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GB 22615-2008Clethodim emulsifiable concentrates (English PDF)

烯草酮乳油

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Issued by

Standardization Administration of China

Level / Type

National · Mandatory

Issue date

December 17, 2008

Implementation date

June 1, 2009

Scope

GB 22615-2008 is the English-translated version of 烯草酮乳油.

GB 22615-2008 — 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.

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Document preview — GB 22615-2008

National Standard of the People's Republic of China

ICS
65.100.20
Classification
G 25

Issued by: Standardization Administration of China

Contents

  • Foreword
  • 1 Scope
  • 2 Normative references
  • 3 Requirements
  • 3.1 Composition and appearance
  • 3.2 Technical Specifications
  • 4.1 Sampling
  • 4.2 Identification Test
  • 4.3 Determination of the mass fraction of clethodim
  • 4.4 Determination of Moisture
  • 4.6 Emulsion stability test
  • 4.7 Low temperature stability test
  • 4.8 Thermal storage stability test
  • 4.9 Product testing and acceptance
  • 5 Marking, labeling, packaging, storage and transportation

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.

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 °C) / (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. pore size of about 0.45µm;

Micro injector. 50µL;

Quantitative sample line. 5µL;

Ultrasonic cleaner.

4.3.4 HPLC operating conditions

Mobile phase. psi (dichloromethane. n-hexane. acetic acid) = 75.25.0.5 by membrane filtration, and degassing;

Flow rate. 1.0mL/min;

Column temperature. 30 °C;

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 rho1 (g/L) by the formula.

1 = A2

359.90

365.84

rho1 =

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) °C 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 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. 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 °C);

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 rho1 (g/L) according to equation (A.2) Calculated.

1 = A2

359.90

365.84

rho1 =

Where.

A1 --- the standard solution, the average peak area clethodim;

A2 --- sample solution, the average peak area clethodim;

Density rho --- 20 °C 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.

......
This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 7 pages — is available in the English PDF.

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