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GB 24758-2009: [GB/T 24758-2009] Thifensulfuron-methyl technical
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[GB/T 24758-2009] Thifensulfuron-methyl technical
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GB 24758-2009
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Basic data | Standard ID | GB 24758-2009 (GB24758-2009) | | Description (Translated English) | [GB/T 24758-2009] Thifensulfuron-methyl technical | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Classification of International Standard | 65.100.20 | | Word Count Estimation | 8,846 | | 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 | | Adopted Standard | FAO 452.201/TC/S-2000, 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 Thifensulfuron original drug requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to thifensulfuron and impurities generated in the production of thifensulfuron original drug. | GB 24758-2009: [GB/T 24758-2009] Thifensulfuron-methyl 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.
Thifensulfuron-methyl technical
ICS 65.100.20
G25
National Standards of People's Republic of China
Thifensulfuron TC
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 modification uses FAO Standard Specification 452.201/T C/S (2000) "thifensulfuron original drug."
This standard modification method using foreign advanced standards for the redrafted law.
This standard FAO Specifications 452.201/T C/S (2000) "thifensulfuron TC" The main technical differences.
This standard specifies --- thifensulfuron mass fraction ≥95.0%, FAO specifications thifensulfuron predetermined mass fraction ≥960g/kg;
--- This standard specifies the original drug thifensulfuron water ≤0.5%, FAO specifications not specified;
This standard specifies --- thifensulfuron TC pH range of 3.0 ~ 7.0, FAO specifications not specified;
--- This standard specifies the original drug thifensulfuron N, N- dimethylformamide insolubles ≤0.3%, FAO specifications not specified.
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 by. the Ministry of Agriculture.
It participated in the drafting of this standard. Anhui Fengle Agrochemical Co., Ltd., Jiangsu Province Institute of hormones.
The main drafters. Wu Jinlong, Hu Qin, Chen Tiechun, Jin Jinsong, Fan Lei, Yu Rong, Li Guoping.
Thifensulfuron TC
This product is an active ingredient of other names, structural formulas and physicochemical parameters of the basic thifensulfuron follows.
ISO common name. thifensulfuron-methyl
CIPAC digital code. 452
CA Registry Number. 79277-27-3
Chemical Name. 3- (4-methoxy-6-methyl-1,3,5-triazin-2-yl) -1- (2-methoxy-formyl thiophen-3-yl) - sulfonyl urea
Structure.
Empirical formula. C12H13N5O6S2
Molecular weight. 387.4 (according to 2005 international relative atomic mass)
Biological activity. weeding
Melting point. 176 ℃ (TC 171 ℃)
Vapor pressure (25 ℃). 1.7 × 10-8Pa
Solubility (g/L, 25 ℃). water 0.223 (pH5), 2.240 (pH7), 8.830 (pH9); hexane < 0.1, o-xylene
0.212, ethyl acetate 3.3, methanol 2.8, 7.7 acetonitrile, acetone, 10.3, 23.8 methylene chloride
Stability. neutral, weakly alkaline aqueous solution more stable, acidic hydrolysis in aqueous solution at accelerated DT504 ~ 6d (pH5)
Range 1
This standard specifies the requirements thifensulfuron original drug, Test Method for marking, labeling, packaging, storage and transportation.
This standard applies to impurities derived from Thifensulfuron composition and production thifensulfuron 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 of goods
GB/T 1605-2001 sampling commercial pesticides
GB 3796 pesticide packaging General
3.1 Appearance. This product should be white to pale yellow loose powder, without visible foreign matter.
3.2 thifensulfuron TC shall comply with the requirements in Table 1.
Table 1 TC thifensulfuron control program Index
Item Index
Thifensulfuron mass fraction /% ≥ 95.0
Moisture /% ≤ 0.5
The pH range of 3.0 to 7.0
N, N- dimethylformamide insolubles a /% ≤ 0.3
When a normal production, N, N- dimethylformamide insolubles every three months, at least once.
Test Method 4
4.1 Sampling
According to GB T 1605-2001 "commodity original drug sample"/carried out. Determined by sampling a random number table method packages, less than the amount of the final sample
100g.
4.2 Identification Test
HPLC --- This identification test can be carried out simultaneously with the measurement of thifensulfuron mass fraction. In the same chromatographic operating conditions
Next, a peak with a retention time of sample solution thifensulfuron standard peak retention time of the solution, the relative difference of 1.5% should be
Or less.
Infrared spectroscopy --- sample and standard in the range of 4000cm-1 ~ 400cm-1 in an infrared absorption spectrum, to be no significant difference
different. Thifensulfuron standard infrared spectrum is shown in Figure 1.
FIG 1 thifensulfuron standard IR spectrum
Determination of mass fraction thifensulfuron thiazol 4.3
4.3.1 Method summary
Sample was dissolved in acetonitrile, methanol + water as the mobile phase, used as a filler C18 stainless steel column and UV detector (250 nm) to
External standard sample thifensulfuron reverse phase high performance liquid chromatography and determination, external standard.
4.3.2 Reagents and solutions
Methanol. HPLC grade;
Acetonitrile. HPLC grade;
Phosphoric acid. AR;
Water. The new secondary steam distilled water;
Thifensulfuron Sample. a known mass fraction, ≥98.0%.
4.3.3 Instruments
HPLC. a variable wavelength UV detector;
Chromatographic data processor or chromatography workstation;
Column. 250mm × 4.6mm (. I.d) stainless steel column, built ZORBAXSB-C18,5μm filler (or other equally effective
Column);
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) = 65.35, adjusted with phosphoric acid where water pH = 3, filtered through a filter membrane and degassed;
Mobile phase flow rate. 1.0mL/min;
Column temperature. 30 ℃;
Detection wavelength. 250nm;
Injection Volume. 5.0μL;
Retention time. thifensulfuron about 4.0min.
The above are typical operating parameters, according to different characteristics of the instrument and the columns for a given operating parameter adjusted as appropriate, in order to obtain the most
Good effect. Typical thifensulfuron HPLC TC shown in Figure 2.
1 --- thifensulfuron.
FIG 2 FIG thiazol HPLC thifensulfuron original drug
4.3.5 Determination Step
4.3.5.1 Preparation of standard solution
Thifensulfuron weighed 0.05 g of standard sample (accurate to 0.0002g), a 100mL volumetric flask, dissolved in acetonitrile and dilute to volume,
Shake well.
4.3.5.2 Preparation of sample solution
Weigh a sample containing thiophene thifensulfuron 0.05g of (accurate to 0.0002g), a 100mL volumetric flask, and dilute with acetonitrile to dissolve
Mark and shake.
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 adjacent needles thifensulfuron peak area becomes relatively
After less than 1.2% of, 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 thifensulfuron peak area are averaged. Sample thiophene
Sulfosulfuron 1 mass fraction (%), according to equation (1).
(1)
Where.
A1 --- the standard solution, thifensulfuron average peak area;
A2 --- sample solution, thifensulfuron average peak area;
--- standard samples thifensulfuron mass fraction, expressed in%.
4.3.7 allows poor
The measurement results of the two parallel error should not exceed 1.2%, and the arithmetic mean value as a measurement result.
4.4 Determination of Moisture
Carried out in GB/T 1600 in the "Karl Fischer" method.
Carried out in GB/T 1601.
Determination of 4.6 N, N- dimethylformamide insolubles
4.6.1 Method summary
Samples with an appropriate amount of N, N- dimethylformamide was heated and dissolved, insolubles were filtered hot and dried, N, N- dimethylformamide containing insolubles
Based on the amount of solid insoluble mass fraction of the sample.
4.6.2 Reagents
N, N- dimethylformamide.
4.6.3 Instruments
Standard ground-stoppered Erlenmeyer flask. 250mL; reflux condenser; glass fritted funnel crucible or G3; suction conical flask. 500mL; oven;
Glass dryer; bath oil pan.
4.6.4 Determination Step
The glass fritted funnel crucible drying (110 ℃, about 1h) to a constant weight (to the nearest 0.0002g), cooled in a desiccator until use. Call
10g sample was taken (accurate to 0.0002g), placed in a conical flask, 150 ml of N, N-dimethylformamide and shaken as far as possible the sample
Dissolved. Then fitted with a reflux condenser and heated to about 120 ℃ in an oil bath, heating was stopped after holding 5min. Crucible assembly fritted funnel
Suction filtration apparatus, under reduced pressure as soon as the hot solution was quickly through the funnel. 60mL with hot N, N- dimethylformamide divided washed 3 times, pumping
Remove the dry glass fritted funnel crucible, which was placed in an oven dried 160 ℃ for 30 min (making constant weight), withdrawn into the dryer, cooled
Was weighed (accurate to 0.0002g).
4.6.5 computing
N, mass fraction N- dimethylformamide 2 insolubles (%), according to equation (2).
(2)
Where.
4.7 product testing and acceptance
Shall comply with the provisions of GB/T 1604's. Process limit values using rounding value comparison method.
5 marking, labeling, packaging, storage and transportation
5.1 flag thiophene thifensulfuron original drug, label, package, should meet the requirements of GB 3796.
5.2 thifensulfuron original drug application of clean, dry plastic liner iron, cardboard, plastic bag or plastic bucket, a net weight of each member
Like to 25kg. Also available upon request or order agreement, other forms of packaging, but to comply with the provisions of GB 3796.
5.3 thifensulfuron 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. This product is moderately toxic pesticides. Symptoms of poisoning the eyes, skin stimulation, generally do not cause systemic poisoning. use
This product should wear protective gloves, goggles and masks, wear clean protective clothing, washed with soap and water immediately after application, to avoid contact with skin and eyes drugs
liquid. If swallowed, should immediately, gastric lavage, activated carbon can also be used with laxatives, symptomatic treatment.
Acceptance of 5.6. thifensulfuron original drug acceptance period of 1 month. From the date of delivery, within a month, complete product quality inspection, its
Indicators should meet the requirements of this standard.
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