HG/T 2467.5-1996 Specification for the preparation of pesticide suspension product standards
Some standard content:
HG/T 2467. 5--1996
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. 1. Added a preface and determined the main contents that the preface should include; 2. Changed the title of Chapter 1 "Subject Content and Scope of Application" to "Scope"; 3. Added a prescribed introduction before citing the standard; 4. Cancelled the product classification chapter;
5. Changed the title of Chapter 3 "Technical Requirements" to "Requirements"; 6. Cancelled the inspection rules chapter, changed the sampling method of the chapter to "Sampling", and put it at the beginning of the test method chapter as one of the clauses; considering that most pesticide product standards are mandatory, the inspection and acceptance rules of the products are still retained and placed in the test method. At the end of the law chapter, and also as one of the articles, 7. The title of marking, packaging, transportation and storage in the original Chapter 7 was changed to marking, labeling, packaging, storage and transportation, as Chapter 5 of the revised version; 8. Some parts of the original standard were also modified and supplemented. For example, it was 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 the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard was mainly drafted People: Hou Yukai, Wang Xuecheng, Zhao Xinxin, Yang Jian, Lou Shaowei.
HG/T2467.5—1996
1 Information about the special partWww.bzxZ.net
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 with the adopted object and the brief reasons; explain the changes in the important technical content of the previous version; explain the relationship with other standard documents or other documents; —Requirements for the implementation of the transition period; explanations on the abolition or replacement of all or part of other standard documents by this standard; indicating which appendices are standard appendices and which are indicative appendices. 2. Basic information
This standard was proposed by.
This standard is managed by.
Drafting unit of this standard: when necessary, the responsible drafting unit and participating drafting units can be specified. Who are the main drafters of this standard: generally no more than 5 people. 267
Chemical Industry Standard of the People's Republic of China
Product Standard Preparation Specification for Pesticide Aqueous Suspension Concentrate HG/T 2467. 5—1996
This standard specifies the specification for the preparation of pesticide water suspension 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 ingredients in this product are as follows: ISO common name:
Trade name:
CIPAC digital code:
Chemical name:
Structural formula:
Empirical formula: ||tt ||Relative molecular weight (measured by 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) 1 Scope
This standard specifies the requirements, test methods, and marking, labeling, packaging, storage and transportation of ·…· (common name) aqueous suspension concentrate. This standard applies to (common name) aqueous suspension concentrate made from (common name) technical, filler and necessary additives that meet the standard.
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 should be arranged in order of standard numbers; standards of different industries should be arranged in alphabetical order of standard codes. GB/T 1601-93 Determination of pH value of pesticides GB/T1604-1995 Acceptance rules for commercial pesticides GB/T1605-79 (89) Sampling methods for commercial pesticides GB3796-83 General rules for pesticide packaging
GB/T4946-85 Terminology for gas chromatography
GB/T14825-93 Determination of suspension rate of wettable powders of pesticides GB/T16150-1995 Determination of fineness of powders and wettable powders of 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 268
Implementation on September 1, 1996
3 Requirements
HG/T 2467. 5--1996
3.1 Appearance: It should be a flowing, easily measurable suspension liquid; during storage, precipitation may occur, but it should return to its original state after being shaken by hand; there should be no lumps.
3.2 (Common name) Aqueous suspension concentrates should meet the requirements of Table 1. Table 1·（Common name）Water suspension concentrate control items Index Items
（Common name）Content, %
…………（Harmful impurity name）Content, %
pH range
Pourability
Suspension rate, %
Residue after pouring, %
Residue after washing, %
Sieve analysis (through 75 μm test sieve), %
Low temperature stability
Hot storage stability
(or specified range)
The listed items are not exhaustive, nor are they required to be fully included in any water suspension concentrate standard. They can be increased or decreased according to the actual situation of different pesticide products.
Low temperature stability and hot storage stability tests shall be conducted at least once a month. 4 Test methods
4.1 Sampling
Carry out in accordance with the "sampling of emulsion and liquid state" method in GB/T1605. The sampled packages are determined by the random number table method; the final sampling volume should generally be no less than 250mL.
4.2 Identification test
Write with reference to 4.2 of HG/T2467.1 (before the identification test, the active ingredients should be extracted first). 4.3 Determination of the content of ... (common name) (taking the wide-bore capillary gas chromatography internal standard method as an example) 4.3.1 Method summary
The sample is dissolved in ...·, and ... is used as the internal standard, using ...· (stationary liquid) coated quartz capillary column and split (or non-split) injection device and detector, and the (common name) in the sample is separated and determined by capillary gas chromatography. 4.3.2 Reagents and solutions
Reagents (specific names)
(common names) Standard samples: known content, ≥…·%; Internal standard solution · Weigh (internal standard) g, dissolve and dilute to mL with .. (solvent), mix well, seal and store. 4.3.3 Instruments
Gas chromatograph: with · detector, split/splitless device (and automatic injection system); capillary column.mXmm (id) fused quartz column, inner wall coated with (fixed liquid), film thickness μm; injection system: with split (or splitless) injection device and fused quartz inner village; split ratio ·|tt|| Chromatography data processor
4.3.4 Capillary gas chromatography operating conditions
HG/T 2467. 5—1996
Temperature (℃). Column chamber; Vaporization chamber·, Detection chamber; Gas flow rate (mL/min);
Carrier gas (H2 or He, N.)··; Carrier gas supplement)·Hydrogen·,
Air;
Retention time (with typical capillary gas chromatogram) (min)); (Common name
(Internal standard)
The above operating parameters are typical and can be appropriately adjusted according to the characteristics of the instrument in order to obtain the best results. 4.3.5 Determination steps
4.3.5.1 Preparation of standard solution
Write according to the specific preparation method.
4.3.5.2 Preparation of sample solution
Write according to the specific preparation method.
4.3.5.3 System balance
Inject 1uL internal standard solution and sample solution (without internal standard) into the gas spectrometer in sequence to check for interference peaks from impurities. Inject several needles of standard solution to balance the system. Set the integration parameters according to the chromatogram information obtained. 4.3.5.4 Determination
Under the above operating conditions, continuously inject several needles of standard solution, calculate the repeatability of the relative response value of each needle, and when the relative response value of the adjacent two needles changes 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 needles of sample solution and the two needles of standard solution before and after the sample to the peak area (peak height) of the internal standard. · (Generic name) mass percentage content Xi, calculated according to formula (1): Xi = 2: mP
—the average value of the peak area (peak height) ratio of (generic name) to the internal standard in the standard solution; where: ri—
the average value of the peak area (peak height) ratio of (generic name) to the internal standard in the sample solution; mi
the mass of the (generic name) standard g
—the mass of the sample, g;
P the mass percentage content of ... (generic name) in the standard sample. It is also possible to calculate the correction factor first and then calculate the effective ingredient content in the sample according to the provisions of GB/T4946. 4.3.7 Allowable difference
The difference between the results of two parallel determinations should not be greater than %, 4.4 The determination of (name of harmful impurities) content shall be written according to the specific determination method adopted.
4. 5 The determination of pH value
shall be carried out in accordance with GB/T1601.
4.6 Pourability test
4.6.1 Method summary
(1)
After placing the water suspension sample in a container for a certain period of time, pour it according to the prescribed procedure and measure the amount of sample remaining in the container; after washing the container with water, measure the amount of sample in the container again. 270
4.6.2 Instrument
HG/T 2467.5—1996
Vacuum with ground stopper: (500±2)mL; the height of the volume is 39cm, and the distance between the upper and lower scales is 25cm (or other equivalent containers suitable for measuring pourability).
4.6.3 Test steps
Mix a sufficient amount of sample and promptly place a part of it in the weighed volume (including the stopper) to 8/10 of the volume of the volume, plug the ground stopper, weigh it, and leave it for a certain time (such as 24h). Open the stopper, pour the cylinder 45, pour for 60s, invert for 60s, and reweigh the cylinder and stopper.
Pour water (20℃) equivalent to 80% of the volume of the cylinder into the cylinder, plug the ground stopper, invert the cylinder 10 times, pour the contents as above, and weigh the cylinder and stopper for the third time. 4.6.4 Calculation
The residue X21(%) after pouring and the residue X2-2(%) after washing shall be calculated according to formula (2-1) and formula (2-2) respectively: mz - mo × 100
X2-1 =
mi -mo
Wherein: mi -
The mass of the measuring cylinder, ground stopper and sample, g; m3 - mo × 100
m - mo
The mass of the measuring cylinder, ground stopper and residue after pouring, m -The mass of the measuring cylinder, ground stopper and residue after washing, g; The mass of the measuring cylinder and ground stopper after constant weight, mto
4.7 Determination of suspension rate
Carry out according to GB/T 14825 (specify the specific operation steps such as sample weight and drying or extraction). 4.8 Sieve analysis
Perform according to the wet sieving method in GB/T16150.
4.9 Low temperature stability test
4.9.1 Method summary
Maintain the sample at 0℃ for 1 hour and observe whether there is any change in appearance. Continue to store at 0℃ for 7 days and test its physical properties. 4.9.2 Apparatus
Refrigerator: Maintain (0±1)℃.
Beaker: 100mL.
4.9.3 Test steps
·(2-1)
.( 2-2)
Take 80mL of sample and place it in a 100mL beaker. Cool it to (0±1)℃ in a refrigerator and keep it for 1 hour. Stir it once every 15min for 15s each time and observe whether there is any change in appearance. Put the beaker back into the refrigerator and keep it at (0±1)℃ for 7 days. After 7 days, take out the beaker and return it to room temperature. Test the suspension rate and sieve analysis. If it meets the standard requirements, it is qualified. 4.10 Hot Storage Stability Test
4.10.1 Instrument
Constant Temperature Box (or Constant Temperature Water Bath): (54±2)℃, Ampoule (or glass bottle with stopper that can still be sealed at 54℃): 50mL; Medical Syringe: 50mL.
4.10.2 Test Steps
Use a syringe to inject about 30mL of sample into a clean ampoule (avoid the sample contacting the bottleneck), cool the ampoule in an ice-salt bath, and seal it with a high-temperature flame (avoid solvent volatilization). Seal at least 3 bottles and weigh them separately. Place the sealed ampoule in a metal container, and then place the metal container in a (54±2)℃ constant temperature box (or constant temperature water bath) and leave it for 14 days. Take out the sample, wipe it clean, weigh it separately, and inspect the specified items within 24 hours for the samples that have not changed in mass (when writing specific product standards, the judgment principles for the qualified hot storage stability test should be specified).
4.11 Inspection and acceptance of products
HG/T2467.5-1996
Should comply with the relevant provisions of GB/T1604. For the processing of limit values, the rounded value comparison method is adopted. 5 Marking, labeling, packaging, storage and transportation
5.1. The marking, labeling and packaging of (common name) water suspension concentrate shall comply with the relevant provisions of GB3796, and shall have the production license (production permit) number and trademark.
5.2 Prepare it based on the specific packaging conditions of each production and processing plant. 5.3 According to user requirements or ordering agreements, other forms of packaging can be used, but they must comply with the relevant requirements of GB3796. The packages should be stored in a ventilated and dry warehouse. 5.41
5.5 During storage and transportation, strictly prevent moisture and sunlight, do not mix with food, seeds, feed, avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: In addition to the corresponding toxicity signs, the instructions for use or packaging containers should also have 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 (generic name) aqueous suspension is at least 2 years from the date of production. During the warranty period,2 Apparatus
HG/T 2467.5—1996
Volume cylinder with ground stopper: (500±2)mL; height of the cylinder 39cm, distance between upper and lower scales 25cm (or other equivalent containers suitable for measuring pourability).
4.6.3 Test steps
Mix a sufficient amount of sample and promptly place a portion of it in the weighed cylinder (including stopper) to 8/10 of the volume of the cylinder, plug the ground stopper, weigh, and leave for a certain time (e.g. 24h). Open the stopper, pour the cylinder 45, pour for 60s, invert for 60s, and reweigh the cylinder and stopper.
Pour water (20℃) equivalent to 80% of the volume of the cylinder into the cylinder, plug the ground stopper, invert the cylinder 10 times, pour the contents according to the above operation, and weigh the cylinder and stopper for the third time. 4.6.4 Calculation
The residue X21(%) after pouring and the residue X2-2(%) after washing shall be calculated according to formula (2-1) and formula (2-2) respectively: mz - mo × 100
X2-1 =
mi -mo
Wherein: mi -
The mass of the measuring cylinder, ground stopper and sample, g; m3 - mo × 100
m - mo
The mass of the measuring cylinder, ground stopper and residue after pouring, m -The mass of the measuring cylinder, ground stopper and residue after washing, g; The mass of the measuring cylinder and ground stopper after constant weight, mto
4.7 Determination of suspension rate
Carry out according to GB/T 14825 (specify the specific operation steps such as sample weight and drying or extraction). 4.8 Sieve analysis
Perform according to the wet sieving method in GB/T16150.
4.9 Low temperature stability test
4.9.1 Method summary
Maintain the sample at 0℃ for 1 hour and observe whether there is any change in appearance. Continue to store at 0℃ for 7 days and test its physical properties. 4.9.2 Apparatus
Refrigerator: Maintain (0±1)℃.
Beaker: 100mL.
4.9.3 Test steps
·(2-1)
.( 2-2)
Take 80mL of sample and place it in a 100mL beaker. Cool it to (0±1)℃ in a refrigerator and keep it for 1 hour. Stir it once every 15min for 15s each time and observe whether there is any change in appearance. Put the beaker back into the refrigerator and keep it at (0±1)℃ for 7 days. After 7 days, take out the beaker and return it to room temperature. Test the suspension rate and sieve analysis. If it meets the standard requirements, it is qualified. 4.10 Hot Storage Stability Test
4.10.1 Instrument
Constant Temperature Box (or Constant Temperature Water Bath): (54±2)℃, Ampoule (or glass bottle with stopper that can still be sealed at 54℃): 50mL; Medical Syringe: 50mL.
4.10.2 Test Steps
Use a syringe to inject about 30mL of sample into a clean ampoule (avoid the sample contacting the bottleneck), cool the ampoule in an ice-salt bath, and seal it with a high-temperature flame (avoid solvent volatilization). Seal at least 3 bottles and weigh them separately. Place the sealed ampoule in a metal container, and then place the metal container in a (54±2)℃ constant temperature box (or constant temperature water bath) and leave it for 14 days. Take out the sample, wipe it clean, weigh it separately, and inspect the specified items within 24 hours for the samples that have not changed in mass (when writing specific product standards, the judgment principles for the qualified hot storage stability test should be specified).
4.11 Inspection and acceptance of products
HG/T2467.5-1996
Should comply with the relevant provisions of GB/T1604. For the processing of limit values, the rounded value comparison method is adopted. 5 Marking, labeling, packaging, storage and transportation
5.1. The marking, labeling and packaging of (common name) water suspension concentrate shall comply with the relevant provisions of GB3796, and shall have the production license (production permit) number and trademark.
5.2 Prepare it based on the specific packaging conditions of each production and processing plant. 5.3 According to user requirements or ordering agreements, other forms of packaging can be used, but they must comply with the relevant requirements of GB3796. The packages should be stored in a ventilated and dry warehouse. 5.41
5.5 During storage and transportation, prevent moisture and sunlight. Do not mix with food, seeds, and feed. Avoid contact with skin and eyes. Prevent inhalation through the mouth and nose. 5.6 Safety: In addition to the corresponding toxicity signs, 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 (generic name) aqueous suspension is at least 2 years from the date of production. During the warranty period,2 Apparatus
HG/T 2467.5—1996
Volume cylinder with ground stopper: (500±2)mL; height of the cylinder is 39cm, and the distance between the upper and lower scales is 25cm (or other equivalent containers suitable for measuring pourability).
4.6.3 Test steps
Mix a sufficient amount of sample and promptly place a portion of it in the weighed cylinder (including the stopper) to 8/10 of the volume of the cylinder, plug the ground stopper, weigh, and leave it for a certain time (such as 24h). Open the stopper, pour the cylinder 45, pour it for 60s, and then invert it for 60s, and reweigh the cylinder and stopper.
Pour water (20℃) equivalent to 80% of the volume of the cylinder into the cylinder, plug the ground stopper, invert the cylinder 10 times, pour the contents according to the above operation, and weigh the cylinder and stopper for the third time. 4.6.4 Calculation
The residue X21 (%) after pouring and the residue X2-2 (%) after washing shall be calculated according to formula (2-1) and formula (2-2) respectively: mz - mo × 100
X2-1 =
mi -mo
Wherein: mi -
The mass of the measuring cylinder, ground stopper and sample, g; m3 - mo × 100
m - mo
The mass of the measuring cylinder, ground stopper and residue after pouring, m -The mass of the measuring cylinder, ground stopper and residue after washing, g; The mass of the measuring cylinder and ground stopper after constant weight, mto
4.7 Determination of suspension rate
Carry out according to GB/T 14825 (specify the sample weight and the specific operation steps such as drying or extraction). 4.8 Sieve analysis
Perform the wet sieving method in GB/T16150.
4.9 Low temperature stability test
4.9.1 Method summary
Maintain the sample at 0℃ for 1 hour and observe whether there is any change in appearance. Continue to store at 0℃ for 7 days and test its physical properties. 4.9.2 Apparatus
Refrigerator: Maintain (0±1)℃.
Beaker: 100mL.
4.9.3 Test steps
·(2-1)
.( 2-2)
Take 80mL of sample and place it in a 100mL beaker. Cool it to (0±1)℃ in a refrigerator and keep it for 1 hour. Stir it once every 15min for 15s each time and observe whether there is any change in appearance. Put the beaker back into the refrigerator and keep it at (0±1)℃ for 7 days. After 7 days, take out the beaker and return it to room temperature. Test the suspension rate and sieve analysis. If it meets the standard requirements, it is qualified. 4.10 Hot Storage Stability Test
4.10.1 Instrument
Constant Temperature Box (or Constant Temperature Water Bath): (54±2)℃, Ampoule (or glass bottle with stopper that can still be sealed at 54℃): 50mL; Medical Syringe: 50mL.
4.10.2 Test Steps
Use a syringe to inject about 30mL of sample into a clean ampoule (avoid the sample contacting the bottleneck), cool the ampoule in an ice-salt bath, and seal it with a high-temperature flame (avoid solvent volatilization). Seal at least 3 bottles and weigh them separately. Place the sealed ampoule in a metal container, and then place the metal container in a (54±2)℃ constant temperature box (or constant temperature water bath) and leave it for 14 days. Take out the sample, wipe it clean, weigh it separately, and inspect the specified items within 24 hours for the samples that have not changed in mass (when writing specific product standards, the judgment principles for the qualified hot storage stability test should be specified).
4.11 Inspection and acceptance of products
HG/T2467.5-1996
Should comply with the relevant provisions of GB/T1604. For the processing of limit values, the rounded value comparison method is adopted. 5 Marking, labeling, packaging, storage and transportation
5.1. The marking, labeling and packaging of (common name) water suspension concentrate shall comply with the relevant provisions of GB3796, and shall have the production license (production permit) number and trademark.
5.2 Prepare it based on the specific packaging conditions of each production and processing plant. 5.3 According to user requirements or ordering agreements, other forms of packaging can be used, but they must comply with the relevant requirements of GB3796. The packages should be stored in a ventilated and dry warehouse. 5.41
5.5 During storage and transportation, prevent moisture and sunlight. Do not mix with food, seeds, and feed. Avoid contact with skin and eyes. Prevent inhalation through the mouth and nose. 5.6 Safety: In addition to the corresponding toxicity signs, 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 (generic name) aqueous suspension is at least 2 years from the date of production. During the warranty period,41
5.5 During storage and transportation, prevent moisture and sunlight. Do not mix with food, seeds, and feed. Avoid contact with skin and eyes. Prevent inhalation through the mouth and nose. 5.6 Safety: In addition to the corresponding toxicity signs, 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 (generic name) aqueous suspension is at least 2 years from the date of production. During the warranty period,41
5.5 During storage and transportation, prevent moisture and sunlight. Do not mix with food, seeds, and feed. Avoid contact with skin and eyes. Prevent inhalation through the mouth and nose. 5.6 Safety: In addition to the corresponding toxicity signs, 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 (generic name) aqueous suspension is at least 2 years from the date of production. During the warranty period,
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