GB 24756-2009 English PDF

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GB 24756-2009: [GB/T 24756-2009] Buprofezin technical
Status: Valid

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GB 24756-2009	319	Add to Cart	3 days	[GB/T 24756-2009] Buprofezin technical	Valid

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Basic data

Standard ID: GB 24756-2009 (GB24756-2009)
Description (Translated English): [GB/T 24756-2009] Buprofezin technical
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Classification of International Standard: 65.100.10
Word Count Estimation: 12,14
Date of Issue: 2009-11-30
Date of Implementation: 2010-07-01
Quoted Standard: GB/T 601; GB/T 603; GB/T 1604; GB/T 1605-2001; GB 3796; GB/T 19138
Regulation (derived from): Announcement of Newly Approved National Standards No. 14 of 2009 (No. 154 overall)
Issuing agency(ies): General Administration of Quality Supervision, Inspection and Quarantine of the People's Republic of China, Standardization Administration of the People's Republic of China
Summary: This Chinese standard specifies the original drug Buprofezin requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to buprofezin and impurities generated in the production thiazinone original drug.

GB 24756-2009: [GB/T 24756-2009] Buprofezin technical

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Buprofezin technical ICS 65.100.10 G25 National Standards of People's Republic of China Buprofenzin original drug Posted 2009-11-30 2010-07-01 implementation Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China Standardization Administration of China released

Foreword

The standard Chapter 3, Chapter 5 is mandatory, the rest are recommended. From the date of implementation of this standard, HG2463.1-1993 "buprofenzin original drug" abolished. Appendix A of this standard is an informative annex. The standard proposed by China Petroleum and Chemical Industry Association. This standard by the National Standardization Technical Committee on Pesticides (SAC/TC133) centralized. This standard is drafted by. Shenyang Chemical Research Institute. Participated in the drafting of this standard. Jiangsu Ampang Electrochemical Co., Ltd., Jiangsu Changlong Chemical Co., Chemical Co., Ltd. Shanghai Yue Jiang Su dragon Chemical Co., Ltd. The main drafters of this standard. Pi-Long, Zan Yan Kun, Jiang Yutian, Ruiyan Chun, Xiang Yu hair of cloud point, Li Maoqing. Buprofenzin original drug The active ingredients of the product thiophene-one hydrochloride other name, structural formula and basic physicochemical parameters are as follows. ISO common name. buprofezin Chemical Name. 2- Laid - butylimino-3-isopropyl-5-phenyl-1,3,5-thiadiazole-4-one Structure. Empirical formula. C16H23N3OS Molecular Weight. 305.4 (according to 2005 international relative atomic mass) Biological activity. Insecticidal Melting point. 104.5 ℃ ~ 105.5 ℃ Vapor pressure (25 ℃). 1.25mPa Density (20 ℃). 1.18 Solubility (25 ℃, g/L). water 0.9mg/L (20 ℃), trichloromethane 520, 370 as benzene, toluene, 320, 240 as acetone, ethanol 80, n Hexane 20 Stability. stable to acid or alkali, light or heat-stable

1 Scope

This standard specifies the buprofenzin original drug requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to the impurities generated by the buprofezin and production consisting of buprofezin original drug.

2 Normative references

The following documents contain provisions which, through reference in this standard and become the standard terms. For dated references, subsequent Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to the agreement are based on research Whether the latest versions of these documents. For undated reference documents, the latest versions apply to this standard. Preparation of GB/T 601 chemical reagent standard titration solution GB/T 603 chemical reagent in test methods - Preparations with GB/T 1604 Goods pesticide regulations for acceptance GB/T 1605-2001 Sampling Method commercial pesticides GB 3796 pesticide packaging General GB/T 19138 Determination of acetone insoluble pesticide

3 Requirements

3.1 Appearance. crystalline powder should be white to pale yellow or white, no visible foreign matter. 3.2 buprofenzin original drug should be consistent with the requirements in Table 1. Table 1 buprofenzin original drug quality control program indicators Item Index Buprofenzin mass fraction /% ≥ 97.0 Loss on drying /% ≤ 0.3 Acidity (H2SO4 dollars) or alkalinity (NaOH meter) /% ≤ 0.1 Acetone insolubles a /% ≤ 0.2 a insoluble in acetone under normal production conditions, measured at least once every three months. Test Method 4 4.1 Sampling According to GB/T 1605-2001 "on the original drug product sampling" approach. Determining sample package using a random number table method; the final sample size Not less than 100g. 4.2 Identification Test Infrared spectroscopy --- sample and standard samples in the IR 4000cm-1 ~ 400cm-1 Scope absorption spectrum should be no significant difference. Thiophene Piperazinone standard infrared spectrum is shown in Figure 1. Figure 1 buprofenzin standard infrared spectrum Gas Chromatography --- The identification test can be carried out simultaneously with the determination of the content of buprofezin. Under the same chromatographic operating conditions, the sample solution The solution buprofezin peak retention time and the retention time of a standard solution peak, the relative difference should be less than 1.5%. 4.3 buprofenzin mass fraction determination 4.3.1 Method summary Sample was dissolved in chloroform, dicyclohexyl phthalate esters as internal standard, using the 5% HP-5 capillary column coated walls and hydrogen Flame ionization detector, the sample of buprofezin gas chromatography separation and determination. You can also use packed column gas chromatography, chromatography strip Member See Appendix A. 4.3.2 Reagents and solutions Chloroform; Buprofenzin standard. a known mass fraction, ≥98.0%; Dicyclohexyl phthalate esters. interference analysis should not contain impurities; Internal standard solution. Weigh 4.0g dicyclohexyl phthalate esters, placed in 500mL flask with chloroform dissolved and diluted to the mark Degree, shake. 4.3.3 Instruments Gas chromatograph. with a hydrogen flame ionization detector; Chromatographic data processor or chromatography workstation; Column. 30m × 0.32mm (i.d.) Capillary column, wall coated HP-5 (5% + 95% diphenyl dimethyl silicone), the film thickness 0.25μm; Micro injector. 10μL. 4.3.4 GC operating conditions Temperature (℃). 230 column temperature, the gasification chamber 270, the detector chamber 280; Gas flow rate (mL/min). carrier gas (N2) 2.0, hydrogen gas 30, air 300, the compensation gas (N2) 25; Split ratio. 20.1; Injection volume (μL). 1.0; Retention time (min). 3.8 buprofezin, internal standard 7.0. GC operating conditions described above, the Department of typical operating parameters. According to the characteristics of different instruments, given operating parameters adjusted as appropriate, In order to obtain the best results. Typical buprofenzin original drug capillary column gas chromatography is shown in Figure 2. 1 --- solvent; 2 --- buprofezin; 3 --- internal standard (phthalate, dicyclohexyl phthalate). Figure 2 buprofenzin original drug and the internal standard capillary column gas chromatogram 4.3.5 measuring step 4.3.5.1 preparation of standard solution Weigh buprofenzin standard 0.08g (accurate to 0.0002g) in 15mL stoppered glass bottle with a pipette accurately added 10mL within Standard solution, shake. 4.3.5.2 preparation of the sample solution Weigh containing buprofezin 0.08g (accurate to 0.0002g) sample in 15mL stoppered glass bottle with a pipette and 4.3.5.1 with Tube accurately added internal standard solution 10mL, shake. 4.3.5.3 Determination Under these operating conditions, the instrument until a stable baseline, the number of continuous injection doses of the standard solution until the two needles buprofezin and the internal standard peak adjacent When the area ratio changes by less than 1.2%, according to the solution, the sample solution, the sample solution and standard sequence of the standard solution was measured. 4.3.6 Calculation The two needle sample solution and measured before and after the two doses of the standard sample solution piperazinone and thiophene internal standard peak area ratios are averaged. test 1 sample mass fraction (%) of buprofezin according to formula (1). (1) Where. --- Standard samples buprofezin mass fraction, expressed as a percentage. 4.3.7 allowable difference Thiophene-one hydrochloride poor quality score measurement results of two parallel, should not exceed 1.2%, and the arithmetic mean as a measurement result. 4.4 Determination of loss on drying 4.4.1 Instruments Weighing bottle. diameter 50mm, height 20mm; Oven. 100 ℃ ± 2 ℃; Dryer. 4.4.2 measuring step Bake bottle weighed into 100 ℃ ± 2 ℃ oven for 30min, and then into the dryer to cool to room temperature, weigh (to the nearest 0.0002g). In weighing bottle was weighed into a 10g sample (paved weighed accurate to 0.0002g). The weighing bottle placed in an oven, uncovered At 100 ℃ ± 2 ℃ bake 1.5h, removed into the drier cooled to room temperature until constant weight was weighed (accurate to 0.0002g). 2 Loss on drying (%) according to equation (2). 100 (2) Where. 4.5 Determination of acidity or alkalinity 4.5.1 Reagents and solutions acetone; Sodium hydroxide standard titration solution. Ba (NaOH) = 0.02mol/L, according to GB/T 601 preparation and calibration; Hydrochloric acid standard titration solution. Ba (HCl) = 0.02mol/L, according to GB/T 601 preparation and calibration; Methyl red solution. 1g/L ethanol solution, according to GB/T 603 preparation; Bromocresol green solution. 1g/L ethanol solution, according to GB/T 603 preparation; Mixed indicator solution. a solution of methyl red + bromocresol green solution = 2 + 10. 4.5.2 measuring step Weigh 2g sample (accurate to 0.0002g) in 250mL conical flask, 50mL acetone solution of mixed indicator solution 5 drops ~ 6 drops of sodium hydroxide standard titration solution was titrated to green as the end point, at the same time make a blank measurement. If the test solution is alkaline, hydrochloric acid required standard Titration solution was titrated to a pink end at the same time make a blank measurement. 3 acidity (%) of the sample according to equation (3) to calculate or alkalinity 4 (%) by (4) Calculation Formula. 3 = Ba · (Vp Vp 1- 0) · M 100 (3) Where. Ba --- the actual concentration of sodium hydroxide standard titration solution, expressed in moles per liter (mol/L); V0 --- titrate blank solution, the volume of consumption of sodium hydroxide standard titration solution, in milliliters (mL); Vp 1 --- titration of the sample solution, the volume of consumption of sodium hydroxide standard titration solution, in milliliters (mL); --- The M sulfuric acid molar mass values, in units of grams per mole (g/mol) [M (12H2SO4 ) = 49]. 4 = Ba ' · (Vp '1- Vp' 0) · M 100 (4) Where. Ba '--- the actual concentration of hydrochloric acid standard titration solution, expressed in moles per liter (mol/L); Vp '0 --- titrate blank solution, hydrochloric acid standard titration solution consumption volume in milliliters (mL); Vp '1 --- titration of the sample solution, hydrochloric acid standard titration solution consumption volume in milliliters (mL); --- NaOH molar mass of the M values, in units of grams per mole (g/mol) [M (NaOH) = 40]. 4.6 Determination of acetone insolubles According to GB/T 19138 performed. 4.7 product testing and acceptance Product inspection and acceptance shall comply with GB/T 1604's. Treatment of extreme values, using the rounding value comparison method. 5 marking, labeling, packaging, storage and transportation 5.1 buprofenzin original drug marking, labeling and packaging should comply with the provisions of GB 3796. 5.2 buprofenzin original drug use clean plastic bucket (bags), barrel (Bag) Net content is generally 25kg, 50kg or 200kg. 5.3 is also available upon request or order agreement, the use of other forms of packaging, subject to the provisions of GB 3796. 5.4 buprofenzin original drug package should be stored in well-ventilated, dry coffers. 5.5 storage, prevent moisture and sunlight, no food, seed, feed mix, avoid contact with skin, eyes, mouth and nose to prevent inhalation. 5.6 Safety. This product is a low-toxic pesticides, are swallowed and inhaled toxic, it can penetrate through the skin. Wear goggles and rubber gloves when using this product And other necessary protective clothing. Such as skin, eyes accidentally stained with the product, rinse immediately with plenty of water. Coverage were immediately sent to hospital first aid. 5.7 of acceptance. Acceptance of buprofenzin original drug for a month. From the date of delivery, product quality inspection completed within a month, its Indicators shall comply with this standard.

Appendix A

(Informative) Buprofenzin quality gas chromatographic method scores packed column A. 1 Method summary Sample was dissolved in chloroform, dicyclohexyl phthalate esters as internal standard, using the 5% OV-101/GaschromQ filler Column and flame ionization detector, the sample of buprofezin gas chromatography separation and determination. A. 2 Reagents and solutions Chloroform; Fixative. OV-101; Carrier. GaschromQ particle diameter of 180μm ~ 250μm; Dicyclohexyl phthalate esters. shall not interfere with the analysis of impurities; Internal standard solution. Weigh 4.0g dicyclohexyl phthalate esters in 500mL flask with chloroform dissolved and diluted to the mark, Shake; Buprofenzin standard. a known mass fraction, ≥98.0%. A. 3 Instrument Gas chromatograph. with a hydrogen flame ionization detector; Chromatographic data processor or chromatography workstation; Column. 1m × 3mm (. I.d) glass column, built 5% OV-101/GasChromQ filler particle size 180μm ~ 250μm (Or other columns with the same column efficiency); Micro injector. 10μL. A. 4 GC operating conditions Temperature (℃).200 column temperature, the gasification chamber 250, the detector chamber 250; Gas flow rate (mL/min). carrier gas (N2) 30, hydrogen gas 40, air 400; Retention time (min). 5 buprofezin; phthalate, dicyclohexyl phthalate 10; GC operating conditions described above, the Department of typical operating parameters. According to the characteristics of different instruments, given operating parameters adjusted as appropriate, In order to obtain the best results. Packed column gas chromatography is shown in Figure A typical buprofenzin original drug A. 1. 1 --- solvent; 2 --- buprofezin; 3 --- internal standard (phthalate, dicyclohexyl phthalate). Figure A. Packed Column Gas Chromatography 1 buprofenzin original drug and the internal standard A. 5 measuring step A. 5.1 preparation of standard solution Weigh buprofenzin standard 0.08g (accurate to 0.0002g) in 15mL stoppered glass bottle with a pipette accurately transferred within 10mL Standard solution, and shake. A. 5.2 Sample preparation solution Weigh about 0.08g sample containing buprofezin the (accurate to 0.0002g) in 15mL stoppered glass vial, with A. With 5.1 used A pipette accurately transferred to the internal standard solution 10mL, shake. A. 5.3 Determination Under these operating conditions, the instrument until a stable baseline, the number of continuous injection doses of the standard solution, calculated for each needle buprofezin and the internal standard peak area The ratio of repeatability. When the relative change to be adjacent to the two-pin buprofezin and the internal standard peak area ratio of less than 1.2%, according to the standard solution, sample solution Solution, sample solution, the order of the standard solution was measured. A. 6 Calculation The two needle sample solution and measured before and after the two doses of the standard sample solution buprofezin and the internal standard peak area ratios are averaged. Buprofezin sample mass fraction of 1 (%) according to equation (A.1) Calculated. (A.1) Where. --- Standard samples buprofezin mass fraction, expressed as a percentage. Book GB 24756-2009 A. 7 allowable difference The difference between two parallel determination results shall not be greater than 1.2%, the arithmetic mean value as a measurement result. ......

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