: 1 mL of solution contains 0.1 mg Pb. 5.9.3 Instruments and equipment
Atomic absorption spectrophotometer: equipped with a lead hollow cathode lamp. 5.9.4 Analysis steps
Use a pipette to transfer four 40 mL portions of test solution A (5.6.4.1) and place them in four 100 mL volumetric flasks, respectively. Add 0, 1.00, 2.00, and 4.00 mL of lead standard solution, respectively, dilute to the mark with water, and shake well. On the atomic absorption spectrophotometer, use an air-acetylene flame, 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 abscissa and the corresponding absorbance as the ordinate to draw a curve. Extend the curve in the reverse direction to intersect with the abscissa. The intersection is the concentration of lead in the tested solution. 5.9.5 Expression of analysis results
The lead (Pb) content X expressed as a mass percentage is calculated according to formula (7): Xy=m,X10-8
Wherein: m1——the mass of lead in the test solution obtained by the graphical epitaxy method, mg; m-——the mass of the sample contained in the test solution A (5.6.4.1), g. 5.9.6 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%. 5.10 Determination of cadmium content
5.10.1 Summary of method
(7)
The sample is dissolved in water and determined on an atomic absorption spectrophotometer using a wavelength of 228.8nm and an air-acetylene flame by the standard addition method.
5.10.2 Reagents and materials
Cadmium standard solution: 1 mL of solution contains 0.1 mgCd. 5.10.3 Instruments and equipment
Atomic absorption spectrophotometer: equipped with a cadmium hollow cathode lamp. 5.10.4 Analysis steps
Use a pipette to transfer four 5 mL portions of test solution A (5.6.4.1) into four 100 mL volumetric flasks, add 0, 0.10, 0.30, and 0.50 mL of cadmium standard solution, dilute to the mark with water, and shake well. On the atomic absorption spectrophotometer, use an air-acetylene flame, adjust to zero with water at a wavelength of 228.8 nm, and measure the absorbance of the above solution 7
.
HG/T2771—1996
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 cadmium in the tested solution. 5.10.5 Expression of analysis results
Cadmium (Cd) content X expressed as mass percentage. Calculate according to formula (8): Xg=miX10-8
Where: m1—the mass of cadmium in the test solution obtained by the graphical extension method, mg; m
5.10.6 Allowable difference
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%. 5.11 Determination of arsenic content
5.11.1 Summary of the method
According to Chapter 3 of GB/T610.1.
5.11.2 Reagents and materials
According to Chapter 4 of GB/T610.1 and
Arsenic standard solution: 1mL of solution contains 1μgAs. (8)
Use a pipette to transfer 1mL of the arsenic standard solution prepared according to GB/T602 into a 100mL volumetric flask, dilute to the mark with water, and shake well. The solution is prepared before use.
5.11.3 Instruments and equipment
According to Chapter 5 of GB/T610.1.
5.11.4 Analysis steps
Weigh 0.50±0.01g of the sample and place it in a wide-mouth bottle. The following operations are carried out according to the method specified in Chapter 6 of GB/T610.1. Preparation of arsenic standard color spot: Use a pipette to transfer 5mL (for superior products) and 10mL (for first-class products) of arsenic standard solution into a wide-mouth bottle and treat it in the same way as the sample.
5.12 Determination of water-insoluble content
5.12.1 Reagents and materials
Silver nitrate solution: 20g/L.
5.12.2 Instruments and equipment
Glass sand crucible: filter plate pore size 515um.
5.12.3 Analysis steps
Weigh about 25g of sample (accurate to 0.001g), place it in a 400mL beaker, and add 100mL of water to dissolve it. Filter it with a glass sand crucible that has been dried to constant weight at 105~110℃, wash it with hot water until there is no chloride ion (check with silver nitrate solution), and dry it at 105~110℃ to constant weight.
5.12.4 Expression of analysis results
Content of water-insoluble matter X expressed as mass percentage. Calculate according to formula (9): ml-m2×100.
Wherein: m1——mass of glass sand crucible and water-insoluble matter, g; m2——mass of glass sand crucible, g;
mass of sample, g.
W.bzsoso.coD5.12.5 Allowable difference
HG/T2771—1996
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 0.005%. 5.13 Determination of chromium content
5.13.1 Summary of method
In sulfuric acid solution, chromium is oxidized to hexavalent with potassium permanganate, and nickel, iron, cobalt and other ions are precipitated with sodium carbonate. Hexavalent chromium reacts with diphenylcarbohydrazide in 0.05~0.2mol/L sulfuric acid solution to form a purple-red complex. Its absorbance is measured by a spectrophotometer at a wavelength of 540nm.
5.13.2 Reagents and materials
5.13.2.1 Sulfuric acid solution: 1+1
5.13.2.2 Potassium permanganate solution: 10g/L
5.13.2.3 Sodium carbonate solution: 200g/L; 5.13.2.4 Diphenylcarbohydrazide ethanol solution: 2.5g/L; Weigh 0.25g of diphenylcarbohydrazide and dissolve it in 94mL of anhydrous ethanol and 6mL of glacial acetic acid, and store it in a brown bottle. 5.13.2.5 Chromium standard solution: 1mL of solution contains 2μgCr. Use a pipette to transfer 2 mL of the chromium standard solution prepared according to GB/T602 into a 100 mL volumetric flask, dilute to the mark with water, and shake well. Prepare the solution before use.
5.13.3 Instruments and equipment
Spectrophotometer: equipped with a 3 cm absorption cell.
5.13.4 Analysis steps
5.13.4.1 Drawing of working curve
In a set of 100mL volumetric flasks, add 0, 1.00, 2.00, 4.00, 7.00, and 10.00mL of chromium standard solution. Add 1mL of sulfuric acid solution, add water to about 90mL, add 3mL of diphenylcarbonyl diethanol solution, dilute to the scale with water, and shake well.
Use a spectrophotometer to measure its absorbance at a wavelength of 540nm with a 3cm absorption cell and water as a reference. Draw a working curve with the chromium content as the horizontal axis and the corresponding absorbance as the vertical axis. 5.13.4.2 Preparation of test solution
Weigh about 1g of sample (accurate to 0.0002g) and place it in a 250mL beaker. Add 1mL of sulfuric acid solution and 30mL of water to dissolve. Add 1mL of potassium permanganate solution and heat and boil until all manganese dioxide is precipitated. Add water to about 90mL, add 30mL sodium carbonate solution slowly in portions while stirring, and cool to room temperature. Transfer to a 250mL volumetric flask. Dilute with water to the mark and shake well. 5.13.4.3 Preparation of blank test solution
Except for not adding the sample, the amount of other reagents added is exactly the same as the preparation of the test solution, and is treated in the same way as the sample. 5.13.4.4 Determination
Dry filter the test solution and blank test solution with double-layer medium-speed filter paper, discard the initial filtrate, and use a pipette to transfer 50mL of the filtrate respectively and place it in a 100mL volumetric flask. Adjust to neutral with sulfuric acid solution, then add 1mL in excess, add water to about 90mL, add 3mL diphenylcarbazide ethanol solution, dilute with water to the mark and shake well. Use a spectrophotometer to measure the absorbance at a wavelength of 540nm, using a 3cm absorption cell and water as a reference. Find out the mass of chromium in the test solution and blank test solution based on the working curve. 5.13.5 Expression of analysis results
The chromium (Cr) content X10 expressed as mass percentage is calculated according to formula (10):9
W.bzsoso.coIHG/T2771—1996
(mm2)X10-×100
m×250
0.0005（m1m2）
Wherein: m1——the mass of chromium in the test solution, ug; m2——the mass of chromium in the blank test solution, ug; m——the mass of the sample, g.
5.13.6 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%. 5.14 Determination of nitrate content
5.14.1 Summary of method
Dissolve the sample in water and precipitate the metal ions with sodium hydroxide. Sodium indigo disulfonate is oxidized by nitrate in acidic solution, making the blue color lighter. Visually compare the color with the standard.
5.14.2 Reagents and materials
5.14.2.1 Sulfuric acid;
5.14.2.2 Sodium hydroxide solution: 100g/L; 5.14.2.3 Sodium chloride solution: 100g/L, 5.14.2.4 Nitrate standard solution: 1mL solution contains 0.01mgNO3; Use a pipette to transfer 10mL of the nitrate standard solution prepared according to GB/T602, place it in a 100mL volumetric flask, dilute to the mark with water, and shake well. This solution is prepared before use. 5.14.2.5 Indigo disulfonate sodium solution: 0.001 mol/L; 5.14.3 Analysis steps
Weigh 2.00 ± 0.01 g of the sample and dissolve it in 30 mL of water. Add 10 mL of sodium hydroxide solution, heat to boiling, cool, transfer to a 100 mL volumetric flask, dilute to scale with water, and shake well. Use a pipette to transfer 10 mL of the upper clear liquid and place it in a 25 mL colorimetric tube. Add 1 mL of sodium chloride solution and 1 mL of indigo disulfonate sodium solution. Under shaking, add 10 mL of sulfuric acid within 1015 seconds and leave it for 10 minutes. The blue color should not be lighter than the standard colorimetric solution. The standard colorimetric solution is 2.00 mL of nitrate standard solution, which is treated in the same way as the test solution. 6 Marking, packaging, transportation, storage
6.1 The packaging of nickel chloride for electroplating should be firmly and clearly marked, including: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, this standard number and the "heat-afraid" mark and "moisture-afraid" mark specified in GB191. 6.2 Each batch of nickel chloride for electroplating shipped out of the factory should be accompanied by a quality certificate. The content includes: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, proof that the product quality meets this standard and this standard number. 6.3 Nickel chloride for electroplating adopts two packaging methods. 6.3.1 Woven bag packaging: The inner packaging is a two-layer polyethylene plastic film bag with a thickness of not less than 0.05mm; the outer packaging is a plastic woven bag, and its performance and inspection method shall comply with the provisions of Type A of GB/T8946. The net weight of each bag is 25kg. 6.3.2 Cardboard barrel packaging: The inner packaging is a two-layer polyethylene plastic film bag with a thickness of not less than 0.05mm; the outer packaging is a cardboard barrel, and its performance and inspection methods shall comply with relevant regulations. The net weight of each barrel is 25kg. 6.4 Two sealing methods are used for nickel chloride for electroplating. 6.4.1 When using woven bags for packaging, the two inner bags are tied manually with vinyl rope or other ropes of equivalent quality, or with equivalent 10
W.bzsosO.cO0.1g sample, dissolved in 30mL water. Add 10mL sodium hydroxide solution, heat to boiling, cool, transfer to a 100mL volumetric flask, dilute with water to the mark, shake well. Use a pipette to transfer 10mL of the upper clear liquid and place it in a 25mL colorimetric tube. Add 1mL sodium chloride solution and 1mL sodium indigo disulfonate solution. Under shaking, add 10mL sulfuric acid within 1015s and let it stand for 10min. The blue color should not be lighter than the standard colorimetric solution. The standard colorimetric solution is 2.00mL of nitrate standard solution, which is treated in the same way as the test solution. 6 Marking, packaging, transportation, storage
6.1 The packaging of nickel chloride for electroplating should be firmly and clearly marked, including: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, this standard number and the "heat-afraid" mark and "wet-afraid" mark specified in GB191. 6.2 Each batch of nickel chloride for electroplating shall be accompanied by a quality certificate. The contents include: manufacturer name, address, product name, trademark, grade, net weight, batch number or production date, proof that the product quality complies with this standard and the number of this standard. 6.3 Two packaging methods are used for nickel chloride for electroplating. 6.3.1 Woven bag packaging: The inner packaging is a two-layer polyethylene plastic film bag with a thickness of not less than 0.05mm; the outer packaging is a plastic woven bag, and its performance and inspection methods shall comply with the provisions of Type A of GB/T8946. The net weight of each bag is 25kg. 6.3.2 Cardboard barrel packaging: The inner packaging is a two-layer polyethylene plastic film bag with a thickness of not less than 0.05mm; the outer packaging is a cardboard barrel, and its performance and inspection methods shall comply with relevant regulations. The net weight of each barrel is 25kg. 6.4 Two sealing methods are used for nickel chloride for electroplating. 6.4.1 When woven bags are used for packaging, the two inner bags shall be tied with nylon rope or other ropes of equivalent quality, or with a rope of equivalent quality.0.1g sample, dissolved in 30mL water. Add 10mL sodium hydroxide solution, heat to boiling, cool, transfer to a 100mL volumetric flask, dilute with water to the mark, shake well. Use a pipette to transfer 10mL of the upper clear liquid and place it in a 25mL colorimetric tube. Add 1mL sodium chloride solution and 1mL sodium indigo disulfonate solution. Under shaking, add 10mL sulfuric acid within 1015s and let it stand for 10min. The blue color should not be lighter than the standard colorimetric solution. The standard colorimetric solution is 2.00mL of nitrate standard solution, which is treated in the same way as the test solution. 6 Marking, packaging, transportation, storage
6.1 The packaging of nickel chloride for electroplating should be firmly and clearly marked, including: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, this standard number and the "heat-afraid" mark and "wet-afraid" mark specified in GB191. 6.2 Each batch of nickel chloride for electroplating shall be accompanied by a quality certificate. The contents include: manufacturer name, address, product name, trademark, grade, net weight, batch number or production date, proof that the product quality complies with this standard and the number of this standard. 6.3 Two packaging methods are used for nickel chloride for electroplating. 6.3.1 Woven bag packaging: The inner packaging is a two-layer polyethylene plastic film bag with a thickness of not less than 0.05mm; the outer packaging is a plastic woven bag, and its performance and inspection methods shall comply with the provisions of Type A of GB/T8946. The net weight of each bag is 25kg. 6.3.2 Cardboard barrel packaging: The inner packaging is a two-layer polyethylene plastic film bag with a thickness of not less than 0.05mm; the outer packaging is a cardboard barrel, and its performance and inspection methods shall comply with relevant regulations. The net weight of each barrel is 25kg. 6.4 Two sealing methods are used for nickel chloride for electroplating. 6.4.1 When woven bags are used for packaging, the two inner bags shall be tied with nylon rope or other ropes of equivalent quality, or with a rope of equivalent quality.
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