Some standard content:
TCS±65. 100
Chemical Industry Standard of the People's Republic of China
(2000)
Published on 2000-06-05
Implemented on 200103-01
Published by the State Administration of Petroleum and Chemical Industry
Registration No. 748:2000
Hf3670-2000
This standard is formulated with reference to the actual quantity of domestic imidacloprid technical and the analysis method of the International Pesticide Analysis Cooperation (CIPAC). This standard was proposed by the Technical Supervision Department of the former Ministry of Chemical Industry of the People's Republic of China: This standard was submitted by Jiuyang Chemical Research Institute. The responsible unit for drafting this standard is Jiuyang Chemical Research Institute. The participating drafting units of this standard are Jiangsu Keshenglai Group and Shandong Jingzun Pharmaceutical Co., Ltd. The main drafters of this standard are Yue Xinsuo, Xing Hong, Chong Yan, Shan Liaoban, and Zhang E. This standard is issued by the National Pesticide Standardization Technical Committee for the purpose of qualification interpretation. 5
Chemical Industry Standard of the People's Republic of China
Imidaeloprid Technical Material
Imidaeloprid Technkcal
The pseudonym, structural formula and herbal chemical structure of the active ingredient of this product are as follows: ISO applicable name: lmicuzlopric.
CIPAC digital code: 582
Chemical name: 1.(6-chloropyritinylmethyl-4-nitro-2-ylamine)Binding formula:
Actual formula: C,HCN.O
Relative molecular weight: 255.0 (international relative atomic mass per 15 years)Biological activity: insecticide
Temperature point: 144r
Vapor pressure (20C>.200mPa
Degree of solubility (g/1.30) in water n.61, ethyl acetate 50, benzene 0.8, methane 5.5L, propanol 1.2HG 3670—2000
Stability; Stable under normal storage conditions and in neutral and limiting media: Stable in non-aqueous media under slow temperature Part 1 Scope
This standard specifies the requirements, test methods, marking, labeling, packaging, storage and transportation of pyridoxine technical materials. This standard is applicable to pyridoxine technical materials containing impurities produced by pyridoxine and its producers. 2 Referenced standards
The provisions contained in the following standards become the provisions of the standards through reference in this standard. When this standard was published, the version shown was All standards will be revised and all parties using the standards shall use the latest versions of the following standards: GB/161-1988 Chemical reagents for quantitative analysis (preparation of standard solutions for quantitative analysis) GB/T1501-1993 Pesticide pH value determination tablets GB/T604-1995 Rules for the acceptance of commercial pesticides GB/T615-15U Method for sampling commercial pesticides 33796-1999 General rules for the packaging of pesticides 3 Requirements 3.1 External specifications Yellow to light yellow solid wood element with visible exogenous hydroxyl groups. 3.2 Control indicators of pyridoxine technical should meet the requirements of Table 1. Approved by the State Administration of Petroleum and Chemical Industry on June 5, 2000, and implemented on March 1, 2001. This product contains: Acidity (ITS), calculated by NaCHI. Dimethylformamide. HG36702000 Control indicators of pyridoxine technical tt||洋: The production situation of the positive potential cattle has changed. The base metal limit has not been melted for at least one month. 4. Transmission method
4.1 Sampling
·Qualified products
According to the "original selection" method in (/T1605-1979 (199), the packaging of the sample is determined by the random number coupon method. The final sampling disk is not less than 100g:
4.2 Identification test
High performance subtraction chromatography: This identification test can be carried out together with the determination of pyridine content. Under the same chromatographic operating conditions, the retention time of a certain peak in the sample package and the retention time of the pyridine color in the standard sample solution should have a difference of less than 1.5 infrared light: the test environment and the standard solution are at 1000-~40) cm-wavenumber. There is no obvious difference in the infrared light diagram. See Figure 1. Figure:
Infrared spectrum of the sample
4.3 Determination of the content of pyrimidine
4.3.1 FTIR
The sample was dissolved in alcohol, with methanol and water as the mobile phase, using Nuvk core, chromatographic and UV-sensitive detector as the filler, and the pyrimidine bands in the test column were separated and determined. 4.32 High-efficiency phase acquisition chromatograph: with UV variable wavelength detection end. Chromatographic data processor:
HG3670-2000
Chromatographic column: 3.9mm (id) [50mn stainless steel. Novapak Cw, ium filler filter: cell membrane pore size 0.45pm.
Micro-injector: 50.,
4-3.3 Reagents and safi
coin, chromatographic grade.
Water, freshly distilled and twice distilled water.
Imidacloprid standard sample, Bacon content greater than or equal to 99.0%, 4.3.4 High performance quasi-phase chromatography working conditions
Mobile phase: methanol (water) = 1U/50.
Mobile phase flow rate: (1.4rrl./mia
Temperature: vehicle temperature (temperature difference should not exceed 2), detection wavelength: 260nm,
Injection volume, 5 minutes.
Retention time: 1.0min.
.The above-mentioned operating conditions are required for typical operating results. According to the characteristics of different instruments, the given operating parameters should be appropriately adjusted to obtain the best operating results. A typical chromatogram of the pyrimidine technical drug is shown in Figure 2. This standard
Figure 2 HPLC chromatogram of the pyrimidine technical drug
4.3.5 Determination
4.3.5.1 Preparation of standard solution
EIC: 36 70—2000
Weigh 0.1% pyrimidine sample (accurate to C.9302), place it in a 13)ml volumetric flask. Add appropriate amount of methanol to dissolve, store in an ultrasonic bath for 5min, return to volume, fix, collect 1ml of the above solution by pipetting and place in a 50ml volumetric flask, make up to volume with methanol, probe
4.3.5.2 Preparation of test tube
Weigh 0.6% pyrimidine sample (accurate to C.9302), place it in a 10ml volumetric flask, add appropriate amount of methanol to dissolve, store in an ultrasonic bath for 5min, fix the temperature, and stir; use a pipette to mix the above solution, put it in a 50ml volumetric flask, stir with methanol.
4.35.3 Test
Under the above working conditions, after the required base is determined, inject the standard sample solution continuously until the area of the two adjacent pyrrolidone peaks is less than 1.5 relative to the cavitation, and then perform the test in the order of standard sample injection, sample injection, sample injection, and standard injection. 4.3. 6 The content of acetylcholine in the sample indicated by mass fraction, % is calculated according to the formula: Aan,r
Wu: A,
The average value of the peak area of acetylcholine in the standard sample solution and the half-mean value of the acetylcholine concentration in the sample solution: The mass fraction of the standard sample:
The mass fraction of the test sample:
The amount of acetylcholine in the standard sample, 4-3.7 The allowable difference
The difference between the results of two strict determinations should not be greater than 1.b%, and the arithmetic average is taken as the determination result. 4.4 The determination of olefin reduction
4.4 .1 Instruments and equipment
Drying 105 ± 2) center,
weighing bottle: inner diameter 2l
lower apparatus,
4.4.2, after finishing the steps
each time you put 1U of sample in the drying oven, take out the sample and cool it to room temperature, weigh the sample on the weighing plate (accurate to 0.0002), until the bottle is weighed, there is 1U of sample in the bottle, put it down, weigh it (accurate to 0.n002), put the weighing plate bottle in the drying oven, do not add any weight, after drying for 1h, add weight, take it out and put it in the lower apparatus to cool to room temperature, weigh it. 4.4.3 Calculation
The mass fraction of the sample x is calculated according to formula (2): x,.
The air volume of the test group!
Quality of the sample and the weighed sample before drying
4.4.4 Tolerance
The deviation between the results of two parallel determinations shall not exceed 15%. Take the arithmetic half mean as the determination result. 4.5 Determination of acidity
4.5.1 Reagents and reagents
The standard titration rate of tin oxide is: cV(>TT)=0.G2mn1/I..Prepare according to GR/T501. 71
HG3670-2000
Standard titration solution: cIn a 25 mL flask, add 0 mL of the test solution, add 5% of the solution, if the solution is yellow, the acidity of the solution is determined; if the solution is blue, the solution is titrated with standard sodium hydride to a blue end point: At the same time, a blank determination is performed. The acidity of the sample expressed as mass fraction X (%) is calculated according to formula (3-1): X = sV: Y3x0 049 × 1cn
b) When the solution is yellow, the blank is determined by titrating with standard hydrochloric acid solution until the solution is reduced to yellow as the end point. The acidity of the sample expressed as mass fraction X (%) is calculated according to formula (3-2): rr.-V,>X0. 040
Vol/L of standard titration solution of sodium hydroxide (salt) : V. I: The volume of standard titration solution consumed by the test solution, ml. The volume of standard titration solution consumed by the blank solution, ml.; m
The mass of the sample
is equivalent to 1.00ml of standard titration solution of sodium hydroxide - (VaC)TI) = 1.CCOmol/L The value expressed in grams of acid is 3.049...
Mass:
is equivalent to 1.00nm hydrochloric acid standard titration solution [c(HL) - 1.00nmol/. The amount of sodium hydroxide expressed in grams
4.5.3 The allowable difference
The relative difference between the results of two and a half determinations should not be greater than ± 0.01. Take the arithmetic mean as the determination result. 4.6 Determination of insoluble matter in dimethylformamide
4.6.1 Reagents
Dimethylformamide
flask, 25 cm3: bZxz.net
Glass core: G..
Sulfate box: (11c ± 2)
4.6.3 Take 1) g of sample accurately to 0.01 and place it in a 250 cm flask, add 60 ml of formamide gel and shake until the substance is dissolved. Use a 60-mL bottle to remove the excess water, wash it twice with 100 mL of straw, and draw out the remaining 110 mL of the sample. Store it in a cold room for 33 minutes. The content of insoluble matter in the sample, expressed as mass fraction, is calculated according to formula (ii). m×100
In the formula, the quality after the test is:
And the quality of the test is:
The quality range of the test is:
4.6.4 Tolerance
H3670-2000
If the sum of the results of two parallel determination stations is not greater than the upper 25 rings, take the arithmetic mean value as the demarcation result. 4.7 Inspection and acceptance of products
shall be in accordance with the provisions of H/T1601: limit numerical processing, use the value comparison method. 5 Marking, labeling, packaging, purchase and transportation
5.1 The marking and labeling of the original drug shall also comply with the provisions of GB36. 5.2 The original drug is about 10 millimeters H, and the inner PVC drum or cardboard drum (with plastic bags) is packed at the entrance of 1 , net content of each barrel is 50kg. 5.3 According to user requirements or order agreement, other forms of packaging can be used. But it must comply with the provisions of G3796. 5.4 The original packaging of the drug should be stored in a dry room away from moisture. 5.5 During transportation, it must be kept away from moisture and food, seeds, and feed. Avoid contact with skin and insects, and prevent inhalation by mouth and nose. 6.6 Safety, this product is a medium-acting insecticide. It can enter through the skin. When using this product, you should wear protective gloves, wear clean protective clothing, and wash it with fertilizer and water immediately after use. If poisoning occurs, go to the doctor for treatment in time. 5.7 Warranty period
Under the formulated storage and transportation policy, the warranty period of the drug is one year from the production month. 72
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