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GB 22605-2008: [GB/T 22605-2008] Tebuconazole emulsifiable concentrates
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[GB/T 22605-2008] Tebuconazole emulsifiable concentrates
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GB 22605-2008
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Basic data | Standard ID | GB 22605-2008 (GB22605-2008) | | Description (Translated English) | [GB/T 22605-2008] Tebuconazole emulsifiable concentrates | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Classification of International Standard | 65.100.30 | | Word Count Estimation | 9,940 | | 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 the tebuconazole EC requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to the original drug with tebuconazole emulsifier dissolved in a suitable solvent in the preparation of tebuconazole EC. | GB 22605-2008: [GB/T 22605-2008] Tebuconazole 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.
Tebuconazole emulsifiable concentrates
ICS 65.100.30
G25
National Standards of People's Republic of China
Tebuconazole 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.
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. Pesticide Co., Ltd. Jiangsu Feng Deng, Jiangsu dragon Chemical Co., Ltd. Jiang Su Qizhou green chemical shares have
Ltd., Shandong Huayang Technology Co., Ltd.
The main drafters of this standard. Jiangmin Yi, Li Xiujie, Gengrong Wei, of cloud point, Hu Chunhong, Bing-Wen.
Tebuconazole EC
The product is an active ingredient tebuconazole pent other name, structural formula and basic physicochemical parameters are as follows.
ISO common name. Tebuconazole
CAS Registry Number. 107534-96-3
CIPAC Numeric Code. 494
Chemical Name. (RS) -1- (4- chlorophenyl) -4,4-dimethyl -3- (1H-1,2,4- triazol-1-ylmethyl) pentan-3-ol
Structure.
Empirical formula. C16H22ClN3O
Molecular Weight. 307.8 (according to 2007 international relative atomic mass)
Biological activity. bactericidal
Melting point. about 102.4 ℃
Vapor pressure (20 ℃). 0.013mPa
Solubility (20 ℃). water 32mg/L; dichloromethane greater than 200g/L; hexane of less than 0.1g/L; isopropanol, toluene, 50g/L ~
100g/L
Stability. at pH 4 ~ 9,22 ℃ hydrolysis DT50 is greater than 1 year.
1 Scope
This standard specifies the tebuconazole EC requirements, test methods and marking, labeling, packaging, storage and transportation.
This standard applies to Tebuconazole original drug formulated with an emulsifier dissolved in a suitable solvent from the tebuconazole 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
Determination of GB/T 1603 pesticide emulsion stability
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 Tebuconazole original drug formulated with an emulsifier dissolved in a suitable solvent, should be stable
Homogeneous liquid without visible suspended matter and sediment.
3.2 tebuconazole EC shall comply with the requirements of Table 1.
Table 1 tebuconazole EC quality control program indicators
Item Index
Tebuconazole mass fraction a /%
Or concentration (20 ℃) / (g/L)
25.0 + 1.5-1.5
+ 15-15 250
Moisture content /% ≤ 1.0
pH range of 6.0 to 9.0
Emulsion stability (200 times) Qualified
Low temperature stability test b qualified
Thermal storage stability test b qualified
When a dispute occurs when mass to the mass fraction of arbitration.
Thermal storage stability test when b normal production, low-temperature stability measured at least once every three months.
Test Method 4
4.1 Sampling
According to GB/T 1605-2001 5.3.2 in "liquid formulations sampling" approach. Determining sample package using a random number table method; final
Sample size should be less than 100g.
4.2 Identification Test
Liquid chromatography --- The identification test can be carried out simultaneously with the determination of the mass fraction of tebuconazole. Under the same chromatographic operating conditions, the test
The retention time of the sample solution and the standard solution to a peak of tebuconazole chromatographic retention time, the relative difference should be 1.5%
Fewer.
4.3 tebuconazole mass fraction (mass concentration) Determination
4.3.1 High performance liquid chromatography (Arbitration Act)
4.3.1.1 Method summary
Sample was dissolved in methanol, methanol + water as the mobile phase, use as filler in Nova-PakC18 stainless steel column and UV detector
(220nm), the sample of tebuconazole high performance liquid chromatography and determination.
4.3.1.2 Reagents and solutions
Methanol;
Water. The new secondary steam distilled water;
Tebuconazole Sample. Known tebuconazole mass fraction ≥99.0%.
4.3.1.3 Instruments
High performance liquid chromatography. a variable wavelength UV detector;
Chromatographic data processor;
Column. 150mm × 3.9mm (. I.d) stainless steel column, built-Nova-PakC185μm filler (or equivalent effect Chromatography
column);
Filter. filter pore size of about 0.45μm;
Micro injector. 50μL;
Quantitative sample line. 5μL;
Ultrasonic cleaner.
4.3.1.4 HPLC operating conditions
Mobile phase. ψ (CH3OH.H2O) = 65.35;
Flow rate. 1.0mL/min;
Column temperature. room temperature (temperature change should not exceed 2 ℃);
Detection wavelength. 220nm;
Injection volume. 5μL;
Retention time. tebuconazole about 7.0min.
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 tebuconazole EC HPLC is shown in Figure 1.
1 --- tebuconazole.
Figure 1 tebuconazole EC HPLC diagram
4.3.1.5 Measurement procedure
4.3.1.5.1 Preparation of standard solution
Weigh 0.1g tebuconazole standard (accurate to 0.0002g), a 50mL volumetric flask, dilute to the mark with methanol, ultrasonic oscillation
5min make sample dissolution, cooled to room temperature and shake well. Using a pipette to take the above solution 5mL to 50mL volumetric flask, diluted with methanol to
Mark and shake.
4.3.1.5.2 Preparation of sample solution
Weigh 0.1g sample containing tebuconazole of (accurate to 0.0002g), a 50mL volumetric flask, dilute to the mark with methanol, ultrasonic
Oscillation 5min make sample dissolution, cooled to room temperature and shake well. Using a pipette to take the above solution 5mL to 50mL volumetric flask with methanol
Dilute to the mark.
4.3.1.5.3 Determination
Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles tebuconazole peak area relative change
After less than 1.5%, according to the solution, sample solution, sample solution, standard order of standard solution was measured.
4.3.1.5.4 Calculation
The two doses of the standard solution was measured before and after the two needles in the sample solution and tebuconazole peak areas are averaged. Sample quality tebuconazole
1 volume fraction (%), according to equation (1) calculation; (2) to calculate the concentration of ρ1 (g/L), according to the formula.
1 =
(1)
ρ1 =
× 10 (2)
Where.
A1 --- the standard solution, the average tebuconazole peak area;
The A2 --- sample solution, alcohol tebuconazole average peak area;
Density ρ --- 20 ℃ when the sample in grams per milliliter (g/mL) (according to GB/T 4472 measured);
--- Tebuconazole standard mass fraction, expressed as a percentage.
4.3.1.6 allowable difference
Determination of the mass fraction of tebuconazole two parallel result of the difference should be not more than 0.5%, the arithmetic mean value as a measurement result.
4.3.2 Capillary Gas Chromatography
4.3.2.1 Method summary
Sample was dissolved in chloroform, dicyclohexyl phthalate esters as internal standard, using a HP-5 (5% phenyl methyl silicone) coated quartz wool wall
Fine column, and a flame ionization detector, the sample of tebuconazole capillary gas chromatography and determination.
4.3.2.2 Reagents and solutions
Chloroform;
Tebuconazole standard. a known mass fraction ≥99.0%;
Dicyclohexyl phthalate ester. not interfere with the analysis of impurities;
Internal standard solution. Weigh 2.0g dicyclohexyl phthalate esters in 500mL volumetric flask, dissolved with chloroform, constant volume,
Shake well.
4.3.2.3 Instruments
Gas chromatograph. with flame ionization detector;
Column. 30m × 0.32mm (. I.d) quartz capillary column, wall coated HP-5 (5% phenyl methyl silicone), film thickness 0.25μm;
Chromatographic data processor or chromatography workstation.
4.3.2.4 GC operating conditions
Temperature (℃). Room 220 column, the gasification chamber 260, detection chamber 280;
Gas flow rate (mL/min). carrier gas (N2) 1.8, hydrogen gas 40, air 400, the compensation gas 25;
Split ratio. 40.1;
Injection volume. 1.0μL;
Retention time. tebuconazole about 7.5min, internal standard about 10.4min.
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. Typical tebuconazole EC and internal standard gas chromatography is shown in Figure 2.
1 --- tebuconazole;
2 --- internal standard.
Figure 2 Gas chromatogram tebuconazole EC and the internal standard
4.3.2.5 Measurement procedure
4.3.2.5.1 preparation of standard solution
Weigh tebuconazole standard 0.05g (accurate to 0.0002g), placed in a glass bottle stopper, with a pipette accurate internal standard was added 10mL
Solution, shake.
4.3.2.5.2 preparation of the sample solution
Weigh the sample containing tebuconazole 0.05g of (accurate to 0.0002g), placed in a glass bottle stopper, with the use and 4.3.2.5.1
With a pipette accurately added internal standard solution 10mL, shake.
4.3.2.5.3 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 tebuconazole 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.
4.3.2.5.4 Calculation
The two needle sample solution and measured before and after the two doses of the standard sample solution tebuconazole and the internal standard peak area ratio of the average, respectively.
(3) calculate the sample mass fraction of tebuconazole '1 (%), according to the type, concentration ρ'1 (g/L), according to equation (4) Calculated.
'1 =
(3)
ρ'1 =
× 10 (4)
Where.
Density ρ --- 20 ℃ when the sample in grams per milliliter (g/mL) (according to GB/T 4472 measured);
--- Standard samples tebuconazole mass fraction, expressed as a percentage.
4.3.2.6 allowable difference
The difference between two parallel determination results shall not be greater than 0.5%, the arithmetic mean value as a measurement 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
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. After the heat storage tebuconazole content should not be less than the reservoir before the mass fraction of tebuconazole
97% emulsion stability should meet the standard requirements.
4.9 product testing 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 tebuconazole EC marking, labeling and packaging should comply with the provisions of GB 4838.
5.2 tebuconazole EC application or polyester glass bottles, cardboard packaging available, corrugated cardboard boxes, bottle net content of 100g, 200g,
100mL, 200mL, each box of net content not more than 15kg. Also available upon request or order agreement, the use of other forms of packaging,
Subject to the provisions of GB 4838.
5.3 tebuconazole EC packages 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
Pull 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, tebuconazole EC guarantee period, from the date of manufacture for 2 years.
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