Some standard content:
1C871.080.30
Chemical Industry Standard of the People's Republic of China
Organic Chemical Products
(1999)
Published on 1999-06-16
Implemented on 2000-06-01
Published by the State Administration of Petroleum and Chemical Industry
Registration No. 3729-1999
HG/T2973-1999
This standard is revised from Chemical Industry Standard 1G/T2973-1958, Aqueous Solution of Diamines. The main technical differences between this standard and HG/T2973-1999 are: The second method for the determination of impurity content is added: gas chromatography, and the first method is specified as the secondary method. The difference between the two methods is that different chromatographic supports and stationary liquids are selected. The end of this standard is the standard. This standard replaces HG/T2573-1388 from the date of implementation. This standard was proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard was jointly drafted by the National Technical Committee for Chemical Standardization. The main drafting units of this standard are: Qinghai Province Jiangming Chemical Factory, Qinghai Province Jiangshan Chemical Industry General. The main drafters of this standard are: Xia Muquan, Jin Lijie, Ji Meng. This standard was first issued as a national standard in 1988, and was upgraded to a recommended chemical industry standard in 1990, and was renumbered. This standard is entrusted to the National Technical Committee for Chemical Standardization and Organic Subcommittee. 13
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Chemical Industry Standard of the People's Republic of China
Industrial 40-way Dimethylamine Aqueous Solution
Solutiuusufgdiuethyluninefurindustriuluse HC/T2973-1999
This standard specifies the requirements, sampling, test methods, marking, packaging, transportation and other aspects of dimethylamine produced by the combined chemical method of methane with a 19% aqueous solution of dimethylamine, with a molecular weight of 1.8 (continuing the 1995 National Standard on Atomic Mass) 2 Reference Standards
The following standards contain provisions that are referenced in this standard and become the provisions of this standard. When this standard is revised, the versions shown are valid. All standards have been replaced. The parties using this standard should explore the possibility of using the latest editions of the following standards: (B19090 Dangerous Goods Packaging Marking
G3/325-91 Packaging Steel Drums
GB/T678-8F Flower Products Sampling List
GR/T8n-86 General Rules for Sampling of Flow Chemical Products G3/T125m): 8S Maximum Limit Value Method and Judgment Method HG/T29711999T Industry A Water Solubility Test Method Railway Dangerous Goods Transfer Rules Soft Overshoot Method (No. 2995104 Document 3 Requirements
3.1 External Colorless Suitable Packaging Fast
3.21 Industry 10-A Water Solubility Question and Weight Recommended Requirements Table 1 Friends 1 Industry 43 2. The quality of the middle water rate supplier is suitable for the source of the cost.
Handy (ENI2)
|A child (CINI
|Three RH, N
1 Parent sample
Superior product
4.1 The following 10 products of the middle water correction are collected by the production plant's single environment cavity department. 4.2 The products are selected for sampling according to the uniform quality ratio: qualified products
4.3 Song sample 8: According to the relevant provisions of GE6678 and GB/T6650, the number of sample units shall comply with GB/T667886, the national petroleum and chemical industry personnel 19990616 approved 20000601 purchase drag
HG/T2973-1959
Table 2, horizontal car packaging, can be Take 4 samples from each batch as a batch, and the total amount of the sampled products shall not be less than 50%. Put the sampled products in two clean, well-sealed bottles, apply new labels on them, and indicate: manufacturer's name, product name, batch number, sample date and sampler's name. Each bottle shall be inspected separately, and two bottles shall be kept for storage. 4.4 Users shall carry out sampling and testing according to the requirements of this standard, and accept the products within 10 days after receiving the products. 4.5 The judgment of the inspection results shall be carried out according to B/T 12=100%. If the basic indicators in the inspection results do not meet the requirements of this standard, the packaging list of twice the number of samples shall be re-inspected: if only one indicator meets the requirements of this standard, the whole batch of products shall be unqualified. ||t t||5 Test method
5.1 Determination of methylamine content
The content of nitrogen, amine and blue powder impurities shall be determined according to 11G/T7971-1999. The content of nitrogen, amine and blue powder impurities shall be determined according to standard 5.2. 5.2 Determination of ammonia, chlorine and chlorine content by gas phase chromatography 5-2.1 Method requirements
The impurities in aqueous solution shall be determined by gas chromatography, thermal conductivity detection, combustion detection and external standard. 5.2.2 Pressure method (arbitration method)
The content of impurities in aqueous solution shall be determined according to 3.2.3 of 1G/T2971-1599. 5.2.3 Method II
5.2.31 Method reagents and materials
5.2.3.7.1 Hydroxide solvent: 5g/L.
5. 2.3.1-2 Acid solution; 1-1, 5.2-3-1.3 Drug A,
5.2.3.1.4 Case II brand 500, chromatographic fixative. 5 Potassium nitrate. www.bzxz.net
5.2.3.1.5
5.2.3.1.6
6 Hexadecanol: chromatographic fixative.
5.2.3.1.7201 Red twist:). 17~c.246m, equivalent to 80~60 days. 5.2.3-2 Apparatus.
5.2.3.2. 1 Phase chromatographic night.
With thermal conductivity detector. Temperature value 0.1℃, sensitivity of the whole machine 1000mVmL/m%: 5.2.3.2.2 spectrum.
Station length 2m, inner diameter 2mm or 3mm, or the user can choose the length and inner diameter required for full separation. Fixed ratio: 201 red acetone: 10% alcohol: 700% potassium hydroxide = 10:1.20.5:0.1. Wash the 207 red support with water to remove ash, use hydrochloric acid to dissolve 24b, select neutral with water, release 21% potassium hydroxide solution, and wash with water to moisten the neutral. Filter the water, cool it in a furnace for 4~8 minutes until it is lukewarm, put it in the blood, weigh about 10g of the 201-color carrier, burn it in 250ml, weigh about 1.2g of 1H 2O3, about 0.1g of ethylene glycol, add 4U~50m of ethanol, mix them evenly, and put them in a furnace continuously to make the liquid cover the carrier. Place the flow cup on the water, shake the beaker with a belt, dry it until it is loose, and bake it in a 75° oven. Filling: After the outlet end of the color filter (including the inspection end) is filled with a little cotton and cloth, the sugar is empty, and the chromatograph sample is tapped with a small wooden hammer. When the color filter can no longer be filled, remove the small color filter, and plug the other end with a glass ladder: The filling of the color filter is about 2.2 mm in the inner scan, and the inner 3 mm is /. Aging of the column: The newly prepared chromatograph is aged for at least 16 hours in a nitrogen atmosphere with a flow rate of about 8°C and a flow rate of about 30 mL/m. Aging technology response detector: 5.2.3.2.3 Chromatographic data processor or change, 5.2.3.2.4 Injector, 11 = 1. Volumetric syringe: 5.2. 3. 3 Standard sample
HG/T 2973-1999
Prepare the standard sample containing each impurity component by weighing method, its relative concentration is higher than that of the test sample, the pure sample space used for preparing the standard sample is: 1-bar, 2-bar, 3-bar, 4-bar, 5-bar, 6-bar, 7-bar, 8-bar, 9-bar, 10-bar, 11-bar, 12-bar, 13-bar, 14-bar, 15-bar, 16-bar, 17-bar, 18-bar, 19-bar, 20-bar, 21-bar, 22-bar, 23-bar, 24-bar, 25-bar, 26-bar, 27-bar, 28-bar, 29-bar, 29-bar, 20 ... 5.2-3.4 Analysis Step 5.2.3.4.1 Start the chromatograph and make necessary adjustments to make it work stably under the best operating conditions. 5.2.3.4.2 Recommended operating parameters: Components: Approximately 100 °C or more. Suitable sequence: Detector: High 120 °C Pre-test temperature: Vaporization temperature: above 1 °C Suitable flow rate: Thermal conductivity: 18 mm/s The user can select the bridge current value that can meet the specific requirements; Gas flow rate, with hydrogen as the gas, the flow rate is 6/m The user can select the carrier gas flow rate that meets the analysis requirements. The color reader will get the specified line in the above working case, and can start the analysis work. 5.2.3.4.3 External standard calibration Before or after each analysis of the sample, perform external standard calibration with the standard sample. Inject the prepared standard sample continuously for more than 10 times. The area A of each impurity drop or the final height, or the calibration positive number of the impurity drop determined by the chromatographic data processor is used as the external standard for quantitative calculation: 5.2. 3.4.4 Calibration Under the same operating conditions as for analyzing the standard sample, use a microsyringe to inject the sample into the inlet (the injection of the sample and the standard sample is alternated). The number of steps should be more than two. The surface area of each impurity peak is expressed as A: and the final height is used for external standard quantitative calculation. The main feature of this method is the chromatographic quality ratio A (standard actual record). 5.2.3.5 Calculation of analysis results The mass content (X:X, X:X, respectively) expressed as mass percentage can be calculated according to formula (1), formula (2), formula (3), or formula (4) or the impurity content can be directly obtained by the chromatographic data processor. 4.
Y,-F,x
,X,XXX-," the content of nitrogen, one cow glue, two formaldehyde, and three impurities in the sample:, point, center, and more in the standard sample, and oh, two middle late, two middle white content of the remaining mass A. Small, A, eight, one sample, - medium glue, two middle, three middle impurities drag area: (1)
A....1 calibrated with two needles or two H with the work of the pine sample, ammonia, one formaldehyde, "amine, three middle recorded wind average peak rainfall area when using the quotient to determine some, the peak height is replaced by formula 1) or (1) the city. 5.2.3.6 Allow indoor storage 3.2.5 Marking, packaging, transportation, storage and disposal 6.1 The packaging should have product markings including: manufacturer name, product name, trademark, production date or batch number, net content, standard number and "Non-toxic" mark. 6.2 All products approved by the manufacturer should be accompanied by quality certificates. 1. Internal information: manufacturer name, product name, trademark, production date or batch number, net content, standard number and "Non-toxic" mark. 2973—1999
6.3 The product can be placed in a truck or steel drum. The truck and steel drum must be intact and in good condition. The packaging steel drum should be inspected and accepted according to GB325. After installation, the cover should be removed and tightly sealed to prevent leakage.
6.4 The product should not be exposed to the environment and should be stored in a room with low humidity, ventilation, away from fire sources and other dangerous goods to avoid high temperature and noise.
6.5 The transportation of this product should be carried out in accordance with the regulations on road transport and other relevant regulations on the transportation of dangerous goods. For safety reasons
7.1 This product is flammable. Avoid mixing with commercial vehicles and contact with fire. 7.2 This product It has been shown that it is corrosive. When used, avoid contact with membranes and skin. 3 This product should be separated from acids, oxidants and other chemicals. HG/T29/3-1999 Appendix A (Standard Appendix) Typical chromatographic parameters A1 Method for determination of dimethylamine water ionization Typical chromatogram of dimethylamine water concentration Typical chromatogram of dimethylamine water concentration See Figure A1. 1-Air 2-Hydrogen-Methylamine 4-Sodium-Fluorocyanate Figure A1 Typical chromatogram of dimethylamine water concentration A2 Chromatographic operating conditions: 50 °C Vaporization chamber temperature = 37 °C
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