Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2079—91
1-Aminocarboxyquinone
Published on July 17, 1991
Ministry of Chemical Industry of the People's Republic of China
Implemented on January 1, 1992
Chemical Industry Standard of the People's Republic of China
1-Aminocarboxylic Acid
Subject Content and Scope of Application
HG2079—91
This standard specifies the technical requirements, test methods, inspection rules, and packaging, marking, storage and transportation requirements of 1-aminocarboxylic Acid. This standard applies to 1-aminocarboxylic Acid obtained by reduction after nitration of carboxylic Acid. 1-Aminocarboxylic Acid is mainly used in the dye industry. Structural formula:
Molecular formula: CuH.O2N
Relative molecular mass: 223.24 (according to the international relative atomic mass in 1987) 2 Reference standards
6 Determination of moisture content in dyes and dye intermediates
GB2386
1 Determination of ash content of organic chemical products
GB7531
3 Technical requirements
The quality of 1-aminoonionaldehyde shall meet the requirements of the following table: Refers to
1-aminoonionaldehyde content (calculated on dry product), %
Total amount of 1,5-diaminoonionaldehyde and 1,8-diaminoonionaldehyde (calculated on dry product), %Ash, %
Moisture, %
4 Test method
4.1 Appearance
Determine by visual method.
Superior grade
Red to brownish red crystalline powder
4.2 Determination of 1-aminoonanal content, total amount of 1,5-diaminoonanal and 1,8-diaminoonanal and other organic impurities 4.2.1 Summary of method
Qualified product
Use high performance reversed phase liquid chromatography on an octadecyl bonded stationary phase column with methanol plus dioxane plus water as the mobile phase to separate 1-aminoonanal and its components. Detect with an ultraviolet detector and quantify by normalization method. 4.2.2 Instruments and Devices
Approved by the Ministry of Chemical Industry of the People's Republic of China on July 17, 1991 and implemented on January 1, 1992
Liquid chromatograph shall meet the following requirements:
HG2079-91
Infusion pump: flow stability within ±1%, maximum usable pressure 30MPa; detector: single wavelength input - 254nm UV detector or UV spectrophotometer with this function; manual injection valve: with 10uL quantitative tube;
Chromatographic column: wet filling with octadecyl-silica gel chemical bonding stationary phase, the theoretical plate number shall not be less than 8000; recording device: full scale 1~5mV recorder or data processor with this function; ultrasonic generator:wwW.bzxz.Net
Micro syringe: 25~50uL flat-head syringe. 4.2.3 Reagents
4.2.3.1 Industrial 1-aminocarboxaldehyde standard; 4.2.3.2 Anhydrous methanol;
4.2.3.3 1,4-Dioxane (HG3-1529). 4.2.4 Chromatographic analysis conditions
According to different devices, select the best chromatographic analysis conditions. Taking LC-6A liquid chromatograph as an example, the chromatographic conditions are as follows: detector: UVD-2 type with a wavelength of 254mm and a range of 0.02; chromatographic column: a stainless steel tube with a length of 100mm and an inner diameter of 5mm, filled with Nucleosil5C1s stationary phase; data processor: C-R3A;
paper speed: 3mm/min;
mobile phase: anhydrous methanol dodecacyclopentacyclopentahydrate = 159+15+126, degassed after preparation; flow rate: 1mL/min;
column temperature: room temperature;
sample concentration: 0.52mg/mL;
injection volume: 10uL.
4.2.5 Preparation of standard solution and determination of correction factor 4.2.5.1 Preparation of standard solution
Weigh about 13 mg (accurate to 0.2 mg) of finely ground and dried 1-aminocarboxaldehyde industrial standard into a 25 mL volumetric flask, dilute to scale with anhydrous methanol, cover the bottle stopper, place in an ultrasonic generator for vibration, and take out for use after the sample is completely dissolved. 4.2.5.2 Determination of relative correction factor
After the instrument is running stably, use a micro-syringe to draw the standard solution and inject it into the manual injection valve (fill the quantitative tube). After the last component has flowed out (see chromatogram), accurately measure the peak width and half peak width of each component, and calculate the peak area of each component (or use a data processor to process the results).
The relative correction factor (f) of each component is calculated according to formula (1): m,·A
ma·A,
Wherein: m. Mass of component i, mg;
m. Mass of -1-aminocarboxaldehyde, mg;
A. Peak area of component i, mm;
A. Peak area of -1-aminocarboxaldehyde, mm.
4.2.6 Analysis steps
Weigh about 13 mg of the finely ground and dried sample to be tested, place it in a 25 mL volumetric flask, dilute to the scale with anhydrous methanol (4.2.3.2), cover the bottle stopper, place it in an ultrasonic generator for vibration, and take it out for use after the sample is completely dissolved. Use a micro syringe to draw the sample solution and inject it into the manual injection valve (fill the quantitative tube). After the last component has completely flowed out (see chromatogram), accurately measure the peak height and half peak height of each component, and calculate the peak area of each component (or use a data processor to process the results). 2
HG2079—-91
Note: The standard solution and sample solution should be filtered with filter paper before injection to reduce column contamination. 1
Chromatogram of 1-aminocarboxaldehyde
1-carboxaldehyde sulfonic acid sodium salt; 2—solvent; 3—solvent; 4—1,7-diaminocarboxaldehyde; 5—1,6-diaminocarboxaldehyde; 6—2-aminocarboxaldehyde; 7—1,5-diaminocarboxaldehyde and 1,8-diaminocarboxaldehyde; 8—1-aminocarboxaldehyde; 9 carboxaldehyde; 10—unknown substance The content of each component (r,) is calculated according to formula (2):
EG,.A,r,)
Wherein: A——peak area of the measured component, mm; f——relative correction factor of the measured component;
\,——signal attenuation of the measured component;
R——ash content determined according to 4.3, %.
X(100-R)
The difference between the two parallel determination results of 1-aminoanthraquinone content should not be greater than 0.5%. The difference between the two parallel determination results of the total amount of 1,5-diaminoanthraquinone and 1,8-diaminoanthraquinone should not be greater than 0.1%. Take the arithmetic mean as the determination result. Note: The correction factor of the unknown substance is calculated according to the correction factor of the adjacent known substance. 4.3 Determination of ash
Carry out in accordance with the provisions of GB7531.
4.4 Determination of moisture
Carry out in accordance with the provisions of GB2386 drying method.
5 Inspection rules
HG207991
5.11-aminoanthraquinone should be inspected by the quality inspection department of the manufacturer. The manufacturer should ensure that all 1-aminoanthraquinone shipped out of the factory meets the requirements of this standard. Each batch of 1-aminoanthraquinone shipped out of the factory should be accompanied by a quality certificate in a certain format. 5.2 The user has the right to inspect the quality of the received 1-aminoaldehyde in accordance with the provisions of this standard to check whether it meets the requirements of this standard.
5.3 Sampling method: Take samples from 10% of the iron barrels of each batch of products (a batch of uniform products). The sampling of small batches of products shall not be less than three barrels. When sampling, use a probe to probe the upper, middle and lower parts of the sample from the opened barrel. The total amount of the sample taken shall not be less than 500g. 5.4 Mix the sample carefully and put it into a clean and dry brown glass bottle with a ground stopper. A label shall be attached to the bottle to indicate the name of the manufacturer, product name, batch number and sampling date. The inspection shall be carried out by the inspection department. 5.5 If one of the indicators in the inspection results does not meet the requirements of this standard, a new sample shall be taken from twice the amount of packaging for verification. Even if only one indicator of the re-verification result does not meet the requirements of this standard, the entire batch of 1-aminoaldehyde cannot be accepted. 5.6 When the supply and demand parties have disputes over product quality and need arbitration, the arbitration institution can be selected by agreement between the two parties. During arbitration, arbitration analysis shall be conducted in accordance with the inspection methods specified in this standard.
6 Packaging, marking, purchase, storage and transportation
6.11-Amino onion shall be packaged in iron barrels lined with plastic bags, with a net weight of 25, 40 or 50 kg per barrel. 6.2 Each batch of packaged products shall be accompanied by a quality certificate. The certificate shall include: manufacturer name, product name, grade, batch number, production date, factory date, product net weight, proof that the product quality meets the requirements of this standard and the number of this standard. 6.3 The packaging container shall be firmly marked, including: manufacturer name, product name, production date, batch number, net weight, tare weight and registered trademark.
6.41-Aminocarboxylic acid should be stored in a dry and ventilated place to prevent heat, moisture and damage. Wear labor protection equipment when using and handling, and be careful when handling.
Additional instructions:
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 Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the Dye Factory of Jilin Chemical Company. The main drafters of this standard are Zheng Shizai, Fan Fang and Zhang Gui. 4
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