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Chemical Industry Standard of the People's Republic of China
HG2323-92
Industrial Zinc Chloride
Published on June 1, 1992
Ministry of Chemical Industry of the People's Republic of China
Implemented on September 1, 1992
WChemical Industry Standard of the People's Republic of China
Industrial Zinc Chloride
1 Subject Content and Scope of Application
HG2323--92
This standard specifies the technical requirements, test methods, inspection rules and marking, packaging, transportation and storage requirements for industrial zinc chloride. This standard applies to solid zinc chloride and zinc chloride solution produced by zinc or zinc oxide and industrial hydrochloric acid. This product is mainly used in industries such as batteries, activated carbon, welding flux, and papermaking. It can also be used as a dehydrating agent, condensing agent, and wood preservative in organic synthesis. Molecular formula: ZnC2
Relative molecular mass: 136.30 (according to the international relative atomic weight in 1989) 2 Reference standards
GB6678
GB6680
GB6682
3 Product classification
Chemical reagents
Preparation of standard solution for titration analysis (volume analysis) Chemical reagents
Preparation of standard solution for impurity determination
Chemical reagents
Preparation of preparations and products used in test methods General rules for sampling of chemical products
General rules for sampling of liquid chemical products
Laboratory water specifications
Industrial zinc chloride is divided into three types: Type I, Type II, and Type III. Type 3.11 is solid zinc chloride for battery industry; Type 3.2 is solid zinc chloride for general industry; Type 3.3I is zinc chloride solution, first-class products are used in battery industry, and qualified products are used in general industry. 4 Technical requirements
4.1 Appearance
Type I and Type II should be white powder or small particles; Type I should be a colorless and transparent aqueous solution. 4.2
Industrial zinc chloride shall meet the requirements of the following table:
Approved by the Ministry of Chemical Industry of the People's Republic of China on June 1, 1992 and implemented on September 1, 1992
Item
Zinc chloride (ZnCl2) content
Balic salt (as ZnO) content
Sulfate (as SO) content
Barium (Ba) content
Iron (Fe) content
Heavy metal (as Pb) content
Content of hydrochloric acid insoluble matter
Zinc sheet corrosion
5 Test method
HG2323-92
Superior product
Passed the test
Qualified product
% (m/m)
0.65~0.85
Qualified products
Passed the test
The reagents and water used in this standard, unless otherwise specified, refer to analytical pure reagents and grade 3 water specified in GB6682. The standard solutions, impurity standard solutions, preparations and products used in the test, unless otherwise specified, are prepared in accordance with the provisions of GB601, GB602 and GB603.
5.1 Determination of zinc chloride content
5.1.1 Summary of the method
Under acidic conditions, diphenylamine is used as an indicator and potassium ferrocyanide standard titration solution is used to titrate until the solution changes from blue-purple to yellow-green. The main reaction formula is:
2K,Fe(CN)s+3Zn+=KzZns(Fe(CN)),★+6K+5.1.2 Reagents and materials
5.1.2.1 Hydrochloric acid (GB622) solution: 1+1. 5.1.2.2
Sulfuric acid (GB625) solution: 1+3.
5.1.2.3 Ammonia (GB631) solution: 2+3. 5.1.2.4 Ammonium sulfate (GB1396) solution: 250g/L. Potassium ferrocyanide [K,Fe(CN). ·3H2O] 5.1.2.5
0.05mol/L.
Preparation and calibration:
(GB1273) standard titration solution: c【K,Fe（CN)） Weigh about 21.6g potassium ferrocyanide, 0.6g potassium ferrocyanide (GB644) and 0.2g anhydrous sodium carbonate (GB639) in a 400mL beaker, add water to dissolve, dilute with water to 1000mL, place in a brown bottle, place for one week, filter and calibrate with a crucible filter (filter plate pore size is 5-15μm). Potassium ferrocyanide standard titration solution should be calibrated at least once every two months; if there is precipitation in the solution, it must be re-filtered and calibrated.
Weigh about 1.7g of standard zinc oxide (GB1260) burned to constant weight at 800℃, accurate to 0.0002g, moisten with a little water, add hydrochloric acid solution until the sample dissolves, transfer to a 250mL volumetric flask, dilute to the scale, and shake well. Use a pipette to transfer 25mL, add 70mL of water, add ammonia solution until a white colloidal precipitate just forms, add 20mL of ammonium sulfate solution and 20mL of sulfuric acid solution, heat to 75-80℃, and titrate with potassium ferrocyanide standard titration solution. Add 2-3 drops of diphenylamine (5.1.2.6) indicator solution when it is close to the end point. When the solution is titrated to a sudden change from blue-purple to yellow-green, and no longer changes to blue-purple within 30S, it is the end point. The solution temperature must not be lower than 60℃ at the end point. Perform a blank test at the same time.
The actual concentration c of potassium ferrocyanide standard titration solution is calculated according to formula (1): x
C(V.-V)×0.1221-1.221(V,-V)
Wherein: m-mass of zinc oxide, g;
V1-volume of potassium ferrocyanide standard titration solution consumed in titration, mL; V-volume of potassium ferrocyanide standard titration solution consumed in blank test, mL; (1)
0.1221-mass of zinc oxide in grams equivalent to 1.00mL of potassium ferrocyanide standard titration solution c (K,Fe（CN)=1.000mol/L).
The result should be expressed to five decimal places,
5.1.2.6 Diphenylamine (GB681) sulfuric acid solution: 10g/L. Weigh 1.0g of diphenylamine and dissolve it in 100mL of concentrated sulfuric acid (GB625) under stirring. 5.1.3 Preparation of sample solution A
In a weighing bottle with a lid, quickly weigh about 3.5g of the sample, accurate to 0.0002g. Transfer the sample to a 250mL beaker, add 50mL of water and a few drops of hydrochloric acid solution (5.1.2.1) until the solution is clear, and then add 3 drops in excess. Transfer to a 250mL volumetric flask, dilute to the mark with water, and shake well.
5.1.4 Analysis steps
Use a pipette to transfer 25mL of test solution A (5.1.3), place it in a conical flask, add 70mL of water, and perform the following operations as described in Section 5.1.2.5, starting from "add ammonia water until a white colloidal precipitate just forms..." to "...simultaneously perform a blank test". 5.1.5 Expression of analysis results
The zinc chloride (ZnCl2) content (X) expressed as mass percentage is calculated according to formula (2): X19(V)0.2044×100-1.675X
204. 4c(V-Vo)-1.675X2
Wherein: c is the actual concentration of the potassium ferrocyanide standard titration solution, mol/L; V is the volume of the potassium ferrocyanide standard titration solution consumed in the titration, mL; V. ——The volume of potassium ferrocyanide standard titration solution consumed in the blank test, mL, m—mass of the sample, g;
X2—the content of basic salt (ZnO) expressed in mass percentage; (2)
0.2044—the mass of zinc chloride equivalent to 1.00mL of potassium ferrocyanide standard titration solution c[K,Fe(CN)g=1.000mol/L], expressed in grams;
1.675—the coefficient for converting zinc monoxide into zinc chloride. 5.1.6 Allowable difference
HG2323—92
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%. 5.2 Determination of basic salt content
5.2.1 Summary of method
Dissolve the sample in water and titrate with standard hydrochloric acid titration solution using methyl orange as the indicator. 5.2.2 Reagents and materials
5.2.2.1 Hydrochloric acid (GB622) standard titration solution: C (HCI) about 0.5 mol/L; 5.2.2.2 Methyl orange indicator solution: 1 g/L.
5.2.3 Analysis steps
In a weighing bottle with a lid, quickly weigh about 10 g of the sample to an accuracy of 0.01g, transfer to a 250mL conical flask, add 50mL water and 1-2 drops of methyl orange indicator solution, and titrate with hydrochloric acid standard titration solution until it turns orange. 5.2.4 Expression of analytical results
The basic salt (ZnO) content (X2) expressed as mass percentage is calculated according to formula (3): X2=cVX0. 040 70x
×1004.070c
Where: c——actual concentration of hydrochloric acid standard titration solution, mol/L; V—volume of hydrochloric acid standard titration solution consumed in titration, mL; m——mass of sample, g;
(3)
0.04070——mass of zinc oxide equivalent to 1.00mL hydrochloric acid standard titration solution [c(HC1)=1.000mol/L], expressed in grams.
5.2.5 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: 0.1% for type 1 and type I; 0.5% for straight type.
5.3 Determination of sulfate content
5.3.1 Summary of method
Under acidic conditions, sulfate ions are precipitated with barium chloride and visually compared with the barium sulfate standard turbidimetric solution. 5.3.2 Reagents and materials
5.3.2.1 Hydrochloric acid (GB622) solution: 1+1; 5.3.2.2 95% ethanol (GB671);
5.3.2.3 Barium chloride (GB652) solution: 100g/L; 5.3.2.4 Sulfate standard solution: 0.1mgSO/mL. 5.3.3 Preparation of test solution B
In a weighing bottle with a lid, quickly weigh 10.00g of the sample, accurate to 0.01g, and place it in a 100mL beaker. Add 40mL of water and a few drops of hydrochloric acid solution until the solution is clear, then add 3 drops in excess, transfer to a 100mL volumetric flask, dilute to the mark with water, and shake for later use. 5.3.4 Analysis steps
Use a pipette to transfer 20mL of test solution B (5.3.3) into a 50mL colorimetric tube, add 1mL of hydrochloric acid solution and 3mL of 95% ethanol, then add 5mL of barium chloride solution, add water to the mark, shake well, and let stand for 30min. The turbidity presented shall not be deeper than that of the standard turbidity solution.
Preparation of standard turbidity solution: Take a certain volume of sulfate standard solution according to the following regulations and treat it in the same way as the sample. Type I superior and first-class products——2mL
First-class products——2mL
Qualified products——10mL
Superior and qualified products——0.8mL
W.bzsoso.coI5.4 Determination of barium content
5.4.1 Summary of the method
HG2323—92
Use sulfuric acid to precipitate the barium ions in the test solution and compare the turbidity with the standard turbidimetric solution of barium sulfate visually. 5.4.2 Reagents and materials
5.4.2.1 Sulfuric acid (GB625) solution: 1+3; 5.4.2.2 95% ethanol (GB671);
5.4.2.3 Barium standard solution: 0.1mgBa/mL. 5.4.3 Analysis steps
Use a pipette to transfer 5 mL of test solution B (5.3.3) into a 50 mL colorimetric tube, add 3 mL of 95% ethanol and 1 mL of sulfuric acid solution, dilute to the mark with water, shake well, and let stand for 30 minutes. The turbidity presented shall not be deeper than that of the standard turbidity solution. Preparation of standard turbidity solution: Take a certain volume of lock standard solution according to the following regulations and treat it in the same way as the test sample. Type I superior and first-class products - 5 mL
First-class products - 5 mL
Qualified products - 10 mL
Type I first-class products and qualified products - 2 mL
5.5 Determination of iron content
5.5.1 Summary of method
In an acidic medium, oxidize divalent iron with ammonium persulfate, add ammonium thiocyanate to develop color, extract with n-butanol, and compare visually with the standard colorimetric solution.
5.5.2 Reagents and materials
5.5.2.1 Hydrochloric acid (GB622) solution: 1+1; 5.5.2.2 Ammonium persulfate (GB655);
5.5.2.3 Ammonium thiocyanate (GB660) solution: 250g/L; 5.5.2.4 n-Butanol (HG3-1012);
5.5.2.5 Iron standard solution: 0.01mgFe/mL, prepared before use. Use a pipette to transfer 10mL of the iron standard solution prepared according to GB602, place it in a 100mL volumetric flask, dilute to the mark with water, and shake well.
5.5.3 Analysis steps
Use a pipette to transfer 10 mL of test solution B (5.3.3) into a 50 mL colorimetric tube, add 10 mL of water, 1 mL of hydrochloric acid solution, and 30 mg of ammonium persulfate, and shake well. Add 5 mL of ammonium thiocyanate solution and extract with 10 mL of n-butanol. The red color of the alcohol layer should not be darker than that of the standard colorimetric solution.
Preparation of standard colorimetric solution: Take a certain volume of iron standard solution according to the following regulations and treat it in the same way as the test sample. Type I superior and first-class products—0.5mL
Type I first-class products—1mL
Qualified products—2mL
Type I—first-class products—0.2mL
Qualified products—0.4mL
5.6 Determination of heavy metal content
5.6.1 Summary of the method
Under alkaline conditions, sodium cyanide (or potassium cyanide) is used to mask interfering ions, sodium sulfide is used to react with heavy metal ions such as lead, and visual colorimetric comparison is carried out with the standard colorimetric solution.
5.6.2 Reagents and materialsWww.bzxZ.net
5.6.2.1 Ammonia (GB631) solution: 2+3; 5
W.bzsoso.coIHG2323—92
5.6.2.2 Sodium cyanide (or potassium cyanide) solution: 200g/L5.6.2.3 Sodium sulfide (HG3-905) solution: 100g/L; 5.6.2.4 Lead standard solution: 0.01mgPb/mL, prepared before use. Use a pipette to transfer 10mL of the lead standard solution prepared according to GB602, place it in a 100mL volumetric flask, dilute to the mark with water, and shake well.
5.6.3 Analysis steps
Use a pipette to transfer 15mL of test solution B (5.3.3) into a 50mL colorimetric tube, neutralize with ammonia solution (pH is about 8.5), then add 20mL of sodium cyanide (or potassium cyanide) solution, and finally add 1mL of newly prepared sodium sulfide solution, shake well, and let stand for 10 minutes. The color should not be darker than the standard colorimetric solution. Preparation of standard colorimetric solution: Transfer 5mL of test solution B (5.3.3), and take a certain volume of lead standard solution according to the following provisions, and treat it in the same way as the test sample.
Type I superior product, first-class product—0.5mL
—Superior product—1mL
Qualified product—2mL
Qualified product—0.2mL
Qualified product—0.4mL
Treat the waste liquid after determination according to the provisions of Appendix A. 5.7 Determination of hydrochloric acid insoluble matter
5.7.1 Summary of method
Dissolve the sample in 80-90℃ hot water, add hydrochloric acid, filter with a crucible filter, wash, dry and weigh. 5.7.2 Reagents and materials
5.7.2.1 Hydrochloric acid (GB622) solution: 1+15.7.2.2 Silver nitrate (GB670) solution: 50g/L. 5.7.3 Instruments and equipment
5.7.3.1 Type filter: the pore size of the filter plate is 5~15μm. 5.7.4 Analysis steps
Use a weighing bottle to quickly weigh about 20g of type 1 sample, accurate to 0.01g, place it in a 250mL beaker, add 150mL of 80-90℃ hot water and 20mL of hydrochloric acid solution, and shake well. Filter with a crucible filter that has been dried to constant weight at 100-110°C in advance, and wash with hot water until the filtrate contains no chloride ions (CI-) (check with silver nitrate solution). Move the crucible filter together with the insoluble matter into an electric drying oven and dry at 100-110°C to constant weight. 5.7.5 Expression of analysis results
The hydrochloric acid insoluble matter content (Xs) expressed as mass percentage is calculated according to formula (4): Xs=ml=m2×100
Where: m1——the mass of the crucible filter together with the insoluble matter, g; m2——the mass of the crucible filter, g;
m——the mass of the sample, g.
5.7.6 Allowable difference
The arithmetic mean of the parallel determination results is taken as the determination result; the absolute difference of the parallel determination results shall not exceed 0.005%. 5.8 Zinc sheet corrosion
5.8.1 Reagents and materials
5.8.1.1 Water sandpaper particle size 140 mesh.
5.8.1.2 Zinc sheet (GB1978): XD2 grade. 5.8.2 Analysis steps
HG2323-92
Weigh 25g of type 1 sample, accurate to 0.01g, place in a 100mL beaker, add 25mL of water, and transfer to a 50mL colorimetric tube; or measure 50mL of type 1 first-class sample and place in a colorimetric tube. Cut the zinc sheet with the surface cleaned with sandpaper into 40mm×8mm, with the lower end at an angle of 45°, place it in the test solution, and keep it in a boiling water bath for 1h. It is qualified when there is no obvious black shadow on the surface of the zinc sheet. 5.9 Determination of pH value
5.9.1 Instruments and equipment
5.9.1.1 Acidity meter: the graduation value is 0.02pH unit and is equipped with a glass measuring electrode and a saturated calomel reference electrode. 5.9.2 Analysis steps
Measure 100mL of type 1 sample, place in a 150mL beaker, and measure with an acidity meter. 5.9.3 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 0.1 pH unit. 6 Inspection rules
6.1 Industrial zinc chloride shall be inspected by the quality supervision and inspection department of the manufacturer in accordance with the provisions of this standard. The manufacturer shall ensure that all products leaving the factory meet the requirements of this standard.
Each batch of products leaving the factory shall be accompanied by a quality certificate, which shall include: manufacturer name, product name, model, grade, batch number, net weight, production date, proof that the product quality meets this standard and the number of this standard. 6.2 The user has the right to inspect and accept the industrial zinc chloride received in accordance with the provisions of this standard. The quality of zinc chloride products shall be inspected within 10 days from the date of receipt of the goods.
6.3 Each batch of zinc chloride products shall not exceed 5t.
6.4 The number of sampling units for sampling of solid zinc chloride shall be determined in accordance with Article 6.6 of GB6678. When sampling, remove the upper layer of the sample with a thickness of about 5 cm, and insert the sampler vertically from the center of the packaging unit to 34 points of the material layer depth to take samples. After mixing the sample, use the alternating shovel method to reduce it to no less than 500g.
The sampling of zinc chloride solution shall be carried out in accordance with Article 2.1 of GB6680, and the sampling volume shall be no less than 500g. The collected samples shall be divided into two clean, dry, and ground-mouth stoppered reagent bottles and sealed. Labels shall be attached to the reagent bottles, indicating the manufacturer's name, product name, model, grade, batch number, sampling date and the name of the sampler. One bottle is for inspection and the other bottle is for reference. The shelf life is 3 months.
6.5 If one of the indicators of the inspection results does not meet the requirements of this standard, re-sampling shall be carried out from twice the amount of packaging units for verification. If even one of the indicators of the verification results does not meet the requirements of this standard, the entire batch of products cannot be accepted. 6.6 When the supply and demand parties have objections to the product quality, they can handle it in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection". 7 Marking, packaging, transportation and storage
7.1 The packaging container should have firm and clear markings, indicating the manufacturer's name, product name, model, grade, net weight, batch number or production date, trademark and the number of this standard. 7.2 Industrial solid zinc chloride should be packaged in galvanized iron drums lined with high-density polyethylene bags, with an iron sheet thickness of 0.5mm; it can also be packaged in plastic drums, cardboard drums or composite plastic woven bags lined with high-density polyethylene bags. The net weight of each packaging unit is 50kg or 25kg. Industrial zinc chloride solution should be packaged in plastic drums or steel tank trucks coated with anti-corrosion materials such as acid-resistant paint. 7.3 Industrial zinc chloride should be covered during transportation to prevent rain and moisture, and should not be mixed with feed and food. 7.4 Industrial solid zinc chloride should be stored in a dry and ventilated warehouse to avoid open-air storage. Industrial zinc chloride solution should be stored in special steel storage tanks and tank trucks. 7.5 The storage period of galvanized iron barrels, cardboard barrels and plastic barrels for type I and I products is 6 months, and the storage period of composite plastic woven bags is 2 months; the storage period of type II products is 2 months, both starting from the date of production. 7
W.bzsoso.coIHG2323—92
Appendix A
Treatment of cyanide waste liquid
In order to prevent the pollution of cyanide waste liquid, the cyanide waste liquid analyzed every day should be post-treated before discharge. A1 Method Summary
Under alkaline conditions, divalent iron and cyanide ions form stable complex ions. A2
Operation Steps
Collect the waste liquid in a 500mL beaker, add 50mL200g/L ferrous sulfate solution, stir, and discharge after sufficient reaction. The above-mentioned reagents are all industrial grade.
Additional Notes:
This standard was proposed by the Science and Technology 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. This standard was drafted by the Tianjin Chemical Research Institute of the Ministry of Chemical Industry, Tianjin Hongguang Chemical Plant and Dalian Jinguang Chemical Plant. The main drafters of this standard are Li Wenqiang, Su Peiji, Fan Ruilan, Wang Jiami, Shen Zhengjia and Yang Zhaohui. This standard adopts the Japanese Industrial Standard JIS K1428-58 (confirmed in 1985) "Zinc Chloride". From the date of implementation of this standard, the original National Standard of the People's Republic of China GB1625-79 "Zinc Chloride" shall be invalid. W.coIHG2323—92
Appendix A
Treatment of cyanide waste liquid
In order to prevent the pollution of cyanide waste liquid, the cyanide waste liquid analyzed every day should be post-treated before discharge. A1 Method Summary
Under alkaline conditions, divalent iron and cyanide ions form stable complex ions. A2
Operation steps
Collect the waste liquid in a 500mL beaker, add 50mL200g/L ferrous sulfate solution, stir, and discharge after sufficient reaction. The above-mentioned reagents are all industrial grade.
Additional remarks:
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Tianjin Chemical Research Institute of the Ministry of Chemical Industry. This standard is drafted by Tianjin Chemical Research Institute of the Ministry of Chemical Industry, Tianjin Hongguang Chemical Plant and Dalian Jinguang Chemical Plant. The main drafters of this standard are Li Wenqiang, Su Peiji, Fan Ruilan, Wang Jiami, Shen Zhengjia and Yang Zhaohui. This standard adopts the Japanese Industrial Standard JIS K1428-58 (confirmed in 1985) "Zinc Chloride". From the date of implementation of this standard, the original National Standard of the People's Republic of China GB1625-79 "Zinc Chloride" will be invalid. W.coIHG2323—92
Appendix A
Treatment of cyanide waste liquid
In order to prevent the pollution of cyanide waste liquid, the cyanide waste liquid analyzed every day should be post-treated before discharge. A1 Method Summary
Under alkaline conditions, divalent iron and cyanide ions form stable complex ions. A2
Operation steps
Collect the waste liquid in a 500mL beaker, add 50mL200g/L ferrous sulfate solution, stir, and discharge after sufficient reaction. The above-mentioned reagents are all industrial grade.
Additional remarks:
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Tianjin Chemical Research Institute of the Ministry of Chemical Industry. This standard is drafted by Tianjin Chemical Research Institute of the Ministry of Chemical Industry, Tianjin Hongguang Chemical Plant and Dalian Jinguang Chemical Plant. The main drafters of this standard are Li Wenqiang, Su Peiji, Fan Ruilan, Wang Jiami, Shen Zhengjia and Yang Zhaohui. This standard adopts the Japanese Industrial Standard JIS K1428-58 (confirmed in 1985) "Zinc Chloride". From the date of implementation of this standard, the original National Standard of the People's Republic of China GB1625-79 "Zinc Chloride" will be invalid. W.
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