GB 22625-2008 English PDF

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GB 22625-2008: [GB/T 22625-2008] Prochloraz emulsion, oil in water
Status: Obsolete

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Basic data

Standard ID: GB 22625-2008 (GB22625-2008)
Description (Translated English): [GB/T 22625-2008] Prochloraz emulsion, oil in water
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Classification of International Standard: 65.100.30
Word Count Estimation: 12,190
Date of Issue: 2008-12-17
Date of Implementation: 2009-06-01
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 prochloraz EW requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to prochloraz meet the standards of the original drug with a suitable additive prepared from prochloraz water emulsions.

GB 22625-2008: [GB/T 22625-2008] Prochloraz emulsion, oil in water

---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.
Prochloraz emulsion, oil in water ICS 65.100.30 G25 National Standards of People's Republic of China Prochloraz water emulsion 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 an informative annex. 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. Participated in the drafting of this standard. Nanjing Red Sun Group, Nantong Jiangshan Agrochemical & Chemical Co., Ltd., Dongguan City, Reid HSBC Biological Technology Ltd., Qingdao Kai Yuen Cheung Chemical Co., Ltd. The main drafters of this standard. Hou Chunqing, Wu Tiejun, Liukui Tao, Wang Zhimin, Li Ou Yan, Wen Shao. Prochloraz water emulsion The product is an active ingredient prochloraz other name, structural formula and basic physicochemical parameters are as follows. ISO common name. prochloraz Chemical name. N- propyl--N- [2- (2,4,6- trichlorophenoxy) ethyl] imidazole-1-carboxamide Structure. Empirical formula. C15H16Cl3N3O2 Molecular Weight. 376.7 (according to 2007 international relative atomic mass) Biological activity. bactericidal Melting point. 46.5 ℃ ~ 49.3 ℃ (purity greater than 99%) Solubility (25 ℃). water 34.4mg/L, soluble in most organic solvents, such as chloroform, ethyl acetate, toluene, xylene 2.5kg/L, Acetone 3.5kg/L, n-hexane 7.5 × 10-3kg/L Stability. In water (pH = 7,20 ℃) stable, light, continuous high temperature heating (200 ℃) or in case of a strong acid, alkali decomposition when

1 Scope

This standard specifies the prochloraz water emulsion of requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to the standards-compliant prochloraz original drug with a suitable adjuvant prepared from prochloraz water emulsion.

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. 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 3796 pesticide packaging General GB/T 4472 chemical product density, relative density measurement General GB/T 14825 method for determination of pesticide suspension 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 prochloraz original drug with suitable additives formulated, should be a stable liquid, long after a small amount of points allowed Layer, a slight shaking or agitation should be uniform. 3.2 Technical Specifications Prochloraz water emulsion should meet the requirements of Table 1. Table 1 prochloraz emulsion in water quality control program indicators project index 25% 45% 450g/L Prochloraz mass fraction a /% Or concentration/(g/L) 25.0 + 45.0 + 2.2-2.2 1.5-1.5 2.0-2.0 40.0 + - - + 22-22 450 2,4,6-trichlorophenol mass fraction b /% ≤ 0.2 0.3 a pH range of 5.5 to 8.5 Pourability After pouring the residue mass fraction /% ≤ 5.0 After washing the residue mass fraction /% ≤ 0.5 Emulsion stability (diluted 200 times) Qualified Persistent amount of foam (placed 1min)/mL ≤ 25 Thermal storage stability test b qualified Low temperature stability test b qualified When a dispute occurs when mass to the mass fraction of arbitration. B when normal production of 2,4,6-trichlorophenol mass fraction, thermal storage stability test, measuring low temperature stability test at least once every three months. Test Method 4 4.1 Sampling According to GB/T 1605-2001 in "liquid formulations sampling" approach. Determining sample package using a random number table method; the final sample size Not less than 1000mL. 4.2 Identification Test Liquid chromatography --- The identification test can be carried out simultaneously with the determination of the mass fraction of prochloraz. Under the same chromatographic operating conditions, the test A sample solution peak retention time and standard solution PROCHLORAZ chromatographic retention time, the relative difference should be 1.5% Fewer. 4.3 Determination of the mass fraction of prochloraz 4.3.1 Method summary Sample was dissolved in methanol, acetonitrile + methanol + water as the mobile phase, to use as filler AgilentTC-C18 stainless steel column and ultraviolet Detector (225nm), the sample of prochloraz reverse phase high performance liquid chromatography, external standard. You can also use capillary gas Chromatography, chromatographic operating conditions given in Appendix A. 4.3.2 Reagents and solutions Methanol. HPLC grade; Acetonitrile. HPLC grade; Water. The new secondary steam distilled water; Prochloraz standard. a known mass fraction ≥98.0%. 4.3.3 Instruments High performance liquid chromatography. a variable wavelength UV detector; Chromatographic data processor or workstation; Column. 250mm × 4.6mm (. I.d) stainless steel column, built AgilentTC-C18,5μm filler (or with equivalent effect Column); 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 (methanol. acetonitrile. water) = 30.40.30 by membrane filtration, and degassing; Flow rate. 1.0mL/min; Column temperature. room temperature (temperature change should not exceed 2 ℃); Detection wavelength. 225nm; Injection volume. 5μL; Retention time. about 12.0min. 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 prochloraz water emulsion HPLC is shown in Figure 1. 1 --- prochloraz. Figure 1 prochloraz water emulsion by high performance liquid chromatogram 4.3.5 measuring step 4.3.5.1 Preparation of standard solution Weigh 0.1g (accurate to 0.0002g) Prochloraz standard in 50mL volumetric flask, dissolved in methanol and diluted to the mark. use Pipette pipette above solution 10mL in 50mL volumetric flask, diluted with methanol to the mark. 4.3.5.2 Preparation of sample solution Weigh containing prochloraz 0.1g (accurate to 0.0002g) sample in 50mL volumetric flask, dissolved in methanol and diluted to the mark, shake uniform. Using a pipette to take the above solution 10mL in 50mL volumetric flask, diluted with methanol to the mark. 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 prochloraz peak area relative change After less than 1.5%, according to the solution, sample solution, sample solution, standard order of standard solution was measured. 4.3.6 Calculation Prochloraz sample mass fraction of 1 (%), according to equation (1) calculation; mass density ρ1 (g/L), according to equation (2). 1 = A2 (1) ρ1 = 10 (2) Where. A1 --- the standard solution, the average peak area prochloraz; A2 --- sample solution, Prochloraz amines mean peak area; Density ρ --- 20 ℃ when the sample in grams per milliliter (g/mL) (according to GB/T 4472 measured); --- Prochloraz standard mass fraction, expressed as a percentage. 4.3.7 allowable difference Prochloraz mass fraction two parallel determination results relative error should not exceed 2.5%, and the arithmetic mean as a measurement result. 4.4 2,4,6-trichlorophenol mass fraction determination 4.4.1 Method summary Sample was dissolved in methanol, acetonitrile + water as the mobile phase, to use as filler AgilentTC-C18 stainless steel column and UV detector (215nm), the sample of 2,4,6-trichlorophenol by reverse phase high performance liquid chromatography, external standard. 4.4.2 Reagents and solutions Acetonitrile. HPLC grade; Water. The new secondary steam distilled water; 2,4,6-trichlorophenol standard. a known mass fraction ≥99.0%. 4.4.3 Instruments High performance liquid chromatography. a variable wavelength UV detector; Chromatographic data processor or chromatography workstation; Column. 250mm × 4.6mm (. I.d) stainless steel column, built AgilentTC-C18,5μm filler (or with equivalent effect Column); Filter. filter pore size of about 0.45μm; Micro injector. 50μL; Quantitative sample line. 5μL; Ultrasonic cleaner. 4.4.4 HPLC operating conditions Mobile phase. ψ (acetonitrile. water) = 55.45, by membrane filtration, and degassing; Flow rate. 1.0mL/min; Column temperature. room temperature (temperature change should not exceed 2 ℃); Detection wavelength. 215nm; Injection volume. 5μL; Retention time. about 4.0min. 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 prochloraz water emulsion of 2,4,6-trichlorophenol was measured by HPLC is shown in Figure 2. 1 --- 2,4,6-trichlorophenol; 2 --- prochloraz. Figure 2 prochloraz water emulsion of 2,4,6-trichlorophenol was measured by high performance liquid chromatogram 4.4.5 measuring step 4.4.5.1 Preparation of standard solution Weigh 0.01g (accurate to 0.0002g) 2,4,6- trichlorophenol standard sample in 50mL volumetric flask, dissolved in methanol and diluted to the mark Degree, shake. 4.4.5.2 Preparation of sample solution Weigh-containing 2,4,6-trichlorophenol 0.01g (accurate to 0.0002g) sample in 50mL volumetric flask, dissolved in methanol and diluted to Mark and shake. 4.4.5.3 Determination Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles 2,4,6-trichlorophenol peak area After the relative change of less than 1.5%, according to the solution, sample solution, sample solution, standard order of standard solution was measured. 4.4.6 Calculation The two needle sample solution and measured before and after the two doses of the standard sample solution of 2,4,6-trichlorophenol peak areas are averaged. test Samples 2,4,6-trichlorophenol 2 mass fraction (%), according to equation (3) Calculated. 2 = A2 (3) Where. A1 --- standard solution, the average of 2,4,6-trichlorophenol peak area; --- The A2 in the sample solution, an average value of the peak area of 2,4,6-trichlorophenol; --- 2,4,6-trichlorophenol standard mass fraction, expressed as a percentage. 4.4.7 allowable difference The relative deviation of two measurements shall be not more than 20% of the arithmetic mean as a measurement result. 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 Determination of dumping 4.7.1 Method summary Once placed in a container of water emulsion sample placed certain period of time, in accordance with prescribed procedures dumping determined trapped in the sample container Volume; the vessel was washed with water, and then measuring the amount of container. 4.7.2 Instruments With ground joint stopper cylinder. 500mL ± 2mL; cylinder height 39cm, between the upper and lower scale distance 25mL (or equivalent for the determination of dumping Down of other containers). 4.7.3 Test procedure Mix well enough samples, some of which have been promptly placed weighed measuring cylinder (including plug), attached to 8/10 of the cylinder, the plug Tight grinding mouth stuffed, place the determined time (24h). The tap is opened, the upright position of the rotating cylinder by a 135 ° angle of dumping 60s, then invert 60s, heavy The new weighing cylinder and a stopper. Would be equivalent to 80% of the cylinder volume of water (20 ℃) was poured into a measuring cylinder, stoppered plug grinding mouth, the cylinder upside down 10 times, according to the above tilting operation Pour the contents of the third weighing cylinder and a stopper. 4.7.4 Calculation Mix well after pouring a sufficient amount of sample residue mass fraction of 3 residue mass (%) and after washing fraction 4 (%), respectively, according to the formula (4) and (5) Calculated. 100 (4) 100 (5) Where. 4.8 Determination of the amount of long-lasting foam 4.8.1 Method summary The sample was mixed with a predetermined amount of standard hard water, after standing foam volume recorded. 4.8.2 Reagents and solutions Standard hard water. ρ (Ca 2 ++ Mg2 +) = 342mg/L, pH = 6.0 ~ 7.0. According to GB/T 14825 preparation. 4.8.3 Instruments and Appliances Stoppered cylinder. 250mL (division value 2mL, 0 ~ 250mL tick 20cm ~ 21.5cm, 250mL scale line to the bottom plug 4cm ~ 6cm); Industrial scale. a sense of the amount of 0.1g. 4.8.4 measuring step The cylinder is added to 180mL standard hard water scale line at set cylinder on balance, weighed into the sample 1.0g (accurate to 0.1g), plus standard Hard water from the bottom of the cylinder to the mark at 9cm, the cover plug for the bottom of the cylinder as the center, upside down 30 times (2s). On trial Test bench standing 1min, record lather volume. 4.9 Thermal storage stability test According to GB/T 19136 in "liquid formulation" to. Thermal storage after prochloraz content should be not less than 95% before the thermal storage, other indicators should Meet the requirements of this standard is qualified. 4.10 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. 4.11 Product inspection and acceptance Product inspection and acceptance shall comply with GB/T 1604's. Treatment of extreme values, using the rounding value comparison method. 5 marking, labeling, packaging, storage and transportation 5.1 prochloraz water emulsion marking, labeling and packaging should comply with the provisions of GB 3796. 5.2 prochloraz water emulsion application PET bottle packaging, packaging boxes are available, corrugated cardboard boxes, bottle net content of 100g, 250g, 500g, 1000g, the net content of each box does not exceed 10kg. Also available upon request or order agreement, the use of other forms of packaging, but need to break The combined provisions of GB 3796. 5.3 prochloraz water emulsion 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. This product is a low toxicity fungicides. Are swallowed and inhaled toxic, it can penetrate through the skin. Wear protective goggles and rubber hand the FDA Jacket, wear the necessary protective clothing. After spraying wash with soap and water. Coverage should be immediately sent to hospital symptomatic treatment. 5.6 Warranty. under the specified storage conditions, warranties of prochloraz water emulsion, starting from the date of manufacture 2 years.

Appendix A

(Informative) The method of capillary gas chromatography mass fraction Prochloraz A. 1 Method summary Sample was dissolved in chloroform, diisooctyl phthalate esters as internal standard, using a HP-5 (5% phenyl methyl silicone) bonded quartz wool Fine column and flame ionization detector to sample prochloraz capillary gas chromatography and determination. A. 2 Reagents and solutions Chloroform; Prochloraz standard. a known mass fraction ≥98.0%; Phthalate Dioctyl. do not interfere with the analysis of impurities; Internal standard solution. Weigh 2.5g of di-iso-octyl phthalate in 500mL volumetric flask, dissolved in acetone, constant volume, shake. A. 3 Instrument Gas chromatograph. with flame ionization detector; Column. 30m × 0.32mm (i.d.) Quartz capillary column, wall bonded HP-5 (5% phenyl methyl silicone), film thickness 0.25μm; Chromatographic data processor or chromatography workstation. A. 4 GC operating conditions Temperature (℃). Room 235 column, the gasification chamber 260, detection chamber 280; Gas flow rate (mL/min). carrier gas (N2) 2.0, the compensation gas (N2) 25, hydrogen gas 40, air 400; Split ratio. 40.1; Injection volume. 1.0μL; Retention time. Prochloraz. about 11.8min, internal standard. about 7.3min. 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 gas chromatogram prochloraz water emulsion and the internal standard, see A. 1. 1 --- prochloraz; 2 --- internal standard. Figure A. 1 prochloraz water emulsion with the internal standard gas chromatograph A. 5 measuring step A. 5.1 preparation of standard solution Weigh prochloraz standard 0.1g (accurate to 0.0002g), placed in a glass bottle stuffed with a pipette 10mL internal standard solution, Shake well. A. 5.2 Sample preparation solution Weigh containing prochloraz 0.1g (accurate to 0.0002g) sample, placed in a glass bottle stopper, with the A. With 5.1 used A pipette internal standard solution 10mL, shake. A. 5.3 Determination Under the above chromatographic operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles prochloraz and internal standard After the change of the relative peak area ratio of less than 1.5%, according to the solution, the sample solution, the sample solution and standard sequence analysis of the standard solution Determination. A. 6 Calculation The two needle sample solution and measured before and after the two doses of the standard sample solution prochloraz and the internal standard peak area ratio of the average, respectively. Sample mass fraction PROCHLORAZ '1 (%), according to equation (A.1) to calculate the mass concentration ρ'1 (g/L), according to equation (A.2) Calculated. (A.1) ρ'1 = (A.2) Where. γ1 --- standard samples Prochloraz amines with the average peak area ratio of the internal standard solution; γ2 --- sample solution prochloraz and the average internal standard peak area ratio; Density ρ --- 20 ℃ when the sample in grams per milliliter (g/mL) (according to GB/T 4472 measured); --- Standard PROCHLORAZ mass fraction, expressed as a percentage. A. 7 allowable difference Prochloraz mass fraction two parallel determination results relative error should not exceed 2.5%, and the arithmetic mean as a measurement result. ......

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