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GB 22624-2008 English PDF

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GB 22624-2008: [GB/T 22624-2008] Prochloraz emulsifiable concentrates
Status: Obsolete
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GB 22624-2008479 Add to Cart 3 days [GB/T 22624-2008] Prochloraz emulsifiable concentrates Obsolete

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Basic data

Standard ID: GB 22624-2008 (GB22624-2008)
Description (Translated English): [GB/T 22624-2008] Prochloraz emulsifiable concentrates
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 EC requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to prochloraz original drug is dissolved in a suitable solvent and emulsifier in the preparation of prochloraz EC.

GB 22624-2008: [GB/T 22624-2008] Prochloraz 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.
Prochloraz emulsifiable concentrates ICS 65.100.30 G25 National Standards of People's Republic of China Prochloraz EC 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 Corporation, Chlorpyrifos Chemical Co., Ltd., Qingdao Otis biotechnology company. The main drafters of this standard. Hou Chunqing, Wu Tiejun, Liukui Tao, Wang Zhimin, Chen was new, Liugui Juan, Duan win. Prochloraz EC 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 EC requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to the prochloraz original drug and preparation of the emulsifier is dissolved in a suitable solvent prochloraz 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 prochloraz original drug is made into a stable homogeneous liquid, free from visible suspended matter and sediment. 3.2 Technical Specifications Prochloraz EC shall comply with the requirements of Table 1. Table 1 Prochloraz EC Control Project Index 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 2.1-2.1 42.0 + - - + 22-22 450 2,4,6-trichlorophenol mass fraction b /% ≤ 0.2 0.3 Moisture content /% ≤ 0.5 a pH range of 5.5 to 8.5 Emulsion stability (diluted 200 times) Qualified Low temperature stability Qualified b Thermal storage stability b qualified When a dispute occurs when mass to the mass fraction of arbitration. B when normal production of 2,4,6-trichlorophenol, 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. 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 mass fraction of prochloraz. In the same chromatographic operating conditions , The sample solution to a chromatographic retention time of the 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 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. 4.3.4 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 EC HPLC is shown in Figure 1. 1 --- prochloraz. Figure 1 Prochloraz EC HPLC diagram 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 The two needle sample solution and measured before and after the two doses of the standard sample solution PROCHLORAZ peak areas are averaged. Sample PROCHLORAZ The mass fraction of 1 (%), according to equation (1) calculation; (2) to calculate the concentration of ρ1 (g/L), according to the formula. 1 = A2 (1) ρ1 = (2) Where. A1 --- the average standard solution PROCHLORAZ peak area; 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 EC 2,4,6-trichlorophenol measured by HPLC is shown in Figure 2. 1 --- 2,4,6-trichlorophenol; 2 --- prochloraz. Figure 2 prochloraz EC 2,4,6-trichlorophenol 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 of 2,4,6-trichlorophenol mean peak area; --- The A2 in the sample solution of 2,4,6-trichlorophenol average peak area; --- 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. 4.5 Determination of Moisture According to GB/T 1600 the "Karl Fischer method". According to GB/T 1601 carried out. 4.7 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. 4.8 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. 4.9 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 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 Prochloraz EC marking, labeling, packaging, should meet the requirements of GB 4838. Prochloraz EC brown glass bottle with an application within the plug and the outer cover, aluminum bottles or fluorinated bottle, bottle net weight 150g (mL), 300g (mL), 500g (mL); overpack Plastic boxes or corrugated boxes, each box of net weight shall not exceed 15kg. Also available upon request Order or agreement, other forms of packaging may be used, subject to the provisions of GB 4838. 5.2 Prochloraz EC packages should be stored in well-ventilated, dry coffers. 5.3 storage, prevent moisture and sunlight, no food, seed, feed mix, avoid contact with skin, eyes, mouth and nose to prevent inhalation. 5.4 Safety. 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 Pull the necessary protective clothing. After spraying wash with soap and water. Coverage should be immediately sent to hospital symptomatic treatment. 5.5 Warranty. under the specified storage conditions, Prochloraz EC guarantee period, from date of manufacture for 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 silica Capillary column and a flame ionization detector, the sample of 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.) fused silica capillary column, the inner wall of the bonding HP-5 (5% phenyl methyl silicone), a 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 EC and the internal standard, see A. 1. 1 --- prochloraz; 2 --- internal standard. Figure A. GC 1 Prochloraz EC and the internal standard 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. PROCHLORAZ sample mass fraction of 1 '(%), according to equation (A.1) to calculate the mass concentration ρ1' (g/L), according to equation (A.2) Calculated. 1 '= γ2 (A.1) ρ1 '= (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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