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Chemical Industry Standard of the People's Republic of China
HG/T2746—1996
Sodium p-aminobenzenesulfonate
Published on April 8, 1996
Published by the Ministry of Chemical Industry of the People's Republic of China and implemented on January 1, 1997
WHG/T2746——1996
This standard is revised on the basis of HG/T2—372—80 "Sodium p-aminobenzenesulfonate". In this revision, the chromatographic method was tried to measure the aniline content in combination with the actual production and inspection situation of the product in China. However, there are still some specific problems that are inconvenient to solve, so the inspection method in the original version has not been changed, but the technical indicators of impurity content have been changed. In this revision, the writing format of the standard has been modified in accordance with the requirements of GB/T1.1—1993. From the date of implementation, this standard will replace HG/T2—372—80. This standard was proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard was jointly drafted by Hebei Baoding Chemical Industry Sanguang and Shenyang Chemical Research Institute. The main drafters of this standard are Wang Zhiwei, Li Chunrong and Wang Gujie. This standard was first issued in 1966 and first revised on July 1, 1982. I
W.bzsoso.cOm1 Scope
Chemical Industry Standard of the People's Republic of China
Sodium p-aminobenzenesulfonate
HG/T2746-1996
Replaces HG/T2-372-80bzxz.net
This standard specifies the requirements, sampling, test methods, inspection rules and marking, packaging, storage and transportation requirements of sodium p-aminobenzenesulfonate. This standard applies to sodium p-aminobenzenesulfonate obtained by sulfonation, baking and treatment of aniline, which is mainly used to make dyes, spices and prevent wheat rust.
Structural formula:
·2H,0
Molecular formula: C.HioOsNSNa
Relative molecular mass: 231.20 (according to the 1991 international relative atomic mass) 2 Referenced standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be revised, and parties using this standard should explore the possibility of using the latest version of the following standards. GB/T601—88
Chemical reagents for the preparation of standard solutions for titration analysis (volume analysis)
3 Requirements
The quality of sodium p-aminobenzenesulfonate should meet the requirements of Table 1. Table 1
Sodium p-aminobenzenesulfonate content, %
Aniline content, %
Insoluble matter in water, %
4 Sampling
Pink or light rose crystals
Select 10% barrels (or bags) from each batch (a batch of uniform products), and the number of small batches shall not be less than 5 barrels (or bags). Use a probe to take samples from the top, middle and bottom of the barrel (or bag), and the total amount of samples shall not be less than 200g. Mix the samples carefully and put them in a glass bottle with a ground stopper and seal them with paraffin. Put a label on the bottle, indicating: manufacturer name, product name, batch number, approved by the Ministry of Chemical Industry of the People's Republic of China on April 8, 1996, implemented on January 1, 1997
W.bzsoso, cOmHG/T2746-1996
and sampling date. One bottle is used for inspection, and one bottle is kept for future reference. 5 Test method
5.1 Appearance
Determine by visual inspection.
5.2 Determination of sodium p-aminobenzenesulfonate content
5.2.1 Reagents and solutions
Hydrochloric acid;
Potassium bromide: 100g/L solution;
Sodium nitrite: c(NaNO2)=0.5000mol/L standard titration solution, prepared and calibrated according to the relevant provisions of GB/T601; potassium iodide-starch test paper.
5.2.2 Determination steps
Weigh about 25g of sample (accurate to 0.0002g), place it in a 500mL beaker, add 200mL of distilled water, heat to dissolve it completely, cool to room temperature, transfer to a 500mL volumetric flask, and dilute to the scale with distilled water. After shaking, use a pipette to measure 50mL of the test solution into a 600mL beaker, add 350mL of distilled water, 20mL of hydrochloric acid, and 10mL of potassium bromide solution, cool to 10~15℃, titrate with sodium nitrite standard titration solution and stir, insert the tip of the burette under the liquid surface during titration, and take out the burette when it is close to the end point, continue titration and test with potassium iodide-starch test paper, when the test solution point appears light blue on the test paper and does not disappear for 3 minutes, it is the end point. Perform a blank test under the same conditions.
The mass percentage of sodium p-aminobenzenesulfonate content is expressed as X, and is calculated according to formula (1): X, 0 212× ×100
-actual concentration of sodium nitrite standard titration solution, mol/L, where: c-
V-volume of sodium nitrite standard titration solution consumed, mL, V-volume of sodium nitrite standard titration solution consumed for blank, mLmi-mass of sample, g;
0.2312-mass of sodium p-aminobenzenesulfonate expressed in grams equivalent to 1.00mL of sodium nitrite standard titration solution [c (NaNO2) = 1.000mol/L].
5.3 Determination of aniline content
5.3.1 Reagents and solutions
Hydrochloric acid;
Sodium nitrite: c(NaNO2)=0.0100mol/L standard titration solution, prepared and calibrated according to the relevant provisions of GB/T601; Potassium bromide;
Bleaching powder: 5% (m/m) solution;
Potassium iodide starch test paper.
5.3.2 Determination steps
Weigh 10g (accurate to 0.002g) of sodium p-aminobenzenesulfonate sample, place it in a 500mL flask, add 150mL of distilled water, connect it to a straight condenser, cool it with cold water, and continue to heat and boil for distillation. Use a 500mL beaker to receive the distillate at the outlet, add 100mL of distilled water and 5mL of hydrochloric acid to the beaker. When the volume of the material in the flask is about 100mL, test the distillate with bleaching powder solution on a white porcelain plate. If no blue color appears, it is the end point of the distillation. Add 1g of potassium bromide to the distillate, titrate it with sodium nitrite standard titration solution at 10-15℃, and test it with potassium iodide-starch test paper until the test paper turns slightly blue and keeps it for 3 minutes without disappearing, which is the end point. Perform a blank test under the same conditions.
The mass percentage of aniline content is represented by X2 and calculated according to formula (2): 2
Ww.bzsoso:comWherein: c1-
HG/T2746—1996
X2=i(V-Vs)×0. 093
actual concentration of sodium nitrite standard titration solution, mol/L; V2——volume of sodium nitrite standard titration solution consumed, mL, Vs—volume of blank sodium nitrite standard titration solution consumed, mLm2
mass of the sample, g;
(2)
the mass of sodium p-aminobenzenesulfonate equivalent to 1.00mL of sodium nitrite standard titration solution [c(NaNOz)=1.000mol/L] expressed in grams.
5.4 Determination of water-insoluble content
Weigh about 20g (accurate to 0.002g) of sodium p-aminobenzenesulfonate sample, place it in a 400mL beaker, add 200mL of distilled water, heat it to dissolve it completely, filter it with a Gs glass crucible filter that has been weighed to a constant weight, rinse the filter with 30-50mL of hot (60-80℃) distilled water 2-3 times, and then dry it at 105-110℃ to a constant weight. The mass percentage of water-insoluble content is represented by X: and calculated according to formula (3). X3
Where: m3——total mass of filter and insoluble matter, g, m—mass of filter, g;
m5——mass of sample, g.
6 Inspection rules
6.1 Inspection classification
All items specified in Table 1 are factory inspection items. 6.2 Inspection by the manufacturer
(3)
Sodium p-aminobenzenesulfonate shall be inspected by the quality inspection department of the manufacturer. The manufacturer shall ensure that the sodium p-aminobenzenesulfonate shipped out of the factory meets the requirements of this standard. Each batch of sodium p-aminobenzenesulfonate shipped out of the factory shall be accompanied by a quality certificate in a certain format. 6.3 User acceptance
The user unit has the right to inspect the sodium p-aminobenzenesulfonate received in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
6.4 Re-test
If one of the indicators in the test results does not meet the requirements of this standard, sodium p-aminobenzenesulfonate should be re-tested from twice the amount of packaging. If only one indicator does not meet the requirements of this standard, the entire batch of sodium p-aminobenzenesulfonate cannot be accepted.
7 Marking, packaging, transportation and storage
7.1 Marking
The outer packaging of sodium p-aminobenzenesulfonate should be painted with a firm mark indicating: manufacturer name, product name, batch number, production date, net weight and gross weight. A certificate should be attached to each bag (or barrel) of packaged finished products. The content includes: manufacturer name, product name, batch number, production date, factory date, product net weight, certificate that the product quality meets the requirements of this standard and the number of this standard. 7.2 Packaging
Sodium p-aminobenzenesulfonate is packaged in woven bags lined with plastic bags, with a net weight of 25kg per bag. 7.3 Transportation and storage
Wbzsoso, cOnHG/T2746—1996
Sodium p-aminobenzenesulfonate should be stored in a dry and ventilated place to prevent moisture and deterioration. Avoid collision during transportation.
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