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GB 22602-2008 English PDF

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GB 22602-2008: [GB/T 22602-2008] Tebuconazole technical
Status: Valid
Standard IDUSDBUY PDFLead-DaysStandard Title (Description)Status
GB 22602-2008319 Add to Cart 3 days [GB/T 22602-2008] Tebuconazole technical Valid

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Basic data

Standard ID: GB 22602-2008 (GB22602-2008)
Description (Translated English): [GB/T 22602-2008] Tebuconazole technical
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Classification of International Standard: 65.100.30
Word Count Estimation: 12,157
Date of Issue: 2008-12-17
Date of Implementation: 2009-06-01
Quoted Standard: GB/T 1600; GB/T 1601; GB/T 1604; GB/T 1605-2001; GB 3796; GB/T 19138
Adopted Standard: FAO 494/TC/S/F-2000, NEQ
Regulation (derived from): Announcement of Newly Approved National Standards No. 21 of 2008 (No. 134 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 tebuconazole original drug requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to tebuconazole and impurities generated in the production of tebuconazole original drug.

GB 22602-2008: [GB/T 22602-2008] Tebuconazole 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.
Tebuconazole technical ICS 65.100.30 G25 National Standards of People's Republic of China Tebuconazole original drug Posted 2008-12-17 2009-06-01 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. This standard FAO specification 494/T C/S/F (2000) "TebuconazoleTechnical" of non-equivalent. 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 Feng Deng Pesticide Co., Shandong Huayang Technology Co., Ltd., Jiang Su Qizhou green chemical shares Limited copies. The main drafters of this standard. Jiangmin Yi, Li Xiujie, Gengrong Wei, Song Dongsheng, Hu Chunhong. Tebuconazole original drug The product is an active ingredient tebuconazole pent other name, structural formula and basic physicochemical parameters are as follows. ISO common name. Tebuconazole CAS Registry Number. 107534-96-3 CIPAC Numeric Code. 494 Chemical Name. (RS) -1- (4- chlorophenyl) -4,4-dimethyl -3- (1H-1,2,4- triazol-1-ylmethyl) pentan-3-ol Structure. Empirical formula. C16H22ClN3O Molecular Weight. 307.8 (according to 2007 international relative atomic mass) Biological activity. bactericidal Melting point. about 102.4 ℃ Vapor pressure (20 ℃). 0.013mPa Solubility (20 ℃). water 32mg/L; dichloromethane greater than 200g/L; hexane of less than 0.1g/L; isopropanol, toluene, 50g/L ~ 100g/L Stability. at pH 4 ~ 9,22 ℃ hydrolysis DT50 is greater than 1 year.

1 Scope

This standard specifies Tebuconazole original drug requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to Tebuconazole original drug impurities generated by tebuconazole and production thereof.

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. GB/T 1600 Determination of Water Pesticides Determination of GB/T 1601 Pesticides pH value 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 White to pale yellow powder. 3.2 Tebuconazole original drug should meet the requirements of Table 1. Table 1 Tebuconazole original drug quality control program indicators Item Index Tebuconazole mass fraction /% ≥ 96.0 Fraction a /% acetone insolubles ≤ 0.2 mass Moisture content /% ≤ 0.5 pH range of 6.0 to 9.0 When a normal production, acetone insoluble content was 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 at 4000cm-1 ~ 400cm-1 Scope of the infrared absorption spectrum should be no significant difference. Mark Like infrared spectrum is shown in Figure 1. Figure 1 tebuconazole standard infrared spectra Liquid chromatography --- The identification test can be carried out simultaneously with the determination of the mass fraction of tebuconazole. Under the same chromatographic operating conditions, the test The retention time of the sample solution and the standard solution to a peak of tebuconazole chromatographic retention time, the relative difference should be 1.5% Fewer. 4.3 Determination of the mass fraction of tebuconazole 4.3.1 High performance liquid chromatography (Arbitration Act) 4.3.1.1 Method summary Sample was dissolved in methanol, methanol + water as the mobile phase, use as filler in Nova-PakC18 stainless steel column and UV detector (220nm), the sample of tebuconazole high performance liquid chromatography and determination. 4.3.1.2 Reagents and solutions Methanol; Water. The new secondary steam distilled water; Tebuconazole Sample. Known tebuconazole mass fraction ≥99.0%. 4.3.1.3 Instruments High performance liquid chromatography. a variable wavelength UV detector; Chromatographic data processor or workstation; Column. 150mm × 3.9mm (i.d.) Stainless steel column, built-Nova-PakC185μm filler (or equally effective column); Filter. filter pore size of about 0.45μm; Micro injector. 50μL; Quantitative sample line. 5μL; Ultrasonic cleaner. 4.3.1.4 HPLC operating conditions Mobile phase. ψ (CH3OH.H2O) = 65.35; Flow rate. 1.0mL/min; Column temperature. room temperature (temperature change should not exceed 2 ℃); Detection wavelength. 220nm; Injection volume. 5μL; Retention time. tebuconazole about 7.0min. It said operating parameters are typical, according to the characteristics of different instruments, given operating parameters adjusted as appropriate, in order to obtain the best results. Typical Tebuconazole original drug HPLC is shown in Figure 2. 1 --- tebuconazole. Figure 2 HPLC Tebuconazole the original drug 4.3.1.5 Measurement procedure 4.3.1.5.1 Preparation of standard solution Weigh 0.1g tebuconazole standard (accurate to 0.0002g), a 50mL volumetric flask, dilute to the mark with methanol, ultrasonic oscillation 5min make sample dissolution, cooled to room temperature and shake well. Using a pipette to take the above solution 5mL to 50mL volumetric flask, diluted with methanol to Mark and shake. 4.3.1.5.2 Preparation of sample solution Weigh 0.1g sample containing tebuconazole of (accurate to 0.0002g), a 50mL volumetric flask, dilute to the mark with methanol, ultrasonic Oscillation 5min make sample dissolution, cooled to room temperature and shake well. Using a pipette to take the above solution 5mL to 50mL volumetric flask with methanol Dilute to the mark. 4.3.1.5.3 Determination Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles tebuconazole peak area relative change After less than 1.5%, according to the solution, sample solution, sample solution, standard order of standard solution was measured. 4.3.1.5.4 Calculation Tebuconazole sample mass fraction of 1 (%), according to equation (1). 1 = A2 (1) Where. A1 --- the standard solution, the average tebuconazole peak area; The A2 --- sample solution, alcohol tebuconazole average peak area; --- Tebuconazole standard mass fraction, expressed as a percentage. 4.3.1.6 allowable difference Determination of the mass fraction of tebuconazole two parallel result of the difference should be not more than 1.2%, the arithmetic mean value as a measurement result. 4.3.2 Capillary Gas Chromatography 4.3.2.1 Method summary Sample was dissolved in chloroform, dicyclohexyl phthalate esters as internal standard, using a HP-5 (5% phenyl methyl silicone) coated quartz wool wall Fine column and flame ionization detector, the sample of tebuconazole capillary gas chromatography and determination. 4.3.2.2 Reagents and solutions Chloroform; Tebuconazole standard. a known mass fraction ≥99.0%; Dicyclohexyl phthalate ester. not interfere with the analysis of impurities; Internal standard solution. Weigh 2.0g dicyclohexyl phthalate esters into 500mL volumetric flask, dissolved with chloroform, constant volume, Shake well. 4.3.2.3 Instruments Gas chromatograph. with flame ionization detector; Column. 30m × 0.32mm (. I.d) quartz capillary column, wall coated HP-5 (5% phenyl methyl silicone), film thickness 0.25μm; Chromatographic data processor or chromatography workstation. 4.3.2.4 GC operating conditions Temperature (℃). Room 220 column, the gasification chamber 260, detection chamber 280; Gas flow rate (mL/min). carrier gas (N2) 1.8, hydrogen gas 40, air 400, the compensation gas 25; Split ratio. 40.1; Injection volume. 1.0μL; Retention time. tebuconazole about 7.5min, internal standard about 10.4min. 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. A typical gas chromatogram Tebuconazole original drug and the internal standard are shown in Figure 3. 1 --- tebuconazole; 2 --- internal standard. Figure 3 Tebuconazole original drug and the internal standard gas chromatograph 4.3.2.5 Measurement procedure 4.3.2.5.1 preparation of standard solution Weigh tebuconazole standard 0.05g (accurate to 0.0002g), placed in a glass bottle stopper, with a pipette accurate internal standard was added 10mL Solution, shake. 4.3.2.5.2 preparation of the sample solution Weigh the sample containing tebuconazole 0.05g of (accurate to 0.0002g), placed in a glass bottle stopper, with the use and 4.3.2.5.1 With a pipette accurately added internal standard solution 10mL, shake. 4.3.2.5.3 Determination Under the above chromatographic operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two needles tebuconazole and the internal standard peak adjacent Changes in the relative area ratio is less than 1.5%, according to the solution, the sample solution, the sample solution and standard sequence analysis of the standard solution was measured. 4.3.2.5.4 Calculation The two needle sample solution and measured before and after the two doses of the standard sample solution tebuconazole and the internal standard peak area ratio of the average, respectively. Tebuconazole sample mass fraction of 1 '(%) according to equation (2). (2) Where. --- Standard samples tebuconazole mass fraction, expressed as a percentage. 4.3.2.6 allowable difference The difference between two parallel determination results shall not be greater than 1.2%, the arithmetic mean value as a measurement result. 4.4 Determination of acetone insolubles According to GB/T 19138 performed. 4.5 Determination of Moisture According to GB/T 1600 the "Karl Fischer method". According to GB/T 1601 carried out. 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 Flag 5.1 Tebuconazole the original drug, labeling and packaging should comply with the provisions of GB 3796. 5.2 Tebuconazole original drug use bags lined with clean plastic bag or cardboard drum lined with clean plastic bag, barrel (Bag) Net content The amount is generally 20kg, 25kg or 50kg. Also available upon request or order agreement, the use of other forms of packaging, but meeting The provisions of GB 3796. 5.3 Tebuconazole original drug package should be stored in well-ventilated, dry coffers. 5.4 storage, prevent moisture and sunlight, no food, seed, feed mix, avoid contact with skin, eyes, mouth and nose to prevent inhalation. 5.5 Security. This product is a low toxicity fungicides. Are swallowed and inhaled toxic, it can penetrate through the skin. Wear protective goggles and rubber hand the FDA Pull the necessary protective clothing. After spraying wash with soap and water. Coverage should be immediately sent to hospital symptomatic treatment. 5.6 of acceptance. Acceptance of Tebuconazole original drug for a month. From the date of delivery, product quality inspection completed within a month, its Indicators should meet the standards.
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