Some standard content:
Chemical Industry Standard of the People's Republic of China
Aminosulfonic acid
Process
1 Subject content and scope of application
HG/T2527-93
This standard specifies the technical requirements, test methods, inspection rules and requirements for marking, packaging, transportation and storage of industrial aminosulfonic acid. This standard applies to industrial aminosulfonic acid produced by the urea process. This product can be used in chemical, construction, textile, food, military and other departments as raw materials for metal electroplating, descaling agent, stabilizer, sulfonating agent, flame retardant, etc.Molecular formula: NH2SO,H
Relative molecular mass: 97.09 (according to the international relative atomic mass in 1989)2Reference standards
GB 190
GB 191
Dangerous goods packaging mark
Pictorial mark for packaging storage and transportation
GB/T 601
GB/T 603
GB1250
Preparation of standard solution for titration analysis (volume analysis) of chemical reagentsPreparation of preparations and products used in chemical reagent test methodsExpression and determination methods of limit valuesGB/T 3049
GB/T 6678
GB/T 6682
3 Technical requirements
General method for determination of iron content in chemical products General rules for sampling of chemical products
Specifications and test methods for water used in analytical laboratories Industrial aminosulfonic acid shall meet the requirements specified in Table 1: Table 1
Aminosulfonic acid (NH, SO, H) content, %
Sulfate (SO), %
Water-insoluble matter, %
Iron (Fe) content, %|| tt||Loss on drying, %
Approved by the Ministry of Chemical Industry of the People's Republic of China on September 8, 1993. O-phenanthroline spectrophotometric method
Superior product
Colorless or white crystals
First-class product
Colorless or white crystals
Qualified product
White powder
Implemented on July 1, 1994
4 Test method
HG/T 2527-93
The reagents and water used in this standard are analytical reagents and grade 3 water in accordance with GB/T6682 unless otherwise specified. 4.1 Determination of aminosulfonic acid content
4.1.1 Summary of the method
In an acidic solution, aminosulfonic acid reacts with sodium nitrite, with starch potassium iodide as the indicator. NH,SO,H + NaNO, = NaHSO, + H,O + N22NaNOz + 2KI + 4HCl = 2KC1 + 2NO + 2H,O + Iz + 2NaCl 4.1.2 Reagents and solutions
4.1.2.1 Hydrochloric acid (GB/T622) solution: 1+1; 4.1.2.2 Sodium nitrite (GB/T633) standard titration solution: c (NaNO2) = 0.1mol/L, prepared and calibrated according to GB/T601, or calibrated as follows:
Weigh 0.5g of standard anhydrous aminosulfonic acid dried to constant weight at 120°C, accurate to 0.0001g. Add 2mL of ammonia water to dissolve, add 200mL of water and 20mL of hydrochloric acid. Insert the lower end of the dropper filled with the prepared sodium nitrite solution into the solution about 10mm, and titrate at 15~~20℃ under stirring. When it is close to the end point, lift the tip of the dropper out of the liquid surface, rinse the tip with a small amount of water, and merge the washing liquid into the solution. Continue to titrate slowly until the titration solution is added and stirred. Use a glass rod to dip a drop of reaction solution on the starch potassium iodide test paper. Light spots should appear. After 5 minutes, light blue spots still appear in the same test method, which is the end point. 4.1.2.3 Starch-potassium iodide test paper: Prepared according to GB/T603. 4.1.3 Analysis steps
Weigh 3g of sample, accurate to 0.0001g, dissolve in a 250mL volumetric flask, dilute to the scale with water, shake well, and set aside. Accurately pipette 25 mL of the above test solution into a 250 mL beaker, add 10 mL of hydrochloric acid solution, dilute to 100 mL with water, and slowly titrate with sodium nitrite standard titration solution at room temperature until a drop of solution is dipped on the starch-potassium iodide test paper with a glass rod and a blue color just appears. Continue stirring for 1 min, then dip another drop of solution and keep the blue color on the test paper for 1 min. The end point is that it does not disappear. 4.1.4 Expression of analysis results
The percentage of aminosulfonic acid (NH,SO:H) expressed as mass percentage X1 is calculated according to formula (1): X = Vc×0 097 09 × 100
m×250
Wherein: V-volume of sodium nitrite standard titration solution, mL; c-actual concentration of sodium nitrite standard titration solution, mol/L; ..(1)
mtMass of the sample, g;
0.09709-mass of aminosulfonic acid equivalent to 1.00mL of sodium nitrite standard titration solution [c(NaNO,)=1.000mol/L], expressed in grams.
4.1.5 Allowable difference
Take the arithmetic mean of the parallel determination results as the determination result. The absolute error value of the parallel determination results shall not exceed 0.6%. 4.2 Determination of sulfate
4.2.1 Method summary
Under acidic conditions, barium chloride reacts with sulfate to form barium sulfate, and turbidimetric determination is performed. 4.2.2 Reagents and solutions
4.2.2.1 Hydrochloric acid (GB/T622) solution: c(HC1)=3mol/L. 4.2.2.2 Barium chloride (GB/T652) solution: 250g/L. 4.2.2.3 Sulfate standard solution: 1ml. Contains 0.1mg sulfate, prepared according to Article 4.28.1 of GB/T602. 504
4.2.3 Instruments and equipment
4.2.3.1 Glass colorimetric tube with stopper, volume 50mL. 4.2.4 Analysis steps
HG/T 2527-- 93
4.2.4.1 Weigh 1g of sample to the nearest 0.01g, dissolve in a 100mL volumetric flask, dilute to the mark with water, shake well, and set aside. 4.2.4.2 Accurately pipette 10mL of the above-mentioned reserve test solution into a colorimetric tube, add 1mL of hydrochloric acid solution and 3mL of barium chloride solution in turn, dilute to 50mL with water, shake well, and leave for 20min. 4.2.4.3 Accurately pipette sulfate standard solution (4mL for superior aminosulfonic acid and 10mL for first-class aminosulfonic acid) into a colorimetric tube and treat it in the same way as the test solution (4.2.4.2). 4.2.4.4 Visually compare the turbidity of the test solution (4.2.4.2) and the standard (4.2.4.3) against a black background. The turbidity of the test solution shall not be greater than that of the standard to be qualified.
4.3 Determination of water-insoluble matter
4.3.1 Summary of the method
After the sample is dissolved in water, the insoluble residue is washed, filtered, dried and weighed to determine the content of water-insoluble matter. 4.3.2 Instruments and equipment
4.3.2.1 Oven;
4.3.2.2 Glass filter crucible No. 4, pore size 5~15μm; 4.3.2.3 Dryer.
4.3.3 Analysis steps
Weigh 10g of sample to the nearest 0.01g, dissolve in about 125mL of water with stirring, then filter with a glass filter that has been weighed constant in advance, wash with 40~50C hot water, and check the filtrate with pH test paper until the pH is 7. Put the glass filter crucible with the residue into an oven and dry it at 105~110℃ to constant weight.
4.3.4 Expression of analysis results
The water-insoluble content X2 expressed as a percentage by mass is calculated according to formula (2): Xz=m×100
Where: m. —The mass of the water-insoluble residue, g; m2 --—The mass of the sample.
4.3.5 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 0.005%. 4.4 Determination of iron content
4.4.1 Summary of the method
See Article 2 of GB/T3049.
4.4.2 Reagents and solutions
Prepare in accordance with Article 3 of GB/T3049, with Article 3.7 changed to Hydroxylamine hydrochloride (GB/T6685): 10g/L solution. 4.4.3 Instruments and equipment
Use Article 4 of GB/T3049.
4.4.4 Analysis steps
4.4.4.1 Preparation of working curve
a. Preparation of standard colorimetric solution:
Add 0.010 mg of iron per ml of iron standard solution to 6 100 mL volumetric flasks as shown in Table 2. (2)
Amount of iron standard solution,ml
Note: 1) Reagent blank solution.
b. Color development:
HG/T 2527-93
Corresponding to the iron mass, ug
Perform according to the procedures specified in Article 5.3.2 of GB/T3049, where "add 2.5mL ascorbic acid solution" is changed to "add 2.5mL hydroxylamine hydrochloride solution".
c. Determination of absorbance:
At a wavelength of 510nm, use a 1cm or 3cm (depending on the iron content in the sample) absorption cell, use water as a reference, adjust the absorbance of the spectrophotometer to zero, and then measure the absorbance of the standard color development solution. d. Draw Preparation of working curve:
Same as Article 5.3.4 of GB/T3049.
4.4.4.2 Determination
Color development: Www.bzxZ.net
Weigh 1g of sample, accurate to 0.001g, place in a 100mL beaker, add 60mL of water to dissolve, adjust the pH to about 2 with ammonia solution, and check the pH with precision pH test paper. Transfer all the solution to a 100mL volumetric flask, and then follow the following procedures in Article 4.4.4.1b\Add 2.5mL of hydroxylamine hydrochloride solution...".
b. Measurement of absorbance:
According to the procedure in Article 4.4.4.1c, measure the absorbance of the above test solution with water as reference. 4.4.4.3 Blank test
While determining the test solution, perform a blank test using the same procedure and the same amount of reagents, but without adding the sample. 4.4.5 Expression of analysis results
Subtract the absorbance value of the blank test (4.4.4.3) from the absorbance value of the test solution (4.4.4.2) and find out the corresponding iron mass from the working curve (4.4.4.1) according to the difference in the obtained absorbances. The iron (Fe) content X3 expressed as mass percentage is calculated according to formula (3): m. ×10-3
Where: ma
-the mass of iron found from the working curve according to the absorbance of the test solution, mg; the mass of the sample, g.
4.4.6 Allowable difference
Take the arithmetic mean of the parallel determinations as the determination result. The absolute difference of the parallel determination results shall not exceed 0.006%. 4.5 Determination of loss on drying
4.5.1 Summary of method
The sample is dried in an oven to constant weight, weighed with a balance, and the content is calculated. 4.5.2 Instruments and Equipment
4.5.2.1 Weighing Bottle: Flat.
4.5.2.2 Oven: Controllable at 70±2℃. HG/T 2527-93
4.5.3 Analysis Steps
Weigh 10g of sample, accurate to 0.01g, and place it in a weighing bottle that has been dried to constant weight in advance. Gently shake the weighing bottle to spread the sample evenly in the weighing bottle, and place it in an oven at 70±2℃ to dry to constant weight. 4.5.4 Expression of Analysis Results
The drying loss X expressed as mass percentage is calculated according to formula (4): X=m×100
Where: m. ---Mass difference before and after drying, g; mA—mass of sample, g.
4.5.5 Allowable Difference
Take the arithmetic mean of parallel determinations as the determination result. The absolute difference of parallel determination results shall not exceed 0.05%. 5 Inspection rules
5.1 Industrial aminosulfonic acid 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 industrial aminosulfonic acid leaving the factory meets the requirements of this standard. Each batch of industrial aminosulfonic acid leaving the factory shall be accompanied by a quality certificate, which shall include: manufacturer name, product name, trademark, grade, batch number, net weight, date of manufacture, and product standard number. 5.2 The user has the right to inspect and accept the industrial aminosulfonic acid received in accordance with the provisions of this standard. 5.3 This product stipulates that the number of finished products of the same specification produced on the same day is one batch. 5.4 The samples for inspection are randomly sampled by barrel. When the total number of units is less than 500 barrels, the number of sampling units can be determined directly according to the provisions of Table 2\Selection of sampling units in Article 6.6.2 of GB/T6678"; if the total number of units is greater than 500 barrels, the number of sampling units is determined by the total number of product units cubed - 3×N (N is the total number of barrels), and if there is a decimal, it is rounded up to an integer. The root of the blue multiple is
From the selected barrel, use a sampling tool to vertically insert the sample from the center of the packaging bag at 2/3 of the material layer, take out a total of about 2kg of the sample, and mix it evenly. Then use the quartering method to reduce it to about 500g, immediately put into two clean, dry ground-mouth bottles, seal with lids, affix labels, and indicate the manufacturer's name, product name, batch number, sampling date and sampler's name, etc. One bottle is used for inspection and the other is used for retention.
5.5 If one indicator in the inspection result does not meet the requirements of this standard, re-sampling should be carried out from twice the amount of packaging bags. After verification, even if only one indicator 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, the provisions of the "Interim Measures for National Product Quality Arbitration Inspection" shall apply. 5.7 Determine whether the test results meet the standards by the rounded value comparison method specified in GB1250. 6 Marking, packaging, transportation and storage
6.1 The packaging bag should have firm and clear markings, including: manufacturer name, product name, trademark, quality, grade, batch number or production date, net weight, this standard number and the "corrosive article" mark specified in GB190 and the "moisture-sensitive" mark specified in GB191. 6.2 The inner packaging of industrial aminosulfonic acid is made of polyethylene plastic film, and the bag mouth is double-tied or heat-sealed, which should be tight and leak-proof. The outer packaging is packed in iron drums. Each drum Net weight 25 or 50kg.
6.3 Industrial aminosulfonic acid should be transported in railway boxcars or other vehicles with curtains and canopies. 6.4 Industrial aminosulfonic acid should be stored in a cool, dry, ventilated warehouse to prevent moisture. 507
Additional instructions:
HG/T252793
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 Nanjing Chemical Industry (Group) Corporation Research Institute. This standard was drafted by the Nanjing Chemical Industry (Group) Corporation Research Institute. The main drafters of this standard are Guo Peihua and Pan Hongyue. 5084 Expression of analysis results
The drying loss X expressed as a percentage of mass is calculated according to formula (4): X=m×100
Where: m. ---Mass difference before and after drying, g; mA—mass of the sample, g.
4.5.5 Allowable difference
The arithmetic mean of the parallel determinations is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.05%. 5 Inspection rules
5.1 Industrial aminosulfonic acid 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 industrial aminosulfonic acid leaving the factory meets the requirements of this standard. Each batch of industrial aminosulfonic acid leaving the factory shall be accompanied by a quality certificate, which shall include: manufacturer name, product name, trademark, grade, batch number, net weight, date of manufacture, and product standard number. 5.2 The user has the right to inspect and accept the industrial aminosulfonic acid received in accordance with the provisions of this standard. 5.3 This product stipulates that the number of finished products of the same specification produced on the same day is one batch. 5.4 The samples for inspection are randomly sampled by barrel. When the total number of units is less than 500 barrels, the number of sampling units can be determined directly according to the provisions of Table 2\Selection of Sampling Units in Article 6.6.2 of GB/T6678"; if the total number of units is greater than 500 barrels, the number of sampling units is determined by the cube of the total number of product units - 3×N (N is the total number of barrels), and any decimals are rounded up to integers. The root multiple is
From the selected barrel, use a sampling tool to vertically insert the sample into the 2/3 of the material layer from the center of the packaging bag, take out a total of about 2kg of samples, and mix them evenly. Then use the quartering method to reduce it to about 500g, immediately put into two clean, dry ground-mouth bottles, seal with lids, affix labels, and indicate the manufacturer's name, product name, batch number, sampling date and sampler's name, etc. One bottle is used for inspection and the other is used for retention.
5.5 If one indicator in the inspection result does not meet the requirements of this standard, re-sampling should be carried out from twice the amount of packaging bags. After verification, even if only one indicator 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, the provisions of the "Interim Measures for National Product Quality Arbitration Inspection" shall apply. 5.7 Determine whether the test results meet the standards by the rounded value comparison method specified in GB1250. 6 Marking, packaging, transportation and storage
6.1 The packaging bag should have firm and clear markings, including: manufacturer name, product name, trademark, quality, grade, batch number or production date, net weight, this standard number and the "corrosive article" mark specified in GB190 and the "moisture-sensitive" mark specified in GB191. 6.2 The inner packaging of industrial aminosulfonic acid is made of polyethylene plastic film, and the bag mouth is double-tied or heat-sealed, which should be tight and leak-proof. The outer packaging is packed in iron drums. Each drum Net weight 25 or 50kg.
6.3 Industrial aminosulfonic acid should be transported in railway boxcars or other vehicles with curtains and canopies. 6.4 Industrial aminosulfonic acid should be stored in a cool, dry, ventilated warehouse to prevent moisture. 507
Additional instructions:
HG/T252793
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 Nanjing Chemical Industry (Group) Corporation Research Institute. This standard was drafted by the Nanjing Chemical Industry (Group) Corporation Research Institute. The main drafters of this standard are Guo Peihua and Pan Hongyue. 5084 Expression of analysis results
The drying loss X expressed as a percentage of mass is calculated according to formula (4): X=m×100
Where: m. ---Mass difference before and after drying, g; mA—mass of the sample, g.
4.5.5 Allowable difference
The arithmetic mean of the parallel determinations is taken as the determination result. The absolute difference of the parallel determination results shall not exceed 0.05%. 5 Inspection rules
5.1 Industrial aminosulfonic acid 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 industrial aminosulfonic acid leaving the factory meets the requirements of this standard. Each batch of industrial aminosulfonic acid leaving the factory shall be accompanied by a quality certificate, which shall include: manufacturer name, product name, trademark, grade, batch number, net weight, date of manufacture, and product standard number. 5.2 The user has the right to inspect and accept the industrial aminosulfonic acid received in accordance with the provisions of this standard. 5.3 This product stipulates that the number of finished products of the same specification produced on the same day is one batch. 5.4 The samples for inspection are randomly sampled by barrel. When the total number of units is less than 500 barrels, the number of sampling units can be determined directly according to the provisions of Table 2\Selection of sampling units in Article 6.6.2 of GB/T6678"; if the total number of units is greater than 500 barrels, the number of sampling units is determined by the cube of the total number of product units - 3×N (N is the total number of barrels), and any decimals are rounded up to integers. The root multiple is
From the selected barrel, use a sampling tool to vertically insert the sample into the 2/3 of the material layer from the center of the packaging bag, take out a total of about 2kg of samples, and mix them evenly. Then use the quartering method to reduce it to about 500g, immediately put into two clean, dry ground-mouth bottles, seal with a cap, affix a label, and indicate the manufacturer's name, product name, batch number, sampling date and sampler's name, etc. One bottle is used for inspection and the other is used for retention.
5.5 If one indicator in the inspection result does not meet the requirements of this standard, re-sample from twice the amount of packaging bags should be checked. After the inspection result, even if only one indicator 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, the provisions of the "Interim Measures for National Product Quality Arbitration Inspection" shall apply. 5.7 Determine whether the test results meet the standards by the rounded value comparison method specified in GB1250. 6 Marking, packaging, transportation and storage
6.1 The packaging bag should have firm and clear markings, including: manufacturer name, product name, trademark, quality, grade, batch number or production date, net weight, this standard number and the "corrosive article" mark specified in GB190 and the "moisture-sensitive" mark specified in GB191. 6.2 The inner packaging of industrial aminosulfonic acid is made of polyethylene plastic film, and the bag mouth is double-tied or heat-sealed, which should be tight and leak-proof. The outer packaging is packed in iron drums. Each drum Net weight 25 or 50kg.
6.3 Industrial aminosulfonic acid should be transported in railway boxcars or other vehicles with curtains and covers. 6.4 Industrial aminosulfonic acid should be stored in a cool, dry, ventilated warehouse to prevent moisture. 507
Additional instructions:
HG/T252793
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 the Nanjing Chemical Industry (Group) Corporation Research Institute. This standard was drafted by the Nanjing Chemical Industry (Group) Corporation Research Institute. The main drafters of this standard are Guo Peihua and Pan Hongyue. 508
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