Some standard content:
ICS 65.100
Registration No.: 10937-2002
Chemical Industry Standard of the People's Republic of China
HG3283-2002
Replaces HG3283-1975 (1983)
Chlormequat-chloride Aqueous Solution
Chlormequat-chloride Aqueous SolutionPublished on September 28, 2002
Implemented on June 1, 2003
Published by the State Economic and Trade Commission of the People's Republic of China
Chapter 3 and Chapter 5 of this standard are mandatory, and the rest are recommended. This standard replaces the mandatory chemical industry standard HG3283-1975 (1983) "Chlormequat-chloride Aqueous Solution". The main differences between this standard and HG3283-1975 (1983) are as follows: "referenced standards" have been added.
HG3283-—2002
Added the control of "mass fraction of 1,2-dichloroethane", "mass fraction of water-insoluble matter", "dilution stability", "low temperature stability" and "hot storage stability" indicators, and cancelled the "specific gravity" indicator. 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 drafting unit of this standard: Shenyang Chemical Research Institute. The participating drafting units of this standard: Quanfeng Pesticide Factory, Anyang City, Henan Province, and Hongcheng Enterprise Co., Ltd., Huanghua City, Hebei Province. The main drafters of this standard: Xu Laiwei, Zhang Xuebing, Xu Xuesong, Zhang Mingyue, and Sun Yunzeng. This standard was first issued on October 1, 1975 and confirmed in 1983. This standard is the first revision.
This standard is entrusted to the Secretariat of the National Pesticide Standardization Technical Committee for interpretation. (3)
Chlormequat-chloride aqueous solution
Other names, structural formulas and basic physicochemical parameters of the active ingredient chlormequat-chloride in this product are as follows:ISO common name: Chlormequat-chlorideCIPAC digital code: 143
Chemical name: 2-chloroethyltrimethylammonium chlorideStructural formula:
CH3—N+
CH2—CH2--Cl
Empirical formula: CsH13NClz
Relative molecular mass: 158.1 (according to the 1997 international relative atomic mass standard)Biological activity: Regulates Plant growth control
Vapor pressure (20℃): less than 10μPa
Melting point: 245℃ (simultaneous decomposition)
Boiling point: 125℃ (66.66mPa)
HG3283-2002
Solubility (g/kg, 20℃): greater than 1000 in water, 320 in ethanol, 50 in methanol, 0.2 in acetone, 0.3 in chloroform, <0.01 in ethyl acetate, insoluble in ether and hydrocarbons
Stability: Very easy to absorb water, the stability of the aqueous solution at 50℃ is more than two years, and it can be quickly degraded by enzymes in the soil. Corrosive to unprotected metals
1 Scope
This standard specifies the requirements, test methods, and marking, labeling, packaging, storage and transportation of chlormequat aqueous solution. This standard applies to chlormequat aqueous solution prepared from chlormequat technical material that meets the standard, appropriate adjuvants and water. 2 Normative references
The clauses in the following documents become the clauses of this standard through reference in this standard. For all dated referenced documents, all subsequent amendments (excluding errata) or revisions are not applicable to this standard. However, the parties who reach an agreement based on this standard are encouraged to study whether the latest versions of these documents can be used. For all undated referenced documents, the latest versions are applicable 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 chemical reagent test methods GB/T1601 Method for determination of pH value of pesticides
GB/T1603
GB/T1604
GB/T1605
Method for determination of stability of pesticide emulsions
Rules for acceptance of commercial pesticides
Sampling methods for commercial pesticides
GB3796 General rules for pesticide packaging
3 Requirements
3.1 Appearance: Light yellow to yellow-brown homogeneous liquid, without visible suspended matter and precipitation. 3.2 The control indicators of chlormequat aqueous solution should meet the requirements of Table 1. (5)
HG 3283—2002
Mass fraction of chlormequat, %
pH range
Mass fraction of 1,2-dichloroethane, %
Mass fraction of water-insoluble matter, %
Dilution stability (diluted 20 times)
Low temperature stability"
Hot storage stability
Table 1 Control item indicators of chlormequat aqueous solution
a During normal production, low temperature stability and hot storage stability shall be tested at least once every three months. 4 Test methods
4.1 Sampling
According to GB/T1605 The "liquid preparation sampling" method is used in the above test. The sampling packages are determined by the random number table method. The final sampling volume should be no less than 200mL.
4.2 Identification test
Thin layer chromatography: Under the same chromatographic operating conditions, the relative difference between the R value of a certain spot of the sample solution and the R value of the main spot of the standard solution should be within 1.5%. [Stationary phase: silica gel G; mobile phase: 0.1mol/L sodium iodide acetonitrile solution; sample solvent: methanol; color developer: Dragenf reagent, i.e. (1.7g bismuth subnitrate + 40g potassium iodide + 220mL glacial acetic acid)/L aqueous solution]. 4.3 Determination of the mass fraction of chlormequat
4.3.1 Principle of the method
After the sample is extracted with ethyl acetate to remove 1,2-dichloroethane, the mass fraction of chlormequat is calculated by measuring the amount of organic chlorine. The amount of organic chlorine is equal to the difference between the amount of total chlorine measured after hydrolysis and the amount of free chlorine measured before hydrolysis. The titration solution is a standard silver nitrate titration solution. 4.3.2 Reagents and solutions
Ethanol.
Ethyl acetate.
Standard silver nitrate titration solution: c(AgNO3)=0.1mol/L (prepared according to the method specified in GB/T601). Sodium hydroxide solution: c(NaOH)=2mol/L. Sodium hydroxide solution: c(NaOH)=0.1mol/L. Nitric acid aqueous solution: 1+3.
Dichlorofluorescent yellow indicator: 2g/L ethanol solution. Phenolphthalein indicator: 10g/L ethanol solution.
Starch indicator: 10g/L aqueous solution. Www.bzxZ.net
4.3.3 Determination steps
4.3.3.1 Preparation of sample solution
Accurately weigh 1.6g of the sample (accurate to 0.0002g), place it in a 50mL test tube, add 5mL of ethyl acetate and shake to extract for 5min. After standing and stratifying, use a pipette to suck out the organic phase as much as possible (discard it); repeat the extraction once according to the above method. Use 40mL of water three times to transfer all the samples to a 100mL volumetric flask, make up to volume, and shake well. 4.3.3.2 Determination of free chlorine
Accurately pipette 25mL of the sample solution into a 250mL conical flask, add 15mL of water, 3 drops of dichlorofluorescent yellow indicator and 10mL of starch indicator, and immediately titrate with silver nitrate standard titration solution until pink just appears, which is the end point. 2
4.3.3.3 Determination of total chlorine
HG3283—2002
Accurately pipette 25mL of sample solution into a 250mL ground-mouth conical flask, add 15mL of 2mol/L sodium hydroxide solution, install a reflux condenser, and heat to reflux on an electric heating mantle. After 15 minutes (starting from boiling), rinse the condenser and the inner wall of the conical flask with water, cool to room temperature, add 1 drop of phenolphthalein indicator, adjust to neutral or slightly acidic with nitric acid solution and 0.1mol/L sodium hydroxide solution, add 3 drops of dichlorofluorescent yellow indicator and 10mL starch indicator, and immediately titrate with silver nitrate standard titration solution until pink just appears, which is the end point. 4.3.4 Calculation
The mass fraction of chlormequat in the sample, Wi (%), is calculated according to formula (1): ur=V 158 1×100=×63. 24
m×100.00
Wherein:
c is the actual concentration of the standard silver nitrate titration solution, in moles per liter (mol/L); V,--the volume of the standard silver nitrate titration solution consumed when titrating free chlorine, in milliliters (mL); V--the volume of the standard silver nitrate titration solution consumed when titrating total chlorine, in milliliters (mL); m--the mass of the sample, in grams (g); 0.1581-the millimole mass of chlormequat, in grams per millimole (g/mmol). 4.3.5 Allowable difference
The difference between two parallel determination results shall not be greater than 0.5%. The arithmetic mean shall be taken as the determination result. 4.4 Determination of pH value
According to GB/T1601, 100 mL of sample shall be measured and determined directly without adding water. 4.5 Determination of mass fraction of 1,2-dichloroethane 4.5.1 Instrument
Gas chromatograph: with hydrogen flame ionization detector. Chromatographic column: 2m×4.0mm(id) glass column or stainless steel column. Filler: 3% polyethylene glycol 20000/GasChromQ (or carrier with equivalent performance), 150μm～180μm. Chromatographic data processor.
Micro-injector: 10μL.
4.5.2 Reagents and solutions
Dichloromethane.
1,2-dichloroethane standard: known mass fraction greater than or equal to 99.5%. 4.5.3 Preparation of chromatographic column
4.5.3.1 Coating of stationary liquid
(1)
Accurately weigh 0.3g of polyethylene glycol 20000 stationary liquid into a 250mL beaker, add an appropriate amount (slightly larger than the volume of the carrier) of chloroform to completely dissolve it, pour in 9.7g of the carrier, shake gently to mix evenly and evaporate the solvent to near dryness, then place the beaker in a 90℃ oven to dry for 1h, take it out and place it in a desiccator to cool to room temperature. 4.5.3.2 Filling of chromatographic column
Connect a small funnel to the outlet of the washed and dried chromatographic column, and fill the prepared filler into the column in batches, while constantly tapping the column wall until it is filled to 1.5cm from the column outlet. Move the funnel to the inlet of the multi-spectrum column, plug a small ball of silanized glass wool at the outlet, connect it to the vacuum pump through a rubber tube, turn on the vacuum pump, continue to slowly add the filler, and tap the column wall continuously to make it evenly and tightly filled. After filling, plug a small ball of glass wool at the inlet and press it properly to prevent the column filler from moving. 4.5.3.3 Aging of the chromatographic column
Connect the inlet end of the chromatographic column to the vaporization chamber, and do not connect the outlet end to the detector for the time being. Pass the carrier gas (N2) at a flow rate of 20mL/min, raise the temperature to 210℃ in stages, and age at this temperature for 48h. After the chromatographic column is aged, connect the outlet end of the column to the detector. (7)
HG3283—2002
4.5.4 Gas chromatography operating conditions
Temperature (℃): column chamber 60, vaporization chamber 200, detection chamber 200. Gas flow rate (mL/min): carrier gas (N2) 15, hydrogen 30, air 300. Injection volume (μL): 2.0.
Retention time (min): 1,2-dichloroethane about 8.5. The above gas chromatography operating conditions are typical operating parameters. According to the characteristics of different instruments, the given operating parameters can be appropriately adjusted to obtain the best effect. The typical gas chromatogram of 1,2-dichloroethane in chlormequat aqueous solution is shown in Figure 1. 1
1-Dichloromethane; 2-1,2-dichloroethane Figure 1 Gas chromatogram of 1,2-dichloroethane in chlormequat aqueous solution 4.5.5 Determination steps
4.5.5.1 Preparation of standard solution
Weigh 0.1g (accurate to 0.0002g) of 1,2-dichloroethane in a 100mL volumetric flask, dilute to volume with dichloromethane, and shake well. 4.5.5.2 Preparation of sample solution
Weigh 20.0g of sample (accurate to 0.0002g) into a 125mL separatory funnel, extract with 70mL of dichloromethane for 4 times, put the extracts into another 100mL volumetric flask, make up to volume with dichloromethane and shake well. 4.5.5.3 Determination
Under the above operating conditions, after the instrument is stable, continuously inject several needles of standard solution until the relative change of the peak area of two adjacent needles of 1,2-dichloroethane is less than 5%, and then inject and determine in the order of standard solution, sample solution, sample solution, and standard solution. 4.5.6 Calculation
Average the peak areas of 1,2-dichloroethane in the two needles of sample solution and the two needles of standard solution before and after the sample. The mass fraction w2 (%) of 1,2-dichloroethane is calculated according to formula (2): W2
Wherein:
A,——the average value of the peak area of 1,2-dichloroethane in the standard solution; A
the average value of the peak area of 1,2-dichloroethane in the sample solution; mi
the mass of the 1,2-dichloroethane standard, in grams (g); the mass of the sample, in grams (g);
P—the mass fraction of 1,2-difluoroethane in the 1,2-dichloroethane standard, expressed in %. (8)
(2)
4.5.7 Allowable difference
The difference between the results of two parallel determinations shall not exceed 0.1%. The arithmetic mean shall be taken as the determination result. 4.6 Determination of water-insoluble matter mass fraction
4.6.1 Summary of the method
Dissolve the sample in water, filter out all the insoluble matter, dry and weigh. 4.6.2 Apparatus
Weighing bottle.
Sintered glass crucible: G3.
Oven: 105℃±2℃.
Buchner suction flask: 100mL.
4.6.3 Determination steps
HG3283—2002
Put the sintered glass crucible in an oven at 105℃±2℃ and dry it to constant weight (accurate to 0.0002g). Accurately weigh 20g of the sample (accurate to 0.01g), rinse it into the measuring cylinder with 200mL of water, cover it with a stopper, and shake it vigorously to dissolve all the soluble matter. Filter the solution through a sintered glass crucible and wash the residue in the crucible with distilled water, 25 mL each time, for three times. Place the sintered glass crucible and the residue in an oven at 105°C ± 2°C and dry to constant weight (accurate to 0.0002 g). 4.6.4 Calculate the mass fraction W3 of water-insoluble matter in the sample by using formula (3): mmo × 100
where:
mass of the sintered glass crucible and the residue after constant weight, in grams (g); m
mass of the sintered glass crucible after constant weight, in grams (g); mo
m—mass of the sample, in grams (g). 4.6.5 Allowable difference
The difference between the results of two parallel determinations shall not be greater than 0.01%. Take the arithmetic mean as the determination result. 4.7 Dilution stability test
4.7.1 Reagents and instruments
Standard hard water: 342 mg/L, prepared according to the corresponding method in GB/T1603. Measuring cylinder: 100 mL.
Constant temperature water bath: 30℃±1℃.
Pipette: 5 mL.
4.7.2 Test steps
Pipette 5 mL of the sample, place it in a 100 mL measuring cylinder, dilute to the scale with standard hard water, and mix well. Place the measuring cylinder in a constant temperature water bath at 30℃±1℃ and let it stand for 1 hour. If the dilution is uniform and there is no precipitate, it is qualified. 4.8 Low temperature stability test
4.8.1 Summary of method
The sample is kept at 0℃ for 1 hour, and the precipitation of solid and oily matter is recorded. Continue to store at 0℃ for 7 days, centrifuge, settle the solid precipitate, and record its volume.
4.8.2 Instruments
Refrigerator: maintain 0℃±2℃.
Centrifuge tube: 100mL, the scale accuracy of the tube bottom is to 0.05mL. Centrifuge: Matching with centrifuge tube.
4.8.3 Test steps
HG3283—2002
Take 100mL±1.0mL of the sample and add it to the centrifuge tube, cool it to 0℃±2℃ in the refrigerator, keep the centrifuge tube and its contents at 0℃±2℃ for 1h, stir it every 15min, each time for 15s, check and record whether there is solid or oily precipitation. Put the centrifuge tube back into the refrigerator and continue to place it at 0℃±2℃ for 7d. After 7 days, take out the centrifuge tube, let it stand for 3 hours at room temperature (not exceeding 20℃), and centrifuge for 15 minutes (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 Thermal storage stability test
4.9.1 Instrument
Thermostatic box (or constant temperature water bath): 54℃±2℃. An (or a stoppered glass bottle that can still be sealed at 54℃). Medical syringe: 50mL.
4.9.2 Test steps
Use a syringe to inject about 30mL of the sample into a clean bottle (avoid the sample from contacting the bottleneck), place the bottle in an ice-salt bath to cool, and quickly seal it with a high-temperature flame (avoid solvent volatilization). Seal at least three bottles and weigh them separately. Place the sealed bottle in a metal container, and then put the metal container in a constant temperature box (or constant temperature water bath) for 14 days. Take it out and cool it to room temperature, wipe the outside of the bottle and weigh it separately. For samples with unchanged mass, measure the mass fraction of chlormequat within 24 hours. After hot storage, the mass fraction of chlormequat is allowed to drop to 95% of the mass fraction measured before hot storage.
4.10 Inspection and acceptance of products
The inspection and acceptance of products shall comply with the provisions of GB/T1604. The rounded value comparison method shall be used for the processing of limit values. 5 Marking, labeling, packaging, storage and transportation
5.1 The marking, labeling and packaging of chlormequat aqueous solution shall comply with the provisions of GB3796. 5.2 The packages of chlormequat aqueous solution should be stored in a ventilated and dry warehouse. 5.3 During storage and transportation, it should be strictly protected from sunlight, and should not be mixed with food, seeds, and feed. Avoid contact with skin and eyes, and prevent inhalation through the mouth and nose. 5.4 Safety: This product is a low-toxic preparation and can penetrate through the skin. When using this product, you should wear protective gloves, masks, 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. 5.5 Warranty period: Under the specified storage and transportation conditions, the warranty period of chlormequat aqueous solution is two years from the date of production.
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