GB 22623-2008 English PDFUS$479.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 22623-2008: [GB/T 22623-2008] Prochloraz technical Status: Obsolete
Basic dataStandard ID: GB 22623-2008 (GB22623-2008)Description (Translated English): [GB/T 22623-2008] Prochloraz technical Sector / Industry: National Standard Classification of Chinese Standard: G25 Classification of International Standard: 65.100.30 Word Count Estimation: 12,197 Date of Issue: 2008-12-17 Date of Implementation: 2009-06-01 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 original drug prochloraz requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to prochloraz and its impurities generated in the production of prochloraz original drug. GB 22623-2008: [GB/T 22623-2008] Prochloraz 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.Prochloraz technical ICS 65.100.30 G25 National Standards of People's Republic of China Prochloraz 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 ForewordThe standard Chapter 3, Chapter 5 is mandatory, the rest are recommended. 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. Chlorpyrifos Chemical Co., Ltd., Nanjing Red Sun Co., Ltd., Nantong Jiangshan Agrochemical & Chemical Co. Shares the company. The main drafters of this standard. Hou Chunqing, Wu Tiejun, Chen was new, Liukui Tao, Wang Zhimin, Duan win. Prochloraz original drug The product is an active ingredient prochloraz other name, structural formula and basic physicochemical parameters are as follows. ISO common name. prochloraz Chemical name. N- propyl--N- [2- (2,4,6- trichlorophenoxy) ethyl] imidazole-1-carboxamide Structure. Empirical formula. C15H16Cl3N3O2 Molecular Weight. 376.7 (according to 2007 international relative atomic mass) Biological activity. bactericidal Melting point. 46.5 ℃ ~ 49.3 ℃ (purity greater than 99%) Solubility (25 ℃). water 34.4mg/L, soluble in most organic solvents, such as chloroform, ethyl acetate, toluene, xylene 2.5kg/L, Acetone 3.5kg/L, n-hexane 7.5 × 10-3kg/L Stability. In water (pH = 7,20 ℃) stable, light, continuous high temperature heating (200 ℃) or in case of a strong acid, alkali decomposition when1 ScopeThis standard specifies the prochloraz original drug requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to the impurities generated by the production of prochloraz and its composition prochloraz original drug.2 Normative referencesThe 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 pesticide3 Requirements3.1 Appearance Light yellow to brown viscous liquid, cooled and solidified. 3.2 Technical Specifications Prochloraz original drug should also meet the requirements of Table 1. Table 1 prochloraz original drug control project indicators Item Index Prochloraz mass fraction /% ≥ 95.0 2,4,6-trichlorophenol mass fraction a /% ≤ 0.5 A mass acetone insoluble fraction /% ≤ 0.2 Moisture content /% ≤ 0.5 a pH range of 5.5 to 8.5 a normal production acetone insoluble, 2,4,6-trichlorophenol is determined 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 Liquid chromatography --- The identification test can be carried out simultaneously with the determination of the mass fraction of prochloraz. Under the same chromatographic operating conditions, the test A sample solution peak retention time and standard solution PROCHLORAZ chromatographic retention time, the relative difference should be 1.5% Fewer. Infrared spectroscopy --- sample and standard prochloraz in the range 4000cm-1 ~ 400cm-1 infrared absorption spectrum should be no significant area do not. Prochloraz standard infrared spectrum is shown in Figure 1. Figure 1 prochloraz standard infrared spectrum 4.3 Determination of the mass fraction of prochloraz 4.3.1 Method summary Sample was dissolved in methanol, acetonitrile + methanol + water as the mobile phase, to use as filler AgilentTC-C18 stainless steel column and ultraviolet Detector (225nm), the sample of prochloraz reverse phase high performance liquid chromatography, external standard. You can also use capillary gas Chromatography, chromatography operating conditions, see Appendix A. 4.3.2 Reagents and solutions Methanol. HPLC grade; Acetonitrile. HPLC grade; Water. The new secondary steam distilled water; Prochloraz standard. a known mass fraction ≥98.0%. 4.3.3 Instruments High performance liquid chromatography. a variable wavelength UV detector; Chromatographic data processor or chromatography workstation; Column. 250mm × 4.6mm (. I.d) stainless steel column, built AgilentTC-C18,5μm filler (or with equivalent effect Column); Filter. filter pore size of about 0.45μm; Micro injector. 50μL; Quantitative sample line. 5μL; Ultrasonic cleaner. 4.3.4 HPLC operating conditions Mobile phase. ψ (methanol. acetonitrile. water) = 30.40.30 by membrane filtration, and degassing; Flow rate. 1.0mL/min; Column temperature. room temperature (temperature change should not exceed 2 ℃); Detection wavelength. 225nm; Injection volume. 5μL; Retention time. about 12.0min. 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 prochloraz original drug HPLC is shown in Figure 2. 1 --- prochloraz. Figure 2 HPLC prochloraz original drug 4.3.5 measuring step 4.3.5.1 Preparation of standard solution Weigh 0.1g (accurate to 0.0002g) Prochloraz standard in 50mL volumetric flask, dissolved in methanol and diluted to the mark. use Pipette pipette above solution 10mL in 50mL volumetric flask, diluted with methanol to the mark. 4.3.5.2 Preparation of sample solution Weigh containing prochloraz 0.1g (accurate to 0.0002g) sample in 50mL volumetric flask, dissolved in methanol and diluted to the mark, shake uniform. Using a pipette to take the above solution 10mL in 50mL volumetric flask, diluted with methanol to the mark. 4.3.5.3 Determination Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles prochloraz peak area relative change After less than 1.5%, according to the solution, sample solution, sample solution, standard order of standard solution was measured. 4.3.6 Calculation The two needle sample solution and measured before and after the two doses of the standard sample solution PROCHLORAZ peak areas are averaged. Sample PROCHLORAZ The mass fraction of 1 (%), according to equation (1). 1 = A2 (1) Where. A1 --- the standard solution, the average peak area prochloraz; A2 --- sample solution, Prochloraz amines mean peak area; --- Prochloraz standard mass fraction, expressed as a percentage. 4.3.7 allowable difference Prochloraz difference between an amine content of two parallel determination results shall not be greater than 1.5%, the arithmetic mean value as a measurement result. 4.4 2,4,6-trichlorophenol mass fraction determination 4.4.1 Method summary Sample was dissolved in methanol, acetonitrile + water as the mobile phase, to use as filler AgilentTC-C18 stainless steel column and UV detector (215nm), the sample of 2,4,6-trichlorophenol by reverse phase high performance liquid chromatography, external standard. 4.4.2 Reagents and solutions Acetonitrile. HPLC grade; Water. The new secondary steam distilled water; 2,4,6-trichlorophenol standard. a known mass fraction ≥99.0%. 4.4.3 Instruments High performance liquid chromatography. a variable wavelength UV detector; Chromatographic data processor or chromatography workstation; Column. 250mm × 4.6mm (. I.d) stainless steel column, built AgilentTC-C18,5μm filler (or with equivalent effect Column); Filter. filter pore size of about 0.45μm; Micro injector. 50μL; Quantitative sample line. 5μL; Ultrasonic cleaner. 4.4.4 HPLC operating conditions Mobile phase. ψ (acetonitrile. water) = 55.45, by membrane filtration, and degassing; Flow rate. 1.0mL/min; Column temperature. room temperature (temperature change should not exceed 2 ℃); Detection wavelength. 215nm; Injection volume. 5μL; Retention time. about 4.0min. 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 prochloraz original drug 2,4,6-trichlorophenol measured by HPLC is shown in Figure 3. 1 --- 2,4,6-trichlorophenol; 2 --- prochloraz. Figure 3 prochloraz original drug 2,4,6-trichlorophenol was measured by high performance liquid chromatogram 4.4.5 measuring step 4.4.5.1 Preparation of standard solution Weigh 0.01g (accurate to 0.0002g) 2,4,6- trichlorophenol standard sample in 50mL volumetric flask, dissolved in methanol and diluted to the mark Degree, shake. 4.4.5.2 Preparation of sample solution Weigh-containing 2,4,6-trichlorophenol 0.01g (accurate to 0.0002g) sample in 50mL volumetric flask, dissolved in methanol and diluted to Mark and shake. 4.4.5.3 Determination Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles 2,4,6-trichlorophenol peak area After the relative change of less than 1.5%, according to the solution, sample solution, sample solution, standard order of standard solution was measured. 4.4.6 Calculation The two needle sample solution and measured before and after the two doses of the standard sample solution of 2,4,6-trichlorophenol peak areas are averaged. test Samples 2,4,6-trichlorophenol 2 mass fraction (%), according to equation (2). 2 = A2 (2) Where. A1 --- standard solution, the average of 2,4,6-trichlorophenol peak area; --- The A2 in the sample solution, an average value of the peak area of 2,4,6-trichlorophenol; --- 2,4,6-trichlorophenol standard mass fraction, expressed as a percentage. 4.4.7 allowable difference The relative deviation of two measurements shall be not more than 20% of the arithmetic mean as a measurement result. 4.5 Determination of acetone insolubles According to GB/T 19138 performed. 4.6 Determination of Moisture According to GB/T 1600 the "Karl Fischer method". According to GB/T 1601 carried out. 4.8 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 prochloraz original drug, labeling and packaging should comply with the provisions of GB 3796. 5.2 prochloraz original drug use clean, dry metal pail, net weight per barrel is generally 200kg or 250kg. Also available upon request Or order agreement other forms of packaging, subject to the provisions of GB 3796. 5.3 prochloraz 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 prochloraz original drug for a month. From the date of delivery, product quality inspection completed within a month, its Indicators should meet the standards.Appendix A(Informative) The method of capillary gas chromatography mass fraction Prochloraz A. 1 Method summary Sample was dissolved in chloroform, diisooctyl phthalate esters as internal standard, using a HP-5 (5% phenyl methyl silicone) bonded silica Capillary column and a flame ionization detector, the sample of prochloraz capillary gas chromatography and determination. A. 2 Reagents and solutions Chloroform; Prochloraz standard. a known mass fraction ≥98.0%; Phthalate Dioctyl. should not interfere with the analysis of impurities; Internal standard solution. Weigh 2.5g of di-iso-octyl phthalate in 500mL volumetric flask, dissolved in acetone, constant volume, shake. A. 3 Instrument Gas chromatograph. with flame ionization detector; Column. 30m × 0.32mm (. I.d) fused silica capillary column, the inner wall of the bonding HP-5 (5% phenyl methyl silicone), film thickness 0.25 m; Chromatographic data processor or chromatography workstation. A. 4 GC operating conditions Temperature (℃). Room 235 column, the gasification chamber 260, detection chamber 280; Gas flow rate (mL/min). carrier gas (N2) 2.0, the compensation gas (N2) 25, hydrogen gas 40, air 400; Split ratio. 40.1; Injection volume. 1.0μL; Retention time. Prochloraz. about 11.8min, internal standard. about 7.3min. 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 prochloraz original drug and the internal standard, see A. 1. 1 --- prochloraz; 2 --- internal standard. Figure A. GC 1 prochloraz original drug and the internal standard Book GB 22623-2008 A. 5 measuring step A. 5.1 preparation of standard solution Weigh prochloraz standard 0.1g (accurate to 0.0002g), placed in a glass bottle stuffed with a pipette 10mL internal standard solution, Shake well. A. 5.2 Sample preparation solution Weigh containing prochloraz 0.1g (accurate to 0.0002g) sample, placed in a glass bottle stopper, with the A. With 5.1 used A pipette internal standard solution 10mL, shake. A. 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 adjacent needles prochloraz and internal standard After the change of the relative peak area ratio of less than 1.5%, according to the solution, the sample solution, the sample solution and standard sequence analysis of the standard solution Determination. A. 6 Calculation The two needle sample solution and measured before and after the two doses of the standard sample solution prochloraz and the internal standard peak area ratio of the average, respectively. PROCHLORAZ sample mass fraction of 1 (%) according to equation (A.1) Calculated. (A.1) Where. γ1 --- standard samples Prochloraz amines with the average peak area ratio of the internal standard solution; γ2 --- sample solution prochloraz and the average internal standard peak area ratio; --- Standard PROCHLORAZ mass fraction, expressed as a percentage. A. 7 allowable difference The difference between two parallel determination results shall not be greater than 1.5%, the arithmetic mean value as a measurement result. ......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB 22623-2008_English be delivered?Answer: Upon your order, we will start to translate GB 22623-2008_English as soon as possible, and keep you informed of the progress. 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