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GB 24752-2009: Methomyl technical
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Methomyl technical
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GB 24752-2009
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Basic data | Standard ID | GB 24752-2009 (GB24752-2009) | | Description (Translated English) | Methomyl technical | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Classification of International Standard | 65.100.10 | | Word Count Estimation | 8,842 | | Date of Issue | 2009-11-30 | | Date of Implementation | 2010-07-01 | | Quoted Standard | GB/T 1600; GB/T 1601; GB/T 1604; GB/T 1605-2001; GB 3796; GB/T 19138 | | Adopted Standard | FAO 264/TC-2002, MOD | | 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 Methomyl drug requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to methomyl and its impurities generated in the production of Methomyl medicine. | GB 24752-2009: Methomyl 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.
Methomyl technical
ICS 65.100.10
G25
National Standards of People's Republic of China
Methomyl original drug
Published 2009-11-30
2010-07-01 implementation
Administration of Quality Supervision, Inspection and Quarantine of People's Republic of China
Standardization Administration of China issued
Foreword
This standard in Chapter 3, Section 5 is mandatory, the rest are recommended.
This standard uses redrafted law revision adopted FAO specification 264/T C (2002) "methomyl original drug" (in English).
This standard FAO Specification 264/T C (2002) The main technical differences are as follows.
Standard control --- This acetone-insoluble matter, water and pH range, without the FAO specifications of the three indicators.
The date of implementation of this standard, the former Chemical Industry Standard HG2611-1994 "Methomyl original drug" abolished.
The standard proposed by China Petroleum and Chemical Industry Association.
This standard by the National Pesticide Standardization Technical Committee (SAC/TC133).
This standard is drafted. Shenyang Chemical Research Institute.
Participated in the drafting of this standard. Haili Guixi Chemical Pesticide Co., Ltd., Shandong Pesticide Research Institute, Jiangsu dragon Chemical Co., Ltd.,
Yancheng Limin Chemical Co., Ltd.
The main drafters. Zhao Xin, Li Xiujie, Running an, Li Dongqin, Feng Xiuzhen, Wei Hongsheng.
Methomyl original drug
Other names, structure and basic physical and chemical parameters of the active ingredient of the product of methomyl as follows.
ISO common name. methomyl
CIPAC digital code. 264
Chemical name. S- methyl-N - [(methylcarbamoyl) oxy] thioacetate imidate
Structure.
CH
CH
NH
CH
Empirical formula. C5H10N2O2S
Molecular weight. 162.20 (according to 2005 international relative atomic mass)
Biological activity. insecticide
Melting point. 78 ℃ ~ 79 ℃
Vapor pressure (25 ℃). 0.72mPa
Solubility (g/L, 25 ℃). 58 water; methanol 1000; 730 acetone; Ethanol 420
Stability. an aqueous solution, decomposing slowly at room temperature in sunlight, exposure to air and accelerated decomposition of alkaline medium
Range 1
This standard specifies the requirements methomyl Granville original drug, test methods and marking, labeling, packaging, storage and transportation.
This standard applies to impurities derived from the production of methomyl and methomyl composition original drug.
2 Normative references
Terms of the following documents become provisions of this standard by reference in this standard. For dated reference documents, all later
Amendments (not including errata content) or revisions do not apply to this standard, however, encourage the parties to agreements based on this standard
Whether the latest versions of these documents. For undated references, the latest version applies to this standard.
GB/T 1600 Pesticide Method Moisture
Determination 1601 pH value pesticides GB/T
GB/T 1604 pesticide regulations for acceptance
GB/T 1605-2001 sampling commercial pesticides
GB 3796 pesticide packaging General
GB/T 19138 Determination of acetone insoluble pesticide
3.1 Appearance
White to off-white crystalline powder.
3.2 Technical Specifications
Methomyl original drug should also meet the requirements of Table 1.
Table 1 Methomyl original drug control project indicators
Item Index
Methomyl content /% ≥ 98.0
Acetone insolubles a /% ≤ 0.2
Moisture /% ≤ 0.3
The pH range of 4.0 to 8.0
When a normal production, the acetone insoluble matter was detected at least once every three months.
Test Method 4
4.1 Sampling
Carried out in GB/T 1605-2001 of "original drug product sampling" approach. Determined by sampling a random number table method packages, the amount of the final sample
Not less than 100g.
4.2 Identification Test
The present liquid chromatography --- identification test can be carried out simultaneously with the determination of the mass fraction of methomyl. Chromatography under the same operating conditions, the test
A solution sample peak retention time of the standard solution Methomyl retention time, the relative difference should be less than 1.5%.
Infrared spectroscopy --- Methomyl sample and standard IR in the range of 4000cm-1 ~ 400cm-1 absorption spectrum should be no significant difference
different. Methomyl standard infrared spectra of Figure 1.
Figure 1 methomyl standard infrared spectrum
4.3 Determination of the mass fraction of methomyl
4.3.1 Method summary
Sample was dissolved in methanol, methanol + water as the mobile phase, used as a filler SpherisorbC8 stainless steel column and UV detector
(235nm), the sample methomyl reverse phase high performance liquid chromatography and determination.
4.3.2 Reagents and solutions
Methanol. HPLC grade;
Water. The new secondary steam distilled water;
Methomyl Standard. Known methomyl content, ≥99.0%.
4.3.3 Instruments
HPLC. a variable wavelength UV detector;
Chromatographic data processor or chromatography workstation;
Column.200mm × 4.6mm (. I.d) stainless steel column, SpherisorbC8,10μm filler contents (or with equivalent effect
C8, C18 bonded phase);
Filter. membrane pore size of about 0.45 m;
Microsyringe. 50μL;
Quantitative sampling tube. 5μL;
Ultrasonic cleaning.
4.3.4 HPLC operating conditions
Mobile phase. [Psi] (methanol. water) = 40.60, by membrane filtration, and degassing;
Flow rate. 1.0mL/min;
Column temperature. room temperature (temperature change should be less than 2 deg.] C);
Detection wavelength. 235nm;
Injection Volume. 5μL;
Retention time. Methomyl about 4.1min.
Are typical operating parameters of the above, according to the characteristics of different instruments, for a given operating parameters appropriately adjusted to obtain the best result.
Typical methomyl original drug by HPLC is shown in Figure 2.
1 --- methomyl.
FIG 2 FIG HPLC original drug methomyl
4.3.5 Determination Step
4.3.5.1 Preparation of standard solution
Weigh 0.10 g methomyl standard (accurate to 0.0002g), a 50mL volumetric flask, diluted with methanol to the mark. accurate
The solution was pipetted 10mL, 50mL volumetric flask, diluted with methanol to the mark.
4.3.5.2 Preparation of sample solution
Methomyl containing weighed about 0.10g sample of the original drug (accurate to 0.0002g), a 50mL volumetric flask, dilute to the mark with methanol
Degree, shake. The solution was accurately pipetted 10mL, 50mL volumetric flask, diluted with methanol to the mark.
4.3.5.3 Determination
Under the above operating conditions, after the instrument is stable, the number of consecutive doses of the standard solution is injected until the two needles methomyl relative change in peak area adjacent
After less than 1.5%, measured according to the standard solution, sample solution, the sample solution, the order of standard solution.
4.3.6 computing
The two needle and the sample solution was measured before and after the two doses of the standard sample solution Methomyl peak area are averaged. Sample Methomyl
A mass fraction (%), according to equation (1).
1 = A2
(1)
Where.
A1 --- the standard solution, the average methomyl peak area;
A2 --- sample solution, the average peak area methomyl;
--- methomyl Granville standard mass fraction, expressed as a%.
4.3.7 allows poor
Results difference methomyl replicates should be less than twice the mass fraction of 1.2%, and the arithmetic mean value as a measurement result.
4.4 Determination of acetone insolubles
According to GB/T 19138 carried out.
4.5 Determination of Moisture
According to GB/T 1600 in the "Karl Fischer method".
Carried out in GB/T 1601.
4.7 product testing and acceptance
Shall comply with the provisions of GB/T 1604's. Limit values rounding processing using the value comparison method.
5 marking, labeling, packaging, storage and transportation
5.1 methomyl sign the original drug Viagra, labeling and packaging should comply with the provisions of GB 3796.
5.2 methomyl original drug application drum lined with plastic bags, woven bag or barrel, a barrel (bags) net weight does not exceed 50kg. Also root
According to user requirements or other forms of ordering agreement package, subject to the provisions of GB 3796.
5.3 methomyl original drug package airiness, dry place.
5.4 storage and transportation to prevent moisture and sunlight, no food, seed, feed mix, avoid contact with skin, eyes, nose and mouth to prevent inhalation.
5.5 Security. instructions for use in or on a packaging container, in addition to the respective signs of toxicity, there should be about the toxicity as follows.
Methomyl is highly toxic carbamate pesticides, toxic inhalation, eating can be deadly. The FDA should avoid direct contact with skin and eyes
Touch, Do not breathe dust and spray. All operations should be carried out in the ventilation, and skin and eye protection to take appropriate measures in case of contact,
Washed with water 15min, then washed with soap and skin, and receive medical treatment. Atropine is a specific antidote.
5.6 Acceptance period. Methomyl original drug acceptance period of one month. From the date of delivery, product quality inspection completed within a month, the indicators
Shall meet the standards.
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