This standard specifies the requirements, test methods, marking, labeling, packaging, storage and transportation of dichlorvos technical materials. This standard applies to dichlorvos technical materials composed of dichlorvos and impurities generated during its production. GB 2549-2003 Dichlorvos technical materials GB2549-2003 Standard download decompression password: www.bzxz.net

The 3rd and 5th rates of this standard are strong and severe, and the rest are recommended. 19a (196s> The main revisions of the original purchase of GB2549 are as follows: This standard is a revision of GB2549-1811989. The main differences between this standard and GB2549-1811989 are as follows: The classification and grading have been cancelled. The mass fraction of diazinon has been uniformly changed to S: 0.1%. The increase in the standard of late increase in temperature has been changed from 0.20% to 0.2%, and the control item of trichloroethylene has been changed to 0.5%, and the control item of diazinon has been cancelled. The change of diazinon is to replace the standard of insecticides in the standard with the standard of insecticides. The standard is published by the China Petroleum and Chemical Industry Association on the day of its entry into force on the 5th of this month. This standard is published on behalf of the China Petroleum and Chemical Industry Association. This standard The National Pesticide Standardization Technical Committee (SAC/T 132) is responsible for the drafting of this standard: Shenyang Chemical Research Institute. The main drafters are: Qiang Bucheng, Shu Jun, This standard was first issued in 1931 and approved in 1989. This is the first revision. CB2549-2003
Text of the original drug
Other names, structural formulas and chemical parameters of the active ingredient of this product are as follows: s) Common name, ichlorws
Chemical name: U,0-dichlorobenzene (2,2-dichlorobenzene) late structural formula:
Experimental formula HCP
Molecular weight, 21.0 (according to the relative atomic mass) Biological activity; Killing point
Food point 231. :C/×10°Pa
Steam sheet (25.2.1×10tala
Relative light intensity () 1.425
Refractive index: (): 1.4533
GB 2549-20D3
Degree of solubility: 18%/125) Kerosene card screen 2%~0.3% (mass fraction) According to the standard formula, the remainder has standard reagent qualitative properties: thermally stable, slowly hydrolyzes in water or alkaline medium, and hydrolyzes faster in alkaline medium to generate diisocyanate and diisocyanate, DT-22C) about 3dH=2,\H7,3.H!, has corrosion effect on iron and mild steel: does not induce, can, and has no It has quality.
1 Scope
This standard specifies the requirements for the source drug, test methods, and marking, labeling, packaging and transportation. This standard is used to identify the original drug of dichlorvos and its residual substances produced during production. 2 Normative references
The clauses in the following documents become the clauses of this standard through the reference of this standard. For referenced documents with dates, all subsequent corrections (excluding the necessary contents of the investigation) or revisions are not applicable to this standard. However, the relevant research institutions that have reached an agreement based on this standard can use the updated versions of these documents: For referenced documents without dates, the latest versions are applicable to this standard. 151601 Chemical test standard GB/16 (Q coating solution determination method)
GR/TICO1 Commercial pesticide collection rules
G3/T16 652001 Commercial Pesticide Purchasing Form E3795 General Rules for Packaging
3 Requirements
3.1 Appearance glassy amber to colorless transparent droplets, no visible foreign matter, 3.2 Improve the original drug list to meet the requirements of Table 1.
GO2549-2D03
European acid slow grass content/%
Triethylsilyl painting effect\/%
Break (in I,M),)/%
Moisture content/%
Table 1 Predicted control indicators of diethylaminophenol
Under normal production conditions, acetaldehyde must be tested at least once every three months. 4 Test methods
4.1 Sampling
The sample of the "body preparation" shall be randomly selected and sampled every day. The inspection rate shall not be less than 100%.
4.2 Identification test
The chromatographic chromatographic method
The identification test can be carried out simultaneously with the pre-test. Under the same negative pressure operation conditions, the retention time of the main peak of the sample in the chromatographic liquid is the retention time of the standard liquid, and its relative value should be within 1.5. Infrared spectroscopy
There should be no obvious difference in the infrared absorption spectrum of the sample and the standard in the range of cm.~100m. The infrared spectrum of the standard is shown in Figure 1. Infrared spectrum of the standard sample
4.3 Determination of mass spectroscopy 4.3.1 Summary of the method The sample was dissolved in dichloromethane with H2O2 as the internal standard. The sample was separated by chromatography on a 1% DC- column and determined by a hydrogen ionization detector. The internal standard method was used for quantification. 4.3.2 Reagents and solvents: Trichloromethane drying; Stationary phase: silicone IKCF5; Obtaining phase: Test 101 (180um~250m) (or other carrier with good performance) was diluted with freshly prepared sodium hydroxide and then dried for 15h~-24h. The effluent was cleaned and sieved for later use. Preparation standard sample: Dispersed matrix content 39.% Internal standard: Normal standard (without new impurities that may interfere with the analysis): 2 CH 2549—2003
Internal standard liquid: Accurately weigh 2.7g of n-15 into a 50ml volumetric flask, dissolve it with dichloromethane and dilute to the mark, shake the spoon. 4.3.3 Instrumentation
Gas chromatograph: It has hydrogen ionization detection; chromatographic data processing!
Color: 2×3.2m () silicon (converted to stainless steel) micro-injector: 1℃
Chemical material: DC-550 101 carrier (1m250m), fixed: (solid + body) = 1C: 004.3.4 gas chromatograph operating strip
temperature (), sticky 171. gasification curtain 230 detector 250 gas volume: m!./): teaching gas N feather + air: 0o guarantee (mia: DDT 2.2: n-pentadecane 3.8 The above selected operating parameters are typical, and the given operating parameters can be appropriately adjusted according to the characteristics of different instruments to achieve the best effect. . The gas phase hazard diagram of the active ingredient is shown in Figure 1. 1--dose
2--limit
3--pentadecane,
4.3.5 Determination steps
4.3.5.1 Weigh the standard sample with a precision of 1g. J2g. The gastric-specific transfer tube is used to transfer the effective product to mL of the internal standard solution, and the content
4.3.5.2 Weigh the test partner containing the active ingredient 3.1 0.0002), placed in a glass bottle with the same standard liquid as used in 4.3.5.1, according to the uniform, 4.3.5.3 determination
in the above case, after the instrument is set up in the room, the number of needles of standard samples are filtered, until the two adjacent needles are less than 1.5% of the internal standard ratio, then the standard group rate changes, or the sample is filtered, the standard sample is broken into pieces in the order specified, 4.3. 6 Calculate the mass distribution of dichlorvos in the sample (%, or (1) Calculate: t
Where:
xnX
-the half mean of the area of ​​dichlorvos in the standard sample and the internal standard; 1
CB2549—2003
-the average value of the peak area of ​​dichlorvos in the sample and the internal standard; - the mass of the standard sample, in gramsDry it and transfer it accurately to 5mL +
mark.
4.4.5.2 Preparation of sample solution
CB2549-2003
Weigh the sample containing 1.1% trichloroacetaldehyde (accurate to 0.W2*), put it in a glass bottle, and dissolve it in 5m at the same point as used in 1.-.5.1. 4.4.5.3 Determination
Under the above conditions, the instrument meets the following conditions: Continuously measure the number of standard deviations: until the relative change of the ratio of the two adjacent dichloroacetaldehyde sieve areas to the internal standard sieve area is less than 1.5 mesh, and the standard deviation is greater than 1.5 mesh, and the liquid is measured and measured in sequence. 4. 4. 6 Calculate the mass fraction of trioxyacetaldehyde in the sample (in %) according to formula 2: #14.4
or in liquid: bZxz.net
in standard sample: the average value of the ratio of the peak area of ​​trioxyacetaldehyde to the area of ​​the internal standard peak;
in liquid: the average value of the ratio of the peak area of ​​chloroacetaldehyde to the positive product of the peak of internal standard;
[47.1] The estimated molecular mass of trioxyacetaldehyde
163.4-The mass fraction of trioxyacetaldehyde in the standard sample. 4.5 Determination of acidity
4.5.1 Reagents and standards
Ethanol solution: H,H2O3 (% aqueous solution)
Sodium hydroxide standard solution: (NaO1H2O=,02ur1/, according to G/T 101 sodium hydroxide solution, 2g/L ethanol. 4.5.2 Determination steps
Weigh the following formula accurately to (.C32) in a 2ml conical flask, add 100ml of the solution, add 3 drops of basic red as the indicator, and titrate with n.02mal/L sodium hydroxide solution until the color changes to white, which is the end point: make a blank sample, and calculate by the formula,
Xr(V. -V>×M/13.
Wu Zhong·
The actual change of sodium hydroxide standard solution droplet, unit is respiration per liter (rm/.): V-elimination formula solution, the actual oxidation standard titration solution volume consumed, unit is set liter! mL) V. One-one pollution self-falling child. The volume of the standard biochemical sodium ion titration solution consumed: the volume is room temperature (m): m-one sample and the unit is gram ():
M-… Sulfur (H, S),) the mass value of the order of grams (/mnl) M19). 4.G Determination of moisture content
According to the "lower limit value" in GB [1600, the appropriate amount of moisture meter is allowed to be determined. 4.7 Inspection and acceptance of products
shall be carried out in accordance with the provisions of (3/10]. The limit value is set by the direct light method. 5 Marking, labeling, packaging and transportation
5.1 The marking, labeling and packaging of the DDT original drug shall comply with the provisions of GI3796.)
GB 2549—2003
5.2 The DDT original drug shall be packed in clear, dry iron drums, with a net weight of 25kg or 200kg per drum. 5.3 According to the user's request or order agreement, other forms of packaging may be used, including the provisions of GB3796. 5.4 The packaging of the DDT original drug shall be stored in a ventilated and dry warehouse. 5.5 During storage and transportation, prevent moisture and sunlight, do not mix with food, seeds, feed, avoid contact with skin, prevent inhalation through mouth and nose. 5.6 Safety: exposure to water may cause poisoning. If the skin and eyes come into contact with the drug, rinse with serum water for more than 15 minutes and consult a doctor: if taken by mistake, induce vomiting immediately.
5.7 Harvest period: The acceptance period for scattered and slow-release products is 1 month. Within one month from the date of delivery, complete the product quality acceptance, and all customer indicators should meet the standard requirements.
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