Some standard content:
Chemical Industry Standard of the People's Republic of China
Industrial Potassium Persulfate
1 Subject Content and Scope of Application
HG/T 2155-91
This standard specifies the technical requirements, test methods, inspection rules, marking, packaging, transportation and storage of industrial potassium persulfate. This standard applies to industrial potassium persulfate produced by electrolysis. This product is mainly used in rubber, plastics, petroleum extraction and reagent industries. Molecular formula: K, S20g
Relative molecular mass: 270.32 (according to the international relative atomic mass of 1987)2
Cited standards
GB 190
GB 601
GB 602
GB3049
GB6678
GB 6682
3Technical requirements
Dangerous goods packaging marking
Pictorial marking for packaging, storage and transportation
Chemical reagentsPreparation of standard solution for titration analysis (volume analysis)Preparation of standard solution for impurity determination
Chemical reagents
Preparation of preparations and products used in test methodsChemical reagents
General method for determination of iron content in chemical productsO-phenanthroline spectrophotometric methodGeneral rules for sampling of chemical products
Specifications for laboratory water
AppearanceWhite crystalline powder.
Industrial potassium persulfate shall meet the requirements of Table 1:
Potassium persulfate (K2S20g) content, %
Free acid (in H,SO.) content, %
Iron (Fe) content, %
Chloride (in CI) content, %
Ammonium salt (in NH.) content, %
Water content, %
Approved by the Ministry of Chemical Industry of the People's Republic of China on September 16, 1991Superior product
First-class product
Qualified product
Implemented on January 1, 1992
4Test method
HG/T 2155—91
The reagents and water used in this standard, unless otherwise specified, refer to analytically pure reagents and grade water specified in GB6682. The standard solutions, impurity standard solutions, preparations and products required in the test, unless otherwise specified, shall be prepared in accordance with the provisions of GB601, GB602 and GB603.
4.1 Determination of potassium persulfate content
4.1.1 Summary of method
Potassium iodide is reacted with potassium persulfate to generate free iodine, which is titrated with sodium thiosulfate standard titration solution in a weakly acidic solution with starch as an indicator.
4.1.2 Reagents and materials
4.1.2.1 Potassium iodide (GB1272);
4.1.2.2 Glacial acetic acid (GB676) solution: 1+2;4 .1.2.3 Sodium thiosulfate (GB637) standard titration solution: c (NazS, O.) about 0.1 mol/L; 4.1.2.4 Soluble starch: 5g/1. Indicator solution. 4.1.3 Analysis steps
Weigh about 0.5g of sample, accurate to 0.0002g, put it in an iodine volumetric flask, dissolve it with 30mL of water, add 4g of potassium iodide, cover, shake well, and place in a dark place for 30min. Add 2mL of acetic acid solution and 25ml. of water, titrate with sodium thiosulfate standard titration solution, when the titration is close to the end point, add 3mL of starch indicator solution, and continue to titrate until the blue color of the solution disappears as the end point. Perform a blank test at the same time.
4.1.4 Expression of analysis results
The potassium persulfate content (X1) expressed as mass percentage is calculated according to formula (1): c(V- Vo) × 0. 135 2 × 100 = X
Wherein: V—
13. 52 × c(V - Vo)
The volume of sodium thiosulfate standard titration solution consumed by the sample, mL; V. - The volume of sodium thiosulfate standard titration solution consumed by the blank test, mL. c—The actual concentration of sodium thiosulfate standard titration solution, mol/L; m——The mass of the sample, g;
0.1352—The mass of potassium persulfate equivalent to 1.00mL sodium thiosulfate standard titration solution c(NazS,O,)-1.000mol/L) in grams.
The result should be expressed to one decimal place.
4.1.5 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.2%, and the arithmetic mean shall be taken as the determination result. 4.2 Determination of free acid content
4.2.1 Method summary
Dissolve the sample in water, use methyl red as the indicator, and titrate with sodium hydroxide standard titration solution. 4.2.2 Reagents and materials
4.2.2.1 Standard titration solution of sodium hydroxide (GB629): c (NaOH) is about 0.01 mol/L, prepared before use. Use a pipette to transfer 10 mL of the standard titration solution of c (NaOH) about 0.1 mol/L prepared and calibrated according to GB601, place it in a 100 mL volumetric flask, dilute to the scale with carbon dioxide-free water, and shake well. 4.2.2.2 Methyl red (HG3--958) indicator solution: 1 g/I. 4.2.3 Analysis steps
Weigh 1 g of sample accurately to 0.01 g, place in a conical flask, add 100 mL of carbon dioxide-free water to dissolve it, add 2 drops of methyl red indicator solution, and titrate with sodium hydroxide standard titration solution until the solution turns yellow. 368
4.2.4 Expression of analysis results
HG/T 2155-91
The free acid content (in terms of H2SO4) expressed as a mass percentage (X,) is calculated according to formula (2): CV × 0.049 04 × 100 = 4
Formula: V—volume of sodium hydroxide standard titration solution consumed by the sample, mL; actual concentration of sodium hydroxide standard titration solution, mol/l-
m——mass of the sample, g;
0.049 04--
(2)
The mass of sulfuric acid equivalent to 1.00mL sodium hydroxide standard titration solution [c (NaOH) - 1.000mol/L), expressed in grams.
The result should be expressed to two decimal places.
4.2.5 Allowable difference
The difference between two parallel determination results shall not exceed 0.03%, and the arithmetic mean shall be taken as the determination result. 4.3 Determination of iron content
4.3.1 Method summary
Same as Article 2 of GB3049.
4.3.2 Reagents and materials
Same as Article 3 of GB3049.
4.3.3 Instruments and equipment
4.3.3.1 Porcelain evaporation blood: volume is about 50mL4.3.3.2 Spectrophotometer: with an absorption cell with a thickness of 3cm. 4.3.4 Analysis steps
4.3.4.1 Drawing of working curve
According to Article 5.3 of GB3049, an absorption cell with a thickness of 3cm and its corresponding amount of iron standard solution are selected to draw the working curve. 4.3.4.2 Determination
Weigh 1g of sample, accurate to 0.01g, place in porcelain evaporator III, add a small amount of water to moisten, cover the surface with blood, slowly heat to 1000 on an electric furnace, and continue to heat until the sample is completely melted, and cool. Add about 20mL of water, heat to dissolve the residue, and cool to room temperature. In a 100ml beaker, add an appropriate amount of water to make a blank test solution. The following is in accordance with Article 5.4 of GB3049, starting from "adjusting the pH to about 2 with hydrochloric acid solution or ammonia water" to "measuring the absorbance of the test solution and reagent blank solution".
4.3.5 Expression of analysis results
The iron (Fe) content (X,) expressed as mass percentage is calculated according to formula (3): m-mo
0. 1(m-mo)
×100=
m × 1 000
-The mass of iron found from the working curve based on the measured absorbance of the test solution, mg; where: m-
m——~The mass of iron found from the working curve based on the measured absorbance of the blank solution, mg; m—The mass of the sample, g.
The result should be expressed to three decimal places.
4.3.6 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.0005%, and the arithmetic mean shall be taken as the determination result. 4.4 Determination of fluoride content
4.4.1 Method summary
In an acidic solution, silver nitrate and chloride are used to generate a white silver chloride precipitate, which is compared with a standard turbidity solution. 4.4.2 Reagents and materials
· (3)
4.4.2.1 Silver nitrate (GB 670) solution: 10 g/L; 4.4.2.2 95% ethanol (GB 679);
4.4.2.3 Nitric acid (GB626) solution: 1+6; HG/T 2155—91
4.4.2.4 Chloride standard solution: 0.0100mgC1/mL, prepared before use. Use a pipette to transfer 10mL of the chloride standard solution prepared according to GB602, place it in a 100mL volumetric flask, dilute it to the mark with water, and shake it well.
4.4.3 Instruments and equipment
4.4.3.1 Colorimetric tube: volume 50mL.
4.4.4 Analysis steps
Weigh 0.5g of the sample, accurate to 0.01g, place it in a beaker, add appropriate amount of water to dissolve it, transfer the solution completely to the colorimetric tube, add 1mL of ethanol, 1mL of nitric acid solution and 2mL of silver nitrate solution, dilute to the mark, shake it well, and let it stand for 10min. Its turbidity shall not be deeper than that of the standard turbidity solution.
The preparation of standard turbidity solution is to take a certain volume of chloride standard solution according to the following regulations and treat it in the same way as the test sample. Superior product ￥2.5mL,
First-class product 5.0mL;
Qualified product 7.5mL.
4.5 Determination of ammonium salt content
4.5.1 Method summary
In alkaline solution, Nessler's reagent is used to react with free ammonia or bound ammonium to form a pale yellow to brownish red insoluble compound, which is visually compared with the standard colorimetric solution.
4.5.2 Reagents and materials
4.5.2.1 Sodium hydroxide (GB629) solution: 100g/L, 4.5.2.2 Nessler's reagent;
4.5.2.3 Ammonium standard solution: 0.001mgNH/mL, prepared before use. Use a pipette to transfer 10mL of the ammonium standard solution prepared according to GB602, place it in a 1000mL volumetric flask, dilute with water to the mark, and shake well. bZxz.net
4.5.3 Instruments and equipment
4.5.3.1 Colorimetric tube: volume 50mL.
4.5.4 Analysis steps
Weigh 1g of the sample, accurate to 0.01g, place it in a beaker, and add appropriate amount of water to dissolve it. Transfer the solution completely to a 200mL volumetric flask, dilute to the mark, and shake well.
Use a pipette to transfer 0.2mL of the test solution, place it in a colorimetric tube, add water to about 25mL, add 2mL of sodium hydroxide solution, 2ml of Nessler's reagent, dilute to the mark, and shake well. Its color shall not be darker than that of the standard colorimetric solution. The preparation of the standard colorimetric solution is to take a certain volume of the ammonium standard solution according to the following regulations and treat it in the same way as the test sample. 5mL for superior products; 7mL for inferior products; 9mL for qualified products.
4.6 Determination of moisture
4.6.1 Instruments and equipment
4.6.7.1 Weighing bottle: 50×30mm.
4.6.2 Analysis steps
Use a weighing bottle that has been dried to constant weight at 70~75℃, weigh about 5g of the sample, accurate to 0.0002g, place it in an electric drying oven, and dry it at 70~75℃ to constant weight.
4.6.3 Expression of analysis results
HG/T 2155-91
The moisture content (X) expressed as a mass percentage shall be calculated according to formula (4): 100(mi m2)
Wherein: m,-mass of the sample and weighing bottle before drying, g; m2-mass of the sample and weighing bottle after drying, g; m-mass of the sample, g.
The result shall be expressed to two decimal places.
4.6.4 Allowable error
The difference between the results of two parallel determinations shall not exceed 0.03%, and the arithmetic mean shall be taken as the determination result. 5 Inspection rules
(4)
5.1 Industrial potassium persulfate 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. The contents include: manufacturer name, product name, grade, batch number, net weight, production date, proof that product quality complies with this standard and the number of this standard. 5.2 The user has the right to inspect and accept the industrial potassium persulfate received in accordance with the provisions of this standard. 5.3 Each batch of products shall not exceed 10t.
5.4 Determine the number of sampling units in accordance with Article 6.6 of GB6678. When sampling, insert the sampler vertically from the center of the packaging bag to 3/4 of the depth of the material layer to take the sample. Mix the collected samples, reduce them to no less than 500g by quartering method, and pack them in two clean, dry wide-mouth bottles with ground stoppers and seal them. Stick labels on the bottles, indicating: manufacturer name, product name, grade, 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. 5.5 If one of the indicators in the test results does not meet the requirements of this standard, samples should be taken from twice the amount of packaging units for verification. If even one of the indicators in the verification results does not meet the requirements of this standard, the entire batch of products cannot be accepted. 5.6 When the supply and demand parties have objections to the product quality, they should handle it in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection". 6 Marking, packaging, transportation and purchase and storage
6.1 The outer packaging of industrial potassium persulfate should be printed with firm and clear markings, indicating: manufacturer name, product name, grade, net weight, gross weight, batch number or production date, trademark, this standard number and the oxidant mark specified in GB190 and the heat-resistant mark and moisture-resistant mark specified in GB191. Export products shall be printed with markings according to foreign trade requirements. 6.2 Industrial potassium persulfate shall be packaged in steel drums or wooden boxes lined with plastic bags or two layers of kraft paper bags, or in composite plastic woven bags lined with plastic bags. The inner and outer packaging shall be sealed. The net weight of each packaging unit is 25kg or 50kg. 6.3 Industrial potassium persulfate should not be stored or transported together with flammable, explosive and reducing substances. During transportation and storage, it should be covered to prevent moisture.
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 and Tianjin Oriental Chemical Plant. The main drafters of this standard are Li Jingge and Wang Yonglin. 3711 Weighing bottle: 50×30mm.
4.6.2 Analysis steps
Use a weighing bottle that has been dried to constant weight at 70~75℃, weigh about 5g of sample, accurate to 0.0002g, place it in an electric drying oven, and dry it at 70~75℃ to constant weight.
4.6.3 Expression of analysis results
HG/T 2155-91
The moisture content (X) expressed as mass percentage is calculated according to formula (4): 100(mi m2)
Where: m,-the mass of the sample and weighing bottle before drying, g; m2-the mass of the sample and weighing bottle after drying, g; m-the mass of the sample, g.
The result should be expressed to two decimal places.
4.6.4 Allowable error
The difference between the results of two parallel determinations shall not exceed 0.03%, and the arithmetic mean shall be taken as the determination result. 5 Inspection rules
(4)
5.1 Industrial potassium persulfate 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. The contents shall include: manufacturer name, product name, grade, batch number, net weight, production date, certificate of product quality in accordance with this standard and this standard number. 5.2 The user has the right to inspect and accept the industrial potassium persulfate received in accordance with the provisions of this standard. 5.3 Each batch of products shall not exceed 10t.
5.4 Determine the number of sampling units in accordance with the provisions of Article 6.6 of GB6678. When sampling, insert the sampler vertically from the center of the packaging bag to 3/4 of the depth of the material layer to take the sample. Mix the collected samples, and use the quartering method to reduce them to no less than 500g, and pack them into two clean, dry wide-mouth bottles with ground 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 for inspection, and the other bottle is kept for three months for reference. 5.5 If one indicator of the inspection result does not meet the requirements of this standard, re-sampling should be carried out from twice the amount of packaging units for verification. Even if one indicator of the verification result does not meet the requirements of this standard, the entire batch of products cannot be accepted. 5.6 When the supply and demand parties have objections to the product quality, they should handle it in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection". 6 Marking, packaging, transportation and purchase and storage
6.1 The outer packaging of industrial potassium persulfate should be printed with firm and clear markings, indicating: manufacturer name, product name, grade, net weight, gross weight, batch number or production date, trademark, this standard number and the oxidant mark specified in GB190 and the heat-sensitive mark and moisture-sensitive mark specified in GB191. Export products shall be printed with markings according to foreign trade requirements. 6.2 Industrial potassium persulfate shall be packaged in steel drums or wooden boxes lined with plastic bags or two layers of kraft paper bags, or in composite plastic woven bags lined with plastic bags. The inner and outer packaging shall be sealed. The net weight of each packaging unit is 25kg or 50kg. 6.3 Industrial potassium persulfate should avoid being mixed with flammable, explosive and reducing substances. During transportation and storage, it should be covered to prevent moisture.
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 Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by Tianjin Chemical Research Institute of the Ministry of Chemical Industry and Tianjin Oriental Chemical Factory. The main drafters of this standard are Li Jingge and Wang Yonglin.1 Weighing bottle: 50×30mm.
4.6.2 Analysis steps
Use a weighing bottle that has been dried to constant weight at 70~75℃, weigh about 5g of the sample, accurate to 0.0002g, place it in an electric drying oven, and dry it at 70~75℃ to constant weight.
4.6.3 Expression of analysis results
HG/T 2155-91
The moisture content (X) expressed as mass percentage is calculated according to formula (4): 100(mi m2)
Where: m, - the mass of the sample and weighing bottle before drying, g; m2 - the mass of the sample and weighing bottle after drying, g; m - the mass of the sample, g.
The result should be expressed to two decimal places.
4.6.4 Allowable error
The difference between two parallel determination results shall not exceed 0.03%, and the arithmetic mean shall be taken as the determination result. 5 Inspection rules
(4)
5.1 Industrial potassium persulfate 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. The content shall include: manufacturer name, product name, grade, batch number, net weight, production date, certificate of product quality in accordance with this standard and this standard number. 5.2 The user unit has the right to inspect and accept the industrial potassium persulfate received in accordance with the provisions of this standard. 5.3 Each batch of products shall not exceed 10t.
5.4 Determine the number of sampling units in accordance with the provisions of Article 6.6 of GB6678. When sampling, insert the sampler vertically from the center of the packaging bag to 3/4 of the depth of the material layer to take the sample. Mix the collected samples, and use the quartering method to reduce them to no less than 500g, and pack them into two clean, dry, wide-mouth bottles with ground 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 for inspection, and the other bottle is kept for three months for reference. 5.5 If one indicator of the inspection result does not meet the requirements of this standard, re-sampling should be carried out from twice the amount of packaging units for verification. Even if one indicator of the verification result does not meet the requirements of this standard, the entire batch of products cannot be accepted. 5.6 When the supply and demand parties have objections to the product quality, they should handle it in accordance with the provisions of the "Interim Measures for National Product Quality Arbitration Inspection". 6 Marking, packaging, transportation and purchase and storage
6.1 The outer packaging of industrial potassium persulfate should be printed with firm and clear markings, indicating: manufacturer name, product name, grade, net weight, gross weight, batch number or production date, trademark, this standard number and the oxidant mark specified in GB190 and the heat-sensitive mark and moisture-sensitive mark specified in GB191. Export products shall be printed with markings according to foreign trade requirements. 6.2 Industrial potassium persulfate shall be packaged in steel drums or wooden boxes lined with plastic bags or two layers of kraft paper bags, or in composite plastic woven bags lined with plastic bags. The inner and outer packaging shall be sealed. The net weight of each packaging unit is 25kg or 50kg. 6.3 Industrial potassium persulfate should avoid being mixed with flammable, explosive and reducing substances. During transportation and storage, it should be covered to prevent moisture.
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 Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by Tianjin Chemical Research Institute of the Ministry of Chemical Industry and Tianjin Oriental Chemical Factory. The main drafters of this standard are Li Jingge and Wang Yonglin.
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