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GB 23551-2009: [GB/T 23551-2009] Clomazone emulsifiable concentrates
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[GB/T 23551-2009] Clomazone emulsifiable concentrates
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GB 23551-2009
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Basic data | Standard ID | GB 23551-2009 (GB23551-2009) | | Description (Translated English) | [GB/T 23551-2009] Clomazone emulsifiable concentrates | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Classification of International Standard | 65.100.20 | | Word Count Estimation | 12,128 | | Date of Issue | 2009-04-27 | | Date of Implementation | 2009-11-01 | | Regulation (derived from) | Announcement of Newly Approved National Standards No. 5, 2009 (No. 145 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 clomazone EC requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to Clomazone Matsubara drugs and emulsifier dissolved in a suitable solvent mixture of the clomazone EC. | GB 23551-2009: [GB/T 23551-2009] Clomazone 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.
Clomazone emulsificable concentrates
ICS 65.100.20
G25
National Standards of People's Republic of China
EC loose grass
Posted 2009-04-27
2009-11-01 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 are 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. Jiangsu Changqing Agrochemical Co., Ltd., Jiangsu dragon Chemical Co., Ltd., Dalian Songliao Chemical Co.
the company.
The main drafters of this standard. Hou Chunqing, Zan Yan Kun, Jerry Hong, of cloud point, Miao innovation.
EC loose grass
Other name, structural formula and basic physicochemical parameters of the active ingredients of the product are as follows.
a) Yi Cao Song
ISO common name. clomazone
CIPAC Numeric Code. 509
Chemical name. 2- (2-chlorobenzyl) -4,4-dimethyl-3-isobutyl ketone
Structure.
Empirical formula. C12H14ClNO2
Molecular Weight. 239.7 (according to 2005 international relative atomic mass)
Biological activity. weeding
Vapor pressure (25 ℃). 19.2mPa
Boiling point. 275.4 ℃
Melting point. 25 ℃
Solubility (20 ℃). water 1.1g/L, soluble in acetone, acetonitrile, chloroform, cyclohexanone, methylene chloride, methanol, toluene, n-hexane, di
Dimethylformamide
Stability. stable for at least 2 years at room temperature at 50 ℃ stable for at least 3 months, the sunlight, the aqueous solution is greater than 30d DT50
b) Azone
English name. Azone
Chemical Name. 1-n-dodecylazacycloheptan-2-one
Structure.
Empirical formula. C18H35NO
Molecular weight. 281.48 (according to 2001 international relative atomic mass)
Solubility. easily soluble in ethanol, acetone, hexane, chloroform, diethyl ether; practically insoluble in water
1 Scope
This standard specifies the different
Grass pine EC requirements, test methods and marking, labeling, packaging, storage and transportation.
This standard applies to the different
Grass Matsubara drugs and preparation of the emulsifier is dissolved in a suitable solvent iso
EC loose grass.
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
GB/T 1601 Pesticides pH value measurement method
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
Determination of GB/T 4472 chemical product density, relative density
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 meet the standards of different
Grass Matsubara drugs made of a stable homogeneous liquid, free from visible suspended matter and sediment.
3.2 Technical Specifications
Grass pine EC should be consistent with Table 1 requirements.
Table 1 Song Yi Cao EC Control Project Index
project
index
480g/L 360g/L
Grass loose concentration (20 ℃) / (g/L)
Or mass fraction of a /%
+ 24-24 480
45.0 + 2.2-2.2
+ 18-18 360
35.0 + 1.7-1.7
Penetrant (Azone) mass fraction b /% ≥ - 2.0
Penetration time/s ≤ - 150
Moisture /% ≤ 0.5
pH range of 5.0 to 8.0
Emulsion stability (diluted 200 times) Qualified
Low temperature stability Qualified c
Thermal storage stability c qualified
When a dispute occurs when mass to the mass fraction of arbitration.
b allow additional penetrant, penetrant other detection methods and its corresponding index requirements in the National Standardization Technical Committee Pesticide obtained.
Thermal storage stability test when c normal production, low-temperature stability measured 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
--- The High Performance Liquid Chromatography with different identification test
Determination of the mass fraction of loose grass simultaneously. In the same chromatographic operating conditions
, The retention time of the standard solution and the sample solution to a chromatographic peaks iso
Grass pine peak retention time, the relative difference should be 1.5%
Fewer.
4.3 Determination of the mass concentration of pine and grass (mass fraction)
4.3.1 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
236nm wavelength, the sample of the different grass pine reverse phase HPLC separation and determination of external standard.
4.3.2 Reagents and solutions
Methanol. HPLC grade;
Acetonitrile. HPLC grade;
Water. The new secondary steam distilled water;
Grass Song Sample. 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 color
The 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. φ (acetonitrile. water) = 50.50, by membrane filtration, and degassing;
Flow rate. 1.0mL/min;
Column temperature. room temperature (temperature change should not exceed 2 ℃);
Detection wavelength. 236nm;
Injection volume. 5μL;
Retention time. iso
Grass pine 11.0min.
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 differences
EC loose grass HPLC is shown in Figure 1.
1 --- Yi Cao loose.
1 Yi Cao Song EC HPLC diagram
4.3.5 measuring step
4.3.5.1 Preparation of standard solution
Weigh 0.2g (accurate to 0.0002g) and grass loose standard in 50mL volumetric flask, dissolved in methanol and diluted to the mark.
Using a pipette to take the above solution 10mL in 50mL volumetric flask, diluted with methanol to the mark.
4.3.5.2 Preparation of sample solution
Weigh Iso
Grass pine 0.2g (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 iso
Peak area becomes relatively loose grass
After less than 1.2% of the solution in accordance with the sample solution, the sample solution and standard sequence of the standard solution was measured.
4.3.6 Calculation
The measured before and after the two-needle sample solution and sample two different doses of the standard solution
Grass Pine Peak area were averaged. Sample different
Grass loose mass fraction of 1 (%) according to equation (1) calculation; (2) to calculate the concentration of ρ1 (g/L) by the formula.
1 = A2
(1)
ρ1 =
10 (2)
Where.
A1 --- the average standard solution and grass Pine Peak area;
A2 --- sample solution and grass Pine mean peak area;
Density ρ --- 20 ℃ when the sample in grams per milliliter (g/mL) (according to GB/T 4472 measured);
--- Yi Cao Song Sample mass fraction, expressed as a percentage.
4.3.7 allowable difference
The measurement results grass loose mass fraction of the difference between the two parallel should not exceed 0.8%, and the arithmetic mean as a measurement result.
4.4 Determination of the mass fraction of nitrogen-one
4.4.1 Method summary
Sample was dissolved in acetonitrile to acetonitrile + water as the mobile phase, to use as filler HypersilGOLDC18 stainless steel column and UV detection
It is, at a wavelength of 210nm on the sample under nitrogen ketone HPLC separation and determination, external standard.
4.4.2 Reagents and solutions
Acetonitrile. chromatographic pure;
Water. freshly distilled twice-distilled water by membrane filtration;
Azone standard. a known mass fraction ≥99.0%.
4.4.3 Instruments
High performance liquid chromatography. a variable wavelength UV detector;
Chromatography data workstations;
Column. 150mm × 4.6mm (i.d.) Stainless steel column. The filler is HypersilGOLDC18, particle diameter of 5 m;
Micro injector. 50μL;
Filter. filter pore size of 0.45μm.
4.4.4 HPLC operating conditions
Mobile phase. φ (acetonitrile. water) = 90.10, by membrane filtration, and degassing;
Flow rate. 1.0mL/min;
Column temperature. room temperature;
Detection wavelength. 210nm;
Injection volume. 10μL;
Retention time. Azone 6.2min.
Above are typical operating parameters can be given operating parameters adjusted as appropriate depending on the characteristics of the instrument, in order to obtain the best results. Texts
Type of 360g/L EC in pine and grass Azone HPLC is shown in Figure 2.
1 --- azone.
Figure 2 Yi Cao Song EC Azone determined by high performance liquid chromatogram
4.4.5 measuring step
4.4.5.1 preparation of standard solution
Weigh Azone standard 0.02g (accurate to 0.0002g), placed in 100mL flask, add acetonitrile dissolved and diluted to the mark with the mobile phase
Degree, shake.
4.4.5.2 preparation of the sample solution
Weigh the sample 1g (accurate to 0.0002g), placed in 100mL flask, add acetonitrile dissolved in mobile phase and dilute to the mark.
4.4.5.3 Determination
Under these operating conditions, the instrument until a stable baseline, the number of continuous injection doses of the standard solution, calculate the response of the needle, two needles to be adjacent ring
Relative change value should be less than 1.0%, according to the solution, the sample solution, the sample solution and standard sequence of the standard solution was measured.
4.4.6 Calculation
The peak area was measured before and after the two-needle sample solution and two doses of the standard sample solution Azone are averaged for sample quality Azone
2 volume fraction (%), according to equation (3) Calculated.
2 = A2
(3)
Where.
A1 --- Azone mean standard peak area;
The average value A2 --- sample Azone peak area;
--- Azone standard mass fraction, expressed as a percentage.
4.4.7 allowable difference
Results of two parallel determination of nitrogen content of ketone relative deviation should not exceed 10% of the arithmetic mean value as a measurement result.
4.5 Determination of the penetration time
4.5.1 Instruments
Beaker.200mL;
Pipette. 2mL;
Straight cylinder. 100mL;
Thermometer. 0 ℃ ~ 100 ℃;
Constant temperature water bath. 25 ℃ ± 2 ℃;
Cotton cloth. 21 × 21 3 shares 3 shares fine canvas, wafers having a diameter of 30.0mm spare.
4.5.2 measuring step
With pipette sample 0.4mL, the sample was slowly dropped into a beaker filled with distilled water of 200mL, stir gently with a glass rod.
The beaker was placed in a water bath to keep the temperature of the solution in the beaker at 25 ℃ ± 2 ℃. Beaker until the solution surface of the foam disappears and canvas circle
Sheet placed on the rear surface of the solution, use a stopwatch, canvas discs until settle to the bottom of the beaker, records from flat to settle to the bottom of the canvas used
Time (in seconds). Repeat the test more than 10 times, and the arithmetic mean of the difference between the 20s and the average of the above data rounding, and then averaged
Value, that is, penetration time.
4.5.3 Calculation
(4)
Where.
--- Like the number of measurement samples.
4.6 Determination of Moisture
According to GB/T 1600 the "Karl Fischer method".
According to GB/T 1601 carried out.
4.8 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.
4.9 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 Thermal storage stability test
According to GB/T 19136 in "liquid formulation" to. After the heat storage and grass pine content shall not be less than 97% before the heat storage, emulsion stability should
Meet the requirements of this standard is qualified.
4.11 Product inspection and acceptance
Shall comply with GB/T 1604's. Limit the use of numerical treatment rounding value comparison method.
5 marking, labeling, packaging, storage and transportation
5.1 Yi Cao Song EC marking, labeling and packaging should comply with the provisions of GB 4838.
Song Yi Cao EC 5.2 Application of glass or plastic PET bottle packaging, bottle net content of 500g or 1000g; each box weighing 10kg, or
12kg. Also available upon request or order agreement other forms of packaging, subject to the provisions of GB 4838.
5.3 Yi Cao Song 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-toxic pesticides. Are swallowed and inhaled toxic, it can penetrate through the skin. Wear protective goggles and rubber gloves when using this product
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 specified conditions of storage, Yi Cao Song EC guarantee period, from date of manufacture for 2 years.
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