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GB 22167-2008: [GB/T 22167-2008] Fomesafen technical
Status: Valid
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| GB 22167-2008 | English | 209 |
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[GB/T 22167-2008] Fomesafen technical
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GB 22167-2008
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Basic data | Standard ID | GB 22167-2008 (GB22167-2008) | | Description (Translated English) | [GB/T 22167-2008] Fomesafen technical | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Classification of International Standard | 65.100.20 | | Word Count Estimation | 8,854 | | Date of Issue | 2008-07-11 | | Date of Implementation | 2009-01-01 | | Quoted Standard | GB/T 1601; GB/T 1604; GB/T 1605-2001; GB 3796; GB/T 19138 | | Regulation (derived from) | Announcement of Newly Approved National Standards No. 12 of 2008 (No. 125 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 Fomesafen original drug requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to fomesafen and impurities generated in the production of fomesafen original drug. | GB 22167-2008: [GB/T 22167-2008] Fomesafen 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.
Fomesafen technical
ICS 65.100.20
G25
National Standards of People's Republic of China
Fomesafen original drug
Posted 2008-07-11
2009-01-01 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 are 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 (CSBTS/T C133) centralized.
This standard is drafted by. Shenyang Chemical Research Institute.
Participated in the drafting of this standard. Dalian Songliao Chemical Co., Ltd., Jiangsu Changqing Agrochemical Co., Ltd., Dalian RAJ Pesticide shares have
Limited.
The main drafters of this standard. High Scenic, Zan Yan Kun, Miao innovation at sea level, Wang Dachun, Wu Tiejun.
The standard commission Secretariat of National Pesticide Standardisation Technical Committee responsible for the interpretation.
Fomesafen original drug
Other name, structural formula and basic physicochemical parameters of the active ingredients of the product fomesafen as follows.
ISO common name. fomesafen
Chemical name. 2-chloro-4-trifluoromethylphenyl 3'-methanesulfonyl-carbamoyl-4'-nitrophenyl ether.
Structure.
Empirical formula. C15H10ClF3N2O6S
Molecular Weight. 438.8 (according to 2005 international relative atomic mass)
Biological activity. weeding
Melting point. 220 ℃ ~ 221 ℃
Vapor pressure (50 ℃). 0.1mPa
Solubility (20 ℃). water 0.05g/L, acetone 300g/L, cyclohexanone 150g/L, methylene chloride 10g/L, hexane
0.5g/L, xylene 1.9g/L
Stability. stable at 50 ℃ for 6 months or more, light unstable and difficult to hydrolysis under acidic or basic conditions
1 Scope
This standard specifies the fomesafen original drug requirements, test methods and marking, labeling, packaging, storage and transportation.
Fomesafen This standard applies to the impurities generated by fomesafen and production consisting of the ether of the original drug.
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.
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
This product should be an off-white powder, free from visible foreign matter.
3.2 Technical Specifications
Fomesafen original drug should meet the requirements of Table 1.
Table 1 fomesafen original drug control project indicators
Item Index
Fomesafen mass fraction /% ≥ 95.0
Acetone insolubles a /% ≤ 0.5
Loss on drying /% ≤ 1.0
pH range 3.5 to 6.0
When a normal production, insoluble in acetone at least every three months, once measured.
Test Method 4
4.1 Sampling
According to GB/T 1605-2001 "on the original drug sampling" approach. Determining sample package using a random number table method; the final sample size should not be
Less than 100g.
4.2 Identification Test
HPLC --- The identification test can be carried out simultaneously with the determination of the content of fomesafen. In the same chromatographic operating conditions
, The sample solution to a chromatographic retention time and standard solution fomesafen chromatographic retention time, the relative difference should
1.5% or less.
Infrared spectroscopy --- sample and standard samples in the infrared range 4000cm-1 ~ 400cm-1 absorption spectrum should be no significant difference, see
Figure 1.
1 fomesafen standard sample infrared spectra in Fig.
4.3 Determination of fomesafen mass fraction
4.3.1 Method summary
Sample was dissolved in methanol, methanol + water + phosphoric acid as the mobile phase, to use as filler HypersilODS stainless steel column and ultraviolet detection
Detector (230nm), the sample of fomesafen reverse phase high performance liquid chromatography, external standard.
4.3.2 Reagents and solutions
Methanol. HPLC grade;
Phosphoric acid;
Water. The new secondary steam distilled water;
Fomesafen Sample. Known fomesafen mass fraction ≥98.0%.
4.3.3 Instruments
High performance liquid chromatography. a variable wavelength UV detector;
Chromatographic data processor;
Column.200mm × 4.6mm (. I.d) stainless steel column, built HypersilODS, 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. [Psi] (methanol. water. phosphoric acid) = 600.400.0.2, filtered through a filter membrane and degassed;
Flow rate. 1.0mL/min;
Column temperature. room temperature (temperature change should not exceed 2 ℃);
Detection wavelength. 230nm;
Injection volume. 5μL;
Retention time. fomesafen 7.8min.
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 fomesafen original drug HPLC is shown in Figure 2.
1 --- fomesafen.
Figure 2 HPLC fomesafen original drug
4.3.5 measuring step
4.3.5.1 Preparation of standard solution
Weigh fomesafen standard 0.1g (accurate to 0.0002g), a 50mL volumetric flask, dissolved in methanol and diluted to the mark,
Shake well. Pipette accurately pipette 5mL above solution was placed in another 50mL volumetric flask, diluted with methanol to the mark.
4.3.5.2 Preparation of sample solution
Weigh fluorine fomesafen 0.1g (accurate to 0.0002g) sample, placed in 50mL volumetric flask, dissolved in methanol and diluted to the mark
Degree, shake. Pipette accurately pipette 5mL above solution was placed in another 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 fomesafen relative peak area
After the change is less than 1.0%, according to the solution, the sample solution, the sample solution and standard sequence of the standard solution was measured.
4.3.6 Calculation
The two needle sample solution measured before and after the peak area of the sample and two doses of the standard solution of fomesafen were averaged. Specimen
Fomesafen mass fraction of 1 (%) according to equation (1).
1 = A2
(1)
Where.
A1 --- the standard solution, the average fomesafen peak area;
A2 --- sample solution, the average fomesafen peak area;
--- Standard samples fomesafen mass fraction, expressed as a percentage.
4.3.7 allowable difference
Determination of fomesafen parallel mass fraction of the difference between the two results should not exceed 1.0%, and the arithmetic mean as a measurement result.
4.4 Determination of acetone insolubles
According to GB/T 19138 Determination.
4.5 Determination of loss on drying
4.5.1 Instruments
Oven. 105 ℃ ± 2 ℃;
Weighing bottle. diameter 70mm, height 40mm;
Dryer.
4.5.2 measuring step
The weighing bottle placed in an oven bake 1h, was brought out in a desiccator to cool to room temperature, weigh (accurate to 0.0002g). Repeat the above steps
Step, until constant weight weighing bottle. 10g sample is placed in the bottle, paving, weighed (accurate to 0.01g), the weighing bottle placed in an oven, without
Cover and bake 1h, remove and put in the dryer to cool to room temperature, weighed (accurate to 0.0002g).
4.5.3 Calculation
Loss on drying of the sample mass fraction 2 (%), according to equation (2).
(2)
Where.
4.5.4 allowable difference
The relative deviation of two parallel determination results shall not be greater than ± 15%; the arithmetic mean value as a measurement result.
According to GB/T 1601 Determination.
4.7 product testing and acceptance
Shall comply with GB/T 1604's. Limit numerical processing using rounding value comparison method.
5 marking, labeling, packaging, storage and transportation
5.1 fomesafen original drug signs, labels, packaging, should meet the requirements of GB 3796.
5.2 fomesafen original drug use clean, dry steel drums lined with plastic or cardboard drum, net weight per barrel should not exceed 25kg.
5.3 According to user requirements or ordering agreement, you can use other forms of packaging, subject to the provisions of GB 3796.
5.4 fomesafen original drug package should be stored in well-ventilated, dry coffers.
5.5 storage, prevent moisture and sunlight, no food, seed, feed mix, avoid contact with skin, eyes, mouth and nose to prevent inhalation.
5.6 Security. fomesafen low toxicity pesticides. The FDA should wear protective gloves, masks, wearing clean protective clothing. Immediately after use with
Wash with soap and water. In case of poisoning, should go to hospital for treatment.
5.7 Acceptance of. fomesafen original drug acceptance period of 1 month. From the date of delivery, within one month, the finished product quality inspection, which each
Indicators should meet the standards.
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