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GB 28148-2011: [GB/T 28148-2011] Pyridaben emulsifiable concentrates
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[GB/T 28148-2011] Pyridaben emulsifiable concentrates
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Basic data
Standard ID: GB 28148-2011 (GB28148-2011)
Description (Translated English): [GB/T 28148-2011] Pyridaben emulsifiable concentrates
Sector / Industry: National Standard
Classification of Chinese Standard: G25
Classification of International Standard: 65.100.10
Word Count Estimation: 11,174
Date of Issue: 2011-12-30
Date of Implementation: 2012-04-15
Quoted Standard: GB/T 1600; GB/T 1601; GB/T 1603; GB/T 1604; GB/T 1605-2001; GB 4838; GB/T 6682-2008; GB/T 8170-2008; GB/T 19136; GB/T 19137
Regulation (derived from): Announcement of Newly Approved National Standards No. 23 of 2011
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 Pyridaben EC requirements, test methods and marking, labeling, packaging, storage and warranty. This standard applies to Pyridaben drugs and emulsifier dissolved in a suitable solvent in the preparation of Pyridaben EC.
GB 28148-2011: [GB/T 28148-2011] Pyridaben 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.
Pyridaben emulsifiable concentrates
ICS 65.100.10
G25
National Standards of People's Republic of China
Pyridaben EC
Issued on. 2011-12-30
2012-04-15 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 was drafted in accordance with GB/T 1.1-2009 given rules.
Please note that some content of this document may involve patents, the issuing authority of this document does not assume responsibility for the identification of these patents.
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 Co., Ltd.
It participated in the drafting of this standard. Jiangsu Suke Sheng Group Co., Ltd., Qingdao Otis biotechnology company.
The main drafters of this standard. Jiangmin Yi Wu tautology, Wang Haixia, Decipher, Lixue Chen.
Pyridaben EC
1 Scope
This standard specifies pyridaben EC requirements, test methods and marking, labeling, packaging, storage and warranty.
This standard applies to the pyridaben the original drug formulated with an emulsifier dissolved in a suitable solvent from the pyridaben EC.
Note. Other name, structural formula and basic physicochemical parameters pyridaben see Appendix A.
2 Normative references
The following documents for the application of this document is essential. For dated references, only the dated version suitable for use herein
Member. For undated references, the latest edition (including any amendments) applies to this document.
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 4838 EC pesticide packaging
GB/T 6682-2008 analytical laboratory use specifications and test methods (ISO 3696. 1987, MOD)
GB/T 8170-2008 revised value represents about rules and limit values and judgment
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 pyridaben the original drug formulated with an emulsifier dissolved in a suitable solvent, it should be stable homogeneous liquid, no
Visible suspended solids and sediments.
3.2 Technical Specifications
Pyridaben EC shall comply with the requirements of Table 1.
Table 1 pyridaben EC Control Project Index
project
index
15% 20%
Pyridaben mass fraction /% 15.0 20.0 1.2-1.2 1.0 to 1.0
Moisture content /% ≤ 0.5
pH range of 4.5 to 8.5
Table 1 (continued)
project
index
15% 20%
Emulsion stability (diluted 200 times) Qualified
Low temperature stability a qualified
Thermal storage stability of a qualified
When a normal production, heat storage stability test was measured at least once every three months.
Test Method 4
Safety Tips. Use of this standard shall have practical experience of laboratory personnel work. This standard does not point out all of the safety issues. Make
With those who have the responsibility to take appropriate safety and health practices and to ensure compliance with the relevant national regulations.
4.1 General provisions
This standard reagents and water in the absence of other requirements specified, refers to three analytical reagent and GB/T 6682-2008 specified in
water. Test results determined in accordance with GB/T 8170-2008 4.3.3 The "rounding value comparison method".
4.2 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 250mL.
4.3 Identification Test
Gas Chromatography --- The identification test can be carried out simultaneously with the determination of the mass fraction of pyridaben. Under the same chromatographic operating conditions, the test
A sample solution peak retention time compared with standard sample solution PYRIDABEN chromatographic retention time, the relative difference should be less than 1.5%.
Liquid chromatography --- The identification test can be carried out simultaneously with the determination of the mass fraction of pyridaben. Under the same chromatographic operating conditions, the test
A sample solution peak retention time compared with standard sample solution PYRIDABEN chromatographic retention time, the relative difference should be less than 1.5%.
4.4 Determination of the mass fraction of pyridaben
4.4.1 High performance liquid chromatography (Arbitration Act)
4.4.1.1 Method summary
Sample was dissolved in methanol, acetonitrile and water as the mobile phase, use as filler in Nova-PakC18 stainless steel column and UV detector
(240nm), the sample of PYRIDABEN high performance liquid chromatography and determination.
4.4.1.2 Reagents and solutions
Methanol;
Acetonitrile. chromatographic pure;
Water. The new secondary steam distilled water;
Pyridaben Sample. Known pyridaben mass fraction w≥99.0%.
4.4.1.3 Instruments
High performance liquid chromatography. a variable wavelength UV detector;
Chromatographic data processor or workstation;
Color 150mm × 3.9mm (id) stainless steel column, built-Nova-PakC18,5μm filler (or the equivalent effect. Column
The column);
Filter. filter pore size of about 0.45μm;
Micro injector. 50μL;
Quantitative sample line. 5μL;
Ultrasonic cleaner.
4.4.1.4 HPLC operating conditions
Mobile phase. Ψ (CH3CN.H2O) = 85.15;
Flow rate. 1.0mL/min;
Column temperature. room temperature (temperature change should not exceed 2 ℃);
Detection wavelength. 240nm;
Injection volume. 5μL;
Retention time. pyridaben about 5.6min.
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 pyridaben EC HPLC is shown in Figure 1.
1 --- pyridaben.
Figure 1 pyridaben EC HPLC diagram
4.4.1.5 Measurement procedure
4.4.1.5.1 Preparation of standard solution
Weigh 0.1g PYRIDABEN 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 the mark.
4.4.1.5.2 Preparation of sample solution
Weigh containing pyridaben 0.1g sample (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.
4.4.1.5.3 Determination
Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles PYRIDABEN Lingfeng area relative change
After less than 1.2%, according to the solution, the sample solution, the sample solution and standard sequence of the standard solution was measured.
4.4.1.6 Calculation
The two needle sample solution and measured before and after the two doses of the standard sample solution PYRIDABEN Lingfeng area were averaged. Sample PYRIDABEN
The mass fraction according to equation (1).
w1 = A2
· M1 · w
A1 · m2
(1)
Where.
w1 --- sample pyridaben mass fraction, expressed as a percentage;
A2 --- sample solution, pyridaben mean Lingfeng area;
m1 --- pyridaben standard mass in grams (g);
w --- pyridaben standard mass fraction, expressed as a percentage;
A1 --- standard solution, pyridaben mean Lingfeng area;
m2 --- sample mass, in grams (g).
4.4.1.7 allowable difference
Difference pyridaben mass fraction of two parallel determination results shall not be greater than 0.5%, the arithmetic mean value as a measurement result.
4.4.2 Capillary Gas Chromatography
4.4.2.1 Method summary
Sample was dissolved in chloroform, dicyclohexyl phthalate esters as internal standard, using a DB-1701 capillary column coated walls, and hydrogen
Flame ionization detector, sample the PYRIDABEN capillary gas chromatography and determination.
4.4.2.2 Reagents and solutions
Chloroform;
Pyridaben standard. a known mass fraction w≥99.0%;
Dicyclohexyl phthalate ester. not interfere with the analysis of impurities;
Internal standard solution. Weigh 5.0g dicyclohexyl phthalate esters into 500mL volumetric flask, dissolved with chloroform, constant volume,
Shake well.
4.4.2.3 Instruments
Gas chromatograph. with flame ionization detector;
Column. 30m × 0.32mm (id) quartz capillary column, wall coated with DB-1701, a film thickness of 0.25μm;
Chromatographic data processor or chromatography workstation.
4.4.2.4 GC operating conditions
Temperature (℃). Room 240 column, the gasification chamber 270, detection chamber 280;
Gas flow rate (mL/min). carrier gas (N2) 1.8, hydrogen gas 30, air 300, the compensation gas 25;
Split ratio. 40.1;
Injection volume. 2.0μL;
Retention time. pyridaben about 8.2min, internal standard about 5.0min.
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 pyridaben EC and the internal standard is shown in Figure 2.
1 --- internal standard;
2 --- pyridaben.
Figure 2 da gas chromatogram mites Ling EC and the internal standard
4.4.2.5 Measurement procedure
4.4.2.5.1 preparation of standard solution
Weigh pyridaben standard 0.05g (accurate to 0.0002g), placed in a glass bottle stuffed with a pipette 5mL internal standard solution,
Shake well.
4.4.2.5.2 preparation of the sample solution
Weigh containing pyridaben 0.05g sample (accurate to 0.0002g), placed in a glass bottle stopper, with the use and 4.4.2.5.1
With a pipette internal standard solution 5mL, shake.
4.4.2.5.3 Determination
Under the above chromatographic operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the peak two needles PYRIDABEN adjacent internal standard
Changes in the relative area ratio is less than 1.5%, according to the solution, the sample solution, the sample solution and standard sequence analysis of the standard solution was measured.
4.4.2.6 Calculation
The two needle sample solution and measured before and after the two doses of the standard sample solution PYRIDABEN and the internal standard peak area ratios are averaged.
Sample PYRIDABEN content according to formula (1 ') Calculated.
w'1 = r2 × m1 × wr1 × m2
(1')
Where.
w'1 --- sample PYRIDABEN mass fraction, expressed as a percentage;
r2 --- the average of the sample solution PYRIDABEN and the internal standard peak area ratio;
m1 --- standard mass in grams (g);
w --- standard samples pyridaben mass fraction, expressed as a percentage;
Mites and the average internal standard peak area ratio r1 --- standard solution clatter;
m2 --- sample mass, in grams (g).
4.4.2.7 allowable difference
The difference between two parallel determination results shall not be greater than 0.5%, the arithmetic mean value as a measurement result.
4.5 Determination of moisture content
According to GB/T 1600 the "Karl Fischer method".
Determination of 4.6 pH value
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, no oil slick measuring cylinder (cream), and precipitation of heavy oil
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. After the thermal storage, pyridaben mass fraction of not less than the average content measured before the heat storage
97%; emulsion stability should meet the standard requirements.
4.10 Product inspection and acceptance
Shall comply with GB/T 1604's.
5 marking, labeling, packaging, storage, security, guarantee
5.1 marking, labeling, packaging
Pyridaben EC marking, labeling and packaging should comply with the provisions of GB 4838. Pyridaben EC application of clean, dry glass or
PET bottle packaging, bottle net content of 250mL (g), 100mL (g), external corrugated packaging, each box weighing no more than 10kg. also may
According to user requirements or the order agreement, the use of other forms of packaging, subject to the provisions of GB 4838.
5.2 Storage
Pyridaben EC packages should be stored in ventilated, dry warehouse; storage and transportation to prevent moisture and sunlight, no food, seed, feed
Mix, avoid contact with skin, eyes, mouth and nose to prevent inhalation.
5.3 Security
This product is moderately toxic mites, pesticides, are swallowed and inhaled toxic, can penetrate through the skin. Wear protective goggles and rubber the FDA
Leather gloves to wear the necessary protective clothing. After application, immediately wash with soap and water. Such as skin, eyes accidentally stained the product immediately with large
The amount of rinse. Coverage should be immediately sent to hospital symptomatic treatment.
5.4 Warranty Period
Under the provisions of storage and transportation conditions, the guarantee period pyridaben EC, two years from date of manufacture.
Appendix A
(Informative)
Pyridaben other name, structural formula and basic physicochemical parameters
This product is an active ingredient pyridaben other name, structural formula and basic physicochemical parameters are as follows.
ISO common name. Pyridaben
CAS Registry Number. 96489-71-3
CIPAC Numeric Code. 583
Chemical name. 2-tert-butyl-5- (4-tert-butyl-benzyl) -4-chloro -3 (2H) - pyridazinone
Structure.
Empirical formula. C19H25ClN2OS
Molecular Weight. 364.9
Biological activity. acaricidal, insecticidal
Melting point. about 111 ℃ ~ 112 ℃
Vapor Pressure. < 0.25mPa (20 ℃)
Solubility (20 ℃, g/L). water, 1.2 × 10-5, 460 acetone, benzene, 110, 320 cyclohexane, 57 ethanol, n-octane 63, hexanes 10,
Xylene 390
Stability. aqueous solution pH4 ~ pH9 and most organic solvents stable, 50 ℃ storage stable for three months under normal storage conditions
At least two years is stable, unstable to light.
1102-
Rights Proprietary Rights Reserved
ISBN. 155 066 · 1-44691
......
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