Some standard content:
HG/T2856-1997
This standard is a revision of GB/T9555-88 "Mepiridone Technical Drug". The main points of this standard revision are as follows:
1 The revision of this standard is mainly the rewriting of the format and text, and the technical indicators and analysis methods are basically the same as GB/T9555--88. 2 The foreword is added.
3 It is stipulated that the rounding value comparison method is used for the treatment of limit values. 4 The chapter on inspection rules is cancelled, and its main contents "sampling" and "inspection rules" are placed as two articles at the beginning and end of the chapter on test methods respectively;
5 Some titles have been changed: "Subject content and scope of application" is changed to "scope", "technical requirements" is changed to "requirements", "inspection methods" is changed to "test methods", and "packaging, marking, transportation, storage" is changed to "marking, labeling, packaging, storage and transportation". In the last chapter, the contents of "safety" and "warranty period" are supplemented.
This standard replaces GB/T9555-88 from the date of implementation. 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 jurisdiction of the Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry. The drafting unit of this standard: Shenyang Institute of Chemical Industry of the Ministry of Chemical Industry. The main drafters of this standard: Lou Shaowei and Zhang Pilong. 1016
Chemical Industry Standard of the People's Republic of China
Mepiqunt chloride technical
Mepiqunt chloride technical
The secret name, structural formula and basic physicochemical parameters of Mepiqunt chloride are as follows: ISO import name: Mepiguatchloride Trade name: Mepiguat chloride, Mepiguat chloride, Mepiguat chloride, Mepiguat chloride, etc. CIPAC digital code: 440
Chemical name: NN-dimethyl chloride Compound Structure:
Experimental CNCI
Relative molecular mass: 149.66 (according to the 1993 international relative atomic mass meter): Biological activity: It has the effect of regulating plant growth; Melting point (C): 285 (decomposition)
Vapor pressure (200): 1X10-sPa
G/T 2856--1997
Generation GB/T9555-88
Dissolution (g/L, 20C): water 1000 ethanol 162 chloroform 11, acetyl glucoside 1 ether ≤1, cyclopentane <1 acid acetaldehyde 1, olive oil 1
Stability The stability of methyl methacrylate is very good. It can be effectively maintained for two years. 1 Scope
This standard specifies the requirements, test methods and labeling, marking, packaging, storage and transportation of methyl methacrylate. This standard is applicable to methyl methacrylate made of methyl methacrylate and impurities generated in its production. 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 issued, the versions shown are valid. All standards will be revised. All parties using this standard are advised to discuss the possibility of using the latest versions of the following standards. GB/T601--88 Preparation of standard solution for titration analysis of chemical reagents (volume analysis) GB/T1604--1995 Acceptance rules for commercial pesticides GB/T1605-79(89) Sampling method for commercial pesticides GB3796-83 General rules for pesticide packaging
3 Requirements
31 Appearance: white or slightly yellowish body,
Approved by the Ministry of Chemical Industry of the People's Republic of China on March 11, 1997 and implemented on January 1, 1998
3.2 The technical version of methylphenidate shall comply with the requirements of Table 1.
Methylpiperidinium content
N-methylpiperidinium hydrochloride content
4 Test methods
4.1 Sampling
HG/T2856—1997
Table 1 Control item indicators of methylpiperidinium technical
First-class products
Qualified products
According to the "Sampling of solid state" method in GB/T1605. Use the random number table method to determine the number of packages to be sampled; the final sampling volume should be no less than 250g.
4.2 Identification test
The identification of the sample can be carried out by paper chromatography: use 18cm×15cm rapid chromatography filter paper Xinhua No. 3 (or filter paper with equivalent performance), trifluoromethane + methanol + ammonia water = 6 + 4 + 1 (V/V) as the developing solvent, spot the sample solution, and use the methylpiperidinium standard sample as a reference. The Rt value of a certain spot obtained by development and the spot developed simultaneously with the control standard solution should be consistent. 4.3 Determination of the content of methylpiperidinium and N-methylpiperidinium hydrochloride 4.3.1 Summary of the method
The sample is dissolved in water, and methylpiperidinium and methylpiperidinium hydrochloride form a complex precipitate with sodium tetraphenylborate, which is dried to constant weight. The methylpiperidinium hydrochloride in the precipitate is dissolved with dimethylformamide, and non-aqueous titration is performed with tetrabutylammonium hydroxide to determine the content of methylpiperidinium hydrochloride and calculate the content of methylpiperidinium.
4.3.2 Reagents and solutions
Nitric acid;
Toluene;
Anhydrous methanol;
Acetone;
Silver oxide;
Benzoic acid;
Isopropanol;
N,N-dimethylformamide;
Tetrabutylammonium iodide;
Crystalline aluminum chloride (AlCl:·6H20): 200g/L; Sodium tetraphenylborate: 20g/L, freshly prepared, filtered; Thymol blue indicator solution: 3g/L methanol solution; Silver nitrate solution: 17g/L,
Tetrabutylammonium hydroxide standard titration solution: c[(C,H,),NOH]=0.1 mol/L; the preparation and calibration method is as follows: weigh 40g of tetrabutylammonium iodide (accurate to 0.0002g), place it in a 250mL conical flask, add 100mL of anhydrous methanol, shake to dissolve the sample, add 20g of silver oxide, cover with a stopper, shake for 1h, centrifuge, take 2 drops of clear liquid and place them on a drip plate, add 2 drops of 17g/L silver nitrate solution, if a yellow precipitate is generated, add 2 drops of concentrated nitric acid, the precipitate dissolves, indicating that there are iodide ions, and 2g of silver oxide should be added, cover with a stopper, shake for 30min, repeat the above inspection until no precipitation is generated in the upper clear liquid. Take the upper clear liquid and place it in a 1000mL volumetric flask, wash the original container and the precipitate with toluene 3 times, 50mL each time, and after centrifugation of the washing liquid, the upper clear liquid is merged into the volumetric flask, fixed to volume with toluene, filled with nitrogen, and sealed for storage. If silver iodide or silver oxide precipitates are precipitated, the upper clear liquid should be separated immediately. Calibration: Weigh 0.3g of benzoic acid standard (accurate to 0.0002g), place it in a 50mL volumetric flask, dissolve it with dimethylformamide and dilute it to the scale, seal and shake well. Use a pipette to draw 10mL of benzoic acid solution, place it in a 150mL iodine volumetric flask, add 3 drops of thymol blue indicator solution, shake, and titrate with a newly prepared tetrabutylammonium hydroxide standard titration solution until the blue color is the end point. At the same time, make a blank determination. The concentration of tetrabutylammonium hydroxide standard titration solution c[(C,H,),NOH], expressed in mol/L, is calculated according to formula (1): C
m×
(Vi-Vo) ×
(V - V.) × 0.610 5
Wherein: V,—-the volume of tetrabutylammonium hydroxide standard titration solution consumed in titrating benzoic acid solution, mL; —the volume of tetrabutylammonium hydroxide standard titration solution consumed in titrating blank solution, mL; V.
-the mass of benzoic acid, nominal,
122.1——the relative molecular mass of benzoic acid. Tetrabutylammonium hydroxide standard titration solution, cL(C,H.),NOH] = 0.02mol/L; preparation method is as follows: · (1) ）
Pull 20mL of the above-standard 0.1mol/L tetrabutylammonium hydroxide standard titration solution into a 100mL volumetric flask, add 5mL of methanol, and then dilute to the scale with toluene, shake well, and the solution should be replaced once a week. 4.3.3 Instruments
One set of suction filtration device,
Micro burette: capacity 10mL, minimum graduation 0.05mL, with 250mL storage bottle; glass sand core funnel: G4, 40mL.
4.3.4 Determination steps
Weigh 1.5-2g (accurate to 0.0002g) of methylpiperidinium chloride original drug, place it in a 100mL volumetric flask, add water to dissolve and dilute to the scale, shake well. Use a pipette to draw 10mL of the sample solution, place it in a 150mL beaker, add 40mL of water and 1 drop of crystalline aluminum fluoride solution, shake well, add 50mL of sodium tetraphenylborate solution, stir evenly, and let it stand for 30 minutes to allow it to precipitate completely. Use a glass sand core funnel that has reached a constant weight to perform vacuum filtration, wash the precipitate with 40~50mL of water, dry it in an oven at 105℃ to constant weight, and weigh it. Carefully dissolve the precipitate in the glass sand core funnel with 10mL of dimethylformamide and transfer it to a 150mL conical flask, wash it with 30mL of acetone, add 20mL of isopropanol,3 drops of thymol blue indicator solution are titrated with 0.02 mol/L tetrabutylammonium hydroxide standard titration solution until the blue color is the end point. At the same time, a blank determination is performed. 4.3.5 Calculation
The content of methylpiperidinium expressed as mass percentage X1 is calculated according to formula (2): (ml - m2) × 149. 66 × 100 = IX
m×433.5×
(m -- mz) × 345. 2
The content of N-methylpiperidinium hydrochloride expressed as mass percentage X2 is calculated according to formula (3): Xx = c(VI-Vo) × 135. 66 × 100 = c(V/-Vo) × 135. 66m×1000×
Wherein: c
V. —
actual concentration of tetrabutylammonium hydroxide standard titration solution, mol/L; m
-volume of tetrabutylammonium hydroxide standard titration solution consumed by titrating sample solution, mL-volume of tetrabutylammonium hydroxide standard titration solution consumed by titrating blank solution, mL; mass of tetraphenylboron complex of methylpiperidinium and N-methylpiperidinium hydrochloride, g, mass of tetraphenylboron complex of N-methylpiperidinium hydrochloride, g; can be calculated according to formula (4): c: (Vi - Vo) × 419. 5
m~mass of sample, g,
433.5--relative molecular mass of tetraphenylboron complex of methylpiperidinium; 419.5--relative molecular mass of tetraphenylboron complex of N-methylpiperidinium hydrochloride. ·（2）
+（4）
4.3.6 Allowable differencebzxZ.net
HG/T2856—1997
The difference between two parallel determination results of methylpiperidin content shall not exceed 1.0%4.4 Inspection and acceptance of products
Should comply with the relevant provisions of GB/T1604, limit value processing, and rounded value comparison method. 5 Marking, labeling, packaging, storage and transportation
5.1 The marking, labeling and packaging of methylpiperidin technical shall comply with the relevant provisions of GB3796, and shall have the production license number and trademark. 5.2 The methylpiperidin technical can be packaged in glass bottles or plastic bottles, 5g or 10g per bottle, and must be sealed and moisture-proof. The outer packaging is made of calcium plastic box or cardboard box, and the net weight of each box shall not exceed 15kg.
5.3 According to user requirements or ordering agreement, other forms of packaging can be used, but they must comply with the relevant provisions of GB3796. 5.4 Packages should be stored in ventilated, dry warehouses. 5.5 During storage and transportation, strictly prevent moisture and sunlight, do not mix with food, seeds, feed, avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: Methylpiperidone is low-toxic, non-flammable, non-corrosive, and belongs to the low-toxic pesticide category. Methylpiperidone is non-irritating to the respiratory tract, skin, and eyes, and is non-toxic to fish, birds, and bees. In case of poisoning, gastrointestinal lavage should be performed. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of Methylpiperidone is 2 years from the date of production. 1020
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