GB 24755-2009 English PDF

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GB 24755-2009: [GB/T 24755-2009] Thiophanate-methyl technical
Status: Valid

Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
GB 24755-2009	259	Add to Cart	3 days	[GB/T 24755-2009] Thiophanate-methyl technical	Valid

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Basic data

Standard ID: GB 24755-2009 (GB24755-2009)
Description (Translated English): [GB/T 24755-2009] Thiophanate-methyl technical
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Classification of International Standard: 65.100.30
Word Count Estimation: 10,113
Date of Issue: 2009-11-30
Date of Implementation: 2010-07-01
Quoted Standard: GB/T 1601; GB/T 1604; GB/T 1605-2001; GB 3796
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 thiophanate-methyl original drug requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to thiophanate-methyl and its impurities generated in the production of methyl thiophanate original drug.

GB 24755-2009: [GB/T 24755-2009] Thiophanate-methyl technical

---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Thiophanate-methyl technical ICS 65.100.30 G25 National Standards of People's Republic of China Thiophanate-methyl original drug 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 draft standard method using the reformed modified using FAO Specifications 262/T C/S/F (1993) "thiophanate-methyl original drug." The main difference between the present technical standard with FAO Specifications 262/T C/S/F (1993) as follows. This standard specifies --- DAP (2,3- diamino phenazine) mass fraction of not more than 5.0mg/kg, FAO Specifications predetermined DAP (2,3- two Diaminophenazine) mass fraction of not more than 0.5mg/kg; --- This standard specifies a pH range of indicators corresponding to a predetermined acidity index FAO specifications; --- This standard specifies the drying loss indicators, FAO specifications not control the indicators. The date of implementation of this standard, the former Chemical Industry Standard HG2462.1-1993 "thiophanate-methyl original drug" void. 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. Shenyang Chemical Research Institute. Participated in the drafting of this standard. Jiangsu abundance of blue and Chemical Corporation, Haili Guixi Chemical Pesticide Co., Ltd., Jiangsu dragon of Studies Limited. The main drafters. Meibao Gui, Xing Hong, XIE Yin Gang, Running an, Feng Xiuzhen, Ma Lin. Thiophanate-methyl original drug The active ingredient other product names, structural formulas and physicochemical parameters of the basic thiophanate-methyl is as follows. ISO common name. Thiophanate-methyl CIPAC Numeric Code. 262 Chemical name. 4,4 '- (1,2-phenylene) bis (3-methyl thioureido) Structure. Empirical formula. C12H14N4O4S2 Molecular weight. 342.40 (according to 2005 international relative atomic mass) Biological activity. bactericide Boiling point. 172 ℃ (decomposition) Vapor pressure (25 ℃). 0.0095mPa Solubility (23 ℃). water 26.6mg/L, acetone 58g/kg, chloroform 26g/kg, cyclohexanone 43g/kg, methanol 29g/kg, Acetonitrile 24g/kg, ethyl acetate 11.9g/kg; slightly soluble in n-hexane Stability., stable in a neutral aqueous solution at room temperature; air and light stability; is very stable at room temperature, the weak acid solution; with a copper salt Form a complex in the plant tissue and long-term storage of the suspension may be formed carbendazim Range 1 This standard specifies the requirements thiophanate-methyl original drug, Test Method for marking, labeling, packaging, storage and transportation. This standard applies to impurities derived from thiophanate-methyl, and the production of the composition of the original drug thiophanate-methyl.

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. 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 White to gray powder. 3.2 Technical Specifications Thiophanate-methyl original drugs should also meet the requirements of Table 1. Table 1 thiophanate-methyl original drug control programs Index Item Index Thiophanate-methyl mass fraction /% ≥ 95.0 HAP (2- amino-3-hydroxy-phenazine) A mass fraction/(mg/kg) ≤ 0.5 DAP (2,3- diamino phenazine) A mass fraction/(mg/kg) ≤ 5.0 The pH range of 5.0 to 8.0 Loss on drying /% ≤ 0.5 When a normal production, HAP content, DAP mass fraction was measured at least once every three months. Test Method 4 4.1 Sampling Carried out in GB/T 1605-2001 of "original drug product sampling" approach. Determined by sampling a random number table method packages, the amount of the final sample Not less than 100g. 4.2 Identification Test HPLC --- This identification test can be carried out simultaneous determination of the content of thiophanate methyl and spirit. In the same chromatographic operating conditions , The peak of a retention time in the sample solution and the standard solution thiophanate-methyl retention time, the relative difference of 1.5% should be Or less. Infrared spectroscopy --- sample and thiophanate-methyl standard IR in the range 4000cm-1 ~ 400cm-1 absorption spectrum should ignorance Significant differences. Thiophanate-methyl standard infrared spectra of Figure 1. FIG 1 thiophanate-methyl standard IR spectrum 4.3 Determination of the mass fraction of thiophanate-methyl 4.3.1 Method summary Sample was dissolved in methanol, methanol + water as the mobile phase, used Hypersil-ODS filler stainless steel column and UV detector (269 nm), thiophanate-methyl of the sample were separated by HPLC, external standard. 4.3.2 Reagents and solutions Methanol. HPLC grade; Water. The new secondary steam distilled water; Thiophanate-methyl Sample. thiophanate-methyl known mass fraction, ≥98.0%. 4.3.3 Instruments HPLC. a variable wavelength UV detector; Chromatographic data processor; Column.200mm × 4.6mm (. I.d) stainless steel column, built-Hypersil-ODS, 5μm packing; Filter. membrane pore size of about 0.45 m; Microsyringe. 50μL; Quantitative sampling tube. 10μL; Ultrasonic cleaning. 4.3.4 HPLC operating conditions Mobile phase. [Psi] (methanol. water) = 60.40, by membrane filtration, and degassing; Flow rate. 1.0mL/min; Column temperature. room temperature; Detection wavelength. 269nm; Injection volume. 10μL; Retention time. thiophanate-methyl about 4.8min. Are typical operating parameters of the above, according to the characteristics of different instruments, for a given operating parameters appropriately adjusted to obtain the best result. Typical thiophanate-methyl original drug by HPLC is shown in Figure 2. 1 --- thiophanate-methyl. Figure 2 HPLC thiophanate-methyl original drug 4.3.5 Determination Step 4.3.5.1 Preparation of standard solution Thiophanate-methyl Weigh 0.1 g of standard sample (accurate to 0.0002g), a 50mL volumetric flask, dissolve and dilute to volume with methanol, Shake well. 5mL pipetted with the above solution diluted further with methanol 50mL volumetric flask to the mark. 4.3.5.2 Preparation of sample solution Thiophanate-methyl, said sample is taken containing 0.1g (accurate to 0.0002g), a 50mL volumetric flask, dissolved in methanol and diluted to Mark and shake. A pipetted sample solution was diluted to 5mL above another in methanol 50mL volumetric flask to the mark. 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, the needle until two adjacent thiophanate methyl pk area opposite After the change is less than 1.2%, measured according to the standard solution, sample solution, the sample solution, the order of standard solution. 4.3.6 computing The measured sample solution and the preceding two needles two doses of the standard sample solution thiophanate-methyl pk area were averaged. A sample Mass fraction of 1-yl thiophanate (%), according to equation (1). 1 = A2 (1) Where. A1 --- the standard solution, the average area of thiophanate-methyl pk; A2 --- sample solution, thiophanate-methyl pk average area; --- Sample mass fraction thiophanate methyl, expressed in%. 4.3.7 allows poor Results difference between the two replicates thiophanate-methyl content should not exceed 1.2%, and the arithmetic mean value as a measurement result. Determination of DAP and 4.4 HAP mass fraction 4.4.1 Method summary Sample dissolved in mobile phase to a potassium dihydrogen phosphate buffer solution pH8.0 + methanol + water as mobile phase, used HypersilODS Stainless steel column filler and UV - VIS detector (453nm), and sample the HAP DAP reverse phase high performance liquid chromatographic From, external standard. (HAP, DAP detection limit of 2 × 10-9g, equivalent to 0.2mg/kg). 4.4.2 Reagents and solutions Methanol. HPLC grade; Potassium dihydrogen phosphate; Water. The new secondary steam distilled water; Sodium hydroxide solution. ρ (NaOH) = 40g/L; Buffer solution. Weigh 6.8g of potassium dihydrogen phosphate in distilled water with the secondary reagent bottle 1000mL, ultrasonic oscillation completely dissolved Solution, with a sodium hydroxide solution to pH 8.0; Sample HAP. known HAP content, ≥97.0%; Sample DAP. DAP known mass fraction, ≥99.0%. 4.4.3 Instruments HPLC. a variable wavelength UV detector; Chromatographic data processor; Column.200mm × 4.6mm (. I.d) stainless steel column, built-Hypersil-ODS, 5μm packing; Filter. membrane pore size of about 0.45 m; Microsyringe. 250μL; Quantitative sampling tube. 50μL; Ultrasonic cleaning; Centrifuge. 4.4.4 HPLC operating conditions Mobile phase. [Psi] (methanol. water. buffer solution) = 45.25.30; Flow rate. 1.0mL/min; Column temperature. room temperature (temperature change should be less than 2 deg.] C); Detection wavelength. 453nm; Injection volume. 50μL; Retention time. HAP about 3.6min; DAP about 10.6min. Are typical operating parameters of the above, according to the characteristics of different instruments, for a given operating parameters appropriately adjusted to obtain the best result. Of HAP, DAP standard sample by HPLC is shown in Figure 3, thiophanate-methyl original drug of HAP assay, HPLC DAP in Figure 4. FIG. 1 --- HAP; 2 --- DAP. FIG 3 HAP and DAP standard liquid chromatography FIG. 1 --- HAP; 2 --- DAP. HPLC FIG. 4 thiophanate-methyl original drug as measured in HAP and DAP 4.4.5 Determination Step 4.4.5.1 Preparation of standard solution 4.4.5.1.1 HAP Preparation of standard solution (A solution) Sample HAP accurately weighed 0.025 g (accurate to 0.0002g) in brown 50mL volumetric flask, diluted with methanol to the mark, the super Was dissolved under sonication 10min, shake well and let to room temperature and set aside. (The solution was stable in the dark at 4 ℃ for 2 months.) 4.4.5.1.2 DAP Preparation of standard solution (B solution) Sample DAP accurately weighed 0.025 g (accurate to 0.0002g) in brown 50mL volumetric flask, diluted with methanol to the mark, the super Was dissolved under sonication 10min, shake well and let to room temperature and set aside. (The solution was stable in the dark at 4 ℃ for 2 months.) Preparation 4.4.5.1.3 DAP, HAP standard solution Pipette 50μLA solution, 50μLB solution, diluted with a 25mL volumetric flask with brown flowing to the mark. (The standard The solution must be prepared before use. ) 4.4.5.2 Preparation of sample solution 10.0 g was weighed accurately (accurate to 0.0002g) sample was brown 100mL volumetric flask, added with a pipette flow 50mL compatibility Was shaken under ultrasound 20min, shake well and let to room temperature. Then at 3000r/min centrifugal 5min, the supernatant was filtered. 4.4.5.3 Determination Under the above operating conditions, after the instrument is stable, the number of continuous injection needle the DAP, HAP standard solution until two adjacent needles HAP, the DAP After the peak area relative variations are less than 20%, measured according to the standard solution, sample solution, the sample solution, the order of standard solution. 4.4.6 computing Sample HAP (DAP) the mass fraction 2 (mg/kg), according to formula (2). 2 = A2 104 (2) Where. A1 --- the standard solution, the average HAP (DAP) peak area; A2 --- sample solution, the average HAP (DAP) peak area; --- standard samples HAP (DAP) mass fraction, expressed in%; 500 --- standard dilution. 4.4.7 allows poor Determination results parallel relative deviation should not exceed 30%, and the arithmetic mean value as a measurement result. Carried out in GB/T 1601. 4.6 Determination of loss on drying 4.6.1 Instruments Oven. 105 ℃ ± 2 ℃; Weighing bottle. an inner diameter of 70mm, 40mm high; Dryer. 4.6.2 Determination Step The weighing bottle placed in an oven bake IH, placed in a desiccator taken cooled to room temperature, weigh (accurate to 0.0002g). Repeating the above steps Step, until a constant weight weighing bottle. 2g sample was placed in the bottle, paving, weighed (accurate to 0.01g), the weighing bottle placed in an oven, without Cap, post-baking IH, removed and placed in a desiccator to cool to room temperature, weigh (accurate to 0.0002g). 4.6.3 computing The mass fraction of the sample 3 Loss on drying (%), according to equation (3) is calculated. (3) Where. 4.6.4 allows poor The measurement results of the two parallel relative deviation should not exceed 30%; and the arithmetic mean as a measurement result. 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 mark thiophanate-methyl original drug, labeling and packaging should comply with the provisions of GB 3796. 5.2 Cleaning packaging applications original drug thiophanate-methyl, dried polyurethane barrel, net content should be less than 200kg. Also be based on User requests or orders for other forms of packaging agreement, subject to the provisions of GB 3796. 5.3 thiophanate-methyl 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 Safety. thiophanate-methyl is a low toxicity fungicides, plant safety. The FDA should wear protective equipment, wash with soap after application net. This product is generally less prone to poisoning. Such as poisoning, atropine detoxification can be used under the guidance of doctors. Acceptance of 5.6. thiophanate-methyl original drug acceptance period of 1 month. Complete product quality inspection from the date of delivery within one month of its finger Standard shall comply with this standard. ......

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