NY/T 1860.4-2010 Guidelines for the determination of physical and chemical properties of pesticides Technical stability NY/T1860.4-2010 |tt||Standard download decompression password: www.bzxz.net
This part specifies the basic requirements for the test method, result evaluation and test report writing for the determination of the thermal stability of pesticide technical (including parent drug) under the influence of temperature, humidity, light and other conditions and the chemical stability to metal/metal ions. This part is applicable to the thermal stability and chemical stability test of pesticide technical to metal/metal ions for the application of pesticide registration.

ICS65.020
Agricultural Industry Standard of the People's Republic of China
NY/T 1860.4—2010
Guidance on the determination of physico-chemical properties of pesticidesPart 4 : Technical material stabilityPublished on May 20, 2010
Implemented from September 1, 2010
Published by the Ministry of Agriculture of the People's Republic of China
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VYT1860 "Guidance on the determination of physico-chemical properties of pesticides" is a series of standards, with a total of 22 parts: Part 1: pH value,
Part 2: Acidity (alkalinity)
Part 3: Appearance;
Part 1: Stability of technical materials;||tt| |-Part 5: UV/Visible Absorption:
-Part 5: Explosiveness:
-Part 7: Photocatalytic Properties in Water;
-Part 8: Alcohol/Water Partition Coefficient;
-Part 9: Hydrolysis;
Part 10: Oxidation-Reduction/Chemical Incompatibility:
Part 11: Flash Point;
Part 12: Fire Point:
Part 13: Miscibility with Non-Polar Organic Solvents;
Part 14: Saturated Vapor Pressure;
-Part 2. Part 15: Flammability of solids;
: - Part 16: Corrosiveness of packaging materials; —- Part 17: Density;
Part 18: Specific rotation;
Part 19: Boiling point
Part 20: Melting point:
- Part 21: Viscosity;
Part 22: Solubility.
This part is Part 1 of the "Guidelines for the Determination of Physical and Chemical Properties of Pesticides". This part is proposed and coordinated by the Crop Production Management Department of the Ministry of Agriculture. Responsible units for this part: Pesticide Control Institute of the Ministry of Agriculture and Hebei Pesticide Control Institute. The main authors of this part: Yu Chai, Gan Xuejie, Li Youshun, Zhang Yanfen, Bo Rui, Luo Shengjun. NY/T 1860. 4—2010. 1 Scope. Guidelines for the determination of physical and chemical properties of pesticides. Part 4: Stability of technical materials. NY/T 1860.4—2010. This part specifies the test methods, result evaluation and basic requirements for the preparation of test reports for the determination of thermal stability and chemical stability of pesticide technical materials (including parent materials) to metals/metal ions under the influence of temperature, humidity, light and other conditions. This part is applicable to the thermal stability and chemical stability tests of pesticide technical materials to metals/metal ions for the application of pesticide registration. 2 Terms and definitions
The following terms and definitions apply to this part.
Thermal stability test includes two determination methods: differential thermal analysis and thermogravimetric analysis. Differential thermal analysis (DTA) is a technique that measures the relationship between the temperature difference and the temperature between a substance and a reference substance at a programmed chamber temperature; thermal gravimetric analysis (TA) refers to the observation of the change in the mass of a sample with temperature or time under programmed temperature. 2.2
Metal/metallic ion chemical stability test refers to the investigation of the stability of the pesticide to metals or metal ions under the coexistence of the pesticide technical and metals or metal ions. 3 Requirements
3.1 The pesticide thermal stability test and chemical stability test should generally be carried out on samples from the same batch. 3.2 The sample used for stability test should be a product produced on a certain scale. It can represent the quality of the product under the conditions of scale production. The batch of technical drug should meet the requirements of the medium scale. The synthesis process, method and steps of technical drug should be consistent with the production scale. 3.3 The thermal stability of pesticides can be carried out by IDTA or TGA method. 3.4 Storage conditions
The stability test is required to be carried out under certain temperature, temperature and light conditions. The setting of these conditions should fully consider the packaging and environmental factors that the pesticide can encounter during storage, transportation and use. 3.5 Environmental control and detection
Various environmental parameters required by the test conditions should be controlled and monitored in the stability test. 4 Test methods
4.1 Thermal stability
4.1.1 DTA method
4.1.1.1 Instrument
Differential thermal analyzer, basic parameters: range: -2000#V; temperature range: home temperature to 850, heating rate: 0℃/min~~100℃/min; temperature accuracy: 0.1℃.
4. 1. 1.2 Test requirements
1) Use different types of sample containers, such as knocked or sealed glass test tubes, gold toilet trays, and the tester is suitable for determination under aerobic conditions.
NY/T 1860.4—2010
2) The test gas is nitrogen or air. When the test gas is air, the sample should be in a loose container. 3) Select an inert reference material that does not change within the test temperature range. The thermal conductivity or heat capacity of the reference material and the sample should be similar. Alumina is an inert material that can be used in most cases. 4.1.1.3 Test steps
4. 1.1.3. 1 Test conditions
Seal 5mg to 50mg of sample in a sample container. Control the heating rate within the range of 2℃/min~20℃/min. 4. 1. 1. 3. 2 Normal pressure DTA
First, record the TTA diagram of the substance under normal pressure. If a thermal effect occurs between room temperature and 150℃, that is, there is an absorption peak or exothermic peak, the following procedures should be followed. 1) When the drop is caused by an exothermic reaction, it is determined to be a decomposition reaction. 2) When the peak is caused by an endothermic reaction, the temperature corresponding to the peak should be compared with the melting point of the substance. If the peak is caused by an endothermic reaction unrelated to the melting point of the substance, proceed according to 1.1.1.8.3. 4.1.1.3.3 Pressurized DTA
Repeat the DIA test at a higher pressure (1X106Pa5×10°Pa) or in a sealed sample container. If the peak shifts to a higher temperature, it is caused by the higher temperature. If the endothermic effect is not caused by melting or evaporation, proceed according to 4.1.1.3.4. 4.1.1.3.4 Cyclic ITA
Repeat the heating cycle around the peak temperature. If the peak disappears, it is determined that a chemical change has occurred. 4.1.2 TGA method
4.1.2.1 Instrument
Thermogravimetric analyzer, basic parameters: Temperature range: 20℃~1000℃ Heating or cooling rate: 0℃/min～100℃/tmin Weighing cell range: 0~-2000mg+ Vacuum degree can reach: 1×10°Pa~2×102Pa. 4.1.2.2 Test requirements
The gases used in the test are usually ammonia and argon gas. When testing oxidation stability and ductility, argon gas should be selected as the test gas. 4.1.2.3 Test steps and judgment
4.1.2.3.1 Test conditions
Place 10mg~500mg of sample in nitrogen and air and heat it. The heating rate should be in the range of 2℃/nain~20%/min. Heat the sample from room temperature to 150℃.
4. 1. 2. 3. 2 TGA test
1) If the mass loss is not caused by the volatilization of the test substance, it is determined that there is a decomposition reaction in the test sample; 2) If decomposition is observed at below 150℃, the decomposition rate is determined by isothermal measurement. 4.2 Chemical stability test of metal/metal ion 4.2.1 Instrument www.bzxz.net
Constant temperature box, temperature control accuracy is -1
4.2.2 Determination
Weigh about 10g of sample (accurate to 0.01g) and add appropriate amount (accurate to 0.01g, determined according to the actual packaging and simulation surface of the sample) of two metals and their metal ion salts (such as iron powder and ferrous acetate, aluminum powder and aluminum acetate, lead powder and lead acetic acid). After grinding and mixing, measure and calculate the mass fraction (X) of the test object. Put the mixed sample into a clean ampoule and cool the ampoule in an ice bath. Seal with an alcohol torch for 11. Place the sealed ampoule into a metal container, place the container in a (5-2)℃ constant temperature box for 14 days, usually at home temperature (54±2)℃ for 14 days, take samples on the 1st, 2nd, 7th and 14th day during the test, and determine the mass fraction of the test substance (Y1),And compare with the sample before storage (0d) respectively. Calculate the decomposition rate. 2
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4.2.3 Result calculation
The decomposition rate of the sample is calculated according to formula (1):
Wu Zhong:
X--the decomposition rate of the sample, %;
X--the mass fraction of the sample before storage, %: X--the mass fraction of the sample after storage, %. The calculation results shall be accurate to two decimal places.
5 Test report
Xe-Xi
The report shall provide sufficient details, including at least the following contents: NY/T1860.4—2010
1) Sample description: It shall include the name, specification, batch number, source, and production period of the pesticide sample to be tested. The properties of the packaging/sealing system shall be accurately described, such as the type, shape and color of the packaging material. Test conditions: It shall clearly include the temperature, light intensity, relative humidity, device type, container, accurate information of the test object and reference 2
, stable range, heating rate and isothermal operation temperature conditions, changes in the treated samples observed during or after the test, the temperature at which chemical changes begin, the maximum value of the sample and the metal or metal ions mixed with it, etc. Test method: It shall describe the requirements of each quality inspection method and project index in the test. 3
Test data: It shall clearly state the questions at the beginning and end of the test. The actual analysis data obtained at each sampling point at the beginning and during the test should generally be submitted in a table with the corresponding typical spectra. Test results: The test results should be expressed as measured data, and it is not appropriate to use expressions such as "meets the requirements". The test results should be expressed using the specified 5)
labeled amount, and a comparison with the test results at the beginning of the test should be given (such as decomposition rate, percentage). Result evaluation: The test results should be analyzed and conclusions should be given. If no decomposition or chemical change is found below 150C when the IDTA or TGA method is used in the thermal stability test, the substance being tested is considered to be sufficiently stable at room temperature: In the chemical stability test with metals/metal ions, if the decomposition rate of the active ingredient analysis results after heat storage is less than 5%, it is considered that the substance being tested is stable when mixed with the metal/metal ions at room temperature. 3
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NY741860.4-2010
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People's Republic of China
Agricultural Industry Standard
Test Guide for Determination of Physical and Chemical Properties of Pesticides
Part 4: Source Stability
NY/T1860.4-2C10
Published by China Agriculture Press
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Format 880nm×1230mm 1/16
2010 5, H first edition
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May 2010 Beijing 1st printing
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