Some standard content:
Record number: 7256--2000
HG/T2960-2000
This standard is based on the current domestic production status and user requirements, and refers to FOCT4164-1979 (85) "Cuprous Chloride" (reagent grade), and is revised from the chemical industry standard HG/T2960-1979 (1988) "Cuprous Chloride". The main differences between this standard and HG/T2960-1979 (1988) are: the potassium dichromate method is added to the cuprous chloride content determination method of the first standard, and the cerium sulfate method is used as the arbitration method. The first standard is graded and the index parameters are greatly adjusted. From the date of implementation, this standard will replace HG/T2960-1979 (1988). Appendix A of this standard is the appendix of the standard.
This standard is proposed by the Policy and Regulations Department of the State Administration of Petroleum and Chemical Industry. This standard is under the jurisdiction of the Inorganic Chemical Branch of the National Technical Committee for Chemical Standardization. This standard was drafted by Tianjin Chemical Research and Design Institute and Chongqing Huaxi Chemical Plant. The main drafters of this standard are Wang Zixian, Zhang Zhilun and Wang Yan. This standard was first issued as a national standard in 1979, confirmed in 1988 and adjusted to a chemical industry standard in 1992. This standard is entrusted to the Inorganic Chemical Branch of the National Technical Committee for Chemical Standardization for interpretation. 892
Chemical Industry Standard of the People's Republic of China
Industrial Cuprous Chloride
Cuprous Chloride for Industrial UseHG/T 2960—2000
Replaces HG/T2960-1979（1988）
This standard specifies the requirements, test methods, inspection rules, and marking, labeling, packaging, transportation and storage of industrial cuprous chloride. This standard applies to industrial cuprous chloride, which is mainly used in industries such as pigments and batteries. Molecular formula: CuCl
Relative molecular mass: 99.00 (according to the 1997 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 the parties using this standard should explore the possibility of using the latest versions of the following standards. GB191-1990 Pictorial markings for packaging, storage and transportation
GB/T601-1988 Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB/T 602--1988
Preparation of standard solutions for determination of impurities in chemical reagents (negISO6353-1:1982) GB/T 603-1988
Preparation of preparations and products used in test methods for chemical reagents (negISO6353-1:1982) GB/T 1250--1989
GB/T 6678-1986
Numerical expression and determination method
General rules for sampling of chemical products
GB/T6682--1992
Specifications and test methods for water used in analytical laboratories (neqISO3696:1987) 3 Requirements
3.1 Appearance: White or off-white powder, loose pieces are allowed. 3.2 Industrial cuprous chloride should meet the requirements of Table 1. Table 1 Requirements
Superior products
Content of cuprous chloride (calculated as CuCl)
Content of divalent copper (calculated as CuCl2)
Content of acid insoluble matter
Content of iron (Fe)
Content of sulfate (calculated as SO,)
Test methodwww.bzxz.net
First-class products
Qualified products
The reagents and water used in this standard, unless otherwise specified, refer to analytical pure reagents and grade 3 water specified in GB/T6682. Approved by the State Administration of Petroleum and Chemical Industry on May 23, 2000, and implemented on December 1, 2000
HG/T 2960—2000
Standard titration solutions, impurity standard solutions, preparations and products used in the test shall be prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603 unless otherwise specified.
Safety Tips: The hydrochloric acid, nitric acid and hydrogen peroxide used in this standard are corrosive. Users should be careful when handling them to avoid splashing on the skin. If splashed on the skin, rinse immediately with plenty of water and seek medical treatment in severe cases. 4.1 Determination of cuprous chloride content
4.1.1 Cerium sulfate method (arbitration method)
4.1.1.1 Summary of the method
Use ferric chloride to oxidize the monovalent copper in the sample to divalent copper, and produce divalent iron in the same amount as the monovalent copper. Take o-phenanthroline as the indicator and use cerium sulfate standard titration solution to determine the divalent iron in the sample. 4.1.1.2 Reagents and materials
a) Hydrochloric acid.
b) Ferric chloride solution.
Weigh 75g of ferric chloride (FeCl:·6H.O) and dissolve it in a mixed solution of 150mL hydrochloric acid and 400mL water. Add 5ml of 30% hydrogen peroxide and boil to remove excess hydrogen peroxide. c) Standard sulfuric acid titration solution: c[Ce(SO,), about 0.1mol/L. d) o-phenanthroline indicator solution.
Weigh 1.49g of o-phenanthroline and 0.695g of ferrous sulfate (FeSO4·7H2O) and dissolve them in 100ml of water. 4.1.1.3 Analysis steps
Use the reduction method to weigh 0.25g~0.30g of the sample (accurate to 0.0002g). Place it in a 250mL iodine volumetric flask with an appropriate amount of glass beads with a diameter of 5mm~7mm and 10mL of ferric chloride solution in advance. Cover the stopper and shake it continuously. After the sample is dissolved, add 50mL of water and 2 drops of o-phenanthroline indicator, and immediately titrate with a standard titration solution of sulfuric acid until the green color appears as the end point. Perform a blank test at the same time.
4.1.1.4 Expression of analysis results
The cuprous chloride content (X,) expressed as mass percentage is calculated according to formula (1): X = c(V-Vo)×0. 099 00 X
Wherein: c—-actual concentration of antimony sulfate standard titration solution, mol/L; X 100
V—volume of sulfuric acid standard titration solution consumed by titrating the test solution, mLV. ——volume of sulfuric acid standard titration solution consumed by titrating the blank solution, mL; -mass of the sample, g;
0.09900—mass of cuprous chloride expressed in grams equivalent to 1.00 mL of antimony sulfate standard titration solution (c[Ce(SO)2]=1.000mol/L).
4.1.1.5 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 0.3%. 4.1.2 Potassium dichromate method
4.1.2.1 Summary of the method
Use ferric chloride to oxidize the monovalent copper in the sample to divalent copper, and produce divalent iron in an amount equal to that of monovalent copper. Use sodium diphenylamine sulfonate as an indicator and potassium dichromate standard titration solution to titrate the reduced divalent iron salt. 4.1.2.2 Reagents and materials
a) Hydrochloric acid.
b) Ferric chloride solution.
Weigh 75g of ferric chloride (FeCl:·6H.O) and dissolve it in a mixed solution of 150ml. hydrochloric acid and 400ml water, add 5ml of 30% hydrogen peroxide, and boil to remove excess hydrogen peroxide. 894
HG/T 2960---2000
c) Potassium dichromate standard titration solution: c(1/6K,CrzO,) is about 0.1mol/L. d) Sulfuric acid solution: 1+8.
e) Sodium diphenylamine sulfonate indicator solution: 5g/L. 4.12.3 Analysis steps
Use the reduction method to weigh 0.25g~~0.30g of the sample (accurate to 0.0002g), place it in a 250mL iodine volumetric flask with an appropriate amount of glass beads with a diameter of 5mm~~7mm and 10ml ferric chloride solution in advance, cover the stopper, shake continuously, and after the sample is dissolved, add 50mL of water, add 20mL of sulfuric acid solution, cover the stopper, shake well, add 5 drops of sodium diphenylamine sulfonate indicator solution, and immediately titrate with potassium dichromate standard titration solution until a purple-blue color appears as the end point.
A blank test is also performed.
4.1.2.4 Expression of analysis results
The cuprous nitride content (X2) expressed as mass percentage is calculated according to formula (2): Xx = c(VV)×0. 099 00×100
Wherein: - the actual concentration of potassium dichromate standard titration solution, mol/L; the volume of potassium dichromate standard titration solution consumed by the titration test solution, mL; V
V. - the volume of potassium dichromate standard titration solution consumed by the titration blank solution, mL; sample mass, g;
0. 099 00-
(KCr.0,)=1.000mol/L equivalent to 1.00mL of potassium dichromate standard titration solution c(the mass of cuprous chloride expressed in grams.
4.1.2.5 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.3%. 4.2 Determination of divalent copper content
4.2.1 Method summary
Under slightly acidic conditions, excess potassium iodide is added to the sample to react with divalent copper to precipitate iodine of the same mass as divalent copper ions. Starch solution is used as an indicator and the precipitated iodine is titrated with sodium thiosulfate standard titration solution. The end point is determined by the color change. 4.2.2 Reagents and materials
4.2.2.1 Sodium fluoride.
4.2.2.2 Potassium iodide.
4.2.2.3 Acetic acid solution: 5+12.
Starch indicator solution: 10 g/L (use limit is two weeks). 4.2.2.4
4.2.2.5 Potassium thiocyanate solution: 100g/L. 4.2.2.6 Sodium thiosulfate standard titration solution: c(NazS,O) about 0.05mol/L. Prepare 0.1mol/L standard titration solution according to GB/T601, dilute - times and calibrate. 4.2.3 Analysis steps
Weigh about 5g of the sample (accurate to 0.01g), place it in a 50mL dry stoppered colorimetric tube, add acetic acid solution to the scale, and place the dry glass Put the glass beads into the tube, cover the tube stopper, make the solution fill the colorimetric tube, and shake for 30 seconds. After clarifying for 30 minutes, take 25mL of the upper clear liquid and put it into the iodine volume bottle, add 1g sodium fluoride, 2g potassium iodide, and then add 25mL water, let it stand for 5 minutes, add 2mL starch indicator and 10ml potassium thiocyanate solution, and titrate with sodium thiosulfate standard titration solution until the blue color disappears. 4.2.4 Expression of analysis results
The content of divalent copper (in terms of CuCl2) expressed as mass percentage (X:) is calculated according to formula (3): X: = V×0.134 5 × 100 = 26. 90 ×cVm
Where: c
HG/T 2960—2000
Actual concentration of sodium thiosulfate standard titration solution, mol/L; V
Volume of sodium thiosulfate standard titration solution consumed by the titration test solution, mL; m—mass of sample, g;
0.1345——-CuCl2 (Cu2O4) equivalent to 1.00mL sodium thiosulfate standard titration solution [c(NazS2Os)=1.000mol/L] in grams Clz）mass.
4.2.5 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 0.1%. 4.3 Determination of acid-insoluble matter content
4.3.1 Summary of method
The sample is dissolved in hydrochloric acid and nitric acid, and the insoluble matter is filtered, washed, dried and weighed. 4.3.2 Reagents and materials
4.3.2.1 Hydrochloric acid.
4.3.2.2 Nitric acid.
4.3.3 Instruments and equipment
Glass sand crucible: filter plate pore size: 5um~~15μm. 4.3.4 Analysis steps
Weigh (5±0.01)g of the sample in a beaker, add 20mL hydrochloric acid and 10mL water, and heat to dissolve it. Add 2 mL of nitric acid to the solution, heat to boiling, let stand for 3 to 5 minutes, add 20 mL of water, and heat in a boiling water bath for 1 hour. Filter with constant-weight glass sand, rinse the filter residue with 100 mL of water acidified with 5 drops of hydrochloric acid, and dry at 105℃ to 110℃ to constant weight. 4.3.5 Expression of analysis results
The acid-insoluble content (X) expressed as mass percentage is calculated according to formula (4): X = m=m2 ×100
-the mass of the acid-insoluble matter and the glass sand crucible after drying, g; where: mj—
the mass of the glass sand crucible after constant weight, g;
the mass of the sample, g.
4.3.6 Tolerance
(4)
The arithmetic mean of the parallel determination results is taken as the determination result. The absolute difference of parallel determination results shall not exceed 0.005% for superior products; and not exceed 0.02% for first-class products and qualified products.
4.4 Determination of iron content
4.4.1 Summary of method
Use nitric acid to convert all the iron in the sample into trivalent iron. The trivalent iron ions are hydrolyzed in an alkaline environment to form iron hydroxide precipitation, which is separated, dissolved, and colored with potassium thiocyanate, and then extracted with isoamyl alcohol for colorimetric comparison. 4.4.2
Reagents and materials
4.4.2.1 Nitric acid.
Ammonium chloride.
4.4.2.3 Ammonia water.
4.4.2.4 Isoamyl alcohol.
5 Ammonia solution: 2+3.
4.4.2.6 Sulfuric acid solution: 1+8.
Potassium thiocyanate solution: 100g/L.
4.4.2.8 Iron standard solution: 1mL of solution contains 0.01mgFe. Preparation: Use a pipette to transfer 10mL of the iron standard solution prepared according to GB/T602, place it in a 100mL volumetric flask, dilute with water to 896
scale, and shake well.
4.4.3 Analysis steps
HG/T2960—2000
Weigh (2±0.01)g of the sample, add 20mL of water, slowly add 3ml of nitric acid, and heat to boiling. Add 20mL of water and 3g of ammonium chloride and heat to boiling. Add ammonia solution under stirring until the precipitate is dissolved. Heat the solution in a boiling water bath for 1h, filter with a rapid qualitative filter paper, wash the filter residue with 100mL of a mixed solution containing 5mL of ammonia solution until the blue color on the filter paper disappears, and then wash it several times with hot water.
Use 5mL sulfuric acid solution to dissolve the residue on the filter paper, wash the filter paper several times with a small amount of water, collect the filtrate and washing solution in a 100mL volumetric flask, and dilute to the scale. After mixing, use a pipette to transfer 10mL to a colorimetric tube, add 4mL potassium thiocyanate solution and 10ml isoamyl alcohol. After sufficient shaking, the red color in the alcohol layer should not be deeper than the standard. The standard colorimetric solution is to transfer 1.00mL (superior, first-class) and 2.00mL (qualified) iron standard solution and treat it in the same way as the sample. 4.5 Determination of sulfate (in terms of SO) content 4.5.1 Summary of the method
In the hydrochloric acid medium, sulfate and barium ions generate white fine barium sulfate precipitates, which are suspended in the solution and compared with the standard turbidity solution. 4.5.2 Reagents and materials
4.5.2.1 Hydrogen peroxide.
4.5.2.2 Hydrochloric acid: 1+2.
4.5.2.3 Sodium chloride solution: 250g/L.
4.5.2.4 Sulfate standard solution: 1mL solution contains 0.1mgSO4.4.5.3 Analysis steps
4.5.3.1 Preparation of test solution
Weigh about (1±0.01)g of the sample, add 20mL of water and 3mL of hydrochloric acid solution, add 5mL of hydrogen peroxide, and heat. After dissolution, cool, filter, and wash. After the filtrate and washing solution are combined, transfer all to a 100mL volumetric flask, dilute with water to the scale, and shake. 4.5.3.2 Determination
Use a pipette to transfer 10mL of the test solution, place it in a 25mL colorimetric tube, add 10mL of water and 1mL of hydrochloric acid solution, keep warm at 30℃~35℃ for 10min, add 3mL of barium chloride solution, dilute with water to the scale, shake well, and let it stand for 30min. Its turbidity shall not be greater than that of the standard turbidity solution.
The standard turbidity solution is to use a pipette to take 0.50mL (superior product), 1.00mL (first-class product), and 3.00mL (qualified product) of sulfate standard solution, add 10mL of cuprous chloride solution without sulfate (preparation see Appendix A), and treat it in the same way as the test solution. 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 in accordance with the provisions of GB/T6678. 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 samples, put the collected samples directly into a clean and dry large glass bottle, seal it immediately, and immediately divide 1/4 of it (not less than 500g) into two clean and dry wide-mouth bottles after shaking the hook, and seal them. A label is attached to the bottle, indicating: manufacturer name, product name, batch number, sampling date and name of the sampler. One bottle is used for inspection and the other is kept for three months for future reference. 5.4 Industrial cuprous nitride shall be inspected by the quality supervision and inspection department of the manufacturer in accordance with the requirements of this standard. The manufacturer shall ensure that each batch of products shipped out of the factory meets the requirements of this standard.
5.5 The user has the right to inspect and accept the received cuprous chloride in accordance with the provisions of this standard. The inspection and acceptance shall be carried out within one month from the date of arrival of the goods.
5.6 If any index of the test result does not meet the requirements of this standard, samples should be taken from twice the amount of packaging for re-testing. If even one index of the re-test result does not meet the requirements of this standard, the whole batch of products shall be unqualified. 5.7 The rounded value comparison method specified in GB/T1250 shall be used to determine whether the test results meet the standards. 897
6 Marking and labeling
HG/T2960—2000
6.1 The packaging of industrial cuprous chloride shall be printed with firm and clear markings. The contents shall include: manufacturer name, address, product name, trademark, grade, net content, batch number or production date and this standard number, as well as the "wet-afraid" mark specified in GB191. 6.2 Each batch of products shipped out of the factory shall have a quality certificate. The contents shall include: manufacturer name, address, product name, trademark, 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 Industrial cuprous chloride is packaged in three layers, with a three-layer composite paper bag as the outer packaging and two layers of polyethylene film bags as the inner lining: one layer must be a black polyethylene film bag with a thickness of 0.08mm; the other layer of polyethylene film bag has a thickness of 0.07mm. The net content of each bag is 35kg and 50kg.
7.2 For industrial cuprous chloride packaging, the inner bag is tied with vinylon or a rope of equivalent quality, or sealed with other equivalent methods to ensure a tight seal. The composite paper bag packaging is sealed with a sewing machine. 7.3 Industrial cuprous chloride products should be stored in a well-ventilated environment and are prohibited from being mixed with oxides. 7.4 During transportation, industrial cuprous chloride products should be protected from sunlight and rain, and the packaging should be kept intact. It is prohibited to transport them together with oxides. 7.5 Under the storage and transportation conditions that meet this standard, the shelf life is three months, and re-sampling and inspection must be carried out after three months. 898
HG/T 2960—2000
Appendix A
(Standard Appendix)
Preparation of cuprous chloride fluoride solution without sulfate Weigh (1±0.01)g of the sample, add 20mL of water and 3mL of hydrochloric acid solution, add 5mL of hydrogen peroxide, heat, dissolve, and cool. Add water to about 30mL, add 10mL of hydrochloric acid solution, keep warm at 30℃～35℃ for 10min, transfer to a 100mL volumetric flask, add 8ml of barium chloride solution, dilute to the scale, shake the hook, and filter for 30min. The filtrate is the cuprous chloride solution without sulfate. 899
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