GB 24758-2009 English PDF

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GB 24758-2009: [GB/T 24758-2009] Thifensulfuron-methyl technical
Status: Valid

Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
GB 24758-2009	209	Add to Cart	3 days	[GB/T 24758-2009] Thifensulfuron-methyl technical	Valid

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Basic data

Standard ID: GB 24758-2009 (GB24758-2009)
Description (Translated English): [GB/T 24758-2009] Thifensulfuron-methyl technical
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Classification of International Standard: 65.100.20
Word Count Estimation: 8,846
Date of Issue: 2009-11-30
Date of Implementation: 2010-07-01
Quoted Standard: GB/T 1600; GB/T 1601; GB/T 1604; GB/T 1605-2001; GB 3796
Adopted Standard: FAO 452.201/TC/S-2000, MOD
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 Thifensulfuron original drug requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to thifensulfuron and impurities generated in the production of thifensulfuron original drug.

GB 24758-2009: [GB/T 24758-2009] Thifensulfuron-methyl technical

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Thifensulfuron-methyl technical ICS 65.100.20 G25 National Standards of People's Republic of China Thifensulfuron TC Published 2009-11-30 2010-07-01 implementation Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China Standardization Administration of China issued

Foreword

This standard in Chapter 3, Section 5 is mandatory, the rest are recommended. This modification uses FAO Standard Specification 452.201/T C/S (2000) "thifensulfuron original drug." This standard modification method using foreign advanced standards for the redrafted law. This standard FAO Specifications 452.201/T C/S (2000) "thifensulfuron TC" The main technical differences. This standard specifies --- thifensulfuron mass fraction ≥95.0%, FAO specifications thifensulfuron predetermined mass fraction ≥960g/kg; --- This standard specifies the original drug thifensulfuron water ≤0.5%, FAO specifications not specified; This standard specifies --- thifensulfuron TC pH range of 3.0 ~ 7.0, FAO specifications not specified; --- This standard specifies the original drug thifensulfuron N, N- dimethylformamide insolubles ≤0.3%, FAO specifications not specified. The standard proposed by China Petroleum and Chemical Industry Association. This standard by the National Pesticide Standardization Technical Committee (SAC/TC133). This standard is drafted by. the Ministry of Agriculture. It participated in the drafting of this standard. Anhui Fengle Agrochemical Co., Ltd., Jiangsu Province Institute of hormones. The main drafters. Wu Jinlong, Hu Qin, Chen Tiechun, Jin Jinsong, Fan Lei, Yu Rong, Li Guoping. Thifensulfuron TC This product is an active ingredient of other names, structural formulas and physicochemical parameters of the basic thifensulfuron follows. ISO common name. thifensulfuron-methyl CIPAC digital code. 452 CA Registry Number. 79277-27-3 Chemical Name. 3- (4-methoxy-6-methyl-1,3,5-triazin-2-yl) -1- (2-methoxy-formyl thiophen-3-yl) - sulfonyl urea Structure. Empirical formula. C12H13N5O6S2 Molecular weight. 387.4 (according to 2005 international relative atomic mass) Biological activity. weeding Melting point. 176 ℃ (TC 171 ℃) Vapor pressure (25 ℃). 1.7 × 10-8Pa Solubility (g/L, 25 ℃). water 0.223 (pH5), 2.240 (pH7), 8.830 (pH9); hexane < 0.1, o-xylene 0.212, ethyl acetate 3.3, methanol 2.8, 7.7 acetonitrile, acetone, 10.3, 23.8 methylene chloride Stability. neutral, weakly alkaline aqueous solution more stable, acidic hydrolysis in aqueous solution at accelerated DT504 ~ 6d (pH5) Range 1 This standard specifies the requirements thifensulfuron original drug, Test Method for marking, labeling, packaging, storage and transportation. This standard applies to impurities derived from Thifensulfuron composition and production thifensulfuron original drug.

2 Normative references

Terms of the following documents become provisions of this standard by reference in this standard. For dated reference documents, all later Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to agreements based on this standard Whether the latest versions of these documents. For undated references, the latest version applies to this standard. GB/T 1600 Pesticide Method Moisture Determination 1601 pH value pesticides GB/T GB/T 1604 pesticide regulations for acceptance of goods GB/T 1605-2001 sampling commercial pesticides GB 3796 pesticide packaging General 3.1 Appearance. This product should be white to pale yellow loose powder, without visible foreign matter. 3.2 thifensulfuron TC shall comply with the requirements in Table 1. Table 1 TC thifensulfuron control program Index Item Index Thifensulfuron mass fraction /% ≥ 95.0 Moisture /% ≤ 0.5 The pH range of 3.0 to 7.0 N, N- dimethylformamide insolubles a /% ≤ 0.3 When a normal production, N, N- dimethylformamide insolubles every three months, at least once. Test Method 4 4.1 Sampling According to GB T 1605-2001 "commodity original drug sample"/carried out. Determined by sampling a random number table method packages, less than the amount of the final sample 100g. 4.2 Identification Test HPLC --- This identification test can be carried out simultaneously with the measurement of thifensulfuron mass fraction. In the same chromatographic operating conditions Next, a peak with a retention time of sample solution thifensulfuron standard peak retention time of the solution, the relative difference of 1.5% should be Or less. Infrared spectroscopy --- sample and standard in the range of 4000cm-1 ~ 400cm-1 in an infrared absorption spectrum, to be no significant difference different. Thifensulfuron standard infrared spectrum is shown in Figure 1. FIG 1 thifensulfuron standard IR spectrum Determination of mass fraction thifensulfuron thiazol 4.3 4.3.1 Method summary Sample was dissolved in acetonitrile, methanol + water as the mobile phase, used as a filler C18 stainless steel column and UV detector (250 nm) to External standard sample thifensulfuron reverse phase high performance liquid chromatography and determination, external standard. 4.3.2 Reagents and solutions Methanol. HPLC grade; Acetonitrile. HPLC grade; Phosphoric acid. AR; Water. The new secondary steam distilled water; Thifensulfuron Sample. a known mass fraction, ≥98.0%. 4.3.3 Instruments HPLC. a variable wavelength UV detector; Chromatographic data processor or chromatography workstation; Column. 250mm × 4.6mm (. I.d) stainless steel column, built ZORBAXSB-C18,5μm filler (or other equally effective Column); Filter. membrane pore size of about 0.45 m; Microsyringe. 50μL; Quantitative sampling tube. 5μL; Ultrasonic cleaning. 4.3.4 HPLC operating conditions Mobile phase. [Psi] (methanol. water) = 65.35, adjusted with phosphoric acid where water pH = 3, filtered through a filter membrane and degassed; Mobile phase flow rate. 1.0mL/min; Column temperature. 30 ℃; Detection wavelength. 250nm; Injection Volume. 5.0μL; Retention time. thifensulfuron about 4.0min. The above are typical operating parameters, according to different characteristics of the instrument and the columns for a given operating parameter adjusted as appropriate, in order to obtain the most Good effect. Typical thifensulfuron HPLC TC shown in Figure 2. 1 --- thifensulfuron. FIG 2 FIG thiazol HPLC thifensulfuron original drug 4.3.5 Determination Step 4.3.5.1 Preparation of standard solution Thifensulfuron weighed 0.05 g of standard sample (accurate to 0.0002g), a 100mL volumetric flask, dissolved in acetonitrile and dilute to volume, Shake well. 4.3.5.2 Preparation of sample solution Weigh a sample containing thiophene thifensulfuron 0.05g of (accurate to 0.0002g), a 100mL volumetric flask, and dilute with acetonitrile to dissolve Mark and shake. 4.3.5.3 Determination Under the above operating conditions, after the instrument is stable, the number of consecutive doses of the standard solution is injected until the two adjacent needles thifensulfuron peak area becomes relatively After less than 1.2% of, measured according to the standard solution, sample solution, the sample solution, the order of standard solution. 4.3.6 computing The two needle and the sample solution was measured before and after the two doses of the standard sample solution thifensulfuron peak area are averaged. Sample thiophene Sulfosulfuron 1 mass fraction (%), according to equation (1). (1) Where. A1 --- the standard solution, thifensulfuron average peak area; A2 --- sample solution, thifensulfuron average peak area; --- standard samples thifensulfuron mass fraction, expressed in%. 4.3.7 allows poor The measurement results of the two parallel error should not exceed 1.2%, and the arithmetic mean value as a measurement result. 4.4 Determination of Moisture Carried out in GB/T 1600 in the "Karl Fischer" method. Carried out in GB/T 1601. Determination of 4.6 N, N- dimethylformamide insolubles 4.6.1 Method summary Samples with an appropriate amount of N, N- dimethylformamide was heated and dissolved, insolubles were filtered hot and dried, N, N- dimethylformamide containing insolubles Based on the amount of solid insoluble mass fraction of the sample. 4.6.2 Reagents N, N- dimethylformamide. 4.6.3 Instruments Standard ground-stoppered Erlenmeyer flask. 250mL; reflux condenser; glass fritted funnel crucible or G3; suction conical flask. 500mL; oven; Glass dryer; bath oil pan. 4.6.4 Determination Step The glass fritted funnel crucible drying (110 ℃, about 1h) to a constant weight (to the nearest 0.0002g), cooled in a desiccator until use. Call 10g sample was taken (accurate to 0.0002g), placed in a conical flask, 150 ml of N, N-dimethylformamide and shaken as far as possible the sample Dissolved. Then fitted with a reflux condenser and heated to about 120 ℃ in an oil bath, heating was stopped after holding 5min. Crucible assembly fritted funnel Suction filtration apparatus, under reduced pressure as soon as the hot solution was quickly through the funnel. 60mL with hot N, N- dimethylformamide divided washed 3 times, pumping Remove the dry glass fritted funnel crucible, which was placed in an oven dried 160 ℃ for 30 min (making constant weight), withdrawn into the dryer, cooled Was weighed (accurate to 0.0002g). 4.6.5 computing N, mass fraction N- dimethylformamide 2 insolubles (%), according to equation (2). (2) Where. 4.7 product testing and acceptance Shall comply with the provisions of GB/T 1604's. Process limit values using rounding value comparison method. 5 marking, labeling, packaging, storage and transportation 5.1 flag thiophene thifensulfuron original drug, label, package, should meet the requirements of GB 3796. 5.2 thifensulfuron original drug application of clean, dry plastic liner iron, cardboard, plastic bag or plastic bucket, a net weight of each member Like to 25kg. Also available upon request or order agreement, other forms of packaging, but to comply with the provisions of GB 3796. 5.3 thifensulfuron original drug package airiness, dry place. 5.4 storage and transportation to prevent moisture and sunlight, no food, seed, feed mix, avoid contact with skin, eyes, nose and mouth to prevent inhalation. 5.5 Security. This product is moderately toxic pesticides. Symptoms of poisoning the eyes, skin stimulation, generally do not cause systemic poisoning. use This product should wear protective gloves, goggles and masks, wear clean protective clothing, washed with soap and water immediately after application, to avoid contact with skin and eyes drugs liquid. If swallowed, should immediately, gastric lavage, activated carbon can also be used with laxatives, symptomatic treatment. Acceptance of 5.6. thifensulfuron original drug acceptance period of 1 month. From the date of delivery, within a month, complete product quality inspection, its Indicators should meet the requirements of this standard. ......

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