HG/T 2467.2-1996 Specification for the preparation of pesticide emulsifiable concentrate product standards
Some standard content:
HG/T 2467.21996
HG/T2467-93 "Specifications for the Preparation of Pesticide Product Standards" industry standard is based on the original national and industry standards for pesticides, absorbs the common points and advantages of international pesticide standards and foreign advanced standards, and is formulated in accordance with the writing requirements of GB1.1-87 "Guidelines for Standardization Work". In 1993, according to Part 3 of the IEC/ISO Guidelines "Rules for the Drafting and Expression of International Standards", GB1.1-87 was revised, and it was required to implement GB/T1.1-1993 from 1995. Therefore, HG/T2467-93, which was compiled in accordance with GB1.1-87, should also be revised in a timely manner to meet the needs of compiling newly formulated and revised national standards, industry standards, local standards and enterprise standards for pesticide products. The main points of this standard revision are as follows:
1. Added the preface and determined the main contents of the preface; 2. Change the title of Chapter 1 "Subject Content and Scope of Application" to "Scope"; 3. Add the introduction specified in the paragraph before citing the standard; 4. Cancel the chapter on product classification;
5. Change the title of Chapter 3 "Technical Requirements" to "Requirements"; 6. Cancel the chapter on inspection rules, change the sampling method of the chapter to "sampling", and put it at the beginning of the chapter on test methods as one of the items. Considering that most pesticide product standards are mandatory, the elements of product inspection and acceptance rules are still retained and placed at the end of the chapter on test methods as one of the items; 7. The title of the original Chapter 7 "Marking, Packaging, Transportation and Storage" is changed to "Marking, Labeling, Packaging, Storage and Transportation" as the revised Chapter 5; 8. Modifications and supplements have also been made to some parts of the original standard. For example, it is clarified that the rounded value comparison method is used for the treatment of limit values. This standard replaces HG/T2467--93 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 Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard was drafted by the 9715th Factory of the Chinese People's Liberation Army. The main drafters of this standard are: Hou Yukai, Wang Xuecheng, Zhao Xinxin, Yang Jian, Lou Shaowei. 248
HG/T2467.2—1996
1. Special part information
Contents that should be included in the foreword of the product standard
-Indicate the degree and version of the adoption of international standards or advanced foreign standards, and explain the adoption of international guidelines or other similar standards and documents.
-Indicate the main technical differences and brief reasons with the adopted object; explain the changes in important technical contents from the previous version; explain the relationship with other standard documents or other documents; requirements for the implementation of the transition period, and explain that this standard leads to the abolition or replacement of all or part of other standard documents; indicate which appendices are standard appendices and which are indicative appendices. 2. Basic part information
This standard is proposed by.
This standard is under the jurisdiction of ·.
—— Drafting unit of a 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. 249
Chemical Industry Standard of the People's Republic of China
Specification for the preparation of pesticide emulsifiable concentrate product standards
HG/T 2467. 21996
This standard specifies the specification for the preparation of pesticide emulsifiable concentrate product standards, and is applicable to the preparation of corresponding national standards, industry standards, local standards and enterprise standards for pesticide products.
Other names, structural formulas and basic physicochemical parameters of the active ingredient … (common name) of this product are as follows; ISO common 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 and heat, half-life) 1 Scope
This standard specifies the requirements, test methods, marking, labeling, packaging, storage and transportation of … … (common name) emulsifiable concentrate. This standard applies to (common name) emulsifiable concentrate prepared by dissolving the (common name) technical drug that meets the standard and the emulsifier in a suitable solvent.
2 Cited 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 version 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 recommendation numbers; standards of different industries are arranged in alphabetical order according to the standard code. GB/T601-88 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 GB/T1604-1995 Acceptance rules for commercial pesticides GB/T1605-79 (89) Sampling methods for commercial pesticides GB3796-83 General rules for pesticide packaging
GB4838-84 Packaging of emulsifiable concentrate pesticides
HG/T2467.1--1996 Specification for the preparation of pesticide technical product standards Approved by the Ministry of Chemical Industry of the People's Republic of China on April 8, 1996 250
Implementation on September 1, 1996
3 Requirements
HG/T 2467.2—1996
3.1 Appearance: It should be a stable homogeneous liquid without visible suspended matter and precipitation. 3.2
Common name) EC should meet the requirements of Table 1.
·(Common name) EC control item index
(Common name content, %
(Harmful impurity name) content, %
Water, %
(or specified range)
Acidity in H,SO) or alkalinity (in NaOH), %Emulsion stability (dilution times)
Low temperature stability
Hot storage stability
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 actual situation of the pesticide product. 1
2 During normal production, low temperature and hot storage stability tests shall be conducted at least once a month. 4 Test method
4.1 Sampling
Carry out in accordance with the method of "sampling of emulsion and liquid state" in GB/T1605. The sampled packages are determined by the random number table method, and the final sampling volume should generally be not less than 250 mL.
4.2 Identification test
Written in accordance with 4.2 of HG/T2467.1 (due to the interference of emulsifiers, infrared spectroscopy identification is generally not used). 4.3 Determination of (common name) content (taking thin layer-ultraviolet spectrophotometry as an example) 4.3.1 Method summary
The sample is subjected to thin layer chromatography to separate the (common name) from impurities, and the band containing ... (common name) is scraped off, and ultraviolet spectrophotometry is performed at ... wavelength.
4.3.2 Reagents and solutions
Reagents: (write the name);
Developing agent: solvent 1 + solvent 2 (or + solvent 3) = X + Y (+ Z) Color developer (if necessary);
Silica gel G (or silica gel GF). Particle size ~ μm;
· (common name) Standard sample·Known content, ≥%·4.3.3 Instruments
UV spectrophotometer;
UV lamp (if required) nm;
Chromatography cylinder;
Chromatography plate. cmXcm smooth glass plate
Volume flask (calibrated): *mL;
(V/V);
Pipette or microinjector calibrate the capacity according to actual operating conditions): mL; 251
Filter· (size, pore size).
4.3.4 Determination steps
a) Preparation of chromatography plate
b) Preparation of standard sample solution
HG/T 2467. 2—1996
Weigh · (common name) standard g (accurate to g), place in a mL volumetric flask, dissolve and dilute to the mark with (solvent), and shake well.
c) Preparation of sample solution
Weigh about (common name).g of sample (accurate to g), place in a mL volumetric flask (the volume of the volumetric flask is the same as that used to prepare the standard sample solution), dissolve and dilute to the mark with (solvent), and shake well. d) Thin layer separation
Take an activated chromatography plate and place it 2.5cm from the bottom and 1.5cm away, use a pipette (or micro-injector) to apply a certain volume of sample solution to form a thin straight line. When the solvent evaporates completely, scrape off 5mm wide silica gel on both sides of the chromatography plate, and then place the plate upright in a chromatography cylinder filled with saturated steam of the developing agent, and control the depth of the chromatography plate immersed in the solvent to be 0.5-1.0cm. When the developing agent rises to the predetermined height, take out the chromatography plate and place it in a fume hood to allow the solvent to evaporate (appropriate heating can be used to accelerate this process). Use (color developer or ultraviolet lamp) to color, mark the outline of the band area of ... (common name), and transfer all this part of silica gel to the filter, use mL.. solvent) to elute in batches and filter into a mL volumetric flask, and make up to volume. The standard solution is also treated in the same way. e) Ultraviolet determination
Pour the sample solution and the standard solution after thin layer chromatography into two cm thick quartz absorption cells respectively, use blank solution 1 as a reference, and measure their absorbance at nm wavelength. 4.3.5 Calculate the mass percentage X of ... (common name) in the sample according to formula (1): A, mP
A,·mz
wherein: A1——absorbance of standard solution; A2——absorbance of sample solution,
mass of standard, g,
m2——mass of sample, g;
mass percentage of (common name) in a standard sample. 4.3.6 Allowable difference
The difference between the results of two parallel determinations shall not exceed %. 4.4 The determination of the content of (name of harmful impurities) shall be written according to the specific determination method adopted.
4.5 Determination of moisture
Carry out according to the Karl Fischer method in GB/T1600. It is allowed to use a micro-moisture meter with equivalent accuracy for determination. 4.6 Determination of acidity (or alkalinity)
Refer to 4.6 in HG/T2467.1 for preparation. 4.7 Emulsion stability testWww.bzxZ.net
Perform according to GB/T1603. It is qualified if there is no floating oil on the top and no sinking oil or precipitation below. 4.8 Low temperature stability test
4.8.1 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 to settle the solid precipitate, and record 1) Use solvent to replace the sample spot plate, expand, scrape off the band area equivalent to the effective ingredient, and the eluted solution is the blank solution. 252
Record its volume.
4.8.2 Apparatus
Refrigerator: maintain (0±1)°C;
HG/T 2467.2—1996
Centrifuge tube: 100mL, scale on the bottom of the tube accurate to 0.05mL; Centrifuge: matched with centrifuge tube.
4.8.3 Test steps
Add (100±1.0)mL sample to the centrifuge tube, cool to (0±1)°C in the refrigerator, keep the centrifuge tube and its contents at (0±1)°C for 1h, stir once every 15min, 15s each time, check and record whether there is solid or oily precipitation. Put the centrifuge tube back into the refrigerator and keep it at (0±1)°C for 7d. After 7 days, take out the centrifuge tube, let it stand for 3 hours at room temperature (not exceeding 20℃), and centrifuge for 15 minutes (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. 4.9 Thermal storage stability test
4.9.1 Instrument
Constant temperature box (or constant temperature water bath): (54±2)℃C; bottle (or glass bottle with a stopper that can still be sealed at 54℃): 50mL, medical syringe, 50mL.
4.9.2 Determination steps
Use a syringe to inject about 30mL of emulsifiable concentrate sample into a clean bottle (or glass bottle) (avoid the sample from contacting the bottleneck), place the bottle in an ice-salt bath for cooling, and quickly seal it with a high-temperature flame (avoid the solvent from falling). Seal at least 3 bottles and weigh them separately. Place the sealed product in a metal container, and then place the metal container in a (54 ± 2) ℃ constant temperature box (or water bath) and keep it covered for 14 days. Take it out and cool it to room temperature. Wipe the outside of the ampoule and weigh it separately. For samples with no change in mass, test the specified items within 24 hours (the judgment principle for the qualified heat storage stability test should be specified when writing specific product standards).
4.10 Inspection and acceptance of products
Should comply with the relevant provisions of GB/T1604. For limit numerical processing, the rounded value comparison method should be adopted. 5 Marking, labeling, packaging, storage and transportation
5.1. The marking, labeling and inclusion of (common name) emulsifiable concentrate shall comply with the relevant provisions of GB3796 and GB4838, and shall have the production license (production permit) number and trademark.
5.2 Prepare it based on the specific packaging regulations of each production and processing plant. 5.3 Other forms of packaging may be used according to user requirements or order agreements, but they must comply with the relevant provisions 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 eye-catching toxicity mark, the instruction manual or packaging container should also have toxicity instructions, precautions for use, symptoms of poisoning, detoxification methods and emergency compress measures. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of (generic name) emulsion is at least 2 years from the production date. During the warranty period,.1 Apparatus
Thermostatic box (or thermostatic water bath): (54±2)℃; Ampoule (or glass bottle with stopper that can still be sealed at 54℃): 50mL, medical syringe, 50mL.
4.9.2 Determination steps
Use a syringe to inject about 30mL of emulsifiable concentrate sample into a clean ampoule (or glass bottle) (avoid the sample contacting the bottleneck), place the ampoule in an ice-salt bath for cooling, and quickly seal it with a high-temperature flame (avoid the solvent from falling). Seal at least 3 bottles and weigh them separately. Place the sealed ones in a metal container, and then put the metal container in a (54±2)℃ thermostatic box (or water bath) and keep it covered for 14 days. Take it out and cool it to room temperature, wipe the outside of the ampoule clean, and weigh it separately. For samples that have not changed in mass, test the specified items within 24 hours (the judgment principle for passing the hot storage stability test should be specified when writing specific product standards).
4.10 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. The marking, labeling and packaging of (common name) 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 in accordance with the specific packaging regulations of each production and processing plant. 5.3 According to user requirements or ordering agreement, other forms of packaging may be used, but they must comply with the relevant provisions 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 eye-catching toxicity mark, the instructions for use or packaging containers should also include toxicity instructions, precautions for use, symptoms of poisoning, detoxification methods and emergency compress measures, etc. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of (generic name) emulsion is at least 2 years from the date of production. During the warranty period,1 Apparatus
Thermostatic box (or thermostatic water bath): (54±2)℃; Ampoule (or glass bottle with stopper that can still be sealed at 54℃): 50mL, medical syringe, 50mL.
4.9.2 Determination steps
Use a syringe to inject about 30mL of emulsifiable concentrate sample into a clean ampoule (or glass bottle) (avoid the sample contacting the bottleneck), place the ampoule in an ice-salt bath for cooling, and quickly seal it with a high-temperature flame (avoid the solvent from falling). Seal at least 3 bottles and weigh them separately. Place the sealed ones in a metal container, and then put the metal container in a (54±2)℃ thermostatic box (or water bath) and keep it covered for 14 days. Take it out and cool it to room temperature, wipe the outside of the ampoule clean, and weigh it separately. For samples with no change in mass, test the specified items within 24 hours (the judgment principle for passing the hot storage stability test should be specified when writing specific product standards).
4.10 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. The marking, labeling and packaging of (common name) 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 in accordance with the specific packaging regulations of each production and processing plant. 5.3 According to user requirements or ordering agreement, other forms of packaging may be used, but they must comply with the relevant provisions 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 eye-catching toxicity mark, the instructions for use or packaging containers should also include toxicity instructions, precautions for use, symptoms of poisoning, detoxification methods and emergency compress measures, etc. 5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of (generic name) emulsion is at least 2 years from the date of production. During the warranty period,
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