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GB 23555-200925% Buprofezin wettable powders (English PDF)

25%噻嗪酮可湿性粉剂

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Issued by

Standardization Administration of China

Level / Type

National · Mandatory

Issue date

April 27, 2009

Implementation date

November 1, 2009

Scope

GB 23555-2009 is the English-translated version of 25%噻嗪酮可湿性粉剂.

GB 23555-2009 — This standard specifies 25% buprofezin WP requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to the buprofezin original drug, suitable additives and fillers processed into 25% buprofezin WP.

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Document preview — GB 23555-2009

National Standard of the People's Republic of China

ICS
65.100.10
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 Buprofenzin mass fraction determination
  • 4.4 Determination of the suspension rate
  • 4.5 Determination of Moisture
  • 4.7 Determination of wetting time
  • 4.8 Determination of fineness
  • 4.9 Thermal storage stability test
  • 4.10 Product inspection and acceptance
  • 5 Marking, labeling, packaging, storage and transportation

Foreword

The standard Chapter 3, Chapter 5 are mandatory, the rest are recommended.

Since the implementation of this standard, HG2463.2-1993 "25% buprofezin WP" abolished.

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 25% buprofezin WP requirements, test methods and marking, labeling, packaging, storage and transportation.

This standard applies to the buprofezin original drug, suitable additives and fillers processed into 25% buprofezin WP.

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 1604 Goods pesticide regulations for acceptance GB/T 1605-2001 Sampling Method commercial pesticides GB 3796 pesticide packaging General GB/T 5451 WP Pesticide wettability measurement method GB/T 14825 method for determination of pesticide suspension GB/T 16150 pesticide powder, wettable powder fineness measurement method GB/T 19136 Determination of Pesticide Thermal storage stability

3 Requirements

3.1 Composition and appearance

This product should be in line with the original drug buprofezin standard with suitable additives and fillers processing is made uniform loose powder, there should be no lumps.

3.2 Technical Specifications

25% buprofezin WP should meet the requirements of Table 1.

Table 1 25% buprofezin WP Control Project Index

Item Index

Buprofenzin mass fraction/25.0 + 1.5-1.5% Moisture /% <= 2.0 Suspension rate /% >= 75 Fineness (through 45µm test sieve) /% >= 98 Wetting time/s <= 90 pH range 6.0 to 10.5 Thermal storage stability of a qualified a thermal storage stability test under normal production conditions, measured at least once every 3 months.

Test Method 4

4.1 Sampling

Carried out according to GB/T 1605-2001 "on solid preparation sampling" method. Determining sample package using a random number table method; the final sample the amount of not less than 300g.

4.2 Identification Test

Gas Chromatography --- The identification test can be carried out simultaneously with the determination of the content of buprofezin. Under the same chromatographic operating conditions, the sample solution the solution buprofezin peak retention time and the retention time of a standard solution peak, the relative difference should be less than 1.5%.

4.3 Buprofenzin mass fraction determination

4.3.1 Method summary

Sample was dissolved in chloroform, dicyclohexyl phthalate esters as internal standard, using a HP-5 (5% diphenyl + 95% dimethylpolysiloxane Ketone) coated wall of the capillary column and flame ionization detector, the sample of buprofezin gas chromatography separation and determination. Also allows with filling column gas chromatography, chromatographic conditions see Appendix A.

4.3.2 Reagents and solutions

Chloroform;

Buprofenzin standard. a known mass fraction >=98.0%;

Dicyclohexyl phthalate esters. interference analysis should not contain impurities;

Internal standard solution. Weigh 4.0g dicyclohexyl phthalate esters, placed in 500mL flask with chloroform dissolved and diluted to the mark Degree, shake.

4.3.3 Instruments

Gas chromatograph. with a hydrogen flame ionization detector;

Chromatographic data processor or chromatography workstation;

Column. 30m × 0.32mm (i.d.) Capillary column, wall coated HP-5 (5% + 95% diphenyl dimethyl silicone), the film thickness 0.25µm;

Micro injector. 10µL.

4.3.4 GC operating conditions

Temperature (°C). 230 column temperature, the gasification chamber 270, the detector chamber 280;

Gas flow rate (mL/min). carrier gas (N2) 2.0, hydrogen gas 30, air 300, the compensation gas (N2) 25;

Split ratio. 20.1;

Injection volume (µL). 1.0;

Retention time (min). 3.8 buprofezin, internal standard 7.0.

HPLC operating conditions described above, the Department of typical operating parameters. According to the characteristics of different instruments, given operating parameters adjusted as appropriate, in order to obtain the best results. A typical 25% buprofezin WP capillary gas chromatography shown in Figure 1.

1 --- solvent;

2 --- buprofezin;

3 --- internal standard (phthalate, dicyclohexyl phthalate).

1 25% buprofezin WP and the internal standard capillary gas chromatogram

4.3.5 Measuring step
4.3.5.1 Preparation of standard solution

Weigh buprofenzin standard 0.08g (accurate to 0.0002g) in 15mL stoppered glass bottle with a pipette accurately added 10mL within Standard solution, shake.

4.3.5.2 Preparation of the sample solution

Weigh containing buprofezin 0.08g (accurate to 0.0002g) sample, in 15mL stoppered glass vial, with a shift with the 4.3.5.1 Pipette accurately added internal standard solution 10mL, shake.

4.3.5.3 Determination

Under these operating conditions, the instrument until a stable baseline, the number of continuous injection doses of the standard solution, calculated for each needle buprofezin and the internal standard peak area the ratio of repeatability to be two adjacent needles buprofenzin relative change and the internal standard peak area ratio of less than 1.2%, the standard solution in accordance with the sample solution Solution, sample solution, the order 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 piperazinone and thiophene internal standard peak area ratios are averaged. test 1 sample mass fraction (%) of buprofezin according to formula (1).

Where.

gamma1 --- standard solution, buprofezin and the internal standard peak area ratio of the average;

gamma2 --- sample solution, buprofezin and the internal standard peak area ratio of the average;

--- Standard samples buprofezin mass fraction, expressed as a percentage.

4.3.7 Allowable difference

Thiophene-one hydrochloride poor quality score two parallel determination results shall be not more than 0.5%, the arithmetic mean value as a measurement result.

4.4 Determination of the suspension rate

4.4.1 Determination

According to GB/T 14825 performed. Weigh 0.5g sample (accurate to 0.0002g), the remaining 1/10 suspension precipitate added Internal standard solution 10mL, plus 10mL chloroform, shaken and extracted. 4.3 Determination of buprofezin by mass calculated suspension rate.

4.4.2 Allowable difference

The difference between two parallel determination results shall not be greater than 5% of the arithmetic mean as a measurement result.

4.5 Determination of Moisture

According to GB/T 1600 in the "azeotropic distillation method".

According to GB/T 1601 carried out.

4.7 Determination of wetting time

According to GB/T 5451 carried out.

4.8 Determination of fineness

According to GB/T 16150 in the "wet sieve method".

4.9 Thermal storage stability test

According to GB/T 19136 "body powder agent" to. Within 24h by 4.3, 4.4 Determination of buprofezin content, suspension rate. The measurement results thiazide One before the mass fraction of the reservoir dropped to allow the determination of 97%, measured suspension rate should not be below 65%.

4.10 Product inspection and acceptance

Shall comply with GB/T 1604's. Limit numerical processing using rounding value comparison method.

5 Marking, labeling, packaging, storage and transportation

5.1 25% buprofezin WP signs, labeling and packaging should comply with the provisions of GB 3796.

5.2 25% buprofezin WP with aluminum foil bag or plastic bag, net weight of 100g, 200g, 250g, 500g; packaging Available cartons, corrugated cardboard box or Plastic boxes, each containing a net weight of not more than 25kg. You can also order or agreement according to user requirements, the use of its Other forms of packaging, subject to the provisions of GB 3796.

5.3 25% buprofezin WP package should be stored in well-ventilated, dry coffers.

5.4 storage, prevent moisture and sunlight, no food, seed, feed mix, avoid contact with skin, eyes, mouth and nose to prevent inhalation.

5.5 Security. buprofezin as low toxicity pesticides, are swallowed or inhaled toxic. When used, should wear protective gloves, masks, wearing clean protective clothing.

Immediately after use with soap and water. In case of poisoning, should go to hospital for examination and treatment.

5.6 Warranty. under specified conditions of storage, from date of manufacture for 2 years.

Appendix A

(Informative)

Buprofenzin quality gas chromatographic method scores packed column A. 1 Method summary Sample was dissolved in chloroform, dicyclohexyl phthalate esters as internal standard, using the 5% OV-101/GaschromQ filler Column and flame ionization detector, the sample of buprofezin gas chromatography separation and determination.

A. 2 Reagents and solutions Chloroform;

Fixative. OV-101;

Carrier. GaschromQ particle diameter of 180µm ~ 250µm;

Dicyclohexyl phthalate esters. shall not interfere with the analysis of impurities;

Internal standard solution. Weigh 4.0g dicyclohexyl phthalate esters in 500mL flask with chloroform dissolved and diluted to the mark, Shake;

Buprofenzin standard. a known mass fraction >=98.0%.

A. 3 Instrument

Gas chromatograph. with a hydrogen flame ionization detector;

Chromatographic data processor or chromatography workstation;

Column. 1m × 3mm (. I.d) glass column, built 5% OV-101/GaschromQ filler particle size 180µm ~ 250µm (Or have other column of the same column efficiency).

A. 4 GC operating conditions Temperature (°C).200 column temperature, the gasification chamber 250, the detector chamber 250;

Gas flow rate (mL/min). carrier gas (N2) 30, hydrogen gas 40, air 400;

Retention time (min). 5 buprofezin; 10 internal standard.

GC operating conditions described above, the Department of typical operating parameters. According to the characteristics of different instruments, given operating parameters adjusted as appropriate, in order to obtain the best results. A typical 25% buprofezin WP packed column gas chromatography is shown in Figure A. 1.

1 --- solvent;

2 --- buprofezin;

3 --- internal standard (phthalate, dicyclohexyl phthalate).

Figure A. Packed Column Gas Chromatography 1 25% buprofezin WP and the internal standard

A. 5 measuring step

A. 5.1 preparation of standard solution Weigh buprofenzin standard 0.08g (accurate to 0.0002g) in 15mL stoppered glass bottle with a pipette accurately transferred within 10mL Standard solution, and shake.

A. 5.2 Sample preparation solution Weigh about 0.08g sample containing buprofezin the (accurate to 0.0002g) in 15mL stoppered glass vial, with A. With 5.1 used A pipette accurately transferred to the internal standard solution 10mL, shake.

A. 5.3 Determination Under these operating conditions, the instrument until a stable baseline, the number of continuous injection doses of the standard solution, calculated for each needle buprofezin and the internal standard peak area Repeatability ratio, when two needles buprofenzin relative change compared with the internal standard peak area of less than 1.2% to be adjacent, in accordance with the standard solution, sample Solution, sample solution, the order of the standard solution was measured.

A. 6 Calculation

The two needle sample solution and measured before and after the two doses of the standard sample solution buprofezin and the internal standard peak area ratios are averaged.

Buprofezin sample mass fraction of 1 (%) according to equation (A.1) Calculated.

Where.

gamma1 --- standard solution, buprofezin and the internal standard peak area ratio of the average;

gamma2 --- sample solution, buprofezin and the internal standard peak area ratio of the average;

--- Standard samples buprofezin mass fraction, expressed as a percentage.

A. 7 allowable difference the difference between two parallel determination results shall not be greater than 0.5%, the arithmetic mean value 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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