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GB 22615-2008: [GB/T 22615-2008] Clethodim emulsifiable concentrates
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[GB/T 22615-2008] Clethodim emulsifiable concentrates
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GB 22615-2008
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Basic data | Standard ID | GB 22615-2008 (GB22615-2008) | | Description (Translated English) | [GB/T 22615-2008] Clethodim emulsifiable concentrates | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Classification of International Standard | 65.100.20 | | Word Count Estimation | 9,969 | | Date of Issue | 2008-12-17 | | Date of Implementation | 2009-06-01 | | Quoted Standard | GB/T 1600; GB/T 1601; GB/T 1603; GB/T 1604; GB/T 1605-2001; GB/T 4472; GB 4838; GB/T 19136; GB/T 19137 | | Regulation (derived from) | Announcement of Newly Approved National Standards No. 21 of 2008 (No. 134 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 requirements of EC clethodim, test methods and marking, labeling, packaging, storage and transportation. This standard applies to clethodim original drug is dissolved in a suitable solvent and emulsifier in the preparation of clethodim EC. | GB 22615-2008: [GB/T 22615-2008] Clethodim emulsifiable concentrates---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.
Clethodim emulsifiable concentrates
ICS 65.100.20
G25
National Standards of People's Republic of China
EC clethodim
Posted 2008-12-17
2009-06-01 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.
Appendix A of this standard is the data appendix.
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.
It participated in the drafting of this standard. Jiangsu Changqing Agrochemical Co., Ltd.
The main drafters of this standard. Meibao Gui, Xing Jun, at sea level, in the light, Lvliang Zhong.
EC clethodim
Other name, structural formula and basic physicochemical parameters of the active ingredient clethodim products are as follows.
ISO common name. Clethodim
Chemical name. (±) -2 - [(E) -3- chloro-allyloxyimino amino] propyl -5- [2- (ethylthio) propyl] -3-hydroxy-cyclohex-2-ene ketone
Structural formula
CH 2CHCH 3
SC2H
5
OH
C C2H 5
N O CH 2 CH 2
C
Cl
Empirical formula. C17H26ClNO3S
Molecular Weight. 359.9 (according to 2007 international relative atomic mass)
Biological activity. Herbicides
Boiling point. decomposition below boiling point
Vapor pressure (20 ℃). less than 1 × 10-2mPa
Solubility. insoluble in water, soluble in most organic solvents
Stability. under ultraviolet light, acidic and alkaline conditions are unstable. Poor thermal stability
1 Scope
This standard specifies the clethodim EC requirements, test methods and marking, labeling, packaging, storage and transportation.
This standard applies to the clethodim original drug and preparation of the emulsifier is dissolved in a suitable solvent clethodim EC.
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.
GB/T 1600 Determination of Water Pesticides
Determination of GB/T 1601 Pesticides pH value
GB/T 1603 Determination of emulsion stability of pesticide
GB/T 1604 Goods pesticide regulations for acceptance
GB/T 1605-2001 Sampling Method commercial pesticides
GB/T 4472 chemical product density, relative density measurement General
GB 4838 EC pesticide packaging
GB/T 19136 Determination of Pesticide Thermal storage stability
GB/T 19137 Pesticide cryogenic stability Determination
3 Requirements
3.1 Composition and appearance
This product should be compliant clethodim original drug is made into a stable homogeneous liquid, free from visible suspended matter or precipitation.
3.2 Technical Specifications
Clethodim EC shall comply with the requirements of Table 1.
Table 1 clethodim EC Control Project Index
project
index
120g/L 240g/L 24%
Clethodim mass fraction a /%
Clethodim or mass concentration (20 ℃) / (g/L)
13.0 + 1.4-0.7
+ 14-7 120
26.0 + 2.6-1.3
+ 24-12 240
24.0 + 2.4-1.2
Moisture content /% ≤ 0.4
pH value of 4.0 to 7.0
Emulsion stability (diluted 200 times) Qualified
Low temperature stability Qualified b
Thermal storage stability b qualified
The mass fraction was measured to arbitration when a dispute occurs when the quality.
B when normal production, low temperature stability test, thermal storage stability test for detection of at least once every 3 months.
Test Method 4
4.1 Sampling
According to GB/T 1605-2001 in "liquid formulations sampling" approach. Determined by sampling a random number table method packages, the final sample size
Not less than 200mL.
4.2 Identification Test
HPLC --- The identification test can be carried out simultaneously with the determination of the content of clethodim. Under the same chromatographic operating conditions, the test
A sample solution peak retention time compared with standard sample solution clethodim chromatographic retention time, the relative difference should be less than 1.5%.
4.3 Determination of the mass fraction of clethodim
4.3.1 Method summary
Sample dissolved in mobile phase to dichloromethane + hexane + glacial acetic acid as the mobile phase, to use as filler stainless Hypersilsilica
Steel column and UV detector (254nm), the sample of clethodim normal phase high performance liquid chromatography, external standard. You can also use
RP-HPLC, chromatography operating conditions, see Appendix A.
4.3.2 Reagents and solutions
Methylene chloride;
N-hexane;
Glacial acetic acid;
Clethodim lithium salt standard. clethodim known lithium salt mass fraction ≥98.0%.
4.3.3 Instruments
High performance liquid chromatography. a variable wavelength UV detector;
Chromatographic data processor;
Column. 150mm × 3.9mm (. I.d) stainless steel column, built Hypersilsilica, 5μm packing;
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 (dichloromethane. n-hexane. acetic acid) = 75.25.0.5 by membrane filtration, and degassing;
Flow rate. 1.0mL/min;
Column temperature. 30 ℃;
Detection wavelength. 254nm;
Injection volume. 5μL;
Retention time. clethodim about 10.4min.
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 EC clethodim normal phase HPLC is shown in Figure 1.
1 --- clethodim.
Figure 1 EC clethodim normal phase HPLC chromatogram
Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles clethodim peak area relative change
After less than 1.2%, according to the solution, the sample solution, the sample solution and standard sequence of the standard solution was measured.
4.3.5 measuring step
4.3.5.1 Preparation of standard solution
Weigh clethodim standard lithium salt 0.1g (accurate to 0.0002g), a 50mL volumetric flask, add 3 drops of glacial acetic acid and shaking the mobile phase
Dissolved, mobile phase and dilute to the mark. With said pipette 5mL 50mL test solution to another flask with the mobile phase
Dilute to the mark.
4.3.5.2 Preparation of sample solution
Weigh 0.1g sample containing clethodim the (accurate to 0.0002g), a 50mL volumetric flask, add the mobile phase was shaken to dissolve with
Mobile phase and dilute to the mark. With said pipette 5mL 50mL test solution to another flask with the mobile phase diluted to the mark,
Shake well.
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 clethodim peak area relative change
After less than 1.2%, 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 and measured before and after the two doses of the standard sample solution clethodim peak areas are averaged. Sample clethodim
(1) calculate the mass fraction of 1 (%) according to the formula, (2) the calculation of the mass concentration of clethodim ρ1 (g/L) by the formula.
1 = A2
359.90
365.84
(1)
ρ1 =
(2)
Where.
A1 --- the standard solution, the average peak area clethodim;
A2 --- sample solution, the average peak area clethodim;
--- Standard samples clethodim lithium salt mass fraction in%;
359.90 --- relative molecular mass clethodim;
Molecular Weight 365.84 --- clethodim lithium salt.
4.3.7 allowable difference
Clethodim mass fraction (concentration) of two parallel determination results relative difference should be less than 4%, and the arithmetic mean as measured
result.
4.4 Determination of Moisture
According to GB/T 1600 the "Karl Fischer method".
According to GB/T 1601 carried out.
4.6 Emulsion stability test
Standard hard water sample was diluted 200-fold, according to GB/T 1603 test, the non-oil slick, no precipitation under qualified.
4.7 Low temperature stability test
According to GB/T 19137 in "homogeneous emulsion and liquid preparations", in the bottom of the centrifuge tube educt volume does not exceed 0.3mL qualified.
4.8 Thermal storage stability test
According to GB/T 19136 in "liquid formulation" to. Heat storage conditions (35 ± 2) ℃ stored for 12 weeks. After the thermal storage, clethodim mass fraction
Number shall not be lower than before the reservoir measured clethodim mass fraction of 90%, emulsion stability should continue to meet the standards.
4.9 product testing and acceptance
Shall comply with GB/T 1604's. Limit the use of numerical treatment rounding value comparison method.
5 marking, labeling, packaging, storage and transportation
5.1 clethodim EC marking, labeling and packaging should comply with the provisions of GB 4838.
5.2 Bulk EC clethodim PU barrel barrel net content of not more than 200kg. EC clethodim small package polyurethane bottle
Packaging, bottle net weight 100g (mL), 200g (mL), 250g (mL), 500g (mL); overpack Plastic boxes or corrugated boxes, each
Box net weight shall not exceed 15kg.
5.3 Other forms of packaging may be used according to user requirements or the order agreement, subject to the provisions of GB 4838.
5.4 clethodim EC packages should be stored in well-ventilated, dry, low temperature warehouse.
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. clethodim as low toxicity herbicides, the FDA should wear protective equipment, application after application, wash with soap, if swallowed, not reminders
Spit, should be sent to the hospital immediately, according to the organic solvent (xylene) poisoning treatment therapy.
5.7 Warranty. under the specified storage conditions, clethodim EC guarantee, from date of manufacture for 2 years.
Appendix A
(Informative)
Clethodim mass fraction of phase high performance liquid chromatographic method
A. 1 Method summary
Sample with acetone petroleum ether was dissolved in acetonitrile + water + phosphoric acid as mobile phase to Nova-PakC18 use as filler and a stainless steel column
UV detector (254nm), the sample of clethodim reverse phase high performance liquid chromatography, external standard.
A. 2 Reagents and solutions
Acetonitrile. HPLC grade;
Water. The new secondary steam distilled water;
acetone;
Petroleum ether;
Phosphoric acid;
Acetone petroleum ether. [Psi] (acetone. petroleum ether) = 1;
Clethodim lithium salt standard. clethodim known lithium salt mass fraction ≥98.0%.
A. 3 Instrument
High performance liquid chromatography. a variable wavelength UV detector;
Chromatographic data processor;
Column. 150mm × 4.6mm (. I.d) stainless steel column, built-Nova-PakC18,5μm 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.
A. 4 RP-HPLC operating conditions
Mobile phase. [Psi] (acetonitrile. water) = 65.35, wherein the water pH was adjusted to 3.0 with phosphoric acid, filtered through a filter membrane and degassed;
Flow rate. 1.0mL/min;
Column temperature. room temperature (temperature change should not exceed 2 ℃);
Detection wavelength. 254nm;
Injection volume. 5μL;
Retention time. clethodim about 5.8min.
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 EC clethodim HPLC is shown in Figure A. 1.
1 --- clethodim.
Figure A. 1 clethodim EC by RP-HPLC Figure
A. 5 measuring step
A. 5.1 preparation of standard solution
Weigh 0.1g clethodim lithium salt standard (accurate to 0.0002g), a 50mL volumetric flask, add 3 drops of glacial acetic acid and a small amount of acetone
Petroleum ether solution was shaken to dissolve, dilute to the mark with acetone petroleum ether solution, shake. Using a pipette to take the above solution 5mL
50mL volumetric flask, dilute to the mark with petroleum ether, acetone, shake.
A. 5.2 Sample preparation solution
Weigh 0.1g sample containing clethodim the (accurate to 0.0002g), a 50mL volumetric flask, dilute with acetone solution to petroleum ether
Mark and shake. Using a pipette to take the above solution 5mL to 50mL volumetric flask, diluted with petroleum ether and acetone to the mark.
A. 5.3 Determination
A. 6 Calculation
The two needle sample solution and measured before and after the two doses of the standard sample solution clethodim peak areas are averaged. Sample clethodim
The mass fraction of 1 (%) according to equation (A.1) calculations, clethodim mass concentration ρ1 (g/L) according to equation (A.2) Calculated.
1 = A2
359.90
365.84
(A.1)
ρ1 =
(A.2)
Where.
A1 --- the standard solution, the average peak area clethodim;
A2 --- sample solution, the average peak area clethodim;
Density ρ --- 20 ℃ when the sample in grams per milliliter (g/mL) (according to GB/T 4472 measured);
--- Standard samples clethodim lithium salt mass fraction in%;
359.90 --- relative molecular mass clethodim;
Molecular Weight 365.84 --- clethodim lithium salt.
A. 7 allowable difference
Two parallel determination results of the relative difference should be less than 4%, and the arithmetic mean as a measurement result.
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