Some standard content:
1CS 65.100
Chemical Industry Standard of the People's Republic of China
HG33003302—2001
Long-lasting phosphorus technical, emulsifiable concentrate, soluble liquid preparation Issued on 20020124
Implemented on 2002-07-01
Issued by the State Economic and Trade Commission
Registration No.: 10085—2002
HG3300—2001
Chapter 3 and Chapter 5 of this standard are mandatory, and the rest are declarative. This standard is equivalent to the determination method of long-term fermentation content in the mandatory chemical industry standard H:3300·1990 long-term data sharing standard G1PA287//M/-force method adopted by the International Pesticide Analysis Cooperation Committee. The main technical content of this standard 3300-1900 is greater than 73.5% of the dry weight of the short-term product, greater than 65.0% of the dry weight of the first-class product. The moisture content of the standard product is greater than or equal to 65.0%. The moisture content of the superior product is less than or equal to .35, and the first-class product is less than or equal to 0.2 %, the standard product is less than or equal to 0.4% and changed to a grade, that is, less than or equal to 0.3%; the superior product is less than or equal to 7.5% and the substandard product is less than or equal to 2.5%. The water absorption of the product is changed from the superior product less than or equal to 0.C5%, the substandard product less than 3.1% and the substandard product less than 1%. The standard for the determination of long-term efficacy is changed from gas chromatography and thin layer chromatography to liquid chromatography: this standard has been implemented since the implementation of the standard, and it also replaces H( R3M-1S9m This standard was issued by the Beijing Municipal Bureau of Industry and Commerce and the Beijing Municipal Administration for Industry and Commerce. This standard was issued by the National Chemical Engineering Committee, and the responsible drafting units of this standard are: Shenyang Chemical Research Institute. The participating drafting units of this standard are: Qingdao Pesticide Factory and Zhangjiajie First Pesticide Factory. The main drafters of this standard are: Xu Laigan, Xing Hong, Zhang Xiebing, Du Laoqiang, Yucheng, and Sheng Cunhe. This standard was first issued in the autumn of 1, and was transformed into a regulatory chemical industry standard in 3, and was newly numbered as G35-. This standard is interpreted by the National Pesticide Standardization Technical Committee of the People's Republic of China, Chemical Industry Standard of the People's Republic of China
Morocrotophos original
Techndca
Other names, formulas and basic physical and chemical parameters of the active ingredient of this product are as follows: Iso Common name, Mdanocratopha
CIPAC digital code: 287
Chemical name: 0,0..methyl (F) L1 methyl-2 (methylcarbamoyl) ethyl phosphate Physical formula:
Experimental formula: HNO
Relative molecular weight 223.2 (based on 1UU7 area relative atomic mass) Biological activity: Insecticidal
Degree of heat (25℃) 290#
Degree of heat (2c ): 1.22g/cm2
Glow point, 54--55
Drying point: 125℃(46.9mP:)
HG3300—2001
Generation HG1300—199m
Solubility g/kg.2℃%): 1000.700 in dihydromethane, 1000.100 in methanol, 250 in methanol, 69.5 in diesel and dye oil
Stability, unstable above 36, thermal decomposition above 55℃. At 20℃:, the half-life of water is based on pH value: 61.pH? When it is 1.H9, it is 17. It is unstable in grade ethanol. Compared with iron plate, rolled steel, stainless steel 304 and yellow Zhao, it is corrosive. This standard specifies the requirements, test methods, marking, labeling, packaging, storage and transportation of long-acting phosphorus technical materials. This standard is applicable to long-acting technical materials composed of long-acting classes and impurities generated during their production: 2 Reference standards The following standards are used to quote the relevant provisions of this standard. When the version is compared, the versions shown are all valid. All standards will be compensated. The parties using this standard should explore the possibility of using non-latest versions of the following standards: GB/T601-Preparation of standard solutions for quantitative analysis (quantity analysis) of chemical reagents GB/160-391080 Method for determination of moisture content in pesticides G/T1604-89. Collection rules for commercial pesticides GB/T1605-979 (1989) Commercial pesticide collection method National Light Economic Fund Conference 2002-01-24 Approved 2002-07-01 Implementation
GB3?S6
3 Requirements
Pesticide packaging general
HG3300---2001
3.1 External age, dark image or solid 4, no visible foreign matter. 3.2 The long-lasting phosphorus technical shall meet the requirements of Table 1. Table 1 Control items of long-lasting phosphorus technical Daily indicators
Long-lasting phosphorus content
Acid (as HSO 100 liters)
To dimethyl ether
Water
Note: Trimethyl ether content, water and other substances, at least 4 test plates are suitable
4.1 Sampling
According to the method of GB/T1615-19/9 (1089) in the milk filter phase, the sample preservation method is carried out according to the state. Before sampling, the long-lasting phosphorus technical shall be incubated at 35~10℃ for rapid baking. The packaging of the sample shall be determined by the energy-saving coating method. The final amount shall be less than 10cm E.4.2 Specific test
High-efficiency phase separation method: The specific test shall be carried out simultaneously with the determination of the long-lasting phosphorus content. Under similar chromatographic operating conditions, the relative value of the retention time of the test solution and the retention time of the chromatographic peak of long-acting phosphorus in the standard solution should be within 1.5. Gas phase hydrogen spectrometry: under similar chromatographic operating conditions, the relative value of the retention time of the chromatographic peak of the test solution and the retention time of the chromatographic peak of long-acting phosphorus in the standard sample should be within 1.3. 4.3 Determination of the content of chlorinated phosphorus
4.3.1 Summary of the method
The sample is dissolved in water, and a mixture of ethyl acetate and water is used as the moving phase. The spectrophotometry is performed on a column with T.ii:hmsplRP-18 (diameter 5um>) as the raw material. A fast-claw UV detector is used. The chlorinated phosphorus is measured with an external standard salt. 4.3.2 Apparatus
Liquid chromatograph: It has an ultraviolet variable wavelength detector and a quantitative inlet valve. Chromatographic data processor
Color: 4.mmti.l.) × 2i)ru stainless steel detector, internal LichrospherR1x (particle size 5um> dot filler (or H has other bonded C with the same effect)
Over-drainage fee, the pore space is about 0.45m.
Metric injector 5.,
4.3.3 Reagents and solutions
Acetyl nitrile: chromatographic grade,
Methanol: chromatographic grade.
Water: freshly distilled water
Mobile phase CHOH:CH,CN:F)=1O
Monocrotophos standard sample: as containing 1 year, greater than or equal to 8.0% 4.3.4 Subtractive chromatography conditions
Column temperature: room temperature,
Moving phase flow rate: 1.0mL/min:
Detection wavelength, 230m.
Injection volume 1IT..
Self-maintenance time: Monocrotophos is about 1.3min.
HG3300
·2001
The reverse liquid chromatography operating conditions are typical operating parameters. According to different collection points, the given operating parameters can be appropriately adjusted. In order to obtain the best effect quickly. The typical long-acting two-drug phase chromatogram is shown in Figure 1. 1 Long-acting
Figure 1 Long-acting crushed original drug phase subtraction chromatogram
4.3.5 Determination steps
4.3.5.1 Preparation of standard phase
Weigh 0.1g of long-acting phosphorus standard sample (accuracy 0.0003g) and put it in a 50ml volumetric flask. Use medium to make it up to volume. According to the following: Use a pipette to draw 5.00ml, put it in another 50mL volumetric flask, use constant volume, and make it up to volume. 5
4.3.5.2 Preparation of sample solution
B3300-2001
Weigh the sample containing 1% chlorpyrifos (if the sample is solid or has crystals, heat the sample to 25~35, let it stand completely, and mix it) to 0.0002g, add 50ml of granules to dissolve, make up to volume, and remove the spoon. Use a pipette to draw 5.00mL, measure it into a 1/4 volumetric flask, and adjust it with methanol. Filter it with a 0.45m membrane filter. 4.3.5.3 Microanalysis
Under the above operating conditions, after continuous injection, continuously inject several injections of standard sample solution until the relative change of the peak area of the two injections is less than 1.0%, and then analyze and determine in the order of standard sample solution, sample solution, sample solution, and standard sample solution. 4.3.6 Calculation
Average the peak areas of the two test solution and the standard sample solution before and after the test, and calculate the mass of the long-acting group in the sample by the formula: Am
the average value of the long-acting phosphorus sieve surface in the standard sample solution: Where A
the average value of the long-acting phosphorus sieve surface in the test solution; R
the mass of the test solution, and R
the mass of the long-acting phosphorus sieve surface in the standard sample solution.
4.3.7 The allowable difference
the two average values shall not be greater than %. The arithmetic mean value shall be taken as the determination result. 4.4 Determination of moisture
Perform according to G/T1600197S (1999). It is allowed to use the appropriate 4.5 Determination of moisture content by water analyzer
4.5.1 Reagents and
Standard sodium hydroxide solution: (NaOH) = 1.12 ml/L, prepare the indicator according to CB/T6U1, 18 ml/L of methyl red alcohol and 2 ml/L of polyol ethanol, mix with ethanol water: CCH3PO4 (precision 0.04002), put it in a 250mL bottle, add ethanol water to 5 ml/L, shake until the sample is evenly dissolved, add 4-6 ml of indicator, and filter with sodium hydroxide standard filter until the color changes from red to dark green. Make a vacuum determination after a certain time.
4.5.3 Calculation
The acidity X of the sample expressed as the mass fraction of sulfuric acid is calculated by (cyclic)-direct formula (2), X: - Yo)xo.oMs
Where: - the actual concentration of the sodium hydride standard titration solution, mol/mol; - the volume of the standard sodium hydroxide standard solution eliminated by the titration sample, m.
); 049
The volume of the sodium hydroxide standard solution eliminated by the titration blank solution, m. The mass selected by the test,
and 1.00L sodium hydroxide standard titrator: c0V-101/Gas ChimmQ or a carrier with the same performance), 15-~180℃, color details heat treatment machine.
Micro single sampler: 0
4.6.1.2 Reduction and solution
Triazine.
Phosphorus tris(III) ester: analytical grade, known content, greater than or equal to 99%, 4.6.1.3 Preparation of color column
a). Coating of stationary solution
Accurately weigh 0.3 μg of V-17 stationary solution in a 25cm3 beaker, add a suitable amount of triazine (slightly larger than the carrier) to completely dissolve it, pour in 5% sodium hydroxide, gently stir, mix it and make the agent nearly stable, then put the filter cup in a 120℃ oven for 1h, take it out and put it in a desiccator to cool to room temperature. b) Filling of the tower
Connect a small vortex funnel to the outlet of the washed color column, fill the prepared filling material in batches, and at the same time continuously lighten the wall, until it is filled to 1.5cm from the outlet of the two rods. Move the funnel to the entrance of the color column, and place a small ball of alkylated glass at the end of the mouth. Through the nuclear leather tube, open the vacuum pump, and continue to fill the filling material, continuously lighten the wall, and the filling is evenly and densely filled. After filling, add a small ball of cotton at the inlet, and add appropriate amount of cotton to prevent the filling from being moved. ) Aging of the chromatographic column
Connect the inlet of the chromatographic column to the gasification column, and do not connect the detection area at the outlet. Use a 20mL/min flow rate to heat the column to 0℃ and age it at this temperature for 481. After the aging of the chromatographic column is completed, connect the outlet of the column to the detector. 4.6.1.4 Gas Chromatography Conditions
Temperature, start: keep for 2min, increase the column chamber to 150℃ at a rate of 6℃/min, and keep it at this temperature for 2min, then increase the column chamber to 240℃ at a rate of 12℃/1min and keep it at this temperature for 1Umin. Chemical group 2:45
Detection chamber fullness: 233--250
Gas flow rate (mL/miu), carrier gas (N) 80. Multigas 80, digital gas 300) injection volume. 1.
Warranty time: phosphoric acid triformic acid about 7min. The above spherical gas chromatography operating conditions are typical operating conditions. According to different instrument characteristics, the given operating parameters can be appropriately adjusted to obtain the best effect. Typical gas chromatography spectra of trimethyl phosphate in monocrotophos emulsions are shown in Table 2.SE-K. 4.6.1.5 Determination steps a) Preparation of standard solution HG3300-2001 Gas chromatography-mass spectrometry [· methyl phosphate] Gas chromatography-mass spectrometry of trimethyl phosphate in monocrotophos emulsions 25.00 g/min) Weigh 1.12 [accurate to 0.1K10 2 s] of dimethyl phosphate and add 50 mL of dimethyl phosphate. b. Preparation of sample condensate
Weigh 2.0 ml of sample <If the sample is solid or has condensate, heat it to 25 °C to allow it to completely dissolve, and adjust the volume to 0.2>, accurately to 0.3>, into a 50 ml volumetric flask, add 3 ml of methyl alcohol, dissolve, adjust to volume, and condense.
Under the operating conditions of the working speed, after the instrument is stable, continuously inject several injections of standard sample solution until the peak areas of two adjacent injections of monomethyl phosphate change by less than 5%. Then, analyze and determine according to the order of standard sample, sample solution, sample solution, and standard sample solution. 4.6.1-6 Calculation
The total area of monomethyl phosphate in the two sample filters and the two standard filter solutions before the test are respectively averaged and the mass fraction of monomethyl phosphate in the two sample filters is calculated according to formula (3): A.-
HG3300--2001
The average peak area of dimethyl phosphate in the standard sample, A, is the average peak area of dimethyl phosphate in the sample solution, and the mass fraction of trimethyl aldehyde standard is calculated according to formula (3).
The mass of phosphoric acid and formaldehyde as the standard trimethyl phosphate is 1.0%. 4.6.1.7 Error
The difference between two parallel determination results should not be greater than 0.3%. The arithmetic mean is taken as the total mass of the determination. 4.6.2 Capillary column gas chromatography [separation method] 4.6.2.1 Instrument
Gas chromatograph: with gas ionization detector and separation injection device. Chromatographic column, 30m×0.25mm (id) double or quartz capillary column. The inner wall is coated with 5% benzene tert-butyl ketone, and the membrane sequence is 0.25um. Chromatographic data processor.
Injection system: with split flow injection device and inlet. Micro-injector: 10L.
4.6.2.2 Reagents and liquids
Methane,
Phosphoric acid trimethylol: known content, about 99.0%, 4.6.2.3 Gas chromatograph working conditions
Room temperature: start at 60℃ + maintain for 20minl then raise the sample room to 220℃ at a rate of 40℃./m, and maintain at this temperature for 10min.
Gasification base temperature, 220F.
Detection room temperature: 230-250 yuan,
Gas flow (ml./mn) Cutting gas (N) 8.0. Supplementary gas (N,) 35, gas 30, air 300. Split ratio 8:1:
Grid volume: 5.0u1.
Retention time: trimethyl phosphate about 16min, the above gas chromatography operation record is a typical operation. According to different characteristics, make appropriate adjustments to the given operation number in order to obtain the best effect. The typical gas chromatogram of dimethyl ester in long-lasting phosphorus emulsifiable concentrate is shown in Figure 2.4.6.2.4 Determination step depth
According to 4.6.1.5.
4.6.2.5 Sieve
According to 4,5.1.6.
4.6.2 6 Allowable difference
The difference between the results of two parallel determinations should not be large! .%, take the arithmetic mean value as the determination result, 4.7 Determination of water content without additives
4.7. 1 Only
suction period of the core type hopper, 63:
oven: (10512)%,
suction bottle: 250
before the density, 2u mL
4.7.2 Steps
HC3300:2001
Put the dust in a glass sand core funnel in a 1C5 oven until constant temperature is reached, weigh 2 samples (accurate to 0.01), rinse with 2 mL of water until the volume is small, cover with a lid, and cook until all the residues are dissolved: drain the solution through a glass sand core funnel, wash the residue in the funnel with water, wash once with 25 mL each time, and place the glass sand core funnel and filter in an oven until the residue is sub-zero.
4. 7. 3. The quality of the water is not divided into ×, (), or (1) sieve: x
In the formula, m is the quality of the core, the quality of the world or the quality of the adjustment bucket is m. The quality of the broken glass sand is selected and tested. g:bzxZ.net
4.8 Inspection and acceptance of products
The inspection and acceptance of products shall comply with the regulations of (H/1104: the numerical value shall be processed by the rounded value comparison method, 5. Marking. Label, packaging, purchase and transportation
5.1 The marking, label and package number of the long-acting phosphorus technical shall comply with the regulations of 6R379h. 5.2 The application of long-acting phosphorus technical shall be in accordance with the regulations of 6R379h. The net content of each insert is 200 kR：5.3 According to user requirements or order agreement, other forms of packaging can be used, and the supply and demand shall comply with the provisions of GB3796. 5.4 The packaging of long-acting phosphorus should be stored in a ventilated and dry room. (4)
5.5 During transportation, it should be strictly prevented from moisture and exposure to the sun, and should not be mixed with food, vegetables, and seasonings. Avoid contact with skin peptides and eyes, and prevent inhalation through the mouth. 5.6 This product is a highly moldy organophosphorus insecticide that can penetrate through the skin. When using this product, protective gloves, mouth and ears should be worn, and semi-clean protective clothing should be worn. After use, it should be washed with soap and water immediately. If the phenomenon of poisoning occurs, go to the hospital for examination and treatment in time. Tetratropine and pralidoxime are special antidotes.
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