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GB 22177-2008: [GB/T 22177-2008] Pendimethalin technical
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[GB/T 22177-2008] Pendimethalin technical
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GB 22177-2008
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Basic data | Standard ID | GB 22177-2008 (GB22177-2008) | | Description (Translated English) | [GB/T 22177-2008] Pendimethalin technical | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Classification of International Standard | 65.100.20 | | Word Count Estimation | 8,851 | | Date of Issue | 2008-07-11 | | Date of Implementation | 2009-01-01 | | Quoted Standard | GB/T 1600; GB/T 1601; GB/T 1604; GB/T 1605-2001; GB/T 3976; GB/T 19138 | | Regulation (derived from) | Announcement of Newly Approved National Standards No. 12 of 2008 (No. 125 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 original drug pendimethalin requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to the production of pendimethalin and impurities resulting from the composition of pendimethalin original drug. | GB 22177-2008: [GB/T 22177-2008] Pendimethalin technical---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.
Pendimethalin technical
ICS 65.100.20
G25
National Standards of People's Republic of China
Pendimethalin drug
Posted 2008-07-11
2009-01-01 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 (CSBTC/T C133) centralized.
This standard is drafted by. Shenyang Chemical Research Institute.
Participated in the drafting of this standard. Shandong Huayang Technology Co., Ltd., Jiangsu Chemical Co., Ltd. dragon.
The main drafters of this standard. Pi-Long, Hou Chunqing, Zhufeng Xia, of cloud point, Li Peng.
The standard commission Secretariat of National Pesticide Standardisation Technical Committee responsible for the interpretation.
Pendimethalin drug
Other name, structural formula and basic physicochemical parameters of the product active ingredients pendimethalin as follows.
ISO common name. pendimethalin
CIPAC digital code. 357
Chemical name. N- (1- ethylpropyl) -2,6-dinitro-3,4-dimethylaniline
Structure.
Empirical formula. C13H19N3O4
Molecular Weight. 281.3 (according to 2005 international relative atomic mass)
Biological activity. weeding
Melting point. 54 ℃ ~ 58 ℃
Vapor pressure (25 ℃). 4.0 × 10-3Pa
Solubility (26 ℃, g/L). Water 3.0 × 10-4 (20 ℃), acetone 700, 148 corn oil, isopropyl alcohol, 77, 628 xylene, heptane 138,
Soluble in benzene, toluene, chloroform and methylene chloride, slightly soluble in petroleum ether and gasoline
Stability. 5 ℃ ~ 130 ℃ stable, water DT50 < 21d, acid, alkali stability, soil DT50 of 30d ~ 90d, see the light slowly
break down
1 Scope
This standard specifies the pendimethalin drug requirements, test methods and marking, labeling, packaging, storage and transportation.
This standard applies to the impurities generated by the production of pendimethalin and pendimethalin in the composition of the original drug.
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 1604 Goods pesticide regulations for acceptance
GB/T 1605-2001 Sampling Method commercial pesticides
GB 3796 pesticide packaging General
GB/T 19138 Determination of acetone insoluble pesticide
3 Requirements
3.1 Appearance. This product should be brown to orange-yellow crystalline powder, free from visible foreign matter and filling the modifier.
3.2 pendimethalin drug should be consistent with the requirements in Table 1.
Table 1 pendimethalin drug quality control program indicators
Item Index
Pendimethalin mass fraction /% ≥ 95.0
Moisture /% ≤ 0.5
pH range 4.0 to 8.0
Insoluble in acetone /% a ≤ 0.5
a insoluble in acetone test under normal production conditions, every 3 months test at least once.
Test Method 4
4.1 Sampling
According to GB/T 1605-2001 "on the original drug product sampling" approach. Determining sample package using a random number table method; the final sample size
Not less than 100g.
4.2 Identification Test
4.2.1 Liquid Chromatography --- The identification test can pendimethalin content simultaneously. Under the same chromatographic operating conditions, the test
A sample solution peak retention time compared with standard sample solution pendimethalin peak retention time, the relative difference should be 1.5%
Fewer.
4.2.2 Gas Chromatography --- The identification test can pendimethalin content simultaneously. Under the same chromatographic operating conditions, the test
A sample solution peak retention time compared with standard sample solution pendimethalin peak retention time, the relative difference should be 1.5%
Fewer.
4.3 Determination of the mass fraction of pendimethalin
4.3.1 Liquid Chromatography (Arbitration Act)
4.3.1.1 Method summary
Sample dissolved in mobile phase acetonitrile + water as the mobile phase, the use of ODS (C18) to filling a stainless steel column and UV detector, for
Pendimethalin in the sample subjected to reverse phase liquid chromatography separation and determination.
4.3.1.2 Reagents and solutions
Acetonitrile. chromatographic pure;
Water. secondary distilled water;
Pendimethalin standard. a known mass fraction ≥99.0%.
4.3.1.3 Instruments
LC. a variable wavelength UV detector and quantitative injection valve;
Chromatographic data processor or chromatography workstation;
Column.200mm × 4.6mm (. I.d) stainless steel column, built HypersilODS5μm filler (or with the same column efficiency
Other reversed phase columns);
Filter. filter pore size of about 0.45μm;
Quantitative sample line. 5μL;
Micro injector. 50μL;
Ultrasonic cleaner.
4.3.1.4 LC operating conditions
Mobile phase. [Psi] (acetonitrile. water) = 60.40;
The mobile phase flow rate. 1.0mL/min;
Column temperature. room temperature (temperature change should not exceed 2 ℃);
Detection wavelength. 240nm;
Injection volume. 5μL;
Retention time. pendimethalin 13.5min.
HPLC 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 pendimethalin drug liquid chromatography is shown in Figure 1.
1 --- pendimethalin.
Figure 1 HPLC pendimethalin drug
4.3.1.5 Measurement procedure
4.3.1.5.1 preparation of standard solution
Weigh pendimethalin standard 0.1g (accurate to 0.0002g), a 50mL volumetric flask, dissolved in acetonitrile and diluted to the mark, shake
uniform. Using a pipette to take the above solution was placed in another 5mL 50mL volumetric flask, mobile phase and dilute to the mark.
4.3.1.5.2 preparation of the sample solution
Weigh containing pendimethalin 0.1g sample (accurate to 0.0002g), a 50mL volumetric flask, dissolved in acetonitrile and diluted to the mark
Degree, shake. Using a pipette to take the above solution was placed in another 5mL 50mL volumetric flask, mobile phase and dilute to the mark.
4.3.1.5.3 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 Lingfeng area with pendimethalin
After the change of less than 1.2%, according to the order of the standard solution, sample solution, sample solution, standard solution injection analysis.
4.3.1.6 Calculation
1 mass fraction (%) sample of pendimethalin according to equation (1).
1 = A2
(1)
Where.
A1 --- the average standard solution of pendimethalin Lingfeng area;
A2 --- sample solution pendimethalin mean Lingfeng area;
--- Pendimethalin pendimethalin standard mass fraction, expressed as a percentage.
4.3.1.7 allowable difference
The difference between two parallel determination results shall not be greater than 1.0%, the arithmetic mean value as a measurement result.
4.3.2 Gas Chromatography
4.3.2.1 Method summary
Sample was dissolved in chloroform, phthalate, di-n-amyl acetate as the internal standard, using to 5% OV-101/ChromosorbW AW
DMCS, 180μm ~ 250μm as filler glass column and flame ionization detector, the sample of pendimethalin into gas
Chromatographic separation and determination.
4.3.2.2 Instruments
Gas chromatograph. with a hydrogen flame ionization detector;
Chromatographic data processor or chromatography workstation;
Column. 1m × 3.2mm (i.d.) glass column, filled with 5% OV-101/ChromosorbW AW DMCS, 180μm ~
250μm filler;
Micro injector. 10μL.
4.3.2.3 Reagents and solutions
Chloroform;
Pendimethalin standard. a known mass fraction ≥99.0%;
Phthalate, di-n-amyl acetate. should not interfere with the analysis of impurities;
Internal standard solution. Weigh 5g of di-n-amyl placed 1000mL volumetric flask, dissolved with chloroform and diluted to the mark
Degree, shake.
4.3.2.4 GC operating conditions
Temperature (℃). 175 Column temperature gasification chamber 200, the detector chamber 200;
Gas flow rate (mL/min). carrier gas (N2) 40, hydrogen gas 35, air 350;
Injection volume (μL). 0.5;
Retention time (min). pendimethalin from about 9.4 to about 14.0 internal standard.
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 pendimethalin drug and internal standard gas chromatography is shown in Figure 2.
1 --- solvent;
2 --- pendimethalin;
3 --- internal standard (n-pentyl phthalate ester).
Figure 2 pendimethalin drug and internal standard gas chromatograph
4.3.2.5 Measurement procedure
4.3.2.5.1 Preparation of standard solution
Weigh pendimethalin standard 0.1g (accurate to 0.0002g), was placed in a 10mL stoppered glass bottle with pipette 10mL
Internal standard solution to dissolve, shake.
4.3.2.5.2 Preparation of sample solution
Weigh containing pendimethalin 0.1g (accurate to 0.0002g) sample, placed in a 10mL glass bottles stoppered with and 4.3.2.5.1
Pipette with an internal standard solution was added to dissolve 10mL, shake.
4.3.2.5.3 Determination
Under these operating conditions, the instrument until a stable baseline, the number of continuous injection doses of the standard solution, calculated for each needle pendimethalin and the internal standard peak area
Volume ratio of repeatability to be two adjacent needles pendimethalin and the internal standard peak area ratio of the relative change of less than 1.2%, according to the standard solution, the test
Sample solution, sample solution, the order of the standard solution was measured.
4.3.2.6 Calculation
1 mass fraction (%) sample of pendimethalin according to equation (2).
1 = γ2
(2)
Where.
γ1 --- standard solution, pendimethalin and the internal standard peak area ratio of the average;
γ2 --- sample solution, pendimethalin and the internal standard peak area ratio of the average;
--- Standard pendimethalin mass fraction, expressed as a percentage.
4.3.2.7 allowable difference
The difference between two parallel determination results shall not be greater than 1.0%, 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 requirements weighed sample with ψ. = 65.35 was dissolved (acetone and water), according to GB/T 1601 Pesticides pH value
Direct measurement method determination.
4.6 Determination of acetone insolubles
According to GB/T 19138 performed.
4.7 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
Flag 5.1 pendimethalin drugs, labeling and packaging should comply with the provisions of GB 3796.
5.2 pendimethalin drug use clean plastic pail or metal pail lined with plastic, careful not to make direct contact with the metal. Net weight per barrel
25kg, 50kg or 200kg.
5.3 is also available upon request or order agreement, the use of other forms of packaging, subject to the provisions of GB 3796.
5.4 pendimethalin drug package should be stored in well-ventilated, dry coffers.
5.5 storage, prevent moisture and sunlight, no food, seed, feed mix, avoid contact with skin, eyes, mouth and nose to prevent inhalation.
5.6 Safety. This product is a low toxicity, are swallowed or inhaled toxic, it can penetrate through the skin. When using this product to wear goggles and rubber gloves and other
Necessary protective clothing. Such as skin, eyes accidentally stained with the product, rinse immediately with plenty of water. Coverage were immediately sent to hospital for treatment.
5.7 of acceptance. Acceptance of pendimethalin drug for a month. From the date of delivery, product quality inspection completed within a month of its
Indicators should meet the standards.
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