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
2002-07-01 Implementation
National Economic and Trade Commission Issued
Service No.: 10087—2002
HG3302—2001
Chapter 3 and Chapter 5 of this standard are mandatory, and the rest are recommended. This standard is a mandatory chemical. 1 Industry Standard HG350%-90&Long-term phosphorus can be used for natural and non-toxic properties. The determination method of long-acting instantaneous content in this standard is equivalent to the International Pesticide Classification Committee (IPA: 28/SL/M/- method. The main technical differences between this standard and IIG33021S9C are: the determination method of temperature-stable components is changed to CIPAC applicable method, and the trimethylol phosphate index is added. The determination method of long-acting phosphorus content is changed from gas chromatography and thin layer chromatography to liquid chromatography. From the implementation of this standard, it will replace 11G33021990. This standard was originally proposed by the National Agricultural Standardization Administration and the Chemical Industry Administration. This standard is under the jurisdiction of the National Pesticide Standardization Technical Committee. This standard is responsible for The drafting unit: Shenyang Chemical Research Institute, Qingdao Pesticide Co., Ltd., Zhangjiagang Second Agricultural Innovation Institute, and the drafting directors of this standard are Xu Laiwei, Xing Hong, Zhang Xuebing, Du Yongqiang, Fang Wei, and Shi Youqing. This standard was first issued in 1993 and converted into a mandatory chemical industry standard in 1999, renumbered as HG3302199n. This standard is entrusted to the Secretariat of the National Pesticide Standardization Technical Committee for reading and interpretation. 21 People's Republic of China and National Chemical Industry Standards
Mnnocnotophos soluble liquid
Mnnocnotophos Other names, structural formulas and non-physical and chemical parameters of the active ingredient of this product are as follows: IS common name Mnnrtotnphas
CIPA digital code: 287
Chemical name dimethyl-1-yl (methyl groupwww.bzxz.net
Formula:
Empirical formula CHNO,F
Relative molecular weight, 223.2 (according to 1S97 international standard) Biological properties: Insecticidal
Hot pressure 20);291Pa
Degree of heat (20t) 1.22g/cm
Point.54-.55*
Point 12s (66.56mP)
HG 33022001
Generation #11GJ302193C
Decomposition (g/kg.20T) 1000 in water, 100 in acetone, 800 in methyl alcohol, 1003 in n-octanol, 250 in toluene, slightly less than diesel and kerosene
Stable above 8, thermal decomposition above EC, at 20, the hydrolysis half-life is 6d when pH value is H5, 66d when pH value is 1/d when pH=9. Not stable in low alcohol: slightly corrosive to black iron plate, high-grade steel, and stainless steel 304.
1 Scope
This standard specifies the requirements, test methods, and labeling, packaging, storage and transportation of long-term phosphorus degradation test. This standard is used for the long-acting phosphorus-containing granules prepared from long-acting instant source drugs and suitable droppers and spurs. 2 Reference Standards
The provisions contained in the following standards constitute the provisions of this standard through their use in this standard: When this standard is published, the versions shown are valid. All standards will be revised, and the parties using this standard should explore the possibility of using the latest version of the following standards. GB/01-158 Chemical analysis (quantity analysis) Preparation of standard soluble sugars GR/1601-1979 1939 Determination of moisture content in pesticides GB/T1603-1971949 Determination of stability of agricultural emulsions B/1604-995 Acceptance test of agricultural products
National Economic and Trade Commission 2002-01-24 Approved 2002-07-01 Buy bottles
GB/T 1E05-1T9 (158U)
IG3302
Method for the collection and purchase of agricultural products
General rules for agricultural product packaging
GB3796-1999
GR 4838-20D0
3 Requirements
Agricultural grape emulsion
3.1 Appearance: Red uniform color, without total floating matter and sediment. 3.2 Long-term phosphorus fusible liquid agent should meet the requirements of Table 1 2001
Table 1 Long-term phosphorus fusible liquid agent preparation project index
Evening seat (with [I, SO, Calculation: ,%
Total rare earth (analysis 20 times)
Phosphamide monomethylamine content -56
Low stability
Perfect stability
Can be used
Note: Purple single three-print enzyme content, tissue sensitivity, spermatogenesis, twice a month, 4 test methods
4.1 Sampling
126 Economic performance plan
According to G1/T1605-197%<1589>\emulsion and micro-body state sampling\ method. Before sampling, mix the long-acting iodine soluble liquid evenly and determine the sampling amount by function table method The final sampling volume should be no less than 200mL. 4.2 Identification test
High-efficiency chromatography: This identification test can be carried out simultaneously with the determination of the long-term effective content. Under the same chromatographic operating conditions, the retention time of the sample chromatographic peak and the retention time of the long-term effective solution in the probe solution should be within 1.5%. Gas chromatography: Under the same chromatographic operating conditions, the retention time of the test chromatographic peak and the retention time of the long-term effective peak in the standard solution should be within 1.5%. 4.3 Determination of long-term effective content
4. 3. 1 Method
The sample is dissolved in alcohol, methanol, ethyl acetate-water mixture is used as the mixture, and reverse phase liquid chromatography separation is performed on a chromatographic phase filled with [ichroher RF-18 (full grid 5m), using an external detector, and the content is measured by external standard method. 4.3.2 Apparatus
Liquid chromatograph: with ultraviolet variable wavelength detection and fixed injection. Chromatographic processor.
Color property: 4.6num(id)X25 0mm stainless steel. 1. Ichrspher RP-18 (particle size 5r) culture medium (or other chain core chromatograph with the same effect?
filter: wrong membrane 0.45gm
micro-inlet filter: 50
4.3.3 test liquid
clear: chromatographic energy,
methanol: chromatographic sensitive,
water: new Lai double distilled water.
[IG3302—2001|| tt||Flow rate: CH.OHCHN:HU)-10:10:B0
Long-acting group standard sample: known content, greater than or equal to 9.5%, 4.3.4 phase chromatography operation conditions
Dufu: room temperature,
Mobile phase flow rate, 1.5 ml./min.
Measurement wavelength: 250mm.
Near sample volume: 10μL,
Reserved words, long-acting operation about 11.3in
The above liquid phase Chromatographic operating conditions are typical operating parameters. According to the characteristics of different instruments, the given operating parameters can be adjusted to obtain the most effective solution: the typical liquid chromatogram of long-acting phosphorus acid degradable agent is shown in Figure 1. Figure 1-Long-acting group
Figure 1 Condensation chromatogram of long-acting acid degradable agent 4.3.5 Steps
4.3.5.1 Standard determination The obtained standard sample (1) is called long-acting enzyme standard (accurate to 0.32) and is dissolved in 4% methanol. The standard sample is determined. 5.00 ml is taken with a transfer tube and placed in a volumetric flask at 1000 mT., and the volume is made up with methanol. 4.3.5.2 Preparation of sample solution
Weigh the sample solution containing 3.1g of long-acting agent (accurately 9.0002g), put it in a 591mL translucent bottle, mix it with a pipette, adjust the volume, and mix well. Use a pipette to draw 0.0m. Place it in another 50mL volumetric bottle, adjust the volume with ethanol, and filter it through a 0.45m filter membrane. 25
4.3.5.3 After the measurement
H33022001
Under the above color selection operating system, after the instrument is stable, continue to inject the standard sample in reverse order until the change of the long-acting agent on the adjacent needle is less than 1.C%, quickly add the standard solution, the sample solution, the sample solution, and the standard sample solution. 4.3. 6. The measured drop of the two samples and the concentration of the long-acting phosphorus in the two standard sample liquids after the sample are averaged. The mass fraction of long-acting phosphorus in the sample is X (%).Calculate according to formula (1): _AF
--the average value of the peak value of long-acting phosphorus in the standard sample: A
A, "the average value of the long-acting phosphorus in the sample solution; m
the surface area of the standard sample·month;
the mass of the sample·5;
P--the mass fraction of long-acting phosphorus in the standard sample,%. 4.3.7 The difference between the two parallel determination results should not be greater than 1.5※, and the average value is taken as the determination result. 4.4 Determination of moisture
According to F160)--19? (93) before \ Karl, the method of rest \. It is allowed to use a moisture determination hinge with equivalent accuracy for determination, 4.5 Determination of alcohol content
4.5.1 Preparation and filtration
Oxidation standard titration solution: 2 (Na2O3)-0.02ml/L. Prepare the mixed indicator according to GB/T60; 1% sodium iodide solution and 1% iodine green ethanol solution 12ml. Mix well. Alcohol-water solution: wCH3CH4OH·H2O3=11
4.5.2 Titration step
Weigh sample 1 (accurate to 0.0m2) in a 250ml small flask, add 50mL of ethyl alcohol, shake to make the solution uniform, add 4~6ml of mixed indicator, and titrate with hydroxyl alcohol until the red color turns to a flash color and the endpoint is determined at the same time
4. 5. 3. Calculate the concentration of the sample by the mass of the acid: (must be calculated according to formula (2): X: -V/-V) x 0.049
Actual concentration of the sodium hydride standard titration solution, mol/.V-volume of the sodium hydroxide standard titration solution consumed by the titration sample, IuL; W
Volume of the sodium hydroxide standard titration solution consumed by the titration blank solution, mL; The mass of the selected solution, more than
. and 1.mT. sodium hydroxide standard are fully determined. The mass of sulfuric acid expressed in grams,
4. Determination of trimethyl ester content in B
4.6.1 Gas chromatograph with stirring
4.6.1. 1. Instruments
Gas chromatograph: flame ionization detector. Chromatographic properties: 2 m×2.2 mm~4.3 mm (i, d, ) silica gel, filler: 3% UV101/G (HramQ or equivalent performance medium>: diameter 15)-.180 μm colorimetric data processor.
Micrometer, 10.
4.6.1.2 Test solution
A little methane.
IC3302---2001
Methyl phosphoric acid: analytical grade, known content is greater than or equal to 99.05%. 4. 6.1.3 Preparation of color reverse drawing
a) Fixing agent coating
Accurately weigh 0.3KV-17 fixing agent 253ml. beaker, add carrier block (slightly larger than the carrier body) and 1,000ml of fluoromethane to make it completely alcoholyzed, pour in 90% carrier, gently stir to make it slightly hydrated and make the agent almost dry, then put the beaker in a 1% supply box to dry for 1h, take out the carrier and cool it in a desiccator until it is dry, b) Filling of chromatogram
Add a small amount of the fixing agent to the outlet of the chromatographic column that has been immersed in the image, and fill the prepared block into the column in batches, while not Tap lightly until the whole column is filled 1.5 cm away from the outlet. Move the column to the inlet of the column and add a small ball of silanized glass wool to the column through a rubber tube. Connect the vacuum pump to the vacuum pump. When the vacuum is complete, continue to add the filling material and tap the column wall continuously to make it evenly filled and tight. When the filling is completed, also use a small valve at the inlet end to keep the column filling material from moving. Connect the inlet end of the column to the vaporization chamber, do not connect the outlet end to the detector for the time being, and let the carrier gas flow through it at a rate of 20 mL/min.30. Hydrogen 30, argon 100, injection volume: 2.L.
Retention time, trimethylol ester?
The above gas chromatograph operating conditions are typical operating parameters. According to the characteristics of different instruments, the given operating parameters can be appropriately adjusted to achieve the desired effect. The typical gas push envelope of trimethylol ester in long-lasting emulsifiable concentrate is shown in Figure 2, 27
.6E+c6
4.6.1.5 Dian Ding Hu Bao
JIG33022001
Clearing Xiang Se
Capillary gas push chromatogram
Figure? Preparation of the sample solution: Weigh 3.0 g of the sample (accurate to 5.000 2 R), add 1% methane monoxide, decompose, make up to volume, and add 5% methane.
Under the above working conditions, after the instrument is connected, continuously inject the standard solution until the phase difference between the adjacent two pairs of required solutions is less than 3%, and then analyze and determine according to the standard solution, sample solution, sample flotation, and standard sample reduction. 26
4.6.1.6 Calculation
3302-2001
The measured peak area of the standard sample before and after the light sample is averaged, and the mass distribution efficiency X is read (%), and calculated according to formula (3): X,
wherein: A-
the average value of the peak area of trimethyl phosphate in the standard sample solution; A-the average value of the peak area of dimethyl aldehyde in the sample solution;-the mass of the trimethyl phosphate standard solution.
The mass of the standard sample, R!
The mass fraction of trimethyl phosphate in the standard consumption of trimethyl phosphate, %F
4.6.1.7 The sum of the two parallel determination results should not be greater than 0.3%. The arithmetic mean is taken as the determination result. 4.6.2 Capillary gas chromatography (capillary method) 4.6.2.1 Apparatus: Gas chromatograph: with hydrogen flame ionization detector and split flow sample introduction device, color tower: 3mm x 0.25mm (mm x 1.8mm) double or quartz thin arm inner wall 5% methyl methacrylate, film thickness 0.25patml. Chromatography treatment machine.
Operation system: with split flow sample introduction device and quartz inner wall charge recorder: 10 meters
4.6.2.2 Reagents and solutions
A kind of methane.
Phosphate diformaldehyde, analytical grade, known content, 99.0% 4.6.2.3 Gas chromatography operating conditions
Chamber temperature: start at 0°C, keep for min. Raise the chamber temperature to 22°C in a min-by-min increment and keep it at this temperature for 10 minutes. n.in.
Chemical cell: 220℃
Test chamber temperature: 200~250℃
Volume chromatogram (mI./min): Carrier gas (N,>A.0, compensation gas N,) 3, oxygen 30, air 300. Split ratio: 8:1
Injection volume: 5.C.
Retention time: triformaldehyde about 1Gmin.
The above gas chromatograph operating conditions are typical operating parameters: according to the characteristics of different instruments, the initial detection times can be appropriately adjusted to obtain the best results. The gas chromatogram of phospho-3-hydroxy ... 1. 6.
4.6.2.6 Allowable error
The difference between the results of two and a half tests shall not be greater than 3%. Take the arithmetic mean as the test result. 4.7 Determination of stability
4.7.1 Reagents and apparatus
Standard hard water: Ca++Mg+) 312mg/T Prepared with GA/T1603, 26
Vacuum: 100mL,
Constant temperature water: (30F1).
4.7.2 Determination steps
HG3302~2001
Use liquid absorption, 1.5ml sample, add 100ml of volume, dilute to the scale with standard hard water, stir and reflux. Let the liquid stand in a (-) solution for 1 hour: if there is precipitate, it is qualified. 4.B Low temperature stability test
4.8.1 Method
Stay at 0 for 1 hour, record the solid and oily matter released. Continue to discard the precipitate, centrifuge, let the precipitate settle, and record its volume.
4.B.2 Instrument
Refrigerator: maintain (0+1)℃,
high centrifuge tube WmL, the bottom scale of the tube is connected to UL
Centrifuge: replace with centrifuge
4.8.3 Test steps
Take (100=1.0) m1 sample and place it in a refrigerator to cool to (0+1). Place the sample in a centrifuge and keep it at (0+1). Stir it every 1 mm for 15% each time. Check and note whether there is any oily substance. Analysis rule: Place the centrifuge tube back into the refrigerator and continue to place it at (0±1)%. After that, take out the centrifuge tube and place it at room temperature (usually above 20℃) for 15 minutes. The relative centrifugal force of the tube is 500g~600g+ acceleration). Record the volume of the precipitate at the bottom of the tube (accurate to 0.C5m[.]. The precipitate shall not exceed C.3ml. It is qualified. 4.9 Thermal stability test
4.9.1 This end
Constant temperature (or constant humidity): 4.512)
Place the stopper in a glass bottle (or one that can still be sealed at 54℃). Medical injector
4.9.2 Test steps
Use an enzyme injector to inject about 3)% of the test liquid into the bottle (prevent the sample from touching the bottleneck), cool the bottle in an ice-salt bath, and then quickly inject and seal it. (to avoid volatility), seal at least one bottle, weigh them separately, put them into the judged safety containers, then put all the containers into a constant temperature box (or constant temperature water bath), place them in a thermostat (or constant temperature water bath), cool them to room temperature for [1d, take them out, wipe the outside of the safety and weigh them separately, take samples, and measure the long-term phosphorus content within 24 hours: after hot storage. Except that the long-term avoidance content is allowed to drop to 8% before hot storage, and the melting deer is allowed to rise to 3.5%, other indicators should still meet the standard requirements. 4.10 Inspection and acceptance of products
The inspection and acceptance of products should meet the requirements of the standard. 1604 regulations. The detection limit number is handled by the comparison method of the value of the contract. 5. Labeling, packaging, storage and transportation
5.1 The marking, labeling and packaging of the long-acting phosphorus liquid preparation shall comply with the current provisions of 6N3796 and G18:A: 5.2 The packaging of the long-acting phosphorus liquid preparation shall be stored in a fast-ventilated and dry warehouse. 5.3 Storage and transportation must be strictly prohibited from moisture and exposure to sunlight. It must not be placed with food, seeds, and feed capsules. Avoid contact with skin and skin, and prevent inhalation through the mouth and nose. 5. This product is a high-percentage organic pesticide, which can be inhaled through the skin. Protective clothing should be worn when using this product. Wear clean gloves, mouthpieces and protective clothing. After use, wash immediately with soap and water. If poisoning occurs, go to the hospital for examination and treatment in time. Atropine and iodine are specific antidotes.
HG.3302—2001
5.5 Under the prescribed storage and transportation conditions, the warranty period of long-acting phosphorus soluble agent is one year from the date of production. When the product leaves the factory: it shall meet the requirements of Chapter 3. Within one year, for 34X liquid agent, the long-acting phosphorus content shall not be less than 3T.0%; for 42% reduced agent, the long-acting phosphorus content shall not be less than 0%,
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