Some standard content:
National Standard of the People's Republic of China
Chloroic acid
Potassium
Industry
Industry
Potassium chlorate for industrial use Subject content and scope of application
1
GB752-94
replaces GB752-85
This standard specifies the technical requirements for industrial potassium chlorate. Test methods, inspection rules and marking, packaging, transportation and storage. This standard applies to industrial potassium chlorate. This product is mainly used in matches and fireworks industry. Molecular formula: KC1O3
Relative molecular mass: 122.55 (according to the 1989 international relative atomic mass) 2 reference standards
GB190
GB191
Dangerous goods packaging mark||tt| |Packaging, storage and transportation pictorial mark
GB/T601
GB/T602
GB/T603bzxZ.net
GB1250
Chemical reagent titration analysis (capacity analysis) Preparation of chemical reagents for use in standard solutions Preparation of standard solutions for impurity determination Chemical reagents Test methods Methods for expressing and judging preparation limit values ??of preparations and products used GB/T3049
GB/T3051
Chemical Industry General method for determination of iron content in products phenanthroline spectrophotometry
General method for determination of chloride content in inorganic chemical products Mercury method test sieve
GB6003
GB/T6678| |tt||General principles for sampling of chemical products
GB/T6682
Analytical laboratory water specifications and test methods 3 technical requirements
3.1 Appearance: white powder.
3.2 Industrial potassium chlorate should comply with the requirements in the following table: Item
Potassium chlorate content, %
Moisture content, %
Water-insoluble matter content, %
Nitride (calculated as CI) content, %
bromate (calculated as BrO,) content, %
acid salt (calculated as SO,) content, %
iron (Fe) Content, %
Screen residue (125μm test sieve), %
National Bureau of Technical Supervision 1994-12-22 approved project
refers to
superior product||tt ||99.5
0.05
0.03
0. 02
0.03
0.01
0.003
0.5||tt ||Standard
First-class product
99.2
0.10
0.10
0.03
0.08
0.03||tt ||0.005
1.0
Implemented on 1995-10-01
4 test methods
GB752-94
The reagents and water used in this standard are not When other requirements are noted, they refer to analytical grade reagents and grade three water specified in GB/T6682. : The standard titration solutions, impurity standard solutions, preparations and products required in the test shall be prepared in accordance with the provisions of GB/T601, GB/T602 and GB/T603 unless other regulations are noted. 4.1 Determination of potassium nitrate content
4.1.1 Method summary
Use a known amount (excess) of iron (1) salt to reduce chlorate, using sodium diphenylamine sulfonate as the indicator, Titrate excess iron(I) salt with standard titration solution of potassium dichromate.
4.1.2 Reagents and materials
4.1.2.1 Sulfuric acid (GB625);
4.1.2.2 Phosphoric acid (GB1282);
4.1.2.3 Ferrous ammonium sulfate ( GB/T661): c[(NH),Fe(SO,),J is about 0.1mol/L solution; 4.1.2.4 Potassium dichromate (GB/T642): c(K.Cr2O,) is about 0.1mol/L Standard titration solution; 4.1.2.5 Sodium diphenylamine sulfonate: 5g/L indicator solution. 4.1.3 Analysis steps
Weigh about 2.5g of sample, accurate to 0.0002g, add water to dissolve, transfer to 1000mL volumetric flask, dilute to volume, shake well. Use a pipette to take 25mL of the above solution and place it in a 500mL Erlenmeyer flask. Use a pipette to take 50mL of ferrous ammonium sulfate solution and place it in a Erlenmeyer flask. Slowly add 20mL of sulfuric acid and 5mL of phosphoric acid while cooling at room temperature. Let stand for 10 minutes. Dilute to about 300mL, add 5mL sodium diphenylamine sulfonate indicator solution, and titrate with potassium dichromate standard titration solution until the solution turns purple as the end point. Do a blank test at the same time.
4.1.4 Expression of analysis results
The potassium chlorate content X expressed as mass percentage is calculated according to formula (1): X = . - V)Xc× 0. 020 42 ×100 0. 958 2 1000×m
25
_ 81. 68 × (Vo - V) In the formula: V. -
V-
-The volume of the potassium dichromate standard titration solution consumed by the blank test, mL; the volume of the potassium dichromate standard titration solution consumed by the titration test solution, mL; Actual concentration of potassium dichromate standard titration solution, mol/L; (1)
- equivalent to 1.00mL potassium dichromate standard titration solution c (1/6KCr0,) = 1.000mol/L in grams The mass of potassium chlorate expressed as 0.02042-
potassium:
0.9582-
Bromate (calculated as BrO:) is converted into potassium chlorate; Content, %; m
mass of sample, g.
4.1.5 Allowable difference
Take the arithmetic mean of the parallel measurement results as the measurement result, and the absolute difference of the parallel measurement results shall not be greater than 0.2%. 4.2 Determination of moisture
4.2.1 Instruments and equipment
4.2.1.1 Weighing bottle: $50mm×30mm. 4.2.2 Analysis steps
GB752-94
Use a weighing bottle with a constant weight to weigh about 10g of the sample, accurate to 0.0002g, place it in an electric oven at 105~110℃ Bake until constant weight. 4.2.3 Expression of analysis results
Moisture X expressed as mass percentage is calculated according to formula (2): tt||The mass of the weighing bottle and the sample before drying, g,
-The mass of the weighing bottle and the sample after drying, g; m
m The mass of the sample, g.
4.2.4 Allowable difference
Take the arithmetic mean of the parallel measurement results as the measurement result, and the absolute difference of the parallel measurement results shall not be greater than 0.01%. 4.3 Determination of water-insoluble matter content
4.3.1 Method summary
Dissolve the sample in hot water, filter with a filter, wash, dry and weigh. 4.3.2 Reagents and materials
4.3.2.1 Sodium nitrite (GB/T633);
4.3.2.2 Nitric acid (GB/T626): 1+1 solution; 4.3.2.3 Silver nitrate (GB /T670): 5g/L solution. 4.3.3 Instruments and equipment
4.3.3.1 Pot filter: The filter plate pore size is 515 μm. 4.3.4 Analysis steps
(2)
Weigh about 20g of the sample, accurate to 0.01g, dissolve it in 300mL hot water, filter it with a constant weight crucible filter, and heat it Wash the water-insoluble matter in the crucible with water until there is no chlorate radical in the filtrate, place it in an electric oven, and dry it to constant weight at 105-110°C. Note: Test for chlorate ions: Use a test tube to take 1 to 2 mL of the washing residue filtrate, add a few grains of solid sodium nitrite and a few drops of nitric acid solution, and then add a few drops of silver nitrate solution. It should not be turbid after adding a few drops of silver nitrate solution.
4.3.5 Expression of analysis results
The water-insoluble matter content X expressed as mass percentage is calculated according to formula (3): |tt||-The mass of water-insoluble matter and type filter, g; where: mi-
m2
m
-mass of crucible filter, g;||tt ||Sample mass, g.
4.3.6 Allowable difference
Take the arithmetic mean of the parallel measurement results as the measurement result, and the absolute difference of the parallel measurement results shall not be greater than 0.005%. 4.4 Determination of chloride content
4.4.1Method summary
Same as Chapter 2 of GB/T3051.
4.4.2 Reagents and materials
Same as Chapter 4 of GB/T3051.
4.4.3 Instruments and equipment
(3)
GB752--94
4.4.3.1 Microburette: The nominal graduation value is 0.01 or 0.02mL. 4.4.4 Analysis steps
Weigh about 10g of the sample, accurate to 0.01g, add 200mL of water to dissolve it, add 3 drops of bromophenol blue indicator solution, and add dropwise c(HNO:) of about 1mol/L Add nitric acid solution until the solution turns yellow, then add 5 drops of excess, add 1mL of diphenyl azocarbon hydrazide indicator solution, and titrate with mercury nitrate standard Hg(NO.)2·HO)=0.02mol/L until the solution changes from yellow to Purple red is the end point. Solution c
2
is used as a blank test.
The titrated mercury-containing waste liquid shall be treated according to Appendix D of GB/T3051. 4.4.5 Expression of analysis results
Chloride content X expressed as mass percentage, calculated according to formula (4): x
(V - V.) X c tt||X100
m
where: V-
V.
0.03545-
The volume of the mercury nitrate standard titration solution consumed in the titration, mL; the volume of the mercury nitrate standard titration solution consumed in the blank test, mL; the actual concentration of the mercury nitrate standard titration solution, mol/L; with 1.00mL mercury nitrate standard titration solution cl chloride (measured as CI) mass;
mass of sample, g.
m
4.4.6 Allowable difference
(4)
-Hg (NO,)·H,O)=1.000mol/L equivalently expressed in grams The arithmetic mean of the parallel measurement results is taken as the measurement result, and the absolute difference of the parallel measurement results is not greater than 0.002%. 4.5 Determination of bromate content
4.5.1 Method summary
In acidic medium, the bromate in the product reacts with potassium iodide to release iodine, and the release is titrated with sodium thiosulfate standard titration solution. out of iodine. 4.5.2 Reagents and materials
4.5.2.1 Hydrochloric acid (GB/T622): 1+10 solution; 4.5.2.2 Potassium iodide (GB/T1272): 100g/L solution, stored in brown bottles; 4.5.2.3 Sodium thiosulfate (GB/T637): c(Na2SO3·5H,O) is about 0.01mol/L standard titration solution; use a pipette to transfer the concentration c(Na2S.O·5H prepared and calibrated according to GB/T601 , O) 50mL of sodium thiosulfate standard titration solution of approximately 0.1mol/L, place it in a 500mL volumetric flask, dilute to the mark, and shake well. 4.5.2.4 Soluble starch: 5g/L solution. 4.5.3 Analysis steps
Weigh about 2g of the sample, accurate to 0.01g, place it in an iodine volumetric bottle, add 100mL of water to dissolve, add 5mL of potassium iodide solution and 5mL of hydrochloric acid solution, place it in the dark for 30 minutes, and use Titrate with sodium thiosulfate standard titration solution. When the end point is near (light yellow), add 3 mL of soluble starch solution and continue titrating until colorless is the end point. Do a blank test at the same time.
4.5.4 Expression of analysis results
The bromate (calculated as BrO) content X expressed as mass percentage, calculated according to formula (5): (V - V.) X c . 021 32.
X,=
The volume of sodium thiosulfate standard titration solution consumed in the blank test, mL; · (5)
GB752-94
The volume of sodium thiosulfate standard titration solution consumed in the blank test, mL; V.
The actual concentration of sodium thiosulfate standard titration solution, mol/L; 0.02132 - equivalent to 1.00mL sodium thiosulfate standard titration solution Cc (Na2S2O, 5H, O) = 1.000mol/L) The mass of bromate (measured as BrO,) expressed in grams; the mass of the sample, g.
4.5.5 Allowable difference
Take the arithmetic mean of the parallel measurement results as the measurement result, and the absolute difference of the parallel measurement results shall not be greater than 0.005%. 4.6 Determination of sulfate content
4.6.1 Method summary
In acidic medium, sulfate reacts with barium chloride to form sulfuric acid precipitate. Adding barium chloride-hydrochloric acid-glycerol mixed reagent can Helps form uniform fine particles and prevents sedimentation from settling into a suspended state for turbidity comparison. 4.6.2 Reagents and materials
4.6.2.1 Barium chloride (GB/T652), pre-ground to less than 1.4mm; 4.6.2.2 Sodium chloride (GB/T1266)-hydrochloric acid (GB/T622)- Glycerol (GB/T687) mixed solution: Weigh 120g sodium chloride and dissolve it in 490mL water, add 10mL hydrochloric acid and 500mL glycerol, and mix evenly; 4.6.2.3 Sulfate standard solution: 1mL contains 0.1mg SO-. 4.6.3 Instruments and equipment
4.6.3.1 Colorimetric tube, 50mL.
4.6.4 Analysis steps
Weigh about 2g of sample, accurate to 0.01g, add water to dissolve it, filter if necessary, move it into a colorimetric tube, add 10mL of mixed solution, and dilute with water to the mark, shake well, add 0.2g barium chloride, shake well, and leave it for 10 minutes. The turbidity should not be deeper than the standard turbidity solution. Preparation of standard turbidity solution: Take a certain volume of sulfate standard solution and process it in the same way as the sample at the same time as specified below. Superior product**
First-class product
4.7 Determination of iron content
4.7.1 Method summary
Same as Chapter 2 of GB/T3049.
4.7.2 Reagents and materials
Same as Chapter S of GB/T3049.
4.7.3 Instruments and equipment
4.7.3.1 Spectrophotometer.
4.7.4 Analysis steps
.2.0mL
6.0mL
4.7.4.1 Drawing of working curve
See Article 5.3 of GB/T3049 , select an absorption cell with a thickness of 3cm and its corresponding iron standard solution dosage, and draw a working curve.
4.7.4.2 Preparation of test solution
Weigh about 1g sample, accurate to 0.01g, place it in a 150mL tall beaker, add 20mL1+3 hydrochloric acid solution to dissolve it, and cover the surface blood, carefully heat and evaporate to dryness, add water to dissolve. 4.7.4.3 Preparation of blank test solution
In a 150.mL tall beaker, use all the reagents used to prepare the test solution with the same dosage and the same operation to prepare the blank test solution. 4.7.4.4 "Measure
For the test solution and blank test solution, follow the provisions of Article 5.4 of GB/T3049. If necessary, add water to 60mL..." and start the operation.
4.7.5 Expression of analysis results
GB752-94
Iron (Fe) content X expressed as mass percentage. Calculate according to formula (6): X, -- (m - mo) × 10-
×100=0.1×(m,-m)
m
m||tt ||In the formula: m: The mass of iron found from the working curve based on the measured absorbance of the test solution, mgm. —The mass of iron found from the working curve based on the measured absorbance of the blank test solution, mg; m-mass of the sample, g.
4.7.6 Allowable difference
Take the arithmetic mean of the parallel measurement results as the measurement result, and the absolute difference of the parallel measurement results shall not be greater than 0.0005%. 4.8 Determination of sieve residue
4.8.1 Instruments and equipment
4.8.1.1 Test sieve (GB6003): R40/3 series, Φ200mm×50mm/0.125mm, with sieve bottom and sieve cover ;4.8.1.2 Paint brush, No. 6 or No. 7 paint brush. 4.8.2 Analysis steps
(6)
Weigh about 50g of the sample, accurate to 0.01g, place it in the test sieve, and sieve (if there are powder balls on the sieve, lightly loosen it) , weigh the residue on the sieve.
4.8.3 Expression of analysis results
The sieve residue content X expressed as mass percentage is calculated according to formula (7): ||In the formula: m - the mass of the residue on the 125μm sieve, gm - the mass of the sample, g.
4.8.4 Allowable difference
Take the arithmetic mean of the parallel measurement results as the measurement result, and the absolute difference of the parallel measurement results shall not be greater than 0.1%. 5 Inspection Rules
·(7)
5.1 Potassium fluoride content, moisture, water-insoluble matter content, chloride content, sulfate content, bromate content, iron content, Eight index items such as sieve residue are type inspection items. Among them, seven indicators, including potassium chlorate content, moisture, water-insoluble matter content, chloride content, bromate content, iron content, and sieve residue, are factory inspection items and should be inspected batch by batch. Under normal circumstances, type inspection is conducted at least once a month.
5.2 Industrial potassium chlorate should be inspected by the quality supervision and inspection department of the manufacturer in accordance with the provisions of this standard. The manufacturer should ensure that all products shipped meet the requirements of this standard.
Each batch of products leaving the factory should be accompanied by a quality certificate, which includes: manufacturer name, factory address, product name, grade, net weight, batch number or production date, quality certificate that the product quality complies with this standard, and this standard serial number. 5.3 The user has the right to inspect and accept the industrial potassium chlorate received within one month in accordance with the provisions of this standard. 5.4 Each batch of industrial potassium chlorate products shall not exceed 60t. 5.5 Determine the number of sampling units in accordance with Article 6.6 of GB/T6678. When sampling, insert the sampler vertically from the center of the packaging bag to 4/5 of the depth of the material layer to sample. After mixing the sampled products, divide them into no less than 500 people according to the four-quarter rule. The samples are divided into two clean, dry, wide-mouth bottles with ground stoppers and sealed. A label should be attached to the bottle to indicate: production name, product name, grade, batch number, sampling date and sampler’s last name GB752-94
. One bottle is used for testing and the other bottle is kept for three months for future reference. 5.6 If any indicator in the inspection results does not meet the requirements of this standard, samples from twice the amount of packaging units should be re-sampled for verification. If even one indicator in the verification results does not meet the requirements of this standard, the entire batch of products will not be accepted. 5.7 When the supply and demand parties have objections to product quality, they shall be handled in accordance with the provisions of the "Product Quality Law of the People's Republic of China". 5.8 Use the rounded value comparison method specified in GB1250 to determine whether the inspection results meet the standards. 6 Marking, packaging, transportation, storage
6.1 Industrial potassium chlorate packaging containers should have firm and clear markings, including: manufacturer name, factory address, product name, trademark, grade, net weight, batch number or production date, and Standard number, mark 11 "oxidizer" mark specified in GB190 and mark 4 "afraid of heat" mark and mark 7 "afraid of moisture" mark specified in GB191.
6.2 Industrial potassium chlorate is double-layered. The inner packaging is made of polyethylene. Plastic film bags with a film thickness of 0.08±0.01mm, or two-layer kraft paper bags. The outer packaging is made of steel drums with a thickness of 0.7mm. When transported by LTL, the steel drums should be packed with transparent cages. Wooden box.
Tie the mouth of the plastic inner packaging bag tightly with Vinyl rope or other ropes of equivalent quality, or seal it in other equivalent ways; use Vinyl thread or other equivalent threads to sew the kraft paper bags. The lid of the steel drum should be tightly sealed. 6.3 Industrial potassium chlorate should be covered during transportation to prevent rain and moisture. It should be handled with care and collisions are strictly prohibited. It should not be mixed with flammable and explosive materials
6.4 Industrial potassium chlorate should be stored in a cool and dry place to prevent exposure to heat, moisture or sunlight. Additional notes:
This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China and is under the jurisdiction of the Tianjin Chemical Industry Research Institute. The standard is drafted by the Tianjin Chemical Industry Research Institute of the Ministry of Chemical Industry and Dalian Potassium Fluorate Factory. The drafters of this standard are Su Peiji, Wang Mingliang, and Li Xia. This standard is based on the former Soviet Union standard OCT2713-74 "Technical Conditions for Industrial Potassium Chlorate". This standard was published in 1965. First published on December 6, 1977. First revised on October 1, 1985; second revised on May 24, 1985.
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