HG/T 2895-1997 Brominic acid sodium salt (sodium 1-amino-4-bromoanthraquinone-2-sulfonate)
Some standard content:
Chemical Industry Standard of the People's Republic of China
HG/T2895—1997
Bromaminic Acid, Sodium Sall
(1-Amino-4-bromoanthraquinone-2-sulfonic acid,sodium This standard adopts the internationally accepted high performance liquid chromatography method to replace the thin layer chromatography-spectrophotometry method used in the original standard to determine the main content and main impurities content of sodium salt of quercetin, and refers to the product specifications of Bayer of Germany, Sumitomo of Japan, Santos of Switzerland and other companies, and is revised according to the needs of domestic and foreign users and the technical and quality levels of manufacturers. Compared with the technical requirements of the original professional standard ZB/TG56003-88: the appearance is changed from paste to crystalline particles or powder; the main organic impurities such as 1-amino-2,4-dibromocarboxyquinone and 1-aminocarboxylic acid-2-sulfonic acid and water-insoluble content are added, and according to GB/T12707-91 "Principles of Industrial Product Quality Grading", the products are divided into three grades: superior products, standard products and qualified products. The indicators of superior products reach the specification level of similar products of Swiss Santos Company, the indicators of standard products are close to the specifications of similar products of German Bayer and Japanese Sumitomo Company, and qualified products are equivalent to the original standard first-class products. In terms of test methods, this standard replaces the original thin-layer chromatography spectrophotometry with advanced high-performance liquid chromatography, the main content is quantified by internal standard peak area, and the impurity components are determined by area normalization method. From the date of entry into force, this standard also replaces ZB/TG56003-88. This standard is 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 supervision of Shenyang Chemical Research Institute of the Ministry of Chemical Industry. The responsible drafting units of this standard are: Sichuan Dye Factory, Shenyang Chemical Research Institute of the Ministry of Chemical Industry. Participating drafting units: Shandong Zhaoyuan Chemical General Plant. The main drafters of this standard are: Wang Jianghong, Lv Qin, Lei Guoming, Yang Jia, Li Chunmei, Yang Xichuan. This standard was first issued in March 1982 and revised for the first time in 1988. I
W.bzsoso.cOmICS71.100.01
Registration No. 431—1997
Chemical Industry Standard of the People's Republic of China
Bromaminic Acid, Sodium Sall
(1-Amino-4-bromoanthraquinone-2-sulfonic acid, sodium salt)1 Scope
HG/T2895—1997
Replaces ZB/TG56003—88
This standard specifies the requirements, sampling, test methods, inspection rules, and marking, packaging, transportation and storage requirements for bromoamic acid sodium salt.
This standard applies to sodium bromine acid salt (sodium 1-amino-4-bromocarboxylic acid-2-sulfonic acid salt) obtained by sulfonation, bromination and purification of 1-aminocarboxylic acid.
Structural formula:
Molecular formula: CuHOsNSBrNa
Relative molecular mass: 404.17 (according to the 1991 international relative atomic mass) 2 Reference 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 the parties using this standard should explore the possibility of using the latest versions of the following standards. GB1250-89 Methods for expressing and determining limit values GB/T2386-80 Methods for determining moisture content in dyes and dye intermediates GB/T6682-92 Specifications and test methods for water used in analytical laboratories (eqvISO3696:1987) 3 Requirements
3.1 Appearance: red or orange-red crystalline particles or powder. 3.2 The quality of sodium bromamine salt shall meet the requirements of Table 1. Approved by the Ministry of Chemical Industry of the People's Republic of China on April 22, 1997 and implemented on October 1, 1997
W.bzsoso.cOm Item
Content of sodium bromamine salt
Content of 1-aminocarboxaldehyde-2-sulfonic acid
Content of 1-amino-2,4-dibromocarboxaldehyde
Content of water-insoluble matterbZxz.net
Moisture content
4 Sampling
HG/T2895—1997
Table 1 Quality requirements of sodium bromamine salt
Superior products
First-class products
Qualified products
Take samples from 10% of the barrels of each batch (a batch of uniform products), and the small batch shall not be less than 3 barrels. When sampling, use a probe to collect samples from the upper, middle and lower parts. The sampling volume shall not be less than 200g. After mixing the collected samples evenly, divide them into two clean and dry brown wide-mouth bottles with ground stoppers. Paste labels on the bottles, indicating: manufacturer name, product name, grade, batch number and sampling date. One bottle is for inspection, and one bottle is sealed with paraffin for future reference. 5 Test method
Unless otherwise specified, the reagents used in this standard refer to analytical pure reagents; water should comply with the third-grade water specifications in GB/T6682. The test results are determined according to the rounded value comparison method in GB1250. 5.1 Appearance
Visual determination is adopted.
5.2 Determination of the content of sodium bromamine salt and other organic impurities 5.2.1 Summary of the method
High performance reverse phase ion pair chromatography was used on an octadecyl bonded stationary phase column with methanol, water and hexadecyltrimethylammonium bromide ion pair reagent as the mobile phase to separate sodium bromamine salt and organic impurity components. The results were detected by UV detector. The sodium bromamine salt was quantified by the internal standard peak area, and the organic impurity components were quantified by the area normalization method. 5.2.2 Instruments and devices
Liquid chromatograph;
Infusion pump: flow range 0.1～5mL/min, within this range, its flow stability is ±1%; Detector: 254nm single wavelength UV detector or spectrophotometer with equivalent performance; Chromatographic column: stainless steel column with inner diameter 4.6mm and length 150mm, wet-filled with 5μm Spherisorb C18 stationary phase; Recording device: full-scale 1~5mV recorder or general chromatography data processor; Manual injection valve: with 10μL quantitative tube;
Micro syringe: 25μL flat-head syringe; Ultrasonic generator.
5.2.3 Reagents
Industrial sodium bromine salt standard (its relevant impurity content is known); methanol;
Hexadecyl trimethyl ammonium bromide;
Wbzsoso.cOnHG/T2895—1997
Benzene chloranone: (industrial refined product, purity greater than 99%). 5.2.4 Chromatographic conditions
According to different liquid chromatographs, select the best chromatographic conditions. Taking HP-1050 chromatograph as an example, the chromatographic conditions are as follows: Mobile phase: methanol + water = 78 + 22 (V/V), add 0.5g hexadecyl trimethyl ammonium bromide per liter of mobile phase, and degas after preparation. Flow rate: 1.0mL/min;
Column temperature: room temperature;
Injection volume: 10μL.
5.2.5 Determination of the content of sodium bromine acid salt
5.2.5.1 Preparation of internal standard solution
Weigh about 0.03g (accurate to 0.0002g) of benzothionone in a 50mL volumetric flask, dilute to the mark with methanol, cover the bottle stopper, and place in an ultrasonic generator for vibration dissolution. 5.2.5.2 Preparation of standard sample solution
Weigh about 0.05g (accurate to 0.0002g) of industrial sodium bromine acid salt standard in a 50mL volumetric flask, dilute to the mark with water, cover the bottle stopper, and place in an ultrasonic generator for vibration dissolution to obtain solution A. Take 5mL each of solution A and internal standard solution in a 25mL volumetric flask, dilute to the mark with methanol, cover the bottle stopper, and place in an ultrasonic generator for vibration dissolution and set aside. 5.2.5.3 Preparation of sample solution
Weigh about 0.05g (accurate to 0.0002g) of sodium bromoamine salt sample into a 50mL volumetric flask, dilute to scale with water, cover the bottle stopper, and place in an ultrasonic generator for vibration dissolution to obtain solution B. Take 5mL each of solution B and internal standard solution into a 25mL volumetric flask, dilute to scale with methanol, cover the bottle stopper, and place in an ultrasonic generator for vibration dissolution for use. 5.2.5.4 Analysis steps
After the instrument runs stably, use a micro-syringe to draw the standard solution and inject it into the manual injection valve (fill the quantitative tube) for injection, and use a data processor to process the results. See Figure 1 for the chromatogram. 3
W.bzsosocom5.00
①—1-aminocarboxaldehyde;
monobromoamic acid sodium salt;
HG/T2895—1997
③—1-aminocarboxaldehyde-2-sulfonic acid;④—internal standard;②carboxaldehyde:
③—1-amino-2-bromocarboxaldehyde,—1-amino-2,4-dibromocarboxaldehyde,③1-hydrocarboxylic acid-2,4-disulfonic acid
Bromamic acid sodium salt HPLC chromatogram examplein
Continuously inject several injections of standard solution until the relative deviation of the ratio of the response values of two adjacent injections (the ratio of the peak area of bromoamic acid sodium salt/the peak area of the internal standard) is not greater than 0.6%, and then perform quantitative analysis in the following order. (The standard solution and the sample solution should be filtered with filter paper before injection to reduce column contamination). 5.2.6.2 Expression of analysis results
The mass percentage of each component (x) is calculated according to formula (2): A
Wherein: A--peak area of component i, mm2. X100
The difference between two parallel determination results should not be greater than 0.1%, and the arithmetic mean is taken as the determination result. 5.3 Determination of water-insoluble matter content
5.3.1 Instrument
G3 glass filter (referred to as filter) 5.3.2 Determination steps
Weigh 1~3g of sample (accurate to 0.0002g) in a 400mL beaker, add 200mL hot water (about 80℃) to dissolve, filter with a filter that has been weighed to a constant weight, and wash with hot water (about 80℃) until the filtrate is colorless, and dry in a 105℃ oven to a constant weight. 4
W.bzsoso，comHG/T2895—1997
The mass percentage of water-insoluble matter (W) is calculated according to formula (3): W_m2-m1
Wherein: m2——mass of filter and water-insoluble matter, g; m1——mass of filter, g;
m——mass of sample, g.
5.4 Determination of moisture
According to the drying method in GB/T2386, the sample weight is 1~2g and the drying temperature is 150±5℃. 6 Inspection rules
6.1 Inspection by the manufacturer
Sodium bromamine salt shall be inspected by the quality inspection department of the manufacturer according to the requirements 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 in a certain format. If one of the indicators in the inspection results does not meet the requirements of this standard, samples shall be taken from twice the amount of packaging for re-inspection. If only one index of the re-inspection result does not meet the requirements of this standard, the entire batch of products cannot be accepted.
6.2 User acceptance
The user unit has the right to inspect the received sodium bromamine salt in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
7 Marking, packaging, transportation and storage
7.1 Marking
The packaging barrel of sodium bromamine salt should have a firm and clear mark, indicating the manufacturer's name, product name, trademark, batch number, grade, gross weight, net weight and production date. Each batch of packaged products should be accompanied by a quality certificate, which includes: manufacturer's name, product name, batch number, grade, net weight, production date, proof that the product quality meets the requirements of this standard and the number of this standard. 7.2 Packaging
Sodium bromamine salt is packaged in iron barrels lined with plastic bags (plastic bags should be tied), with a net weight of 25kg or 50kg per barrel. If the user requires other packaging, it can be negotiated and determined.
7.3 Transportation
Prevent exposure to sunlight and collision during transportation.
7.4 Storage
The product should be stored in a cool, dry and ventilated warehouse. 5
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