HG 2988-1999 Analysis method for permethrin content

HG 2988-1999 Permethrin content analysis method HG2988-1999 standard download decompression password: www.bzxz.net

Chemical Industry Standard of the People's Republic of China
Analytical method of content for permethrin
Analytical method of content for permethrin1Subject content and scope of application
This standard specifies the analytical method for permethrin content. This standard is applicable to the determination of the effective content of permethrin technical and emulsifiable concentrate. Active ingredient: Permethrin
UDC632.95
HG/T2988-1988(1997)
Replaces GB9566-88
Chemical name: m-phenoxybenzyl (±) cis, trans-2,2-dimethyl-3-(2,2-dichlorovinyl) cyclopropanecarboxylate Molecular formula: CHzoO,Cl
Structural formula:
CH,-0-CO
Molecular weight: 391.29 (international atomic weight in 1983) 2 Analysis method
Gas chromatography
CH=CClh
2.1 Summary of method: Gas chromatography analysis was carried out on a QF-1/ChromosorbWAWDMCS column with di-n-octyl sebacate as the internal standard.
2.2 Reagents
Permethrin standard: known accurate content; internal standard: dioctyl sebacate (no impurity peaks inseparable from permethrin); chromatographic stationary liquid: QF-1;
Support: ChromosorbWAWDMCS60~80 mesh; acetone (GB686) analytical grade.
2.3 Instruments
Gas chromatograph, hydrogen flame ionization detector; recorder or integrator;
Chromatographic column: 2m long, 3mm inner diameter stainless steel column or glass column; filling material: 8%QF-1/ChromosorbWAWDMCS6080 mesh; approved by the Ministry of Chemical Industry of the People's Republic of China on May 19, 1988 38·
Yuan Xiaosheng Daoke Processing
Implementation on February 1, 1989
Micro syringe: 10μL.
2.4 Operation steps
2.4.1 Preparation of chromatographic column
2.4.1.1 Coating of stationary liquid
HG/T2988-1988 (1997)
Weigh 0.8g QF-1 stationary liquid into a beaker, add an appropriate amount of acetone solvent, and add enough to just cover the support. Stir thoroughly to dissolve it completely. Then pour 10g of dried 60-80 mesh Chromosorb WAWDMCS support into the above solution at once, shake it gently, put it in a fume hood to let the solvent evaporate naturally, and shake it gently frequently. After the solvent evaporates completely, put it in an oven and bake it at 105-110℃ for 2h, take it out and put it in a desiccator for use. 2.4.1.2 Filling and aging of chromatographic columns
Put the above-coated column filling material into the clean and dried chromatographic column by vacuum pump or manually, tap the column wall gently while filling, and plug the column mouth with a little clean glass wool after filling. Then connect the inlet end of the column to the vaporization chamber of the chromatograph, pass nitrogen at a flow rate of about 10ml per minute, gradually raise the temperature to 240℃ in stages, and age at this temperature for no less than 24h. 2.4.2 Chromatographic operating conditions
Temperature:
Column chamber: 230℃
Vaporization chamber: 250℃
Detection chamber: 250℃
Gas flow rate:
Carrier gas nitrogen: 30ml/min
Hydrogen: 40ml/min
Air: 350~400ml/min
Sensitivity×attenuation: 100×1/2
Paper speed: 60mm/h
Relative retention time:
Cis-permethrin: 1.00 (about 7.3min) trans-permethrin: 1.14 (about 8.3min) Sebacic acid dioctanoic acid: 2.09 (about 15.3min) The above gas chromatography operating conditions are typical operating parameters. Analysts can make appropriate adjustments to the operating parameters according to the performance of the instrument to obtain the best effect.
2.4.3 Determination of relative correction factor f value
Accurately weigh 0.10-0.12g (accurate to 0.0002g) of dioctyl decanoate and 0.06-0.07g (accurate to 0.0002g) of permethrin standard with known accurate content into a stoppered sample bottle, add appropriate amount of acetone to dissolve, and shake well. Under the above chromatographic operating conditions, use a 10uL syringe to draw the sample solution and inject it into the chromatographic column, and calculate the relative correction factor f value according to formula (1). f=mi·P:A
wherein: m:, m,
are the mass of permethrin standard and di-n-octyl sebacate, g; the percentage of permethrin standard;
A; and A, are the peak areas of permethrin standard and di-n-octyl sebacate, mm2. 2.4.4 Determination of sample contentbzxz.net
... (1)
Accurately weigh 0.10-0.12 g (accurate to -0.0002 g) of permethrin sample and 0.10-0.12 g (accurate to 0.0002 g) of internal standard di-n-octyl sebacate in a stoppered sample bottle, dissolve them in appropriate amount of acetone, spread them thoroughly, and under the same chromatographic operating conditions for determining the f value, use a 10μL syringe to draw the sample solution and inject it into the chromatographic column. 2.4.5 Calculation
·39·
HG/T2988-1988（1997)
The mass percentage content X of cis-permethrin shall be calculated according to formula (2): X,(%))=
The mass percentage content X of trans-permethrin shall be calculated according to formula (3): A
m', ·A'2
X2(%)=f×
The mass percentage content X of permethrin sample shall be calculated according to formula (4): X = X, + X2
Wherein: m, m—are the masses of sample and di-n-octyl sebacate, respectively, in g; A\a, A2, A are the peak areas of cis-permethrin, trans-permethrin and di-n-octyl sebacate, respectively, in mm; —relative correction factor.
2.4.6 Method Deviation
The parallel deviation of this method is within 1.5% for original drug and within 0.3% for emulsifiable concentrate. Additional Notes:
This standard is under the jurisdiction of the Pesticide Standardization Office of Shenyang Chemical Research Institute. This standard was drafted by Jiangsu Pesticide Research Institute. The main drafter of this standard is Tong Lu.
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