GB 6694-1998 Cypermethrin technical

This standard specifies the requirements, test methods, marking, labeling, packaging, storage and transportation of cypermethrin technical. This standard applies to cypermethrin technical consisting of cypermethrin and impurities generated during production. GB 6694-1998 Cypermethrin technical GB6694-1998 Standard download decompression password: www.bzxz.net

GB 6694-1998
This standard is revised on the basis of the original national standard GB6694-86 "Cypervalerate Technical Material" in accordance with the format of the industry standard HG/T2467.1-1996 "Specifications for the Preparation of Pesticide Technical Material Product Standards". The main points of this standard revision are as follows:
1. The three grades (first-class, second-class, and third-class) divided in the original standard are adjusted to superior, first-class, and qualified products. 2. The quality specifications have been changed to a certain extent, and the moisture control items have been added. Among them, the various indicators of superior products are equivalent to the standard indicators of FAO Specification 334/TC/S (1991). 3. In the determination method of active ingredient content, the quantitative method is changed from peak height method to peak area method, and the gas chromatography determination method with N2 as carrier gas is placed in the main text of the standard, while the gas chromatography determination method with H2 as carrier gas is included in the appendix of the standard. 4. The allowable difference of the meaning of active ingredient is adjusted to 1.5%. 5. In Chapter 5, the contents about "safety" and "guarantee period" are supplemented. This standard replaces GB6694-86 from the date of implementation. Appendix A of this standard is the appendix of the standard. This standard is proposed by the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of Shenyang Chemical Research Institute of the Ministry of Chemical Industry. This standard is drafted by Shanghai Zhongxi Pharmaceutical Co., Ltd., and Kaifeng Pesticide Chemical Research Institute (Henan Tianlaoda Company) participated in the drafting.
The main drafters of this standard are Tao Hongying, Zhu Zhenming, Wu Rong, Zhang Changhong, Zhao Lanzhen, and Liu Jigang.
This standard was first issued in August 1986.
National Standard of the People's Republic of China
Cenvalerate Technical
Fenvalerate technical
Other names, structural formulas and basic physicochemical parameters of fenvalerate are as follows: ISO common name: fenvalerate
Trade name: fenvalerate
CIPAC digital code: 334
Chemical name: RS-α-cyano-3-phenoxybenzyl-R,S-2-(4-chlorophenyl)-3-methylbutyl ester. GB 6694—1998
Replaces GB6694--86
Among them: R-α-cyano-3-phenoxy-S-2-(4-chlorophenyl)-3-methylbutyl ester and S-α-cyano-3-phenoxybenzyl-R-2-(4-chlorophenyl)-3-methylbutyl ester are α-form of cypermethrin;
R-α-cyano-3-phenoxybenzyl-R-2-(4-chlorophenyl)-3-methylbutyl ester and S-α-cyano-3-phenoxybenzyl-S-2-(4-chlorophenyl)-3-methylbutyl ester are β-form of cypermethrin.
Structural formula:
CH,--CH--CH-
Empirical formula: C2H22CINO
Relative molecular weight: 419.91 (according to the 1993 international relative atomic mass) Biological activity: insecticide
Vapor pressure (25C): 3.7×10-5Pa
Solubility (g/L, 20℃): less than 1.0×10-3 in water; less than 77 in hexane; greater than 4.5×10° in acetone, cyclohexanone, ethanol, xylene, and chloroform.
Stability: easily decomposed in alkaline medium, stable in slightly acidic medium. 1 Scope
This standard specifies the requirements, test methods, marking, labeling, packaging, storage and transportation of cypermethrin technical. This standard applies to cypermethrin technical composed of cypermethrin and impurities generated during production. 2 Reference 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. GB/T601-88 Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB/T1250-89 Methods for expressing and determining limit values ​​Approved by the State Administration of Quality and Technical Supervision on October 19, 1998 520
Implementation on April 1, 1999
GB 6694-1998
GB/T1600-79 (89) Method for determining moisture content in pesticides GB/T1604-1995 Acceptance rules for commercial pesticides GB/T1605-79 (89) Sampling methods for commercial pesticides GB/T3796-83 General rules for pesticide packaging
3 Requirements
3.1 Appearance: Yellow to brown viscous liquid or solid. 3.2 Cypermethrin technical shall comply with the requirements of Table 1. Table 1www.bzxz.net
Cyperthrin content, %
Water content, %
Acidity (in HSO,), %
α/β (peak area ratio)
Note: α/β is a reference item.
4 Test method
4.1 Sampling
Cyperthrin technical control item index
Superior product
Qualified product
Carry out according to the "sampling of emulsion and liquid state" method in GB/T1605-79 (89). Before sampling, the product must be heated in the drying room to a homogeneous liquid state before sampling. The sampling package is determined by the random number table method, and the final sampling volume should be not less than 250g. 4.2 Identification test
This identification test can be carried out simultaneously with the determination of cyperthrin content. Under the same gas chromatography operating conditions, the relative difference between the retention time of a chromatographic peak of the sample solution and the retention time of the chromatographic peak of fluvalerate in the standard solution should be within 1.5%. 4.3 Determination of cypermethrin content
4.3.1 Method Summary
The sample was dissolved in acetone, and didecyl phthalate was used as the internal standard. A glass column with 1.5% DC-11 + 5% QF-1/Chromosorb W, AW-DMCS (147μm～175μm) as the filling material and a hydrogen flame ionization detector were used to separate and determine the cypermethrin in the sample by gas chromatography.
4.3.2 Reagents and solutions
a) Acetone;
b) Chloroform;
c) n-Butanol;
d) Cypermethrin standard: known content, ≥98.0%; e) Internal standard: didecyl phthalate, which should not contain impurities that interfere with the analysis; f) Stationary phase: QF-1; DC-11;
g) Carrier: ChromosorbWAW-DMCS (147μm~175μm). 4.3.3 Apparatus
a) Gas chromatograph: with hydrogen flame ionization detector; b) Chromatographic data processor;
c) Chromatographic column: 2m×2mm(id) glass column; 521
GB6694-1998
d) Column packing: QF-1+DC-11 coated on Chromosorb W AW-DMCS (147 μm~~175 μm), DC-11:QF-1:(carrier+stationary liquid)=1.5:5:100 (m/m). 4.3.4 Preparation of chromatographic column
a) Coating of stationary liquid
Accurately weigh the required amount of DC-11 and QF-1 (accurate to 0.0002g) into a beaker, add an appropriate amount of a mixed solvent of n-butanol + chloroform + acetone (1 + 1 + 1) (it is best to make the solvent just immerse the entire carrier), stir to dissolve, and if necessary, place it in a water bath to heat it slightly to accelerate the dissolution. Pour the weighed carrier into the above solution at once, shake it gently to mix it evenly, then place it under an infrared lamp to completely evaporate the solvent, and finally bake it in an oven at 100℃ for 2h for use. b) Filling of chromatographic column
Connect a small funnel to the outlet of the washed and dried chromatographic column, and fill the prepared filler into the column in batches, while constantly tapping the column wall until it is filled to 1.5cm from the column outlet. Move the funnel to the entrance of the chromatographic column, plug a small ball of silanized glass wool at the outlet, connect it to the vacuum pump through a rubber tube, turn on the vacuum pump, continue to slowly add the filler, and tap the column wall continuously to make it evenly and tightly filled. After filling, plug a small ball of glass wool at the inlet and press it properly to prevent the filler from moving. c) Aging of the chromatographic column
Connect the inlet of the chromatographic column to the vaporization chamber, do not connect the outlet to the detector for the time being, pass the carrier gas (N2) at a flow rate of 10mL/min, raise the temperature to 245℃ in stages, and age at this temperature for at least 24h. 4.3.5 Gas chromatography operating conditions
a) Temperature (℃): column chamber 230, vaporization chamber 270, detector chamber 270; b) Gas flow rate (mL/min): carrier gas (N2) 15, hydrogen 30, air 300; c) Retention time (min): fluvalerate α-form 22; fenvalerate β-form 24, internal standard 29. The gas chromatogram of fenvalerate technical is shown in Figure 1. 1-fenvalerate α-form,2—β-form of cypermethrin; 3—Internal standard: didecyl phthalate Figure 1 Gas chromatogram of cypermethrin technical
The above operating parameters are typical. According to the characteristics of different instruments, the given operating parameters can be appropriately adjusted to obtain the best results. 4.3.6 Determination steps
a) Preparation of standard solution
Weigh 0.13g of cypermethrin standard (accurate to 0.0002g) and 0.10g of didecyl phthalate (accurate to 0.0002g) into a 10mL stoppered volumetric flask, dissolve and dilute to the mark with acetone, and shake well. Pipette 5mL of this solution into another 10mL stoppered volumetric flask, dilute to the mark with acetone, and shake well. b) Preparation of sample solution
Weigh a sample containing 0.13g (accurate to 0.0002g) of fenvalerate and 0.10g (accurate to 0.0002g) of didecyl phthalate into a 10mL stoppered volumetric flask, dissolve it with acetone and dilute to the mark, shake well. Use a pipette to draw 5mL of this solution into another 10mL stoppered volumetric flask, dilute to the mark with acetone, and shake well. c) Determination
Under the above operating conditions, after the baseline of the instrument is stable, inject several needles of standard solution continuously, calculate the repeatability of the relative response value of each needle, and when the relative response value of two adjacent needles changes less than 1.0%, measure in the order of standard solution, sample solution, sample solution, and standard solution. 522
4.3.7 Calculation
GB 6694—1998
According to the chromatograms obtained from the two needles of standard solution, measure the peak areas of fenvalerate and internal standard respectively, calculate the quantitative correction factor (f) of fenvalerate according to formula (1), and calculate the average value. miXp
In the formula: ml,m2—
+A + A2 /
are the masses of fenvalerate and internal standard in the standard solution, g; - the mass fraction of fenvalerate in the standard sample, %; Ai,A2,A: are the peak areas of α-isomer, β-isomer and internal standard in the standard solution, respectively. (1)
Based on the chromatograms obtained from the two injections of the sample solution, measure the peak areas of fenvalerate and the internal standard respectively, calculate the percentage of fenvalerate (X,) according to formula (2), and calculate the α/β ratio according to formula (3). And take their average values ​​respectively. 4
{ A + A,
× 100
Wherein: the average quantitative correction factor of fenvalerate; A4
m3, m4 are the masses of the sample and the internal standard in the sample solution, g; A4, A, A are the peak areas of the α-isomer, β-isomer and the internal standard of fenvalerate in the sample solution. 4.3.8 Allowable difference
The difference between the results of two parallel determinations shall not exceed 1.5%. 4.4 Water content determination
Carry out according to the Karl Fischer method in GB/T1600-79(89). It is allowed to use a micro-moisture meter with equivalent accuracy for determination. 4.5 Determination of acidity
4.5.1 Reagents and solutions
a) Sodium hydroxide standard titration solution: c(NaOH)=0.05mol/L, prepared according to the method specified in GB/T601; b) 95% ethanol;
c) Indicator solution: a mixture of 2mL2g/L methyl red ethanol solution and 10mL2g/L bromocresol green ethanol solution. 4.5.2 Determination steps
Weigh 2g of the sample (accurate to 0.002g), place it in a 250mL conical flask, add 100mL95% ethanol, shake to dissolve the sample, add 5 drops of indicator solution, and titrate with 0.05mol/L sodium hydroxide standard solution until the color changes from orange-yellow to blue-green as the end point, and perform a blank determination at the same time.
The acidity X of the sample expressed in mass percentage is calculated according to formula (4): X, = cVi- V × 0. 049 × 100m
Where: °C-actual concentration of sodium hydroxide standard titration solution, mol/L; VI—-volume of sodium hydroxide standard titration solution consumed by titrating the sample solution.mL; Vo
volume of sodium hydroxide standard titration solution consumed by titrating the blank solution, mL; m—mass of the sample, g;
The mass of sulfuric acid in grams equivalent to 1.00mL of sodium hydroxide standard titration solution [c(NaOH)=1.000mol/L].
4.6 Inspection and acceptance of products
shall comply with the relevant provisions of GB/T1604, and the rounding value comparison method in GB/T1250 shall be used for the processing of limit values. 523
5 Marking, labeling, packaging and storage and transportation
GB6694-1998
5.1 The marking, labeling and packaging of cypermethrin technical shall comply with the relevant provisions of GB3796. As a commodity circulating technical, it shall also have a trademark and production license number.
5.2 Cypermethrin technical shall be packaged in clean, dry iron drums coated with protective film. The net weight of each package shall not exceed 250kg: 5.3 Other forms of packaging may be used according to the specific situation of the enterprise, user requirements or order agreement, but they must comply with the relevant provisions of GB3796.
5.4 Packages shall be stored in ventilated and dry warehouses. 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: Cypermethrin technical is a pyrethroid insecticide with moderate toxicity. It is poisonous to people if swallowed or inhaled, and irritating to the skin. When using this product, you should pay attention to personal protection, wear protective gloves, do not let the liquid enter the eyes, nose, and mouth, wash your hands with soap after using the medicine, and if poisoning occurs, please seek medical treatment according to the doctor's instructions.
5.7 Warranty period: Under the specified storage and transportation conditions, the warranty period of cypermethrin technical is 2 years from the date of production. During the warranty period, all indicators should meet the requirements of this standard.
Method Summary
GB 6694 —1998
Appendix A
(Standard Appendix)
Gas chromatography determination of fenvalerate content with hydrogen as carrier gas The sample was dissolved in acetone, didecyl phthalate was used as internal standard, and a glass column filled with 1.5% DC-11 + 5% QF-1/Chromosorb AW-DMCS (147μm~175μm) was used and a hydrogen flame ionization detector to separate and determine the fenvalerate in the sample by gas chromatography.
Reagents and solutions
a) Acetone;
b) Trifluoromethane;
c) n-Butanol;
d) Cyanthrin standard, known content, ≥98.0%;
Internal standard: didecyl phthalate, which should not contain impurities that interfere with analysis;
g) Carrier: Chromosorb W AW-DMCS (147 μm~175 μm);3Instruments
Gas chromatograph: with hydrogen flame ionization detector; chromatographic data processor;
Chromatographic column: 2mX3mm(id) glass column;
Column filling: DC-11→+QF-1 coated on Chromosorb W AW-DMCS (147 μm～175 μm), DC-11: QF-1 : (carrier + stationary liquid) = 1.5:5:100 (m/m). A4 Preparation of chromatographic column
See 4.3.4 of this standard.
5 Gas chromatography operating conditions
a) Temperature (C): column chamber 230, vaporization chamber 270, control and detection chamber 270; b) Gas flow rate (mL/min): carrier gas (Hz) 36, air 500; c) Retention time (min): α-form of fenvalerate 22, β-form of fenvalerate 24, internal standard 29. The gas chromatogram of cypermethrin technical drug is shown in Figure A1. 525
GB 6694 — 1998
1—Cypermethrin α-body, 2—Cypermethrin β-body; 3—Internal standard: didecyl phthalate Figure A1 Gas chromatogram of cypermethrin technical drug
The above operating parameters are typical. According to the characteristics of different instruments, the given operating parameters can be appropriately adjusted to obtain the best effect. A6 Determination steps
a) Preparation of standard solution
Weigh 0.13g of cypermethrin standard (accurate to 0.0002g) and 0.10g of didecyl phthalate (accurate to 0.0002g) in a 10 mL stoppered volumetric flask, add acetone to dissolve and dilute to the scale, and shake well. b) Preparation of sample solution
Weigh a sample containing 0.13 g (accurate to 0.0002 g) of cypermethrin technical, 0.10 g (accurate to 0.0002g) in a 10mL stoppered volumetric flask, add acetone to dissolve and dilute to the scale, shake well. c) Determination
Under the above operating conditions, after the instrument is stable, 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 two adjacent needles changes less than 1.0%, determine in the order of standard solution, sample solution, sample solution, and standard solution. A7 Calculation
Refer to 4.3.7 of this standard.
3 Allowance
Refer to 4.3.8 of this standard.
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