Some standard content:
Chemical Industry Standard of the People's Republic of China
HG2464.1—93
Phorate Technical
Published on July 5, 1993
Ministry of Chemical Industry of the People's Republic of China
Implemented on January 1, 1994
Chemical Industry Standard of the People's Republic of China
Phorate Technical
Subject Content and Scope of Application
HG2464.1—93
This standard specifies the technical indicators of phorate technical and its inspection methods and inspection rules as well as the requirements for marking, packaging, transportation and storage.
This standard applies to phorate technical synthesized by condensation of 0,0-diethyl dithiophosphoric acid, ethyl mercaptan and formaldehyde. Active ingredient: phorate
Chemical name: O,O-diethyl-S-(ethylthiomethyl) dithiophosphate Structural formula:
Molecular formula: CH1O,PS3
SCH2S-CHs
Relative molecular mass: 260.38 (according to the international relative atomic mass in 1989) 2 Reference standards
Dangerous goods packaging mark
Packaging storage and transportation pictorial mark||tt| |Preparation of standard solution for titration analysis (volumetric analysis) of chemical reagents GB/T1600
GB1604
GB1605
GB3796
3 Technical requirements
Method for determination of moisture content in pesticides
Pesticide acceptance rules
Sampling method for commercial pesticides
General rules for pesticide packaging
3.1 Appearance: Yellow-brown to brown transparent liquid. 3.2 Phorate technical shall meet the following requirements: %
Phorate
Acidity (in HSO.)
Superior product
Approved by the Ministry of Chemical Industry of the People's Republic of China on July 5, 1993
First-class product
Qualified product
Implemented on January 1, 1994
4 Inspection method
4.1 Determination of phorate content
HG 2464.1—93
4.1.1 Summary of method: The sample is dissolved in acetone with lindane as internal standard, 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 (without impurities interfering with the gas chromatography analysis); Phorate standard: known content ≥98% (m/m); Chromatographic stationary liquid: Silicone DC-550
Carrier: chromosorbWAWDMCS (or other carriers with the same performance) 180250μm (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/chromosorbWAWDMCS.
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 two 250mL 24-gauge round-bottom flasks, 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 cleaned 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 filling material from the funnel in batches. At the same time, tap the column tube continuously to make the filling material even and tightly fill the chromatographic column, then stop the vacuum pump. Also plug a small ball of glass wool into the inlet end and press it tightly to prevent the filling material from moving. (3) "Aging" of the chromatographic column
Connect the inlet end of the chromatographic column to the vaporization chamber of the gas chromatograph, and do not connect the outlet end 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" at this temperature for 24h. After cooling down, connect the column outlet end to the detector. 4.1.4.2 Chromatographic operating conditions
Column box: 180℃±2℃;
Vaporization: 250℃±2℃;
Detection: 250℃±2℃;
Gas flow rate
Carrier gas (N2): 50mL/min;
Hydrogen: 40mL/min;
Air: 300~400mL/min;
Amplification and attenuation: Adjust the amplification and attenuation to make phorate and the internal standard peak height is 60-80% of the full scale of the recorder. 2
HG2464.1—93
Gas chromatogram of phorate
1-phorate; 2-internal standard.
Retention time: phorate is about 6 minutes, and the internal standard lindane is about 8 minutes. The analyst 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 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 solutionWww.bzxZ.net
Weigh phorate technical drug Place 0.1g (accurate to 0.0002g) of the sample in another glass bottle with a stopper, use a pipette to accurately draw 10mL of the 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, continuously inject several needles of the standard solution, 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 a, d and b, c ratios of the peak area of methyl parathion to the internal standard. The mass percentage content of methyl parathion X is calculated according to formula (1):
Where: 1-methyl parathion and the standard solvent The average value of the ratio of the peak area of the internal standard; 12——The average value of the ratio of the peak area of the sample solution phorate to the internal standard; mi—The mass of the phorate standard, g;
m2——The mass of the phorate sample, g; milk——The mass percentage of the phorate standard. 4.1.4.5 Allowable difference
The difference between the results of two parallel determinations should not be greater than 1.5%. Take the average value as the reported result. 4.2 Determination of acidity
4.2.1 Reagents and solutions
95% ethanol (GB679);
HG2464.1-93
Sodium hydroxide (GB629) standard titration solution: c(NaOH)=0.02mol/L, prepared according to GB601; Methyl red (HG3-958): 1g/ethanol solution. 4.2.2 Determination steps
Accurately weigh 1-2g (accurate to 0.0002g) of the sample, 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 X of the sample is calculated according to formula (2): X=×0.049×100+
Where: c—actual concentration of sodium hydroxide standard titration solution, mol/L, V—volume of sodium hydroxide standard titration solution consumed, mL; m—mass of the sample, g,
0.049—mass of sulfuric acid in grams equivalent to 1.000mL sodium hydroxide standard titration solution Lc(Na0H)=1.000mol/LJ. 4.3 Determination of water content
Determine according to the Karl Fischer method in GB/T1600. 5 Inspection rules
5.1 Phorate technical should be inspected by the quality inspection department of the manufacturer. The manufacturer should ensure that all phorate technical shipped out of the factory meets the requirements of this standard. Each batch of phorate technical shipped out of the factory should be accompanied by a quality certificate. 5.2 The acceptance rules for phorate technical shall be carried out in accordance with GB1604. 5.3 The sampling method shall be carried out in accordance with GB1605.
5.4 The quantity of each batch of phorate technical should 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 inspection results does not meet the requirements of this standard, the sample should be doubled and the results should be re-tested. If even one item does not meet the requirements of this standard, the entire batch of products cannot be accepted. 5.6 In case of objection to product quality, the supply and demand parties can negotiate to resolve it, or the selected arbitration institution can conduct arbitration inspection according to this standard. 6 Marking, packaging, transportation and storage
6.1 Each barrel should be marked with: manufacturer name, product name, trademark, batch number, net weight, grade, production license number, pesticide registration number and this standard number; and the relevant marks should be marked according to the provisions of GB190, GB191 and GB3796. 6.2 Phorate technical should be packaged in clean, dry and firm coated iron barrels (barrel skin thickness 1.2~1.5mm), no leakage, and the net weight of each barrel is 200kg.
6.3 Each batch of packaged finished products should be accompanied by a quality certificate, which includes: manufacturer name, product name, batch number, date of manufacture, net weight, and this standard number and quality grade. 6.4 During storage and transportation, it must not be violently hit or inverted. It must be strictly protected from moisture, heat and sunlight. It must be well ventilated and must not be mixed with food, seeds, or feed. It must be avoided from inhalation through the mouth or nose and contact with the skin. 6.5 Warranty period: Under the specified storage and transportation conditions, the warranty period of phorate technical is 2 years from the date of production. 4
Additional notes:
HG2464.1—93
This standard was 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 was drafted by Tianjin Pesticide General Factory. The main drafters of this standard are Miao Tianzeng, Wang Yulan, Li Junge, and Hou Wei. 5
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