other information
drafter:Zhao Xinxin, Xing Hong, Wu Chongyan, Ge Heping, Zhang Yi
Drafting unit:Shenyang Research Institute of Chemical Industry
Focal point unit:Shenyang Research Institute of Chemical Industry
Proposing unit:Technical Supervision Department of the former Ministry of Chemical Industry of the People's Republic of China
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.: 7481--2000
HG3671--2000
This standard is formulated based on the actual quality of domestic imidacloprid wettable powder and the classification method of the International Cooperation Committee on Pesticide Analysis (CIIAC).
This standard is issued by the Technical Supervision Department of the former Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Beijing Chemical Industry Research Institute. The responsible unit for the reform of this standard: Beijing Chemical Industry Research Institute. The drafting organizations of this standard are: Jiangsu Kesheng Group, 11 Tokyo Pharmaceutical Co., Ltd. The main editors of this standard are: Yue Xinxin, Xing Hong, Guan Genyan, Shu Hezang, Zhang Guche. The standard is under the charge of the National Pesticide Standardization Technical Committee. 73
Chemical Industry Standard of the People's Republic of China
Imidacloprid Wettable Powder
Iaidurluprid Vettnble Other names, structural formulas and basic chemical properties of the active ingredient in Ponders products are as follows: [S] General name: Imidacloprid
CIPA code: 582
Chemical name: (3-chloropyridylmethyl)-2-nitroimidazolidin-2-ylamine Structural formula,
Empirical formula: CH.CN.O
Moisture content: 235.7 (according to the international atomic mass standard of 1990) Biological activity:
Melting point, 144℃
Vapor pressure 20: 200mPa
Degree of fragmentation g/L, 2 0> Water.51, acetonitrile 50, benzene 5.58, difluoromethane bb, isocyanate 1.2H+3671—2000
Stability: Stable under normal storage conditions and in volatile and micro-solid media; Decomposed within a range of 1 in a reducing water environment
This standard specifies the requirements, test methods and marking, labeling, packaging and transportation of pyrimidine spherical mixed agents. This standard is applicable to pyrimidine spherical powders prepared by adding 1 to the original drug, bulk materials and active ingredients of the standard. 2 Reference standards
~ The provisions contained in the standard are cited in this standard and constitute the text of this standard. When this standard is published, the version shown is valid. All standard parts are subject to revision. The parties using the standard should use the following standard when the latest version is possible. （/T1f011993 Determination of 5H value of pesticides Ancient method GB/T1604-1995 Current acceptance rules for commercial pesticides GB1619791989 Commercial acceptance standards www.bzxz.net
379-1995 General rules for pesticide packaging
（/T54511S85 Determination of mixability of wettable powders for pesticides Pesticide tax avoidance Suspension rate determination method GR/1483E-15U3
GR/T161=(1-1995 Method for determining the fineness of table powders and flexible powders 3 Requirements
3-1 External alkane: The loose content of the group should be uniform and there should be no lumps. Approved by the State Red Petroleum and Chemical Industry on 2000-06-05 2001- 03-01 Implementation
HG3671-20G0
32. The control index of pyrrolidone hygroscopic powder should meet the requirements of Table 1. The instantaneous index of hygroscopic wettable powder is n5
the content of pyrrolidone in the powder
and the derivative,
please pass the test (through 45n: standard research)-%
and the test method is difficult to carry out
Note: Under normal circumstances, the accelerated test is carried out once every % of the class, and the 4 test method is 6.0~·16.G
according to the "powder and hygroscopic powder sampling method" in (FI3/T1%051979 (8S). Use the machine effect table method to determine the sample size. 3.1.2 Specific tests
High performance chromatography method. The specific test can be carried out simultaneously with the determination of imidacloprid content: Under the same chromatographic conditions, the retention time of the sample solvent and the retention time of imidacloprid in the standard sample shall have a relative difference of less than 1.5%: When the above methods have doubts about the identification of the active ingredients, other effective methods can be used for identification. 4.3 Determination of the content of imidacloprid
4.3.1 Method summary
The test should be carried out by decomposition, with monoalcohol and water as the mobile phase, using NevapakCuim as the chromatographic medium and a UV variable wavelength detector: The samples in the test group should be Separation and determination of pyrrolidone. 4.3.2 Apparatus and equipment
Acquisition phase chromatography: It has a UV variable length detector, a colorimetric data processor,
Package: 3.9mm td) × 15mm non-swirl column, an inner surface Novupk5am deionized water filter, and the pore size of the filter membrane is about .L.
Micro-injector: 5UL,
4.3.3 Reagents and liquids
Methanol: chromatographic grade.
Water: freshly distilled water.
Sample, 8. .
4.3.4 Phase chromatography coupling conditions
Mobile phase: ethanol (water) · 4.
Mobile phase resolution: 0.1 ml./min,
Humidity: room temperature (humidity change: 2T:) Detection time: 250m
Injection volume.5
Retention time: 5.in.
HG3671-2000
The above liquid chromatography operating conditions are typical operating parameters. According to the different return solution points, the specific operating parameters can be appropriately adjusted to obtain the best effect. The typical high-efficiency phase chromatogram of pyridine is shown in Figure 1. 4.3.5 Determination steps of wettable non-powders
4.3.5.1 Preparation of standard sample
Weigh 0.1 g of pyrrolidone (accurate to 0.002 g) in a 10.9 mL volumetric bottle, add appropriate amount of diethyl ether solution, shake in a vortex for 5 min, return to original volume, and make up to volume; use a pipette to transfer 5 L + 6 mL of the above liquid into a 50 mL volumetric chromatogram. Use a distilled water to make up to the volume.
4.3 5-2 Preparation of sample
Weigh 5.1 g of pyrrolidone (accurate to 0.0002 g) in a 10.9 mL volumetric bottle. Add appropriate amount of diethyl ether solution, incubate in an ultrasonic bath for 5 min, make up to volume; use a 1.4 mm diameter diaphragm to filter. 4.3.5.3 Under the above operating conditions, after the instrument is stable, continue to inject the standard solution until the change in the adjacent standard solution is less than 1. Then proceed in the order of standard solution, sample solution, and sample solution. 4.3.6 Calculate the content of the sample expressed in mass number according to the formula: 77
Where: 4,
IG 3671—2000
X=AmXIO
Average value of the product of the peaks of pyrrolidone in the standard sample
Average value of the peaks of pyrrolidone in the sample, A
Quality of the standard sample·Four:
Approximately the sample is determined·R1
The pressure fraction of the standard sample, %,
4.3-7Tolerance
The result of two measurements should be less than 0.1% for wettable powder and less than 1% for wettable powder. Take the arithmetic mean as the measurement result.
4.4 Determination of pH
It is carried out according to the pH calculation method in GB/T1601-1993. 4.5 Determination of suspension
4.5.1 Determination method
Adapt GB/T148
Weigh 0.1 μl of the test sample (accurate to 0.0 μl). Transfer the remaining 1/1 of the suspension and the precipitate to 130 ml of 1 mL ethanol. Add 25 μl of the residue to a 100 ml volumetric flask in 3 times. Remove the bacteria in an ultraviolet filter for 5 min, return to room temperature, make up to volume, and aliquot. Filter with a pore size of 0.45 μm. Determine the quality according to the method in step 3 and calculate its total elasticity. 4.5.2 Permissible difference
If the test results are parallel, the difference should not exceed 5%. The arithmetic mean is taken as the determination boundary: 2.6 Determination of immersion time
According to GB/T5151.
4.7 Determination of thickness
According to the pump-screen method of GB/T30--1995. 4.8 Accelerated storage test
4.8.1 Method summary
Through the pressurized heat rot test, the product is accelerated to age. The performance changes of the product stored at room temperature are measured. 4.2 Instruments and equipment
Machine and box: (12).
Beaker, 250ml, inner diameter 6.35.5cm.
The diameter of the plate should match the cup, and the average bed of 2.45ka should be produced.
Wrap the 236 sample around the body without any positive force, so that the sample can be evenly layered. Press the air plate on the sample, and the cup should be placed in the supply and sales, at 54, store for 14 days, take out the beaker, put it in the container, and cool the sample to room temperature. Complete the determination of the active ingredient content and suspension rate within 241. The test results of the active ingredient plate are allowed to drop to S? before expansion, and the suspension rate should still meet the standard requirements. 4.9 Inspection and acceptance of products
It should comply with the provisions of GB/T11, the limit value processing, and the standard value comparison method. 5 Marking, labeling, packaging, storage and transportation
5.1 The marking, labeling and packaging of pyrrolidone wettable powder should comply with the provisions of B3796. 5.2 Pyridoxine wettable powder should be packaged in plastic composite film bags: the net content of each bag should not exceed 1gdg, the outer packaging should be cardboard or plastic, and the net content should not exceed 1ukg. 5-3 According to the user's cumulative request or order agreement, other forms of packaging can be used, but they must comply with the provisions of GR796. 5.4 Pyridoxine wettable powder packages should be stored in a ventilated and low-lying warehouse: 5.5 During transportation, strictly prevent moisture and sunlight, do not mix with food, drugs, and materials, avoid contact with skin, eyes, and prevent people from mouth and nose: Safety: This product is a low-toxic preparation, which is harmful to the human body. Others who use this product should wear protective gloves, masks, and clean protective clothing. After use, wash with soap and water immediately. If poisoning occurs, go to the hospital for examination and treatment in time. 5.7 Warranty period Under the specified transportation conditions, the warranty period of pyrimidine is 2 years from the date of production.
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