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Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 28129-2011: [GB/T 28129-2011] Fluoroglycofen-ethyl technical material Status: Valid
Basic dataStandard ID: GB 28129-2011 (GB28129-2011)Description (Translated English): [GB/T 28129-2011] Fluoroglycofen-ethyl technical material Sector / Industry: National Standard Classification of Chinese Standard: G25 Classification of International Standard: 65.100.20 Word Count Estimation: 11,170 Date of Issue: 2011-12-30 Date of Implementation: 2012-04-15 Quoted Standard: GB/T 601-2002; GB/T 1604; GB/T 1605-2001; GB 3796; GB/T 19138 Regulation (derived from): Announcement of Newly Approved National Standards No. 23 of 2011 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 Fluoroglycofen ether original drug requirements, test methods and marking, labeling, packaging, storage and acceptance period. This standard applies to Fluoroglycofen ether and impurities generated in the production of Fluoroglycofen ether original drug. GB 28129-2011: [GB/T 28129-2011] Fluoroglycofen-ethyl technical material---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.Fluoroglycofen-ethyl technical material ICS 65.100.20 G25 National Standards of People's Republic of China B fluoroglycofen original drug Issued on. 2011-12-30 2012-04-15 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. This standard was drafted in accordance with GB/T 1.1-2009 given rules. Please note that some of the content of this document may involve patents. Release mechanism of the present document does not assume responsibility for the identification of these patents. 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 Co., Ltd. It participated in the drafting of this standard. Jiangsu Changqing Agrochemical Co., Ltd. The main drafters of this standard. in bright, Li Xiujie, Jerry Hong, Ji Yuping. B fluoroglycofen original drug1 ScopeThis standard specifies the B fluoroglycofen original drug requirements, test methods and marking, labeling, packaging, storage and acceptance period. This standard applies to the impurities generated by Fluoroglycofen ether acetate composition and production fluoroglycofen original drug. Note. Other name, structural formula and basic physicochemical parameters Fluoroglycofen ether in Appendix A.2 Normative referencesThe following documents for the application of this document is essential. For dated references, only the dated version suitable for use herein Member. For undated references, the latest edition (including any amendments) applies to this document. Preparation of GB/T 601-2002 Chemical Reagent standard titration solution 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 White to yellowish brown granular or powdery solid, no visible foreign matter and filling the modifier. 3.2 Technical Specifications B fluoroglycofen original drug should be consistent with the requirements in Table 1. Table 1 B fluoroglycofen original drug quality control program indicators Item Index Fluoroglycofen ether mass fraction /% ≥ 95.0 Loss on drying /% ≤ 0.5 Acidity (H2SO4 meter) /% ≤ 0.5 Acetone insoluble mass fraction /% ≤ 0.3 Test Method 4 4.1 Sampling According to GB/T 1605-2001 "on the original drug product sampling" approach. Determined by sampling a random number table method packages, the final sample size Not less than 100g. 4.2 Identification Test You can choose one of the following methods. When not identify one way, then use another method should be determined. 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 B fluoroglycofen standard infrared spectrum HPLC --- The identification test can be carried out simultaneously with the determination of ethyl fluoroglycofen mass fraction. In the same chromatographic operating conditions Under parts, the sample solution to a chromatographic retention time and Fluoroglycofen ethyl ether standard solution fluoroglycofen chromatographic retention time, relative Of the difference should be less than 1.5%. 4.3 Determination of B fluoroglycofen mass fraction 4.3.1 capillary gas chromatography (Arbitration Act) 4.3.1.1 Method summary Sample was dissolved in chloroform, dicyclohexyl phthalate esters as internal standard, using a HP-5 fused silica capillary column coated walls, and hydrogen fire Flame ionization detector, a sample with acetic fluoroglycofen capillary gas chromatography and determination. 4.3.1.2 Reagents and solutions Chloroform; B fluoroglycofen standard. a known mass fraction w≥99.0%; Dicyclohexyl phthalate ester. not interfere with the analysis of impurities; Internal standard solution. Weigh 7.5g dicyclohexyl phthalate esters into 1000mL volumetric flask, dissolved with chloroform, constant volume, Shake well. 4.3.1.3 Instruments Gas chromatograph. with flame ionization detector; Column. 30m × 0.32mm (id) quartz capillary column, wall coated HP-5, film thickness 0.25μm; Chromatographic data processor or chromatography workstation. 4.3.1.4 GC operating conditions Temperature (℃). Room 230 column, the gasification chamber 260, detection chamber 280; Gas flow rate (mL/min). carrier gas (N2) 1.8, hydrogen gas 30, air 300, the compensation gas 25; Split ratio. 30.1; Injection volume. 1.0μL; Retention time. Fluoroglycofen ether about 10.8min, internal standard about 7.9min. 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 B fluoroglycofen original drug and the internal standard gas chromatography is shown in Figure 2. 1 --- internal standard; 2 --- Fluoroglycofen ether. Figure 2 B fluoroglycofen original drug and the internal standard gas chromatograph 4.3.1.5 Measurement procedure 4.3.1.5.1 preparation of standard solution Weigh Fluoroglycofen ether standard 0.05g (accurate to 0.0002g), placed in a glass bottle stopper, with a pipette accurately added 5mL within Standard solution, shake. 4.3.1.5.2 preparation of the sample solution Weigh containing ethyl fluoroglycofen 0.05g of the sample (accurate to 0.0002g), placed in a glass bottle stopper, and with the 4.3.1.5.1 With the use of a pipette accurately added internal standard solution 5mL, shake. 4.3.1.5.3 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 Fluoroglycofen ether and the internal standard After the relative change of the peak area ratio was less than 1.5%, according to the solution, the sample solution, the sample solution and standard sequence analysis of the standard solution Determination. 4.3.1.5.4 Calculation The measured before and after the two-needle sample solution and two doses of the standard sample solution Fluoroglycofen ether and the internal standard peak area ratios are flat all. Sample B fluoroglycofen content according to equation (1). w1 = r2 × m1 × wr1 × m2 (1) Where. Quality w1 --- sample Fluoroglycofen ether fraction, in%; r2 --- sample solution Fluoroglycofen ether and the average internal standard peak area ratio; m1 --- standard mass in grams (g); w --- standard samples Fluoroglycofen ether mass fraction, expressed as a percentage; r1 --- standard samples Fluoroglycofen ether and the average peak area ratio of the internal standard solution; m2 --- sample mass, in grams (g). 4.3.1.6 allowable difference The difference between two parallel determination results shall not be greater than 1.2%, the arithmetic mean value as a measurement result. 4.3.2 High Performance Liquid Chromatography 4.3.2.1 Method summary Sample was dissolved in acetonitrile, methanol and acetic acid water as the mobile phase, use as filler in Nova-PakC18 stainless steel column and ultraviolet detection Detector (230nm), the sample of Fluoroglycofen ether HPLC separation and determination. 4.3.2.2 Reagents and solutions Methanol. HPLC grade; Acetonitrile. chromatographic pure; Water. The new secondary steam distilled water; Fluoroglycofen ether Sample. Known Fluoroglycofen ether content w≥99.0%. 4.3.2.3 Instruments High performance liquid chromatography. a variable wavelength UV detector; Chromatographic data processor or workstation; Column. 150mm × 3.9mm (id) stainless steel column, built-Nova-PakC18,5μm filler (or equivalent effect Chromatography column); Filter. filter pore size of about 0.45μm; Micro injector. 50μL; Quantitative sample line. 5μL; Ultrasonic cleaner. 4.3.2.4 HPLC operating conditions Mobile phase. Ψ (CH3OH.H2O.CH3COOH) = 75.25.0.2; Flow rate. 1.0mL/min; Column temperature. room temperature (temperature change should not exceed 2 ℃); Detection wavelength. 230nm; Injection volume. 5μL; Retention time. B fluoroglycofen 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 B fluoroglycofen original drug HPLC is shown in Figure 3. 1 --- Fluoroglycofen ether. HPLC Figure 3 Fluoroglycofen grass ether original drug 4.3.2.5 Measurement procedure 4.3.2.5.1 Preparation of standard solution Weigh 0.1g Fluoroglycofen ether standard (accurate to 0.0002g), a 50mL volumetric flask, dilute to the mark with acetonitrile, 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 acetonitrile Dilute to the mark. 4.3.2.5.2 Preparation of sample solution Weigh containing ethyl fluoroglycofen sample of 0.1g (accurate to 0.0002g), a 50mL volumetric flask, dilute to the mark with acetonitrile, super Acoustic oscillations 5min make sample dissolution, cooled to room temperature and shake well. Using a pipette to take the above solution 5mL to 50mL volumetric flask Acetonitrile and diluted to the mark, shake. 4.3.2.5.3 Determination Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles Fluoroglycofen ether relative peak area After the change of less than 1.5%, according to the solution, sample solution, sample solution, standard order of 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 Fluoroglycofen ether peak areas are averaged. Sample B Fluoroglycofen mass fraction according to equation (2). w2 = A2 · M1 · w A1 · m2 (2) Where. Quality w2 --- sample Fluoroglycofen ether fraction, in%; A2 --- sample solution B carboxymethyl fluoride grass ether the average peak area; m1 --- B fluoroglycofen standard mass in grams (g); w --- B fluoroglycofen standard mass fraction, expressed as a percentage; A1 --- Sample mean fluoride grass ether peak areas of ethyl in solution; m2 --- sample mass, in grams (g). 4.3.2.6 allowable difference Results - ethyl difference fluorine content Ethoxyfen two parallel determinations should not exceed 1.2%, and the arithmetic mean as a measurement result. 4.4 Determination of the mass fraction of the loss on drying 4.4.1 measuring step With constant weight after weighing bottle Weigh 5g sample (accurate to 0.01g), paving the thickness of no more than 3mm, placed in 105 ℃ ± 2 ℃ of 1h after oven drying in a desiccator, cool to room temperature, and weighed. 4.4.2 Calculation Sample Loss on drying w3 (%) according to equation (3) Calculated. w3 = m0-m1m × 100 (3) Where. W3 --- Loss on drying of the sample, expressed in%; Mass m1 --- dried weighing bottle and the sample, in grams (g); Mass m0 --- weighing bottle and the sample, in grams (g); M --- the quality of the sample, in grams (g). 4.5 Determination of the mass fraction of acidity 4.5.1 Reagents and solutions Sodium hydroxide standard titration solution c (NaOH) = 0.02mol/L, according to GB/T 601-2002 4.1 preparation and calibration; Ethanol. [Psi] (ethanol. water) = 95 Bromocresol green ethanol solution. ρ = 1g/L; Methyl red ethanol solution. ρ = 2g/L; Indicator. Ψ (Bromocresol green solution. methyl red solution) = 3. 4.5.2 measuring step Weigh the sample 1g (accurate to 0.002g), placed in a 150mL conical flask, 50mL ethanol was shaken to dissolve the sample. Add 5 drops of indicator, with 0.02mol/L sodium hydroxide standard titration solution, titration, titration of the solution from yellow to green as the end point, at the same time Blank determination. 4.5.3 Calculation The acidity of the sample, according to equation (4) Calculated. w4 = c (V1-V0) × M m × 1000 × 100 (4) Where. W4 --- acidity of the sample, expressed in%; C --- the actual concentration of sodium hydroxide standard titration solution, expressed in moles per liter (mol/L); V1 --- titration of the sample solution, the volume of consumption of sodium hydroxide standard titration solution, in milliliters (mL); V0 --- titrate blank solution, the volume of consumption of sodium hydroxide standard titration solution, in milliliters (mL); --- The M values of the molar mass of sulfuric acid, in units of grams per mole (g/mol), [M 12H2SO ÷ 4 = 49.04]; M --- the quality of the sample, in grams (g). 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. 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, security, acceptance of 5.1 marking, labeling, packaging B fluoroglycofen original drug marking, labeling and packaging should comply with the provisions of GB 3796; Fluoroglycofen ether bag lined with clean original drug application Plastic bags or cardboard drum lined with clean plastic bag, net weight per barrel is usually 50kg. Also available upon request or order Agreement other forms of packaging, subject to the provisions of GB 3796. 5.2 Storage B fluoroglycofen original drug package should be stored in ventilated, dry warehouse; storage and transportation to prevent moisture and sun, not with food, seeds, Feed-mixing, avoid contact with skin, eyes, mouth and nose to prevent inhalation. 5.3 Security The goods on the skin moderate irritation of the eyes has a strong stimulating effect. Wear protective goggles when using this product wear rubber gloves and necessary Protective clothing. After application, immediately wash with soap and water. Such as skin, eyes accidentally stained with the product, rinse immediately with plenty of water. error Clothing should be immediately sent to hospital symptomatic treatment. 5.4 Acceptance of B fluoroglycofen original drug acceptance period is one month. From the date of delivery, the quality of the finished product acceptance within one month, the indicators should be Compliance.Appendix A(Informative) Other name, structural formula and basic physicochemical parameters Fluoroglycofen ether This product is an active ingredient B carboxymethyl fluoride grass ether other name, structural formula and basic physicochemical parameters are as follows. Generic Name. B fluoroglycofen ISO common name. fluoroglycofen-ethyl CAS Registry Number. 77501-90-7 Chemical Name. O- [5- (2-chloro -α, α, α- trifluoro - on - tolyloxy) -2-nitrobenzoyl] hydroxy ethyl Structure. Empirical formula. C18H13ClF3NO7 Molecular Weight. 447.8 Biological activity. Herbicides Melting point. 65 ℃ Vapor Pressure. Less than 133Pa (25 ℃) Solubility (25 ℃). water 0.6mg/L; most organic solvents greater than 100g/kg Stability. 0.25mg/L aqueous solution at 22 ℃ about the DT50 231d (pH5), 15d (pH7), 0.15d (pH9); a water suspension It was due to the rapid decomposition of ultraviolet light; and soil degradation due to rapid microbial, DT50 about 11h. Rights Proprietary Rights Reserved ISBN. 155 066 · 1-44786 ......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB 28129-2011_English be delivered?Answer: Upon your order, we will start to translate GB 28129-2011_English as soon as possible, and keep you informed of the progress. The lead time is typically 1 ~ 3 working days. 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