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GB 24753-2009: Isocarbophos technical
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Isocarbophos technical
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GB 24753-2009
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Basic data | Standard ID | GB 24753-2009 (GB24753-2009) | | Description (Translated English) | Isocarbophos technical | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Classification of International Standard | 65.100.10 | | Word Count Estimation | 9,983 | | Date of Issue | 2009-11-30 | | Date of Implementation | 2010-07-01 | | Quoted Standard | GB/T 601; GB/T 1600; GB/T 1604; GB/T 1605-2001; GB 3796; GB/T 19138 | | Regulation (derived from) | Announcement of Newly Approved National Standards No. 14 of 2009 (No. 154 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 Isocarbophos requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to isocarbophos and impurities generated in the production of Isocarbophos original drug. | GB 24753-2009: Isocarbophos 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.
Isocarbophos technical
ICS 65.100.10
G25
National Standards of People's Republic of China
Isocarbophos original drug
Posted 2009-11-30
2010-07-01 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. Hubei cents Lung Chemical Co., Ltd., Hebei Weiyuan Biological and Chemical Corporation.
The main drafters of this standard. Jiangmin Yi, in bright, Zhang Xue, Yang Jinrong, Ko Wing Man.
Isocarbophos original drug
Other name, structural formula and basic physicochemical parameters of the active ingredients of the product Isocarbophos as follows.
ISO common name. Isocarbophos
CAS Registry Number. 24353-61-5
Chemical Name. O- methyl -O- (2- isopropoxy-formylphenyl) Thioxophosphamide
Structure.
Empirical formula. C11H16NO4PS
Molecular Weight. 288.0 (according to 2003 international relative atomic mass)
Biological activity. insecticide, acaricide
Melting point. 45 ℃ ~ 46 ℃
Solubility. soluble in alcohol, ether, benzene, acetone and ethyl acetate, insoluble in water and petroleum ether
Stability. stable under neutral and acidic conditions, the case of alkali easy to decompose
1 Scope
This standard specifies the Isocarbophos original drug requirements, test methods and marking, labeling, packaging, storage and transportation.
This standard applies to the impurities generated by Isocarbophos composition and production Isocarbophos 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.
Preparation of GB/T 601 chemical reagent standard titration solution
GB/T 1600 Determination of Water Pesticides
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
White to pale yellow crystals.
3.2 Isocarbophos original drug should be consistent with the requirements in Table 1.
Table 1 Isocarbophos original drug quality control program indicators
Item Index
Isocarbophos mass fraction /% ≥ 95.0
Moisture /% ≤ 0.3
Acetone insolubles a /% ≤ 0.5
Acidity (H2SO4 meter) /% ≤ 0.3
Insoluble in acetone measured at least once every 3 months a normal production.
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
Infrared spectroscopy --- Isocarbophos sample and standard samples in the range 4000cm-1 ~ 400cm-1 infrared absorption spectrum should not significantly
the difference. Isocarbophos standard infrared spectrum is shown in Figure 1.
Figure 1 Isocarbophos standard infrared spectra
Liquid chromatography --- The identification test can be carried out simultaneously with the determination of the mass fraction of Isocarbophos. Under the same chromatographic operating conditions,
The sample solution to a chromatographic retention time and standard solution in the chromatographic peaks Isocarbophos retention time, the relative difference should
Less than 1.5%.
4.3 Determination of the mass fraction of Isocarbophos
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, to use as filler BDSHypersilC18 stainless steel column and UV detector
(225nm), the sample Isocarbophos high performance liquid chromatography and determination.
4.3.1.2 Reagents and solutions
Methanol;
Water. The new secondary steam distilled water;
Isocarbophos standards. a known mass fraction, ≥97.5%.
4.3.1.3 Instruments
High performance liquid chromatography. a variable wavelength UV detector;
Chromatographic data processor or workstation;
Color 150mm × 4.6mm (i.d.) Stainless steel column, built BDSHypersilC185μm 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.
4.3.1.4 HPLC operating conditions
Mobile phase. ψ (CH3OH.H2O) = 60.40;
Flow rate. 1.0mL/min;
Column temperature. room temperature (temperature change should not exceed 2 ℃);
Detection wavelength. 225nm;
Injection volume. 5μL;
Retention time. Isocarbophos 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 Isocarbophos original drug HPLC is shown in Figure 2.
1 --- Isocarbophos.
Figure 2 HPLC Isocarbophos original drug
4.3.1.5 Measurement procedure
4.3.1.5.1 Preparation of standard solution
Weigh 0.1g Isocarbophos standard (accurate to 0.0002g), a 50mL volumetric flask, dilute to the mark with methanol, ultrasonic transducer
Dang 5min to dissolve the sample was cooled to room temperature and shake well. Using a pipette to take the above solution 5mL to 50mL volumetric flask, dilute with methanol
Release to the mark.
4.3.1.5.2 Preparation of sample solution
Weigh aqueous Isocarbophos 0.1g sample (accurate to 0.0002g), a 50mL volumetric flask, dilute to the mark with methanol, ultrasonic
Wave 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 A
Alcohol diluted to the mark, shake.
4.3.1.6 Determination
Under these operating conditions, after the instrument is stable, continuous injection of several doses of the standard solution until the two adjacent needles Isocarbophos peak area becomes relatively
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.
4.3.1.7 Calculation
1 sample mass fraction (%) Isocarbophos, according to equation (1).
1 = A2
(1)
Where.
A1 --- the standard solution, the average Isocarbophos peak area;
A2 --- sample solution, the average Isocarbophos peak area;
--- Isocarbophos standard mass fraction, expressed as a percentage.
4.3.1.8 allowable difference
Isocarbophos poor quality score of two parallel determination results shall not be greater than 1.2%, the arithmetic mean value as a measurement result.
4.3.2 Gas Chromatography
4.3.2.1 Method summary
Sample was dissolved in ethyl acetate, n-butyl sebacate to as the internal standard, using the 5% OV-3 packed column, and a hydrogen flame ionization detector
, A sample of Isocarbophos gas chromatographic separation and determination.
4.3.2.2 Reagents and solutions
Ethyl acetate;
N-butyl sebacate. Do not interfere with the analysis of impurities;
Isocarbophos standards. a known mass fraction, ≥97.5%;
Internal standard solution. Weigh 5g of n-butyl sebacate in 250mL volumetric flask, dissolved in ethyl acetate and diluted to the mark,
Shake;
Fixative. OV-3;
Carrier. 101 silanized carrier body (180μm ~ 250μm).
4.3.2.3 Instruments
Gas chromatograph. with flame ionization detector;
Chromatographic data processor or chromatography workstation;
Column. 1m × 3mm (. I.d) glass column (or stainless steel column), built-in 5% OV-3/101 silylation white support body (180μm ~
250 m) filler.
4.3.2.4 GC operating conditions
Temperature (℃). Room 210 column, the gasification chamber 270, detection chamber 270;
Gas flow rate (mL/min). carrier gas (N2) 60, hydrogen gas 40, air 400;
Injection volume. 0.6μL;
Retention time. Isocarbophos about 6.1min, internal standard about 9.5min.
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 Isocarbophos original drug and the internal standard are shown in Figure 3.
1 --- Isocarbophos;
2 --- internal standard.
Figure 3 Isocarbophos original drug and the internal standard gas chromatograph
4.3.2.5 Measurement procedure
4.3.2.5.1 preparation of standard solution
He said water Isocarbophos standard 0.2g (accurate to 0.0002g), placed in a glass bottle stopper, with a pipette accurately added 5mL internal standard
Solution, shake.
4.3.2.5.2 preparation of the sample solution
Weigh aqueous Isocarbophos 0.2g sample (accurate to 0.0002g), placed in a glass bottle stopper, with manipulation and 4.3.2.5.1
With a pipette accurately with added internal standard solution 5mL, shake.
4.3.2.6 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 Isocarbophos internal standard
After the peak area ratio of relative change is less than 1.2%, according to the solution, the sample solution, the sample solution, the order of standard sample of standard solution was analyzed
Determination.
4.3.2.7 Calculation
The peak area was measured before and after the two-needle sample solution and two doses of the standard sample solution Isocarbophos and the internal standard ratio were flat
all. Sample Isocarbophos 2 mass fraction (%) according to equation (2).
(2)
Where.
--- Standard ISO CARBOPHOS mass fraction, expressed as a percentage.
4.3.2.8 allowable difference
The difference between two parallel determination results shall not be greater than 1.2%, the arithmetic mean value as a measurement result.
4.4 Determination of Moisture
According to GB/T 1600 the "Karl Fischer method".
4.5 Determination of acetone insolubles
According to GB/T 19138 performed.
4.6 Determination of acidity
4.6.1 Reagents and solutions
Ethanol;
Sodium hydroxide standard titration solution Ba (NaOH) = 0.02mol/L, according to GB/T 601 preparation and calibration;
Bromophenol blue in ethanol. ρ (bromophenol blue) = 1g/L.
4.6.2 measuring step
Weigh the sample 2g (accurate to 0.002g), placed in a 250mL Erlenmeyer flask, adding ethanol 20mL, shake the sample solution
solution. Add 3 drops of bromophenol blue indicator, 0.02mol/L sodium hydroxide standard titration solution, titration to blue is the end. Meanwhile blank
Determination.
4.6.3 Calculation
The acidity of the sample 3 (%), according to equation (3) Calculated.
3 = Ba
(Vp Vp 1- 0) × M
100 (3)
Where.
Ba --- the actual concentration of sodium hydroxide standard titration solution, expressed in moles per liter (mol/L);
Vp 1 --- titration of the sample solution, the volume of consumption of sodium hydroxide standard titration solution, in milliliters (mL);
V0 --- titrate blank solution, the volume of consumption of sodium hydroxide standard titration solution, in milliliters (mL);
--- The M sulfuric numerical molar mass in grams per mole (g/mol), [M (12H2SO4
) = 49g/mol].
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 Isocarbophos original drug, labeling and packaging should comply with the provisions of GB 3796.
5.2 Isocarbophos original drug use clean, dry sturdy plastic (iron) pail, barrel net content should not exceed 200kg. It can also be used in accordance with
User requirements or other forms of ordering agreement package, subject to the provisions of GB 3796.
5.3 Isocarbophos original drug 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 highly toxic organophosphate pesticides. Are swallowed and inhaled toxic, it can penetrate through the skin. Wear protective goggles and the FDA
Rubber gloves, wear the necessary protective clothing. After spraying, wash immediately with soap and plenty of water. Such as poisoning, should be immediately sent to hospital
Symptomatic treatment. Atropine or pralidoxime detoxification.
5.6 of acceptance. Acceptance of Isocarbophos original drug for a month. From the date of delivery, product quality inspection completed within a month of its
Indicators shall comply with this standard.
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