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GB 13649-2009 English PDF

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GB 13649-2009: [GB/T 13649-2009] Fenitrothion technical
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GB 13649: Evolution and historical versions

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GB 13649-2009English289 Add to Cart 3 days [Need to translate] [GB/T 13649-2009] Fenitrothion technical Valid GB 13649-2009
GB 13649-1992English319 Add to Cart 3 days [Need to translate] Fenitrothion technical Obsolete GB 13649-1992

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Basic data

Standard ID GB 13649-2009 (GB13649-2009)
Description (Translated English) [GB/T 13649-2009] Fenitrothion technical
Sector / Industry National Standard
Classification of Chinese Standard G25
Classification of International Standard 65.100.10
Word Count Estimation 11,15
Date of Issue 2009-11-30
Date of Implementation 2010-07-01
Older Standard (superseded by this standard) GB 13649-1992
Quoted Standard GB/T 1600; GB/T 1604; GB/T 1605-2001; GB 3796
Adopted Standard FAO 35/TC/S-1988, MOD
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 requirements fenitrothion original drug, test methods and marking, labeling, packaging, storage and transportation. This standard applies to fenitrothion and its impurities generated in the production of fenitrothion original drug.

GB 13649-2009: [GB/T 13649-2009] Fenitrothion 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.
Fenitrothion technical ICS 65.100.10 G25 National Standards of People's Republic of China Replacing GB 13649-1992 Fenitrothion 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 are mandatory, the rest are recommended. This standard uses redrafted law revision using FAO specifications 35/T C/S (1988) "fenitrothion original drug." The FAO standards and specifications 35/T C/S (1988) The main technical differences are as follows. --- This standard specifies fenitrothion content of not less than 95.0%, FAO specifications prescribed fenitrothion content of not less than 930g/kg. This standard replaces GB 13649-1992 "fenitrothion original drug." This standard compared with GB 13649-1992, the main differences are as follows. --- Fenitrothion original drug by the mass fraction of not less than 93%, 85% and 70% to not less than 95%; --- Increase S- methyl fenitrothion control indicators; --- By the acidity of not more than 0.3%, 0.4% and 0.5% to not more than 0.1%; --- By the water not more than 0.2% to not more than 0.1%. Appendix A of this standard is an informative annex. 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. the Ministry of Agriculture. Participated in the drafting of this standard. Zhejiang Jiahua Group Co., Ltd., Sinochem Ningbo Chemicals Co., Ltd. The main drafters of this standard. Jiang Yifei, Li Youshun, Wang Xiaoli, Chen Tiechun, United Kingdom, Li Guoping, Xu Qiang Hua Tang light transmission. This standard replaces the standards previously issued as follows. --- GB 13649-1992. Fenitrothion original drug This product is an active ingredient fenitrothion other name, structural formula and basic physicochemical parameters are as follows. ISO common name. fenitrothion CIPAC numerals. 35 CA registration number. 122-4-5 Chemical Name. O, O- dimethyl -O- (4- nitro-3-methylphenyl) phosphorothioate Structural formula  division O2 N CH3 O P (OCH3) 2 S Empirical formula. C9H12NO5 Molecular Weight. 277.2 (according to 2005 international relative atomic mass) Biological activity. Insecticidal Melting point. 0.3 ℃ Boiling point. 140 ℃ ~ 145 ℃/1mmHg (decomposition) Vapor pressure (20 ℃). 18mPa Solubility. water 14mg/L (30 ℃), soluble in alcohols, esters, ketones, aromatic hydrocarbons and chlorinated hydrocarbons, hexane 24, isopropanol 138 (g/L, 20 ℃) Stability. under normal conditions are relatively stable, hard to be hydrolyzed

1 Scope

This standard specifies the original drug fenitrothion requirements, test methods and marking, labeling, packaging, storage and transportation. This standard applies to the original drug Fenitrothion Fenitrothion impurities generated by the production and composition.

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 1604 Goods pesticide regulations for acceptance GB/T 1605-2001 Sampling Method commercial pesticides GB 3796 pesticide packaging General

3 Requirements

3.1 Composition and appearance. This product should Fenitrothion and impurities generated in the production of the composition, should be pale yellow to dark brown liquid, no visible FOD. 3.2 fenitrothion original drug should be consistent with the requirements in Table 1. Table 1 Fenitrothion original drug control project indicators Item Index Fenitrothion content /% ≥ 95.0 S- methyl fenitrothion mass fraction /% ≤ 2.0 Moisture /% ≤ 0.1 Acidity (H2SO4 meter) /% ≤ 0.3 Test Method 4 4.1 Sampling According to GB/T 1605-2001 5.3.1 "commodity original drug sample" to. Determining sample package using a random number table method, the final sample The amount of not less than 100g. 4.2 Identification Test Gas Chromatography --- The identification test can be carried out simultaneously with the determination of fenitrothion (S- methyl fenitrothion) mass fraction. In the same Chromatographic operating conditions, the sample solution to a chromatographic retention time and standard solutions fenitrothion (S- methyl fenitrothion) peaks Retention time, the relative difference should be less than 1.5%. Infrared spectroscopy --- sample and standard samples in 4000cm-1 ~ 400cm-1 wave number range of the infrared spectrum, there should be no significant difference different. Fenitrothion standard infrared spectrum is shown in Figure 1. Figure 1 fenitrothion standard infrared spectrum 4.3 Determination of fenitrothion, S- methyl fenitrothion mass fraction 4.3.1 Method summary Sample was dissolved in acetone to diallyl phthalate esters as internal standard, using a HP-5 capillary column and a flame ionization detector, Sample of fenitrothion, S- methyl fenitrothion and measured by gas chromatography, internal standard. You can also use a packed column gas chromatography Determination of spectrum, chromatographic operating conditions, see Appendix A. 4.3.2 Reagents and solutions Acetone. AR; Fenitrothion standard. a known mass fraction, ≥98.0%; Internal standard. dimethyl phthalate, propylene carbonate, should not interfere with the analysis of impurities; Internal standard solution. Weigh diallyl phthalate esters 2.5g, placed in 500mL volumetric flask, dissolved in acetone and diluted to the mark, Shake well. 4.3.3 Instruments Gas chromatograph. with a hydrogen flame ionization detector, split/splitless inlet; Chromatographic data processor or chromatography workstation; Column. 30m × 0.32mm (i.d.) HP-5 capillary column, film thickness 0.25 m; Micro injector. 10μL. 4.3.4 GC operating conditions Temperature (℃). Room 210 column, the gasification chamber 230, detection chamber 270; Gas flow rate (mL/min). carrier gas (N2) 1.5, makeup gas (N2 of) 30, hydrogen gas 30, air 300; Split ratio. 50.1; Injection volume. 1.0μL; Retention time. fenitrothion 4.9min, S- methyl fenitrothion 6.4min, diallyl phthalate esters 3.2min. The above operating conditions, the Department of typical operating parameters, according to the characteristics of different instruments and columns for a given operating parameters to make appropriate adjustments to To obtain the best results. Typical fenitrothion original drug GC is shown in Figure 2. 1 --- internal standard (diallyl phthalate esters); 2 --- fenitrothion; 3 --- S- methyl fenitrothion. Figure 2 fenitrothion original drug gas chromatogram 4.3.5 measuring step 4.3.5.1 Preparation of standard solution Weigh fenitrothion standard 0.1g (accurate to 0.0002g), placed in 15mL stoppered glass bottle with a pipette accurately added 10mL Internal standard solution, shake well. 4.3.5.2 Preparation of sample solution Weigh the sample containing fenitrothion 0.1g of (accurate to 0.0002g), placed in 15mL stoppered glass vial with 4.3.5.1 with the same A pipette accurately added internal standard solution 10mL, shake. 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 fenitrothion and the internal standard peak area After the change of the relative volume ratio is less than 1.2%, according to the solution, the sample solution, the sample solution and standard sequence of the standard solution was measured. 4.3.6 Calculation The two needles in the sample solution and measured before and after the two-pin standard sample solution fenitrothion and the internal standard peak area ratios are averaged. 1 sample mass fraction (%) of fenitrothion according to equation (1). (1) Where. --- Fenitrothion standard mass fraction, expressed as a percentage. The two needles in the sample solution is measured with S- methyl fenitrothion fenitrothion peak areas are averaged. Sample S- methyl fenitrothion 2 mass fraction (%) parathion according to formula (2). 2 = A2A1 × 1 (2) Where. A1 --- sample solution, fenitrothion mean peak area; A2 --- sample solution, the average S- methyl fenitrothion peak area; 1 --- sample fenitrothion mass fraction, expressed as a percentage. 4.3.7 allowable difference The difference between two parallel determination results, fenitrothion should be less 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 acidity 4.5.1 Reagents and solutions 95% ethanol; Sodium hydroxide standard titration solution. Ba (NaOH) = 0.02mol/L; Methyl red - bromocresol green mixed indicator solution. take 2mL methyl red ethanol solution (1g/L) and 10mL bromocresol green ethanol solution (1g / L) were mixed shake. 4.5.2 measuring step Weigh the sample 4g (accurate to 0.002g), placed in a 250mL conical flask, 40mL95% ethanol, shaking the sample solution Solution was added 2mL mixed indicator solution, titration with sodium hydroxide standard titration solution to dark green as the end point. Meanwhile blank determination. 4.5.3 Calculation The acidity of the sample 3 (%), according to equation (3) Calculated. 3 = Ba * Vp Vp 1- () 0 · M (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 values of the molar mass of sulfuric acid, in units of grams per mole (g/mol), [M (1/2H2SO4) = 49g/mol]. 4.6 product testing 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 fenitrothion original drug, labeling, packaging, should meet the requirements of GB 3796. 5.2 fenitrothion original drug application, clean, dry wall is coated with a protective layer of iron drum, barrel, net weight should be less than 200kg. Also root According to user requirements or the order agreement, the use of other forms of packaging, but to comply with the provisions of GB 3796. 5.3 fenitrothion 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 toxic organophosphate insecticides pesticides are swallowed or inhaled toxic to the eyes, skin irritation. The FDA should wear Protective gloves, masks and goggles, wear clean protective clothing, wash with soap and water immediately after application to avoid skin and eye contact with liquid. in case Wrongly, should be sent to hospital for treatment. 5.6 Acceptance period. Fenitrothion original drug acceptance period of 1 month. From the date of delivery, within a month, the finished product quality inspection, its Indicators should meet the requirements of this standard.

Appendix A

(Informative) Fenitrothion quality gas chromatographic method scores packed column A. 1 Method summary Sample was dissolved in chloroform to lindane as internal standard, using the 5% OV-101/ChromosorbW-HP for the stainless steel filler Column and a flame ionization detector, the sample of fenitrothion, S- methyl fenitrothion and measured by gas chromatography internal standard method Quantified. A. 2 Reagents and solutions Chloroform; Fenitrothion standard. a known mass fraction, ≥98.0%; Internal standard. lindane, should not interfere with the analysis of impurities; Fixative. OV-101; Vector. ChromosorbW-HP, diameter of 125μm ~ 150μm (100 mesh to 120 mesh); Internal standard solution. Weigh Lindane 5g, placed in 500mL flask with chloroform dissolved and diluted to the mark. A. 3 Instrument Gas chromatograph. with a hydrogen flame ionization detector; Chromatographic data processor or chromatography workstation; Column. 500mm × 2.2mm (i.d.) Stainless steel column, filled with 5% OV-101/ChromosorbW-HP filler; Micro injector. 10μL. A. 4 GC operating conditions Temperature (℃). Column Room 155 ± 5, the gasification chamber 220, detection chamber 250; Gas flow rate (mL/min). carrier gas (N2) 15, hydrogen gas 30, air 300; Injection volume. 1.0μL; Retention time. fenitrothion about 11min, S- methyl fenitrothion about 16min, lindane about 5min. The above operating conditions, the Department of typical operating parameters, according to the characteristics of different instruments and columns for a given operating parameters to make appropriate adjustments to To obtain the best results. Typical fenitrothion original drug GC is shown in Figure A. 1. 1 --- internal standard (lindane); 2 --- fenitrothion; 3 --- S- methyl fenitrothion. Figure A. TC 1 Fenitrothion gas chromatogram A. 5 measuring step A. 5.1 Preparation of standard solution Weigh fenitrothion standard 0.1g (accurate to 0.0002g), placed in 15mL stoppered glass bottle with a pipette accurately added 10mL Internal standard solution, shake well. A. 5.2 Preparation of sample solution Weigh the sample containing fenitrothion 0.1g of (accurate to 0.0002g), placed in 15mL stoppered glass vial, with the A. 5.1 in the same Only pipette accurately added internal standard solution 10mL, shake. A. 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 fenitrothion and the internal standard peak area After the relative change in volume of less than 1.5%, according to the solution, the sample solution, the sample solution and standard sequence of the standard solution was measured. A. 6 Calculation The two needles in the sample solution and measured before and after the two-pin standard sample solution fenitrothion and the internal standard peak area ratios are averaged. 1 sample mass fraction (%) of fenitrothion according to formula (A.1) Calculated. (A.1) Where. Book GB 13649-2009 --- Fenitrothion standard mass fraction, expressed as a percentage. The two needles in the sample solution is measured with S- methyl fenitrothion fenitrothion peak areas are averaged. Sample S- methyl fenitrothion Parathion 2 mass fraction (%) according to equation (A.2) Calculated. 2 = A2A1 × 1 (A.2) Where. A1 --- sample solution, fenitrothion mean peak area; A2 --- sample solution, the average S- methyl fenitrothion peak area; 1 --- sample fenitrothion mass fraction, expressed as a percentage. A. 7 allowable difference The difference between two parallel determination results, fenitrothion should be less than 1.2%, the arithmetic mean value as a measurement result. 9002-

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