Some standard content:
1CS 65.100
Chemical Industry Standard of the People's Republic of China
HG33003302—2001
Long-term phosphorus technical, emulsifiable concentrate, soluble liquid 20020124 Issued
Implementation on 2002-07-01
Issued by the State Economic and Trade Commission
Title No.: 10086—2002
EIG 33012001
Chapter 3 and Chapter 5 of this standard are mandatory, and the rest are recommended. This standard is a customized version of the mandatory chemical industry standard HG33011550 Long-term phosphorus. The determination method of the content of small-term long-acting pesticides in this standard is equivalent to that of the International Pesticide Analysis Cooperation Committee (JPAC287/T(/M/-) as the method: the main technical differences between the technical standard and HG3311-1991 are: the determination method of the micro-qualitative determination of the emulsion is changed from the required group 500 to the dilution group 200 times, the determination method of low stability is changed to the IPAC general method, the tri-ester index of lysate is added, and the determination method of the long-acting pesticide content is changed from the strength and colorimetric method and the layer colorimetric method to the liquid phase chromanometry. From the implementation of this standard, it will replace 1TG 3:01-190. This standard was issued by the State Administration of Petroleum and Chemical Industry and revised by the Technical Committee of the National Agricultural Standardization Promotion Committee. The responsible drafting unit of this standard is Shenyu Chemical Research Institute. The drafting units of this standard are Qingdao Pesticide Factory and Zhangjiagang Second Pesticide Factory. The main drafters of this standard are Xu Laijian, Xing Hong, Zhang Xuebing, Du Nanya, and You Xiao. This standard was first revised and issued in 1990 and converted into a mandatory chemical industry registration in 1999. The production code is 133011990. This standard is entrusted to the Secretary of the National Pesticide Standardization Technical Committee. 11
Chemical Industry Standard of the People's Republic of China
Mourocroophos Emulsifiable Concentrate
Mourocroophos Emulsifiable Concentrate ConcentrnteThe other names, formulas and chemical combinations of the active ingredients in this product are as follows: IS Generic name Mumu
CTPAC code 28?
Chemical name: dimethyl ([1-chloro-2-yl) acrylate Structure,
Empirical formula: CH.NOP
Relative density 22.3.2 (according to the 1997 International Standard for the determination of molecular weight) Biological activity: Soft insect
Heat gas jade (292
Density (20r): 1. 22 g/rm
Melting point: 54~55℃
Boiling point: 125℃(36.66ma)
HG3301—2001
Generation 33011990
Solubility (g/kg, 20%): 1000 in water, 700 in acetone, 800 in dichloromethane, 1030 in methanol, 250 in n-octanol, soluble in diesel and kerosene
Stability: unstable above 38, thermal decomposition is severe above 55. At 20℃, the hydrolysis half-life depends on the pH value. 5 is 96d. pH=7 is 65d. pH=9 is Ed. At low levels, it is not changed. It has peeling properties for the required plate, the stolen steel, and stainless steel 304.
1 Scope
This standard specifies the requirements, test methods, and marking, labeling, packaging and transportation of long-lasting emulsifiable concentrates. This standard applies to long-lasting phosphorus emulsifiable concentrates prepared from long-lasting phosphorus technical materials that meet the standards and suitable emulsifiers and dispersants. 2 Reference standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard was published, the versions shown were all valid. All standards will be revised. Parties that stop using this standard will be advised to use the following standards as soon as possible: G1/T601-1988 Preparation of standard solution for titration analysis (volume analysis) of chemical reagents GB/T16001S79(1989) Method for determination of moisture content of pesticides CB/T16U3-1579(1989) Method for determination of the water content of pesticide emulsions GH/T1604-1995 Acceptance rules for commercial pesticides State Economic and Trade Commission 2002-01-24 Approved 2002-07-01 Purchase and implementation
Method for sampling commercial pesticides
GET :503-
701589
(3HR790-1999 General Rules for Pesticide Packaging
G3H-2000 Emulsion Packaging
3 Requirements
3.1 It should be a brown or reddish brown liquid with no visible floating matter or debris. 3.2 Long-lasting emulsion should meet the requirements in Table 1
1 Long-lasting commercial emulsion Ear index
Effective research content
Water,
Acid waste (in H)),
Earthaldehyde content (confirmed to be 200%)
Branded aldehyde dimethyl methacrylate content, %
Low light secretion qualitative
Thermal qualitative
Note: Trimethylolpropane is significantly reduced, low temperature storage qualitative, at least once every three months. The test method|| tt||4.1 Sampling
According to the sampling method of emulsion and liquid state in GB/T16051979 (198S), the long-lasting storage emulsion oil should be wetted before sampling. The packages to be sampled are determined by a random number table. The final sampling volume should be no less than 2 m2. 4.2 Specific test
For the effective chromatographic method, this specific test can be carried out simultaneously with the determination of effective phosphorus. Under the same chromatographic operating conditions, the relative difference between the retention time of one peak of the sample solution and the chromatographic retention time of the effective phosphorus in the standard solution should be within 1.5%. 4.3 Determination of the content of effective phosphorus
4. 3.1 Method Summary
In the sample preparation, the aqueous solution of ethyl encephalate was used as the mobile phase, and the reverse phase chromatography was performed on a chromatograph filled with iebrospher RP-1% (diameter m), using an old UV detector and the long-acting phosphorus content was determined by an external standard. 4.3.2 Instrument
Phase chromatograph: equipped with a UV detector and a quantitative injection valve. Chromatographic data processor:
Chromatography: 4. Fanmti.il.) × 25Gmm stainless steel tube - filled with Iichrn5pher RP-18 (rotation diameter 5m) filler (or other with the same social effect but with C free spectrum tube)
Filter: filter membrane pore size about 0.45pm.
Micro-inlet, 50E.
4.3.3 Reagents and energy
: Chromatographic grade: www.bzxz.net
Methyl acetate: chromatograph.
Water, new condensate water.
HG 3301.2001
Mobile phase: CH:OH:CH, CN-H0) = 10:10:80. Long-term accurate standard sample, known content, greater than or equal to 98.0%. 4.3.4 Liquid chromatography operation
Column, cross temperature.
Mobile phase flow rate: 1.0L/min.
Detection tube length: 2301m.
Injection volume, 10 μl
Retention time: 1.3min
The above-mentioned chromatographic operation conditions are typical operation parameters. According to the characteristics of different instruments, the given operation parameters can be appropriately adjusted to obtain the best effect. The typical chromatographic diagram of chromatographic analysis ... 4.3.5.2 Preparation of sample solution
Weigh the sample containing C.1k (previously diluted to 0.0302R) in methanol and add 5.00mL of the sample to a 50mL volumetric bottle. Dilute with methanol, mix well, and then sterilize with a 45 μm membrane for 15 min.
4.3.5.3 Determination
H 3301—2001
Under the above operating conditions, after the instrument is stable, add the standard sample solution until the relative change of the area of the two adjacent long-term sample solutions is less than 1.0 μg, and then perform analysis in the order of standard solution, reading solution, sample solution, and standard solution. 4.3.6 Calculation
The peak areas of the long-acting phosphorus in the two standard sample drops before the two needles of the test range are averaged. The mass fraction of the long-acting phosphorus in the sample (%) is calculated according to formula (1): X, = Amp
Where: A, is the average value of the long-acting phosphorus area in the standard solution! A.—The average value of the effective area of the sample solution tThe mass of the standard sample B
t-··The mass of the sample g
The effective area of the standard sample,
4.3.7 The difference between the results of two parallel determinations shall not be greater than 1.5%. The arithmetic mean shall be taken as the determination result. 4.4 Determination of water content
The Karl-Fischer method in GB/T 160 (1979 (1969) is followed. The water determination method according to the conditions is allowed to be used. 4.5 Determination of acidity
4.5.1 Reagents and reagents
Standard titration solution of sodium hydroxide: (rNuH) 0.0n1/. Prepare according to the G/TG: mixed indicator: 1g/L methyl ethyl ethanol solution 8mL and 1g/L cresol green ethyl solution 12mL. 4.5.2 Determination of light intensity
Weigh sample 1 to an accuracy of 0.0002) in a 2-mL flask, add ethanol water solution to make the mixture uniformly dissolved, and use sodium hydride standard solution to filter until the color changes from pale red to green, and at the same time make a white determination.
4.5.3 Calculate the acidity X (%) of the sample expressed as a fraction of
age, and calculate r(V.-V.X0. u49.
：-00
Wherein:
actual concentration of sodium hydroxide standard titration solution, nl/L; volume of sodium hydroxide standard titration solution consumed in titration, mL; volume of sodium hydroxide standard titration solution consumed in titration, mL;
0.049-mass of sodium hydroxide equivalent in grams to 1.00% sodium hydroxide standard titration solution [(Na0H)=1.00DI/L]
4.6 Determination of trimethylol phosphate content
4.6.1 Filling gas chromatograph
4.6. 1.1 Only the gas chromatography instrument
gas color collection: and the gas chromatography instrument with fire enhancement ionization: 2 m>2. 2 mT~-4. 0 mn:ti. d. >Silica gel filler: 3% Q-1)! /GasChrnmQ (or carrier with similar performance), particle size 150--180 μm chromatographic phase single machine.
Microdisc pusher:
4.6.1.2 Reagents and solutions
Trimethyl methane.
HG3301-2001
Trimethyl phosphate: analytical grade, with a substance content of greater than or equal to. 0%：4.6.1.3 Preparation of chromatographic batches
a) Fixation
Accurately weigh 0.3R0V17 fixation to obtain 250ml. Add an appropriate amount (slightly larger than the volume of the solvent> chloroform) to the solution and dissolve it completely. Pour 9.7g of the solvent and gently stir to make it uniform and make the solvent almost absorbed. Then dry the solution in a 120℃ medium for 1h, take it out and place it in a dry and cold place.||t t||6) Filling of the color column
Put a small funnel into the exit of the washed and dried color column, and fill the prepared filling material into the column in batches, while continuously lightly covering the column wall until the whole point is 1.5n away from the exit. Insert the funnel into the entrance of the color column, and fill a small ball of silica gel at the exit end, connect it to the vacuum machine through a rubber tube, open the vacuum system, and continue to fill the environment with materials: and continuously lightly generate energy Reduce the filling width and fill it completely. Use cotton at the entrance and use proper pressure to keep the filling from moving. Aging of the color wall at the left side
Connect the color column end to the vaporization chamber, and do not connect the detector at the outlet. Pass the carrier gas (N) at a flow rate of mL/min, and heat it to 24℃ in stages and age it at this temperature for 43h. After the color column aging is completed, connect the column outlet to the detector. 4.5.1.4 Gas-bearing color column operation system
Temperature of the color chamber: start from 80℃, keep it for 2tnin: raise the temperature of the color chamber to 10℃ at a rising rate of 6℃/tmin, and keep it at this temperature for 2m. Then raise the temperature outside the color chamber to 24℃ at a rising rate of 12t/min, and keep it at this temperature for 15mim. Temperature of the vaporization chamber: 230℃.
Detection temperature: 230~250.
Gas flow rate (mi./min) Gas N, s0.3.0 Air 0 Injection volume; 2.1mL.
Retention time: Trimethyl phosphate about min
Upward reverse gas sweep chromatographic operation conditions, other product operation dream number: according to different instrument holding points, most of the given operations are adjusted appropriately in order to obtain the best effect, the typical long-term emulsion in the succinic acid diol gas cabinet color is shown in Figure 2, 17
2 (E106
4. 6.1.5 Determination steps a) Preparation of standard solution HC3301-2001 Gas chromatography chromatogram of 1-dry trimethylol ester 2-drying milk solution of methanol 25-30 mL) Weigh 1.0 μl of phosphine-1-one accurately to 0.02 μl, put it in a 50 mL volume bottle, add three kinds of metal, put it in the bottle, and make up to volume. b) Preparation of sample solution Weigh 3.0 μl of sample (accuracy 0.000 2 g), EC ml. Add chloroform to the sample, determine the concentration and the amount of trimethylol ether. Under the above operating conditions, after the instrument is stable, inject several injections of standard sample solution continuously until the area of two adjacent injections of trimethylol ether sample changes by less than 3%. Then, analyze and determine in the order of standard sample solution, test solution, sample solution and standard sample solution. 4.6.1.6 The areas of trimethylol ether in the adjustment solution prepared from the first injection and the two injections of standard sample solution before the sample are averaged. The mass fraction of trimethyl phosphate in the standard sample, x, (), is calculated according to (3): x,
wherein, 11 is the average area of monomethyl phosphate in the standard sample, A is the average area of trimethyl phosphate in the sample solution, A
the amount of standard precipitate of trimethyl phosphate, area
the pressure of the sample,
the mass fraction of trimethyl phosphate in the standard sample,%. 4.6.1.7 The difference between the results of two parallel determinations shall not be too large. Meaning: Take the arithmetic mean as the determination result. 4.6.2 Capillary in gas chromatograph (heat transfer) 4.6.2.1 Instrument
Gas chromatograph, with hydrogen flame ionization controller and split injection device, chromatographic column: 30 11: c0. 25 mmr. (id) double or non-flammable capillary, inner wall coated with 5% benzyl silicone, membrane sequence 0. 25 μm, other spectrum data processor,
injection system: with split injection transfer tube and quartz inner village: micro injection, 10JrL
4.6.2.2 Test and
Trisomethane.
Monomethyl phosphate: analytical grade, chromatographic content, 10% isocyanate. 4.6.2.3 Gas Spectroscopy Conditions
Chamber temperature: 50°C initially, maintained for 2 min; then the temperature in the chamber is raised to 220°C at a rate of 49°C/min and maintained at this temperature for 10 min.
Vaporization chamber temperature: 220°C.
Detection room leakage, 280~250℃
Gas pressure (/m: cutting gas (N2) 8.0, make-up gas (N2) 3, hydrogen 30, settling gas 300. Separation ratio: 8:1,
Inlet volume: 5.0L
Maintain the time, methyl antacid 16min.
The above-mentioned gas chromatography operating conditions are typical operating conditions. According to the characteristics of different receivers, the parameters can be appropriately adjusted to obtain the best effect. The typical gas chromatographic analysis of trimethyl phosphate in long-acting group milk sleeves is shown in Figure 2. 4.6.2.4 Determination steps
According to 4, 6.1. =.
4.6.2.5Calculation
According to 4.6.1. .
4.6.2.6 The difference between the results of the two parallel determinations within a certain period of time shall not be less than 0. The average value shall be taken as the determination result. 4.7 The qualitative determination of milk chain species
The formula is as follows: Dilute the selected sample 20 times with standard hard water and test it according to 6/T1 3. If there is no oil on the surface and no large precipitate on the bottom, it is qualified. 4.8 Low temperature barrier qualitative test
4.8.1 The test sample is kept in a centrifuge for 1 hour, and the presence of solid and precipitated substances is recorded. Continue to heat at ℃, centrifuge, and reduce the solid precipitate to 4
and record its properties.
4.8.2. Instrument end
Remove the temperature and keep it at 0±1).
HC3301—2001
Centrifuge tube: mL tube bottom with an accuracy of 5m
Classic centrifuge, equipped with high speed centrifuge tube.
4.8.3 Test steps
Take (10~1). Add the sample into the centrifuge, cool it in the refrigerator to (0±1)℃. Keep the centrifuge tube and the contents at (0±1)℃ for 1h, then adjust it once every two times, 155 each time, check whether there is any solid or oily substance separated, centrifuge it and place it in the refrigerator at (0±1)℃ for continuous vortexing. d, d later, take out the centrifuge tube. Stand at room temperature (not more than 20°C) for 3h, centrifuge for 15min (relative centrifugal force at the bottom of the tube is 50rg--500g+g is the acceleration), record the amount of precipitate at the bottom of the tube (specific oxygen 0.05mL). The precipitate is qualified if it does not exceed 0.3mL. 4.9 Thermal transfer qualitative test
4.9.1 Receiver
Standard temperature box (or constant temperature water bath): (54℃). 4.9.2 Medical reflector, 50ml.
4.9.2 Test time
Use an injection to inject about 30ml of emulsifiable concentrate sample into the clean mixture (avoid the sample contacting the bottle), place the bottle in ice salt solution to heat, and seal it with a high temperature flame (avoid the sample from leaking). At least one of them should be sealed, and the sealed ampoule should be placed in a metal container, and then the metal container should be placed in a constant temperature or constant temperature water for 14 days, and then taken out to cool to room temperature, and the outside of the ampoule should be wiped and weighed. For the sample with no change in the pressure plate, the long-term phosphorus content should be measured within 2 hours. After heating, except that the long-term phosphorus content is allowed to drop to 85% of the content measured before heating, the temperature is allowed to rise by 3%. Other indicators should still meet the standard requirements. 4.10 Inspection and acceptance of products
Inspection and acceptance of products shall comply with the provisions of GH/11604. For the handling of limit values, the static mean value comparison shall be adopted. 5 Marking, labeling, patina, transportation
5.1 The marking, labeling and packaging of long-lasting phosphorus emulsifiable concentrate shall comply with the provisions of GB37 and (K4838). 5.2 Long-lasting phosphorus emulsifiable concentrate packaging shall be stored in a ventilated and dry warehouse. 5.3 During transportation, strictly prevent moisture and fire. Do not place with food, chemicals, or other materials, avoid contact with skin and eyes, and prevent Prevent inhalation: 5.4 This product is a highly harmful organic iodine insecticide, which can enter the body through the skin. When using this product, you should wear protective hands, mouth and clean protective clothing. After use, wash it with soap and water immediately. If poisoning occurs, go to the hospital for examination and treatment in time. Atropine and chlorpyrifos are effective antidotes.
5.5 Under the specified storage and transportation conditions, the warranty period of long-acting emulsion is one year from the date of production. When the product is manufactured, it shall meet the requirements of Article 3. Within two years, the long-acting phosphorus content shall not be less than 31.0%, 20
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