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                    [GB/T 24751-2009] Clomazone technical
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  Basic data             |  Standard ID  |          GB 24751-2009 (GB24751-2009) |               |  Description (Translated English)  |          [GB/T 24751-2009] Clomazone technical |               |  Sector / Industry  |          National Standard |               |  Classification of Chinese Standard  |          G25 |               |  Classification of International Standard  |          65.100.20 |               |  Word Count Estimation  |          8,882 |               |  Date of Issue  |          2009-11-30 |               |  Date of Implementation  |          2010-07-01 |               |  Quoted Standard  |          GB/T 601; GB/T 603; GB/T 1600; GB/T 1604; GB/T 1605-2001; GB 3796; GB/T 19138 |               |  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 Clomazone Matsubara drug requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to clomazone and impurities generated in the production of Clomazone Matsubara drugs.  |         
  GB 24751-2009: [GB/T 24751-2009] Clomazone 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.  
Clomazone technical
ICS 65.100.20
G25
National Standards of People's Republic of China
Grass Matsubara drugs
Posted 2009-11-30
2010-07-01 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.
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 Changqing Agrochemical Co., Ltd., Jiangsu dragon Chemical Co., Ltd., Dalian Songliao Chemical Co.
the company.
The main drafters of this standard. Hou Chunqing, Zan Yan Kun, Jerry Hong, of cloud point, Miao innovation.
Grass Matsubara drugs
Other name, structural formula and basic physicochemical parameters of the active ingredient and grass loose product as follows.
ISO common name. Clomazone
CIPAC Numeric Code. 509
Chemical name. 2- (2-chlorobenzyl) -4,4-dimethyl-3-isobutyl ketone
Structure.
Empirical formula. C12H14ClNO2
Molecular Weight. 239.7 (according to 2005 international relative atomic mass)
Biological activity. weeding
Vapor Pressure. 19.2mPa (25 ℃)
Boiling point. 275.4 ℃
Melting point. 25 ℃
Solubility (20 ℃). water 1.1g/L, soluble in acetone, acetonitrile, chloroform, cyclohexanone, methylene chloride, methanol, toluene, n-hexane, di
Dimethylformamide
Stability. stable for at least 2 years at room temperature at 50 ℃ stable for at least 3 months, the sunlight, the aqueous solution is greater than 30d DT50
1 Scope
This standard specifies the different
Grass Matsubara drugs requirements, test methods and marking, labeling, packaging, storage and transportation.
This standard applies to the different
Different impurity generated in the production of grass and pine composition
Grass Matsubara drugs.
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.
Preparation of GB/T 601 chemical reagent standard titration solution
GB/T 603 chemical reagent in test methods - Preparations with
GB/T 1600 Determination of Water Pesticides
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
Colorless to pale yellow viscous liquid or white to pale yellow solid, semi-solid substance.
3.2 Technical Specifications
Grass Matsubara drugs should also meet the requirements of Table 1.
Table 1 and grass Matsubara drugs control projects index
Item Index
Grass loose mass fraction /% ≥ 93.0
Acidity (H2SO4 meter) /% ≤ 0.3
Moisture /% ≤ 0.5
Acetone insolubles a /% ≤ 0.2
Insoluble in acetone measured at least once every 3 months a normal production.
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
--- The liquid chromatography with different identification test
Determination of the mass fraction of loose grass simultaneously. Under the same chromatographic operating conditions,
The sample solution to a chromatographic retention time and different standard solution
Pine grass chromatographic retention time, the relative difference should be 1.5%
Fewer.
Infrared spectroscopy and different specimen ---
Grass loose standard in the range 4000cm-1 ~ 400cm-1 infrared absorption spectrum should not significantly
the difference. different
Grass loose standard infrared spectrum is shown in Figure 1.
1 Yi Cao loose standard infrared spectrum
4.3 Determination of the mass fraction of pine and grass
4.3.1 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
236nm wavelength, the sample of the different grass pine reverse phase HPLC separation and determination of external standard.
4.3.2 Reagents and solutions
Methanol. HPLC grade;
Acetonitrile. HPLC grade;
Water. The new secondary steam distilled water;
Grass Song Sample. 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 color
The 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 (acetonitrile. water) = 50.50, by membrane filtration, and degassing;
Flow rate. 1.0mL/min;
Column temperature. room temperature (temperature change should not exceed 2 ℃);
Detection wavelength. 236nm;
Injection volume. 5μL;
Retention time. iso
Grass loose about 11.0min.
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 differences
Grass Matsubara drugs HPLC is shown in Figure 2.
1 --- Yi Cao loose.
Figure 2 HPLC and grass Matsubara drugs
4.3.5 measuring step
4.3.5.1 Preparation of standard solution
Weigh 0.2g (accurate to 0.0002g) and grass loose standard in 50mL volumetric flask, dissolved in methanol and diluted to the mark.
Using a pipette to take the above solution 10mL in 50mL volumetric flask, diluted with methanol to the mark.
4.3.5.2 Preparation of sample solution
Weigh Iso
Grass pine 0.2g (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 iso
Peak area becomes relatively loose grass
After less than 1.2% of the solution in accordance with the sample solution, the sample solution and standard sequence of the standard solution was measured.
4.3.6 Calculation
The measured before and after the two-needle sample solution and sample two different doses of the standard solution
Grass Pine Peak area were averaged. Sample different
Grass loose mass fraction of 1 (%), according to equation (1).
1 = A2
(1)
Where.
--- Yi Cao Song Sample mass fraction, expressed as a percentage;
A1 --- the standard solution, the average peak area of pine and grass;
A2 --- sample solution, the average peak area of pine and grass;
4.3.7 allowable difference
Poor quality grass pine fraction of two parallel determination results shall not be greater than 1.5%, 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".
4.6 Determination of acidity
4.6.1 Reagents and solutions
95% ethanol;
Sodium hydroxide standard titration solution. Ba (NaOH) = 0.02moL/L, according to GB/T 601 preparation;
Mixed indicator solution. bromocresol green ethanol solution (1g/L) + methyl red ethanol solution (2g/L) = 3 + 1, according to GB/T 603 formulation.
4.6.2 measuring step
Weigh iso
Pine grass samples 2g (accurate to 0.002g), placed in 250mL flask, add 100mL95% ethanol, 3 drops instructions
Solution, titrated with sodium hydroxide standard titration solution to green, do not fade in the 30s for the end. Make a blank test simultaneously.
4.6.3 Calculation
2 sample acidity (%), according to equation (2).
Ba 1- Vp Vp = 2 () 0
· M
100 (2)
Where.
Ba --- the actual concentration of sodium hydroxide standard titration solution, expressed in moles per liter (moL/L);
Vp 1 --- sample solution of sodium hydroxide standard titration solution consumption volume in milliliters (mL);
V0 --- blank solution of sodium hydroxide standard titration solution consumption volume 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.
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
5.1 Yi Cao flag Matsubara drugs, labeling and packaging should comply with the provisions of GB 3796.
5.2 Yi Cao Matsubara pharmaceutical lined iron drum, net weight per barrel is generally 50kg, 100kg or 200kg. Also available upon request or
Ordering protocol uses other forms of packaging, subject to the provisions of GB 3796.
5.3 and grass Matsubara drugs packages 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-toxic pesticides. Are swallowed and inhaled toxic, it can penetrate through the skin. Wear protective goggles and rubber gloves when using this product
Wear 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 different grass Matsubara drugs for a month. From the date of delivery, product quality inspection completed within a month of its
Indicators shall comply with this standard.
   
   
  
  
    
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