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GB 23552-2009: [GB/T 23552-2009] Thiophanate-methyl wettable powders
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[GB/T 23552-2009] Thiophanate-methyl wettable powders
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Basic data | Standard ID | GB 23552-2009 (GB23552-2009) | | Description (Translated English) | [GB/T 23552-2009] Thiophanate-methyl wettable powders | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Classification of International Standard | 65.100.30 | | Word Count Estimation | 12,181 | | Date of Issue | 2009-04-27 | | Date of Implementation | 2009-11-01 | | Older Standard (superseded by this standard) | HG 2462.2-1993 | | Quoted Standard | GB/T 1601; GB/T 1604; GB/T 1605-2001; GB 3796; GB/T 5451; GB/T 14825; GB/T 16150; GB/T 19136 | | Adopted Standard | FAO 262/WP/S/P-1993, MOD | | Regulation (derived from) | Announcement of Newly Approved National Standards No. 5, 2009 (No. 145 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 thiophanate-methyl WP requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to thiophanate-methyl original drug with a suitable additives and fillers processed into thiophanate-methyl WP. | GB 23552-2009: [GB/T 23552-2009] Thiophanate-methyl wettable powders---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.
Thiophanate-methyl wettable powders
ICS 65.100.30
G25
National Standards of People's Republic of China
Thiophanate-methyl wettable powder
Published 2009-04-27
2009-11-01 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 standard FAO Specification 262/WP/S/P (1993) "thiophanate-methyl wettable powders" (Thiophanate-methyl
WettablePowders).
This standard modification method using foreign advanced standards for the redrafted law.
This standard FAO "thiophanate-methyl wettable powders" (Thiophanate-methylWettablePowders) the main technical
difference.
This standard specifies --- 70%, 50% in two sizes DAP (2,3- diamino phenazine) mass fraction ≤4.0mg/kg, ≤3.0mg/kg,
FAO Specifications predetermined DAP (2,3- diamino phenazine) mass fraction ≤0.4mg/kg, ≤0.3mg/kg;
--- This standard specifies a pH range of 6.0 ~ 9.0, FAO Specifications predetermined pH range 4.0 to 7.0;
--- This standard suspension rate ≥70%, FAO Specifications predetermined suspension ratio ≥60%;
--- FAO specifications lasting foam control volume indicators, this standard does not control the indicators;
--- This standard specifies the wetting time ≤90s, FAO specifications prescribed wetting time ≤60s.
The date of implementation of this standard, the former Chemical Industry Standard HG2462.2-1993 "thiophanate-methyl WP" void.
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. Jiangsu abundance of blue and Chemical Corporation, Haili Guixi Chemical Pesticide Co., Ltd., Jiangsu dragon of
Studies Limited.
The main drafters. Meibao Gui, Xing Hong, XIE Yin Gang, Running an, Feng Xiuzhen, Ma Lin.
Thiophanate-methyl wettable powder
The active ingredient other product names, structural formulas and physicochemical parameters of the basic thiophanate-methyl is as follows.
ISO common name. thiophanate-methyl
CIPAC Numeric Code. 262
Chemical name. 4,4 '- (1,2-phenylene) bis (3-methyl thioureido)
Structure.
Empirical formula. C12H14N4O4S2
Molecular weight. 342.40 (according to 2005 international relative atomic mass)
Biological activity. bactericide
Boiling point. 172 ℃ (decomposition)
Vapor pressure (25 ℃). 0.0095mPa
Solubility (23 ℃). water 26.6mg/L, acetone 58g/kg, chloroform 26g/kg, cyclohexanone 43g/kg, methanol 29g/kg, B
Nitrile 24g/kg, ethyl acetate 11.9g/kg; slightly soluble in n-hexane
Stability., stable in a neutral aqueous solution at room temperature; air and light stability; is very stable at room temperature, the weak acid solution; with a copper salt
Form a complex in the plant tissue and long-term storage of the suspension may be formed carbendazim
Range 1
This standard specifies thiophanate-methyl wettable powder of requirements, test methods and marking, labeling, packaging, storage and transportation.
This standard applies to thiophanate-methyl wettable powder made of thiophanate-methyl of the drug and appropriate processing auxiliaries and fillers.
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 1601 method for measuring the pH of pesticides
GB/T 1604 pesticide regulations for acceptance of goods
GB/T 1605-2001 sampling commercial pesticides
GB 3796 pesticide packaging General
GB/T 5451 method for measuring the wettability of agrochemical wettable
GB/T 14825 Method for determination of pesticide suspension
GB/T 16150 pesticide powders, wettable powder fineness measurement method
GB T 19136 Determination of heat storage stability of pesticide /
3.1 Composition and appearance
This product should meet the criteria of thiophanate-methyl of the drug and appropriate processing auxiliaries and fillers are made as loose powder uniformly, there should be
Clumps.
3.2 Technical Specifications
Thiophanate-methyl wettable powder should meet the requirements of Table 1.
Table benomyl wettable powder Item Index 1 control methylsulfanyl
project
index
70% 50%
Thiophanate-methyl mass fraction /% 70.0 + 50.0 + 2.5-2.5 2.5-2.5
HAP (2- amino-3-hydroxy-phenazine) mass fraction a/(mg/kg) ≤ 0.4 0.3
DAP (2,3- diamino phenazine) mass fraction a/(mg/kg) ≤ 4.0 3.0
pH range 6.0 to 9.0
Fineness (45μm standard sieve) /% ≥ 98
Suspension rate /% ≥ 70
Wetting time/s ≤ 90
Thermal storage stability test a /% passing
When a normal production, the mass fraction of HAP, the mass fraction of the DAP, the thermal storage stability test for detecting at least every 3 months once.
Test Method 4
4.1 Sampling
Carried out in GB/T 1605-2001 of "solid preparation sampling" approach. Determining Sample packages with a random number table method; final sample size
Not less than 300g.
4.2 Identification Test
HPLC --- This identification test can be conducted simultaneously measuring the mass fraction of benomyl and thiophanate-methyl. In the same chromatographic operating conditions
The lower member, and the retention time of peaks benomyl solution of methylthio the retention time of a standard sample peak relative difference in the sample solution should be
1.5% or less.
When using the above method of identification of active components in doubt, other effective means may be employed for authentication.
4.3 Determination of the mass fraction of thiophanate-methyl
4.3.1 Method summary
Sample was dissolved in methanol, methanol + water as the mobile phase, used Hypersil-ODS filler stainless steel column and UV detector
(269 nm), thiophanate-methyl of the sample were separated by HPLC, external standard.
4.3.2 Reagents and solutions
Methanol. HPLC grade;
Water. The new secondary steam distilled water;
Thiophanate-methyl Sample. thiophanate-methyl known mass fraction ≥98.0%.
4.3.3 Instruments
HPLC. a variable wavelength UV detector;
Chromatographic data processor;
Column.200mm × 4.6mm (. I.d) stainless steel column, built-Hypersil-ODS, 5μm packing;
Filter. membrane pore size of about 0.45 m;
Microsyringe. 50μL;
Quantitative sampling tube. 10μL;
Ultrasonic cleaning.
4.3.4 HPLC operating conditions
Mobile phase. [Phi] (methanol. water) = 60.40, by membrane filtration, and degassing;
Flow rate. 1.0mL/min;
Column temperature. room temperature;
Detection wavelength. 269nm;
Injection volume. 10μL;
Retention time. thiophanate-methyl about 10.4min.
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 thiophanate-methyl wettable powder shown in Figure 1 HPLC.
1 --- thiophanate-methyl.
Figure 1 HPLC thiophanate-methyl wettable powder
Under the above operating conditions, after the instrument is stable, the number of consecutive doses of the standard solution is injected, the needle until two adjacent thiophanate methyl pk area opposite
After the change is less than 1.2%, measured according to the standard solution, sample solution, the sample solution, the order of standard solution.
4.3.5 Determination Step
4.3.5.1 Preparation of standard solution
Thiophanate-methyl Weigh 0.1 g of standard sample (accurate to 0.0002g), a 50mL volumetric flask, dissolve and dilute to volume with methanol,
Shake well. A pipetted sample solution was diluted to 5mL above another in methanol 50mL volumetric flask to the mark.
4.3.5.2 Preparation of sample solution
Thiophanate-methyl, said sample is taken containing 0.1g (accurate to 0.0002g), a 50mL volumetric flask, dissolved in methanol and diluted to
Mark and shake. A pipetted sample solution was diluted to 5mL above another in methanol 50mL volumetric flask 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, the needle until two adjacent thiophanate methyl pk area opposite
After the change is less than 1.2%, measured according to the standard solution, sample solution, the sample solution, the order of standard solution.
4.3.6 computing
The measured sample solution and the preceding two needles two doses of the standard sample solution thiophanate-methyl pk area were averaged. A sample
Mass fraction of 1-yl thiophanate (%), according to equation (1).
1 = A2
(1)
Where.
A1 --- the standard solution, the average area of thiophanate-methyl pk;
A2 --- sample solution, thiophanate-methyl pk average area;
--- Sample mass fraction thiophanate methyl, expressed in%.
4.3.7 allows poor
Results difference between the two replicates thiophanate-methyl content should not exceed 1.0%, and the arithmetic mean value as a measurement result.
Determination of DAP and 4.4 HAP mass fraction
4.4.1 Method summary
Sample dissolved in mobile phase to a potassium dihydrogen phosphate buffer solution pH8.0 + methanol + water as mobile phase, used HypersilODS
Stainless steel column filler and UV - VIS detector (453nm), and sample the HAP DAP reverse phase high performance liquid chromatographic
From, external standard (HAP, DAP detection limit of 2 × 10-9g, equivalent to 0.1mg/kg).
4.4.2 Reagents and solutions
Methanol. HPLC grade;
Potassium dihydrogen phosphate;
Water. The new secondary steam distilled water;
Sodium hydroxide solution. ρ (NaOH) = 40g/L;
Buffer solution. Weigh 6.8g of potassium dihydrogen phosphate in distilled water with the secondary reagent bottle 1000mL, ultrasonic oscillation completely dissolved
Solution, with a sodium hydroxide solution to pH 8.0;
Sample HAP. HAP known mass fraction ≥97.0%;
Sample DAP. DAP known mass fraction ≥99.0%.
4.4.3 Instruments
HPLC. a variable wavelength UV detector;
Chromatographic data processor;
Column.200mm × 4.6mm (. I.d) stainless steel column, built-Hypersil-ODS, 5μm packing;
Filter. membrane pore size of about 0.45 m;
Microsyringe. 250μL;
Quantitative sampling tube. 50μL;
Ultrasonic cleaning;
Centrifuge.
4.4.4 HPLC operating conditions
Mobile phase. [Phi] (methanol. water. buffer solution) = 45.25.30;
Flow rate. 1.0mL/min;
Column temperature. room temperature (temperature change should be less than 2 deg.] C);
Detection wavelength. 453nm;
Injection volume. 50μL;
Retention time. HAP about 3.3min; DAP about 7.5min.
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.
HAP, DAP standard sample by HPLC is shown in Figure 2, thiophanate-methyl wettable powders HAP, DAP measured by HPLC
Shown in Figure 3.
1 --- HAP;
2 --- DAP.
FIG 2 HAP and DAP standard liquid chromatography FIG.
1 --- HAP;
2 --- DAP.
HPLC FIG. 3 thiophanate-methyl wettable powder and HAP DAP assay
4.4.5 Determination Step
4.4.5.1 Preparation of standard solution
4.4.5.1.1 DAP Preparation of standard solution (A solution)
Sample DAP accurately weighed 0.025 g (accurate to 0.0002g) in brown 50mL volumetric flask, diluted with methanol to the mark, the super
Was dissolved under sonication 10min, shake well and let to room temperature, the standby (the solution was stable for 2 months at dark at 4 ℃ conditions).
4.4.5.1.2 HAP Preparation of standard solution (B solution)
Sample HAP accurately weighed 0.015 g (accurate to 0.0002g) in brown 50mL volumetric flask, diluted with methanol to the mark, the super
Was dissolved under sonication 10min, shake well and let to room temperature, the standby (the solution was stable for 2 months at dark at 4 ℃ conditions).
Preparation 4.4.5.1.3 DAP, HAP standard solution
Pipette 50μLA solution, 50μLB solution, diluted with a 25mL volumetric flask with brown flowing to the mark (the standard solutions
Solution to be prepared before use).
4.4.5.2 Preparation of sample solution
20.0 g of accurately weighed (accurate to 0.0002g) sample was brown 100mL volumetric flask, added with a pipette flow 50mL compatibility
Was shaken under ultrasound 20min, shake well and let to room temperature. And then filtered at 3000 rpm/min centrifuge 5min, the supernatant.
4.4.5.3 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 HAP, the DAP relative peak area
After variations are less than 20%, measured according to the standard solution, sample solution, the sample solution, the order of standard solution.
4.4.6 computing
Sample HAP (DAP) the mass fraction 2 (mg/kg), according to formula (2).
2 = A2
104 (2)
Where.
A1 --- the standard solution, the average HAP (DAP) peak area;
A2 --- sample solution, the average HAP (DAP) peak area;
--- standard samples HAP (DAP) mass fraction, expressed in%;
500 --- standard dilution.
4.4.7 allows poor
Determination results parallel relative deviation should not exceed 30%, and the arithmetic mean value as a measurement result.
Carried out in GB/T 1601.
4.6 Determination of fineness
According to GB/T 16150 in the "wet sieve method".
4.7 Determination of the suspension rate
According to GB/T 14825 carried out. Weigh 0.35g sample containing thiophanate methyl (accurate to 0.0002g). 50mL methanol with an amount of
The remaining 25mL cylinder suspension and the precipitate was all transferred to 100mL volumetric flask to volume with methanol, shaken at ultrasonic
3min, shake, filtration. 4.3 Determination by mass spirit thiophanate-methyl, calculate suspensibility.
4.8 Determination of wetting time
Carried out in GB/T 5451.
Thermal storage stability test 4.9
According to GB/T 19136 of "powder formulation" performed. After the heat storage, thiophanate-methyl content should be greater than the measured mass fraction before hot storage
97% was still the suspension should meet standard requirements.
4.10 product inspection 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
Flag benomyl WP 5.1 methyl sulfide, labeling and packaging should comply with the provisions of GB 3796.
Benomyl thiophanate-methyl wettable powder 5.2 packaging applications, clean, dry aluminum foil bags, net weight 200g, 250g, 500g. and also
Other forms of packaging can be employed according to user requirements or ordering protocols, subject to the provisions of GB 3796.
5.3 thiophanate-methyl wettable powder package and 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 Safety. thiophanate-methyl is a low toxicity fungicides, plant safety. The FDA should wear protective equipment, wash with soap after application
net. This product is generally less prone to poisoning. Such as poisoning, atropine detoxification can be used under the guidance of doctors.
5.6 guarantee. Storage conditions specified in, benomyl thiophanate-methyl wettable powder warranty period from the production date of 2 years.
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