Some standard content:
ICS65.100
Registration No.: 10928--2002
Chemical Industry Standard of the People's Republic of China
HG 3700--2002
Dicofole emulsifiable concentrates2002-09-28 Issued
2003-06-01 Implementation
National Economic and Trade Commission of the People's Republic of China Foreword
Chapter 3 and Chapter 5 of this standard are mandatory, and the rest are recommended. HG3700-2002
This standard is formulated based on the quality level of domestic dicofol emulsifiable concentrate, with reference to the FAO standards of the Food and Agriculture Organization of the United Nations and the analytical methods of the International Pesticide Analysis Coordination Committee (CIPAC). This standard was proposed by the Policy and Regulations Department of the former State Administration of Petroleum and Chemical Industry. This standard is under the jurisdiction of the National Pesticide Standardization Technical Committee (CSBTS/TC133). The responsible unit for the chapter of this standard is the Pesticide Testing Institute of the Ministry of Agriculture. The participating drafting unit of this standard is Jiangsu Yangnong Chemical Group Co., Ltd. The main drafters of this standard are Li Guoping, Zhao Yonghui, Fan Wenzhong, Liu Ping, and Ji Ying. The Secretariat of the National Pesticide Standardization Technical Committee is responsible for the interpretation of this standard. I
Dichlorodichlorobenzene EC
Other names, structural formulas and basic physical and chemical parameters of the active ingredient dicofol in this product are as follows:ISO common name: dicofol
CAS registration number: 115-32-2
CIPAC digital code: 123
Chemical name: 2,2,2-trifluoro-1,1-bis(4-fluorophenyl)ethanolStructural formula:
Empirical formula: CuHClsO
Relative molecular mass: 370.5 (according to the 1997 international relative atomic mass)Biological activity: Acaricide
Melting point: 78.5 ℃79.5℃
Relative density: 1.45 (25℃)
Vapor pressure: 0.053mPa
HG3700—2002
Solubility: slightly soluble in water, soluble in most organic solvents, such as ether, acetone, lysine, toluene, chloroform, dichloromethane Stability: stable in acid, unstable in alkali and hydrolyzed, stable below 80℃ The isomers of trichlorodicofol, o- and p-dicofol also have biological activity, and its structural formula is as follows: OH
1Scope
This standard specifies the requirements, test methods, and marking, labeling, packaging, storage and transportation of trichlorodicofol emulsifiable concentrates. This standard applies to trichlorodicofol emulsifiable concentrates prepared by dissolving the dicofol technical material that meets the standard and the emulsifier in a suitable solvent.
2 Normative references
The clauses in the following documents become clauses of this standard through reference in this standard. For any dated referenced document, all subsequent amendments (excluding errata) or revisions are not applicable to this standard. However, parties to an agreement based on this standard are encouraged to investigate whether the latest versions of these documents can be used. For any undated referenced document, the latest version applies to this standard. Preparation of standard solutions for titration analysis (volume analysis) of chemical reagents GB/T601
GB/T603
Preparation of preparations and products used in test methods for chemical reagents GB/T1250
GB/T1600
GB/T16Q1
GB/T1604
GB/T1605
Expression and determination methods of limit values Pesticide moisture determination method
Pesticide pH determination method
Commercial pesticide acceptance rules
Commercial pesticide sampling method
GB37962
General rules for pesticide packaging
HG3700-2002
GB4838 Pesticide emulsifiable concentrate packaging
3 Requirements
3.1 Appearance: Brown transparent liquid, without obvious suspended matter and sediment. 3.2 The control item indicators of triazine emulsifiable concentrate should meet the requirements of Table 1. Table 1 Control Items of Dicofol EC Index Items
Total active ingredient content (dicofol + o-, p-dicofol), % Dicofol content/total active ingredient content, % DDT content, %
PH range
Water content, %
Emulsion stability (diluted 200 times)
Low temperature stability
Hot storage stability.
8p-, p-dicofol.
b In this standard, DDT impurities include o-, p-DDT), p-, p-DDT (PP-DDT), p-, p-DDE and p-, p-chlorinated DDT (p-CIDDT). Under normal circumstances, the low temperature and hot storage stability tests shall be inspected at least once every three months. 4 Test methods
4.1 Sampling
The test is carried out in accordance with the "Sampling of Liquid Preparations" method in GB/T1605. The sampled packages are determined by random sampling (the temperature shall not exceed 75°C when melting the sample). The final sampling volume shall not be less than 100g. 4.2 Identification test
High performance liquid chromatography: This identification test can be carried out simultaneously with the determination of the content of the active ingredient. Under the same chromatographic operating conditions, the relative difference between the retention time of two chromatographic peaks in the sample solution and the retention time of the chromatographic peaks of dicofol, o-, and p-dicofol in the standard solution should be within 1.5%.
4.3 Determination of dicofol, o-, and p-dicofol 4.3.1 Summary of the method
The sample uses methanol decahydrate + glacial acetic acid as the mobile phase, uses a Cs column and a UV detector, and uses the external standard method to separate and determine the active ingredients in the sample by high performance liquid chromatography.
4.3.2 Instruments
High performance liquid chromatograph: with variable wavelength ultraviolet detector. Chromatographic data processor.
Chromatographic column: 250mm×4.6mm(id) stainless steel column, filled with SUPELCOSILLC-8 (or other similar), 5μm filler. Micro-injector: 50uL.
4.3.3 Reagents and solutions
Methanol: high purity.
Water: freshly distilled and double distilled water. wwW.bzxz.Net
Glacial acetic acid.
Trichlorodicofol standard: known content.
O,P-Trichlorodicofol standard: known content. 4.3.4 High performance liquid chromatography operating conditions
Mobile phase: methanol + water + glacial acetic acid = 75 + 25 + 0.2. Mobile phase flow rate: 1.3mL/min.
Column temperature: 30℃.
Detection wavelength: 235nm.
Injection volume: 10μL.
Retention time: o-, p-dicofol about 9min, dicofol about 13min. HG37002002
The above operating parameters are typical. According to the characteristics of different instruments, the given operating parameters can be appropriately adjusted to obtain the best effect. A typical HPLC chromatogram of dicofol emulsifiable concentrate is shown in Figure 1. 1-ortho, para-dicofol, 2-dicofol Figure 1 HPLC chromatogram of dicofol emulsifiable concentrate 4.3.5 Determination steps
4.3.5.1 Preparation of standard solution
Weigh 0.05g (accurate to 0.0002g) of dicofol standard and 0.01g (accurate to 0.0002g) of ortho, para-dicofol standard in a 100mL volumetric flask, dissolve and dilute to volume with methanol, and mix well. 4.3.5.2 Preparation of sample solution
Weigh a sufficient amount of sample (accurate to 0.0002g) that matches the concentration of the standard solution in a 100mL volumetric flask, dissolve and dilute to volume with methanol, mix well, and filter if necessary.
4.3.5.3 Determination
Under the above operating conditions, after the instrument is stable, continuously inject several needles of standard solution, calculate the relative response value of each needle, and when the relative response value of two adjacent needles changes less than 1.5%, inject the needle in the order of standard solution, sample solution, sample solution, and standard solution. 4.3.6 Calculation
Average the peak areas of the isomers of dicofol in the two needles of sample solution and the two needles of standard solution before and after the sample solution.
The content of dicofol expressed as mass fraction w (%) and the content of o-,p-dicofol expressed as mass fraction 4.3.6.1
ws (%) are calculated according to formula (1) and formula (2) respectively: r
Wherein:
A.a--the average value of the peak area of dicofol in the sample solution; msi
-the mass of the dicofol standard, in grams (g); P--the mass fraction of dicofol in the standard, expressed in %; A.--the average value of the peak area of dicofol in the standard solution; (91)
HG3700-2002
m--the mass of the sample, in grams (g); Az
--the average value of the peak area of o-, p-dicofol in the sample solution: P--the mass fraction of o-, p-dicofol in the standard, expressed in %; Aa
--the average value of the peak area of o-, p-dicofol in the standard solution; o-, p-dicofol standard, in grams (g). 4.3.6.2 The total active ingredient content expressed as mass fraction ws (%) is calculated according to formula (3): Ww +
Wherein:
Mass fraction of dicofol, expressed as %; o-, p-dicofol mass fraction, expressed as % 4.3.6.3 The percentage of dicofol content/total active ingredient content X is calculated according to formula (4): X-×100
Wherein:
Mass fraction of dicofol, expressed as %; Mass fraction of total active ingredients, expressed as %. 4.3.7 Permissible difference
The difference in dicofol content between two parallel determinations shall not be greater than 1.0%, and the difference in o-, p-dicofol content shall not be greater than 0.5%. 4.4 Determination of the content of droplet-delay impurities (DDTY) 4.4.1 Summary of the method
The sample is dissolved in methanol, methanol decahydrate decaacetic acid is used as the mobile phase, a C column and a UV detector are used, and the DDT? impurity in the sample is separated and determined by high performance liquid chromatography using the Pp-DDE standard. 4.4.2 Instruments
Same as 4.3.2.
4.4.3 Reagents and solutions
P, p-DDE standard: known mass fraction greater than or equal to 98.0%.
P, p-DDT standard: no interference peak.
P, P-DDT standard: no interference peak.
P, P'-CIDDT standard, no interference peak
Qualitative solution: 0.004 mg/mL DDT methanol solution. Methanol: chromatographic grade.
Water: freshly distilled double distilled water.
Glacial acetic acid: analytical grade.
4.4.4 HPLC operating conditions
Same as 4.3.4.
Retention time 0, p-DDT 20min; pp-DDT 22min, p'-DDE 23min; p, p-CIDDT 36min. 4.4.5 Determination steps
4.4.5.1 Preparation of standard solution
Weigh about 0.020g (accurate to 0.0001g) of p, p-DDE standard sample in a 50mL volumetric flask, dissolve and dilute with methanol, mix well, and use it as solution A. Accurately transfer 0.5mL of solution A to a 50mL volumetric flask, dilute with methanol, mix well, and use it as standard solution. 4.4.5.2 Preparation of sample solution
Weigh 1.25g of 40% or 2.5g of 20% emulsion (accurate to 0.0001g) into a 50mL volumetric flask, dissolve and dilute with methanol, and mix well.
4.4.5.3 Determination
HG3700—2002
4.4.5.3.1 Solvent blank: Under the above operating conditions, after the instrument is stable, inject 10uL of methanol used to dissolve the sample. There should be no chromatographic peaks that interfere with the determination of impurities.
4.4.5.3.2 Qualitative analysis of impurity peaks: Inject 10uL of qualitative solution and determine the retention time of the four DDT peaks. 4.4.5.3.3 Continuously inject several needles of standard solution, calculate the relative response value of each needle, and when the relative response value of two adjacent needles changes by less than 1.5%, inject the needles in the order of standard solution, sample solution, sample solution, and standard solution. The separation effect is shown in Figure 2. If the peak of dicofol is tailing, the peak processing parameters of the integrator should be set correctly so that the peaks of DDT-related impurities located on its tail are integrated as tail peaks or peak-to-valley integration. 1--ortho, para-dicofol, 2-dicofol; 3-ortho, para-DDT: 4-para, para-DDT; 5-ortho, para-DDT; 6-para, para-DDT; 7-para, para-chlorinated DDT Figure 2 DDTY sample separation chromatogram
4.4.5.4 Calculation
The mass fraction w (%) of DDT is calculated according to formula (5): AmP
w=AmzX100
Where:||tt| |A,—-Average value of the peak area of P,p'-DDE in the standard solution; (5)
A2—Average value of the sum of the areas of all peaks of o,-DDT, p,P-DDT, p,p-DDE and P,p'-CIDDT in the sample solution; The mass of the P,p-DDE standard, in milligrams (mg); m
The mass of the sample, in milligrams (mg); The mass fraction of P·P'-DDE in a standard sample, expressed in %. P
4.4.5.5 Allowable difference
The relative deviation of the results of two parallel determinations shall not be greater than 20%. 4.5 Determination of moisture
The determination shall be carried out according to the Karl Fischer method in GB/T1600. It is allowed to use a moisture meter with equivalent accuracy. 4.6 Determination of pH value
The determination shall be carried out according to the method in GB/T1601.
4.7 Emulsion stability test
The sample is diluted 200 times with standard hard water and tested according to GB/T1603. It is qualified if there is no floating oil on the top and no sinking oil or precipitation below. 4.8 Low temperature stability test
4.8.1 Method summary
The sample is kept at 0℃ for 1min, and the presence of solid and oily matter is recorded. Continue to store at 0℃ for 7d, centrifuge to settle the solid precipitate, and record its volume.
4.8.2 Instrument
HG3700—2002
Refrigerator: Maintain (0±1)℃.
Centrifuge tube 100mL, the scale on the bottom of the tube is accurate to 0.05mL. Centrifuge: Matching with centrifuge tube.
4.8.3 Test steps
Take (100±1.0)mL of the sample and place it in a centrifuge tube, cool it to (0±1)℃ in a refrigerator, and keep it at this temperature for 1h. Stir it every 15min, and check and record whether there is solid and oily precipitation every 15s. Put the centrifuge tube back into the refrigerator and continue to place it at (0±1)℃ for 7d. After 7d, take out the centrifuge tube, let it stand at room temperature (not exceeding 20℃) for 3h, and centrifuge it for 15min (the relative centrifugal force at the top of the tube is 500g~600g, g is the acceleration of gravity). Record the volume of the precipitate at the bottom of the tube (accurate to 0.05mL). The precipitate is qualified if it does not exceed 0.3mL.
4.9 Hot storage stability test
4.9.1 Apparatus
Thermostatic box (or thermostatic water bath): (54+2)℃, ampoule (or glass bottle with stopper that can still be sealed at 54℃). Medical syringe: 50mL.
4.9.2 Test steps
Use a syringe to inject 15mL of emulsifiable concentrate sample into a clean ampoule (to avoid the sample from removing the bottleneck), place the ampoule in an ice-salt bath to cool, and quickly seal it with an alcohol blowtorch (to avoid solvent evaporation). Seal at least 3 bottles and weigh them separately. Place the sealed ampoule in a metal container, and then put the metal container in a thermostatic box for 14 days. Take it out and cool it to room temperature, wipe the outside of the ampoule and weigh it separately. For samples that have not changed in mass, test the specified items within 24 hours. Except that the mass fraction of the active ingredient is allowed to drop to 95% of the pre-storage mass, the results of other items still meet this standard and are qualified.
4.10 Inspection and acceptance of products
Carry out in accordance with the relevant provisions of GB/T1604. The processing of limit values adopts the rounded value comparison method of GB/T1250. 5 Marking, labeling, packaging, storage and transportation
5.1 The marking, labeling and packaging of dicofol emulsifiable concentrate shall comply with the relevant provisions of GB3796 and GB4838, and shall have the pesticide production approval certificate number, pesticide registration certificate number, standard number and trademark. 5.2 Dicofol emulsifiable concentrate shall be packaged in polyester bottles, each with a net capacity of 100mL, and a calcium plastic box shall be used as the outer packaging. 5.3 According to user requirements or ordering agreements, other forms of packaging may be used, but they must comply with the relevant provisions of GB3796. 5.4 Packages should be stored in ventilated and dry warehouses. 5.5 During storage and transportation, strictly prevent moisture and sunlight, do not mix with food, seeds and feed, avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.6 Safety: Trichlorfon EC is a low-toxic acaricide. When using this product, you should wear protective gloves and clean protective clothing. After applying the product, you should immediately wash it with soap and water. If it gets into your eyes, wash it with water. There is no special antidote. If you take it orally, you should induce vomiting. Do not mix it with alkaline pesticides to avoid decomposition and loss of efficacy.
5.7 Warranty period: Under the specified storage and transportation conditions, the quality warranty period of dicofol emulsifiable concentrate is two years from the date of production. (94)
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