GB 13649-2009Fenitrothion technical (English PDF)
杀螟硫磷原药
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Issued by
Standardization Administration of China
Level / Type
National · Mandatory
Issue date
November 30, 2009
Implementation date
July 1, 2010
Scope
GB 13649-2009 is the English-translated version of 杀螟硫磷原药.
GB 13649-2009 — 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.
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Document preview — GB 13649-2009
National Standard of the People's Republic of China
- ICS
- 65.100.10
- Classification
- G 25
- Replacing
- GB 13649-1992
Issued by: Standardization Administration of China
Contents
- Foreword
- 1 Scope
- 2 Normative references
- 3 Requirements
- 4.1 Sampling
- 4.2 Identification Test
- 4.3 Determination of fenitrothion, S- methyl fenitrothion mass fraction
- 4.4 Determination of Moisture
- 4.5 Determination of acidity
- 4.6 Product testing and acceptance
- 5 Marking, labeling, packaging, storage and transportation
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.
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 (°C). 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).
Where.
--- Fenitrothion standard mass fraction, expressed as a percentage.
The two needles in the sample solution is measured with S- methyl fenitrothion peak areas are averaged. Sample S- methyl fenitrothion 2 mass fraction (%) parathion according to formula (2).
2 = A2A1 ×
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
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 (°C). 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.
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 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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