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GB 22604-2008: [GB/T 22604-2008] Tebuconazole emulsion, oil in water
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[GB/T 22604-2008] Tebuconazole emulsion, oil in water
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GB 22604-2008
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Basic data | Standard ID | GB 22604-2008 (GB22604-2008) | | Description (Translated English) | [GB/T 22604-2008] Tebuconazole emulsion, oil in water | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Classification of International Standard | 65.100.30 | | Word Count Estimation | 9,987 | | Date of Issue | 2008-12-17 | | Date of Implementation | 2009-06-01 | | Adopted Standard | FAO 494/FW/S/F-2000, NEQ | | 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 EW requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to the original drug tebuconazole formulated with suitable additives tebuconazole water emulsions. | GB 22604-2008: [GB/T 22604-2008] Tebuconazole 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.
Tebuconazole emulsion, oil in water
ICS 65.100.30
G25
National Standards of People's Republic of China
Tebuconazole EW
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.
This standard FAO specification 494/FW/S/F (2000) "Tebuconazoleemulsion, oilinwater" degree of non-conformity
Equivalent.
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. Shenzhen Knopp letter Agrochemical Co., Ltd., Shandong Huayang Technology Co., Ltd., Jiangsu dragon chemistry
Ltd., Qingdao Kai Yuen Cheung Chemical Co., Ltd.
The main drafters of this standard. Jiangmin Yi, Li Xiujie, Li Ou Yan, Song Dongsheng, of cloud point, Lixue Chen.
Tebuconazole EW
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 EW requirements, test methods and marking, labeling, packaging, storage and transportation.
This standard applies to Tebuconazole original drug with suitable additives formulated tebuconazole water emulsions.
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 Tebuconazole original drug with suitable additives formulated, it should be a stable liquid, long after Yun
Xu small amount of layering, slight shaking or agitation should be uniform.
3.2 tebuconazole water emulsion should meet the requirements of Table 1.
Table 1 tebuconazole EW quality control program indicators
project
index
250g/L 12.5%
Tebuconazole mass fraction a /%
Or concentration (20 ℃) / (g/L)
25.0 + 1.5-1.5
+ 15-15 250
12.5 + 0.6-0.6
a pH range of 4.5 to 8.0
Pourability
After pouring the residue /% ≤ 3.0
After washing the residue /% ≤ 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, 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 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 equally effective 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. 5L;
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 EW HPLC is shown in Figure 1.
1 --- tebuconazole.
Figure 1 tebuconazole water emulsion by high performance liquid chromatogram
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) to calculate the mass concentration ρ1 according to formula (2).
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 water emulsion with an internal standard gas chromatography is shown in Figure 2.
1 --- tebuconazole;
2 --- internal standard.
Figure 2 tebuconazole water emulsion with an internal standard gas chromatograph
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 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
(4) Calculation of fractional 1 '(%), according to equation (3) Calculate the mass concentration ρ1' according to the formula.
(3)
ρ1 '=
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.
According to GB/T 1601 carried out.
4.5 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.
4.6 Determination of dumping
4.6.1 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.
4.6.2 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).
4.6.3 Test procedure
A sufficient sample size to fully shake, some of which have been promptly placed weighed measuring cylinder (including plug), attached to the cylinder of 8/10
At the mill plugged gag, placed 24h. The tap is opened, the upright position of the rotating cylinder by a 135-degree angle dumped 60s, then invert 60s, again called
The amount of the 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.
4.6.4 Calculation
The residue was dumped after the sample 3 (%) and the residue washed 4 (%), respectively, according to equation (5) and (6) Calculated.
100 (5)
100 (6)
Where.
4.7 Determination of the amount of long-lasting foam
4.7.1 Method summary
The sample was mixed with a predetermined amount of standard hard water, after standing foam volume recorded.
4.7.2 Reagents and solutions
Standard hard water. ρ (Ca
2 ++ Mg2 +) = 342mg/L, pH = 6.0 ~ 7.0. According to GB/T 14825 preparation.
4.7.3 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.
4.7.4 measuring step
Added 180mL graduated cylinder standard hard water, 1.0g sample was weighed into a graduated cylinder (accurate to 0.1g), added to standard hard water from the cylinder
Plug at the bottom tick 9cm, the cover plug to the bottom of the cylinder as the center, upside down 30 times (2s). Stand on the test stand
1min, record lather volume.
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 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.
4.10 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 tebuconazole EW logo, labeling and packaging should comply with the provisions of GB 3796.
5.2 tebuconazole EW application or polyester glass bottles, cardboard packaging available, corrugated cardboard boxes, bottle net weight 100g,
250g, 100mL, 200mL, each box of net weight does not exceed 15kg. Also available upon request or order agreement, the use of other forms of
Packaging, subject to the provisions of GB 3796.
5.3 tebuconazole EW 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
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, warranties of tebuconazole water emulsions, starting from the date of manufacture 2 years.
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