HG/T 2743.1-1996 Specification for the preparation of pesticide compound emulsifiable concentrate product standards
Some standard content:
HG/T2743.1—1996
The compound preparations scientifically mixed with different pesticides can greatly improve the efficacy, reduce the resistance and delay the emergence of resistance. Therefore, the development and application of compound preparations of pesticides are important ways to use pesticides rationally and effectively prevent and eliminate diseases, insects and weeds. At present, there are hundreds of compound preparations of pesticides in my country, but many varieties lack scientific experimental basis. The compilation of compound preparation standards is mostly chaotic and of different levels. In order to standardize the compilation format of pesticide compound preparation product standards and improve the standard level, this standard is formulated on the basis of GB/T1.1--1993 "Guidelines for Standardization Work Unit 1: Drafting and Expression Rules of Standards Part 1: Basic Provisions for Standard Compilation" and the industry standard ZBG23001-86 of the Ministry of Chemical Industry "Principles and Procedures for Naming Common Names of Pesticides", and on the basis of HG/T2467 "Format for Compilation of Pesticide Product Standards". Appendix A of this standard is the appendix of the standard. 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 Shenyang Chemical Industry Research Institute, Ministry of Chemical Industry. This standard was drafted by Shenyang Chemical Industry Research Institute, Ministry of Chemical Industry. The main drafters of this standard are: Hou Yukai, Wang Xuecheng, Lou Shaowei, Yang Jian, Zhao Xinxin.
HG/T 2743. 1—1996
Contents to be included in the preface of pesticide compound preparation product standards 1. Special part information
- The number and degree of adoption of international standards or foreign advanced standards, the differences and reasons with the adopted standards; the purpose and basis of standard drafting: the test comparison results of toxicity, toxicity and efficacy of compound preparations and each active ingredient of the compound preparations should be provided, and the degree of improvement in efficacy and reduction in toxicity of compound preparations should be explained; for revised standards, the key points of revision should be explained; requirements for the transition period of standard implementation: the explanation of the abolition or replacement of all or part of other standard documents by this standard;- Indicate which appendices are standard appendices and which are suggestive appendices. 2. Basic part information
This standard is proposed by.
This standard is under the jurisdiction of.
Drafting unit of this standard: When necessary, the responsible drafting unit and participating drafting units may be specified. Main drafters of this standard: Generally no more than 5 people. 285
Chemical Industry Standard of the People's Republic of China
Standard for the preparation of pesticide compound emulsifiable concentrate products HG/T 2743.1—1996
This standard specifies the standard for the preparation of pesticide compound emulsifiable concentrate products, and is applicable to the preparation of corresponding national standards, industry standards, local standards and enterprise standards for pesticide compound emulsifiable concentrate products. Other names, structural formulas and basic physicochemical parameters of each active ingredient in this product are as follows: a) (Generic name of active ingredient 1)
ISO Generic name:
Trade name:
CIPAC digital code:
Chemical name:
Structural formula:
Empirical formula:
Relative molecular mass (calculated according to 19×× international relative atomic mass): Biological activity·(insecticide, acaricide, fungicide, herbicide) Melting point.…℃
Boiling point℃
Vapor pressure (20℃): ·Pa
Solubility (g/L, 20℃):
Stability: (stability to acid, alkali, light, heat, etc., half-life) b) · (Generic name of active ingredient 2)
Contents are the same as a.
c) (Generic name of active ingredient 3)
Contents are the same as a.
1 Scope
This standard specifies the requirements, test methods, and marking, labeling, packaging, storage and transportation of (name of compound preparation) emulsifiable concentrate. This standard applies to **(name of compound preparation) emulsifiable concentrate prepared by dissolving the technical drugs of …(common name of active ingredient 1), …(common name of active ingredient 2), (common name of active ingredient 3) that meet the standard and emulsifiers in a suitable solvent. 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 published, the versions shown are valid. All standards will be revised, and all parties using this standard should explore the possibility of using the latest versions of the following standards. The order of arrangement of referenced standards is domestic first and then foreign; standards of all levels should be arranged step by step, with national standards first and then industry standards; standards of the same level are arranged in the order of standard numbers; standards of different industries are arranged in alphabetical order according to standard codes. GB/T 601—88 Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB/T1600-79 (89) Determination of moisture content in pesticides GB/T1603-79 (89) Determination of stability of pesticide emulsions Approved by the Ministry of Chemical Industry of the People's Republic of China on April 8, 1996 286
Implemented on September 1, 1996
HG/T 2743.1-1996
GB/T1604--1995 Rules for acceptance of commercial pesticides GB/T1605.-79 (89) Sampling methods for commercial pesticides GB/T3796-83 General rules for pesticide packaging
GB/T4838-84 Packaging of emulsifiable concentrate pesticides
GB/T4946-85 Terminology for gas chromatography
HG/T2467--93 Format for writing pesticide product standards ZBG23001-86 Principles and procedures for naming common names of pesticides 3 Requirements
3.1 Appearance: It should be a stable homogeneous liquid without visible suspended matter and sediment. 3.2 (Name of compound preparation) The emulsifiable concentrate should meet the requirements of Table 1. Table 1 (Name of compound preparation) EC control items Index Items
… (Generic name of active ingredient 1) content, % (Generic name of active ingredient 2) content, %
(Generic name of active ingredient 3) content, %
… (Name of harmful impurities) content, %
Moisture, %
Acidity (in H2SO4), %
or Alkalinity (in NaOH), %
Emulsion stability (dilution ·… times)
Low temperature stability
Hot storage stability
(or specified range)
(or specified range)
(or specified range)
The listed items are not exhaustive, nor are they required to be included in any EC standard. They can be increased or decreased according to the specific conditions of different compound pesticide products.
2 Low temperature stability and hot storage stability tests shall be conducted at least once every month. 4 Test methods
4.1 Sampling
Carry out in accordance with the "sampling of emulsions and liquid states" method in GB/T1605. The number of packages to be sampled is determined by the random number table method, and the final sampling volume should generally be no less than 250mL.
4.2 Identification test
When there is doubt about the identification of the active ingredient using the specified test method, at least another effective method should be used for identification. If chromatographic C including gas spectroscopy (GC), high performance liquid spectroscopy (HPLC), thin layer chromatography (TLC)> and infrared spectroscopy (IR) are used for identification, the following statement is recommended:
GC, HPLC This identification test can be carried out simultaneously with the determination of the content of (common name of active ingredient) (the determination of the content of active ingredient also uses the same method). Under the same chromatographic operating conditions, the relative difference between the retention time of a chromatographic peak of the sample solution and the retention time of the standard solution (common name of active ingredient) should be within 1.5%. 287
HG/T 2743. 1—1996
TLC--The R value of a spot obtained by developing the sample solution and the spot developed simultaneously with the control standard solution should be consistent. IR--After separation and removal of emulsifiers and other active ingredients, there should be no obvious difference between the infrared spectra of the sample and the standard (since emulsifiers and other active ingredients are not easy to remove, emulsifiable concentrates are generally not identified by this method). Note: For test methods not included in the standard, the test conditions and operating steps should be clearly stated. 4.3 Determination of ··(common name of active ingredient 1) content (taking HPLC internal standard method as an example) 4.3.1 Method summary
The sample is dissolved, the internal standard ... is used as the mobile phase, and a stainless steel column and detector filled with ... are used to separate and determine the ·…(common name of active ingredient 1) in the sample by HPLC. 4.3.2 Reagents and solutions
Reagents (specific names):
(common name of active ingredient 1) standard sample, known content, ≥…%; internal standard, should not contain impurities that interfere with analysis; internal standard solution: (specify the specific preparation and storage methods); 4.3.3 Instruments
High performance liquid chromatograph, with wavelength ultraviolet detector; chromatographic data processor;
Chromatographic column · mmXmm (id) stainless steel column, filled with filler, am. 4.3.4 High performance liquid chromatography operating conditions
Mobile phase ·
Flow rate. mL/min;
Column temperature · ℃ bZxz.net
Detection wavelength. nm;
Injection volume · μL;
Detector sensitivity (AUFS)..…
Retention time (with typical HPLC chromatogram) (min): (generic name of active ingredient 1),
*·** (internal standard)
The above operating parameters are typical and can be adjusted appropriately according to the characteristics of the instrument in order to obtain the best results. 4.3.5 Determination steps
a) Preparation of standard solution
Written according to the specific preparation method.
b) Preparation of sample solution
Written according to the specific preparation method.
c) Determination
Under the above operating conditions, after the baseline of the instrument is stable, continuously inject several needles of standard solution, calculate the relative response value of each needle, and when the relative response value of two adjacent needles changes by less than %, perform the determination in the order of standard solution, sample solution, sample solution, and standard solution. 4.3.6 Calculation
Average the ratio of the peak area (peak height) of the two sample solutions and the two standard solutions before and after the sample. The mass percentage content of ... (generic name of active ingredient 1) X1 is calculated according to formula (1): r2'mi·P
r,·m2
HG/T2743.1—1996
wherein r--
the average value of the ratio of the peak area (peak height) of ... (generic name of active ingredient 1) to the internal standard in the standard solution; r2-the average value of the ratio of the peak area (peak height) of ... (generic name of active ingredient 1) to the internal standard in the standard solution; the mass of the standard sample (generic name of active ingredient 1), g; mi
the mass of the sample, g:
the mass percentage content of ...·(generic name of active ingredient 1) in the standard sample. P
Also, according to the provisions of GB/T4946, the correction factor f is calculated first, and then the active ingredient content in the sample is calculated. 4.3.7 Allowable difference
The difference between the results of two parallel determinations shall not be greater than %. 4.4…** (Generic name of active ingredient 2) The determination of content shall be written in accordance with the same method format as in HG/T2467 and this standard. 4.5 (Generic name of active ingredient 3) The determination of content shall be written in accordance with the same method format as in HG/T 2467 and this standard. 4.6 (Name of harmful impurities) The determination of content shall be written according to the specific method used.
4.7 Determination of moisture
It shall be carried out according to the Karl Fischer method (when moisture <1.0%) or the azeotropic distillation method (when moisture ≥1.0%) in GB/T1600. It is allowed to use a micro-moisture meter with equivalent accuracy for determination. 4.8 Determination of acidity (or alkalinity)
4.8.1 Reagents and solutions
Sodium hydroxide standard titration solution, c(NaOH)=mol/L, prepared according to the method specified in GB/T601; hydrochloric acid standard titration solution, g(HCI)=…mol/L; prepared according to the method specified in GB/T601, indicator solution: (explain the preparation method; about the concentration unit, if the indicator is solid, it is expressed in g/L; if it is liquid, it is expressed in % (V/V).)
4. 8. 2 Determination steps
Weigh g sample (accurate to g), put it in a 250mL conical flask, add mL (solvent), shake to dissolve the sample (or mix it), add… drops (or mL) of indicator solution, shake, and titrate with sodium hydroxide (or hydrochloric acid) standard titration solution until the color changes from . to color as the end point. At the same time, make a blank determination.
The acidity X, of the sample expressed as mass percentage (in HzSO,) is calculated according to formula (2-1): X, = c(Vi - Vo) × 0. 049
The basicity X'z of the sample expressed as mass percentage (in NaOH) is calculated according to formula (2-2): X', = c(Vi- Vo) × 0. 040
In the formula: -
The actual concentration of the sodium hydroxide (or hydrochloric acid) standard titration solution, mol/L; V,——the volume of the sodium hydroxide (or hydrochloric acid) standard titration solution consumed for titrating the sample solution, mL; V. —The volume of sodium hydroxide (or hydrochloric acid) standard titration solution consumed in titrating the blank solution, mL; m-the mass of the sample, g
(2-2)
0.049—m-the mass of sulfuric acid in grams equivalent to 1.00 mL sodium hydroxide standard titration solution [c(NaOH)=1.000 mol/L];
-the mass of sodium hydroxide in grams equivalent to 1.00 mL hydrochloric acid standard titration solution [c(HCI)=1.000mol/L). 0.040-
If the test solution is dark in color and it is difficult to indicate the end point with the indicator solution, the potentiometric titration method can be used for determination. 4.8.3 Allowable difference
The difference between two parallel determination results should not be greater than %. 289
4.9 Emulsion stability test
HG/T 2743. 1—1996
The sample is diluted with standard hard water… times and tested according to GB/T1603. It is qualified if there is no floating oil on the top and no precipitation on the bottom. 4.10 Low temperature stability test
4.10.1 Method summary
The sample is kept at 0℃ for 1h, and the precipitation of solid and oily substances is recorded. Continue to store at 0℃ for 7d, centrifuge, settle the solid precipitate, and record its volume.
4.10.2 Instruments
Refrigerator: maintain 0±1℃;
Centrifuge tube: 100ml, the scale on the bottom of the tube is accurate to 0.05mL; Centrifuge: matched with centrifuge tube.
4.10.3 Test steps
Take (100±1.0)mL of sample and add it to a centrifuge tube. Cool it to (0±1)℃ in a refrigerator. Keep the centrifuge tube and its contents at (0±1)℃ for 1h. Stir once every 15min for 15s each time. Check and record whether there is any solid or oily matter precipitated. Put the centrifuge tube back into the refrigerator and continue to place it at (0±1)℃ for 7d. After 7d, take out the centrifuge tube, let it stand at room temperature (not exceeding 20℃) for 3h, and centrifuge for 15min (the relative centrifugal force at the top of the tube is 500~600G, G is the acceleration of gravity). Record the volume of the precipitate at the bottom of the tube (accurate to 0.05mL). The precipitate is qualified if it does not exceed 0.3mL. 4.11 Hot Storage Stability Test
4.11.1 Apparatus
Thermostatic box (or thermostatic water bath): (54±2)℃: bottle (or glass bottle with stopper that can still be sealed at 54℃): 50mL; medical syringe: 50mL.
4.11.2 Test Procedure
Use a syringe to inject about 30mL of emulsifiable concentrate sample into a clean bottle (avoid the sample from contacting the bottleneck), place the bottle in an ice-salt bath to cool, and seal it with a high-temperature flame (avoid solvent volatilization). Seal at least 3 bottles and weigh them separately. Place the sealed bottles in a metal container, and then place the metal container in a (54±2)℃ thermostatic box (or thermostatic water bath) for 14 days. Take out, wipe the outside of the bottle clean and weigh them separately. For samples that have not changed in mass, inspect the specified items within 24 hours (when writing specific product standards, the judgment principles for passing the hot storage stability test should be specified).
4.12 Inspection and acceptance of products
Should comply with the relevant provisions of GB/T1604. For the processing of limit values, the rounded value comparison method shall be adopted. 5 Marking, labeling, packaging, storage and transportation
5.1 (Name of compound preparation) The marking, labeling and packaging of emulsion shall comply with the relevant provisions of GB3796 and GB4838, and shall have the production license (production permit) number and trademark. 5.2 Prepared based on the specific packaging conditions of each production and processing plant. 5.3 Other forms of packaging may be used according to user requirements or ordering agreements, but they must comply with the relevant requirements of GB4838. 5.4 Packages should be stored in ventilated and dry warehouses. 5.5 During storage and transportation, strictly prevent moisture and sunlight, do not mix with food, seeds, and feed, avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: In addition to the corresponding cystic mark, the instructions for use or packaging containers should also include toxicity instructions, poisoning symptoms, detoxification methods and first aid measures.
5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of ……… (name of compound preparation) emulsifiable concentrate is at least 2 years from the date of production. During the warranty period, …,
HG/T2743.1—1996
Appendix A
(Appendix to the standard)
The naming principles of the common names of pesticide compound preparations are based on ZBG23001-86 "Principles and procedures for naming common names of pesticides" 1.Article 2 The common name of pesticide preparations (single or mixed) should include three parts, namely, the mass percentage of the active ingredient, the common name of the active ingredient and the dosage form. The common name of the mixed preparation can be composed of the prefixes or pronouns of the common names of each active ingredient. The naming of the common name of pesticide compound preparations is divided into three parts: one is the total content of each active ingredient in the compound preparation (mass percentage or g/L (20℃)], the second is the common name of the compound preparation, which is composed of the prefixes (or the first few words) of the common names of each active ingredient. A dot is inserted between the prefixes (or the first few words) to reflect how many components of the compound preparation it is; the order of each active ingredient The order should generally be determined by the content, with the higher content in front and the lower content in the back; it can also be sorted by the contribution to the efficacy, with the greater contribution to the efficacy in the front; the third is the dosage form of the compound preparation, such as powder, emulsion, wettable powder, water-based suspension, etc. For example, 3% methyl phthalate powder, 40% dimethoate emulsion, 20% cypermethrin emulsion, 50% polysulfide suspension, etc. If a synergist is added to the compound preparation, the synergist is not counted as an active ingredient, and the proportion it occupies does not enter the total content of the active ingredient. 291
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