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Chemical Industry Standard of the People's Republic of China
HG2464.2-93wwW.bzxz.Net
Phorate EC
1993-07-05 Issued
Ministry of Chemical Industry of the People's Republic of China
1994-01-01 Implementation
Chemical Industry Standard of the People's Republic of China
Phorate EC
Subject Content and Scope of Application
HG2464.2-93
This standard specifies the technical indicators of phorate EC and its inspection methods and inspection rules as well as marking, packaging, transportation and storage. This standard applies to phorate EC prepared from phorate technical and suitable emulsifiers and solvents. Active ingredient: Phorate
Chemical name: O,O-diethyl-S-(ethylthiomethyl) dithiophosphate Structural formula:
Molecular formula: CH17O2PSs
SCH2S-CH
Relative molecular mass: 260.38 (according to the international relative atomic mass in 1989) Reference standards
Dangerous goods packaging mark
Packaging storage and transportation pictorial mark
Preparation of standard solution for titration analysis (volume analysis) of chemical reagents GB/T 1600
Method for determination of moisture content in pesticides
GB1603
GB1604
GB1605
GB3796
GB4838
Technical requirements
Method for determination of stability of pesticide emulsions
Pesticide acceptance rules
Sampling method for commercial pesticides
General rules for pesticide packaging
Emulsifiable concentrate pesticide packaging
3.1 Appearance: Yellow-brown to brown transparent liquid. Phorate emulsifiable concentrate shall meet the following requirements:
Phorate, %
Acidity (in HSO.), %
Water, %
Emulsion stability (diluted 200 times)
Hot storage stability test1)
Low temperature stability test\)
Note: 1) Test at least once every six months.
Approved by the Ministry of Chemical Industry of the People's Republic of China on July 5, 1993
Implementation on January 1, 1994
4 Test methods
4.1 Determination of phorate content
HG2464.2-93
4.1.1 Summary of the method: The sample is dissolved in acetone and lindane is used as the internal standard. It is separated on a 12% DC-550 column and determined by a hydrogen flame ionization detector.
4.1.2 Reagents and solutions
Acetone: (GB686);
Lindane: (GB9559-88) internal standard (no impurities that interfere with the gas chromatography analysis); Phorate standard: known content ≥98.0%; Chromatographic stationary liquid: Silicone DC-550;
Carrier: chromosorbW·AW-DMCS (or other carriers with the same performance) 180~250μm (60~80 mesh); Internal standard solution: weigh 1.2g (accurate to 0.0002g) of internal standard lindane and place it in a 100mL volumetric flask, dissolve and dilute to the scale with acetone, and shake well.
4.1.3 Instruments
Gas chromatograph: with hydrogen flame ionization detector; recorder or integrator;
Chromatographic column: 2000×2mm (inner diameter) glass or stainless steel column tube, filled with 12% silicone DC-550/chromosorbW. AW-DMCS;
Micro-injector: 10uL.
4.1.4 Operation steps
4.1.4.1 Preparation of chromatographic column
(1) Coating of stationary liquid
Accurately weigh 1.2g of DC-550 and place it in a 250mL round-bottom flask with a standard opening of No. 24. Add enough chloroform to dissolve it, add a certain amount of carrier according to the ratio of the stationary liquid so that it is just immersed in the stationary liquid solution, and then use a rotary evaporator to coat it. Start the rotary evaporator under reduced pressure and heat it with a water bath or infrared lamp until the solvent is almost dry. Then place it in a 120℃ oven and dry it for 2 hours. Take it out and cool it down before sieving it for later use.
(2) Filling of the chromatographic column
Connect a small funnel to the inlet of the clean and dried column tube, and plug an appropriate amount of glass wool into the outlet, wrap it with gauze, and connect it to the vacuum pump through a rubber tube. Start the vacuum pump and add the column filler from the funnel in batches. At the same time, tap the column tube continuously to make the filler fill the chromatographic column evenly and tightly, then stop the vacuum pump. Also plug a small ball of glass wool into the inlet and press it appropriately to prevent the filler from moving. (3) "Aging" of the chromatographic column
Connect the inlet of the chromatographic column to the vaporization chamber of the gas chromatograph, and do not connect the outlet to the detector for the time being. Raise the temperature to 230℃ in stages at a carrier gas (nitrogen) flow rate of about 15mL/min and "age" it at this temperature for 24 hours. After cooling down, connect the outlet of the column to the detector. 4.1.4.2 Chromatographic operating conditions
Column box: 180℃±2℃;
Gasification: 250℃±2℃;
Detection: 250℃±2℃;
Gas flow rate
Carrier gas (N,): 50mL/min;
Hydrogen: 40mL/min;
Air: 300~400mL/min;
Amplification and attenuation:
HG2464.2—93
Adjust amplification and attenuation so that the chromatographic peak height of phorate and internal standard is 60~80% of the full scale of the recorder. Retention time
Phorate is about 6min, and internal standard lindane is about 8min. Gas chromatogram of phorate
1-phorate; 2-internal standard.
Analysts can adjust the chromatographic operating conditions appropriately according to the differences in instrument performance and chromatographic columns in order to obtain the best results. 4.1.4.3 Determination steps
(1) Preparation of standard solution
Weigh 0.1g (accurate to 0.0002g) of phorate standard sample and place it in a stoppered glass bottle. Use a pipette to accurately draw 10mL of internal standard solution and add it to the same bottle. Then add an appropriate amount of acetone to fully dissolve and shake well. (2) Preparation of sample solution
Weigh 0.15g (accurate to 0.0002g) of phorate emulsifiable concentrate sample and place it in another stoppered glass bottle. Use a pipette to accurately draw 10mL of internal standard solution and add it to the same bottle. Then add an appropriate amount of acetone to fully dissolve and shake well. (3) Determination
Under the above chromatographic conditions, after the instrument baseline is stable, inject several needles of standard solution continuously, calculate the repeatability of the relative response value of each needle, and when the relative response values of two adjacent needles are basically close, perform chromatographic analysis in the following order. The injection volume is 1uL. a. Standard solution; b. Sample solution; c. Sample solution; d. Standard solution. 4.1.4.4 Calculation
Average the measured ratios of the peak areas of a, d and b, c of phorate to the internal standard. The mass percentage content of phorate X1 is calculated according to formula (1):
Where: \1-the average value of the peak area ratio of phorate to the internal standard in the standard solution; 12-the average value of the peak area ratio of phorate to the internal standard in the sample solution; m1-the mass of phorate standard, g;
the mass of phorate sample,;
the mass percentage content of phorate standard. 4.1.4.5 Allowable error
The difference between the results of two parallel determinations of this method shall not exceed 1.5%. The average value shall be taken as the reported result. (1)
4.2 Determination of acidity
4.2.1 Reagents and solutions
95% ethanol (GB679);
HG2464.2-93
Sodium hydroxide (GB629); c(NaOH)=0.02mol/L standard titration solution, prepared according to GB601; methyl red (HG3-958); 1g/L ethanol solution. 4.2.2 Determination steps
Accurately weigh 1~2g of sample (accurate to 0.0002g) and place it in a 250mL conical flask. Add 25mL of 95% ethanol, mix well, add 3 drops of methyl red indicator solution, and titrate with sodium hydroxide standard titration solution until it just turns yellow. The acidity mass percentage of the sample (X2) is calculated according to formula (2): cV×0.049×100
Wherein: c—actual concentration of sodium hydroxide standard titration solution, mol/L; V—volume consumed by sodium hydroxide standard titration solution, mL; m——mass of the sample, g;
0.049——mass of sulfuric acid in grams equivalent to 1.00mL sodium hydroxide standard titration solution Lc(Na0H)=1.000mol/L. 4.3 Determination of water content
Determine according to the Karl Fischer method in GB/T1600. 4.4 Determination of emulsion stability
Determination is carried out according to GB1603. The dilution ratio is 200 times, and the determination temperature is 30±1℃. 4.5 Hot storage stability test
4.5.1 Instrument
4.5.1.1 Constant temperature water bath: control the temperature to 54±2℃; 4.5.1.2 Ampoule: capacity is about 10mL, long neck. 4.5.2 Determination
Pour about 5~7mL of sample into a clean ampoule, seal it with a gas lamp, and store it in a constant temperature water bath at 54±2℃ for 14 days. The relative decomposition rate of the active ingredient of the sample after hot storage is not more than 5% compared with that before hot storage. 4.6 Low temperature stability test
4.6.1 Instrument
Ice water bath: control the temperature to 0±1℃.
4.6.2 Operation steps
Take about 50mL of the sample into a 100mL beaker, put it into an ice-water bath, keep the temperature at 0±1℃, leave it for 1h, stir it once every 15min, and stir it for 0.5min each time, then observe whether there is solid precipitation in the cup. If not, it is qualified. 5 Inspection rules
5.1 Phorate EC should be inspected by the quality inspection department of the manufacturer. The manufacturer should ensure that all phorate EC shipped out of the factory meets the requirements of this standard. Each batch of phorate EC shipped out of the factory should be accompanied by a quality certificate. 5.2 The acceptance rules of phorate EC shall be carried out in accordance with GB1604. 5.3 The sampling method shall be carried out in accordance with GB1605.
5.4 The amount of each batch of phorate EC shall not exceed the capacity of the packaging storage tank (metering tank), and the inspection batch number, production batch number and packaging batch number must be consistent.
5.5 If one of the indicators in the test results does not meet the requirements of this standard, the sample should be doubled and the test results should be retested. If even one item does not meet the requirements of this standard, the entire batch of products cannot be accepted. 5.6 If there is any objection to the product quality, it can be resolved through negotiation between the supply and demand parties, or the selected arbitration institution can conduct arbitration inspection according to this standard. 4
6 Marking, packaging, transportation and purchase and storage
HG2464.2—93
6.1 Each box and each bottle should be marked with: manufacturer name, product name, trademark, production batch number, net weight, production permit number, pesticide registration number, this standard number and usage and precautions (limited to the bottle label) and the relevant signs should be marked according to the provisions of GB190, GB191, GB3796 and GB4838. It should be marked that this preparation should not be directly sprayed with alcohol and is only used for seed treatment. 6.2 Phorate EC should be packaged in clean and dry glass bottles. The net weight of each bottle is allowed to fluctuate by ±2%, but the net weight of each box shall not be less than the marked weight. The bottles are padded with appropriate materials such as straw covers and straw mats, and are tightly arranged in wooden boxes or calcium plastic boxes. 6.3 Each batch of packaged finished products should be accompanied by a quality certificate, which includes: manufacturer name, product name, production batch number, factory date, net weight and the number of this standard. 6.4 During storage and transportation, it should be strictly prevented from moisture, heat and sunlight, and maintained in good ventilation. It should not be mixed with food, seeds, and feed, and should avoid contact with the skin and inhalation through the mouth and nose.
6.5 Warranty period: Under the specified storage and transportation conditions, the warranty period of phorate EC is 2 years from the date of production. Additional remarks:
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the technical jurisdiction of the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard is drafted by Tianjin Pesticide General Factory. The main drafters of this standard are Miao Tianzeng, Wang Yulan, Li Junge and Hou Wei.
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