Some standard content:
Professional Standard of the People's Republic of China
ZBG25011—90
Published on April 11, 1990
Alachlor EC
Implemented on January 1, 1991
Published by the Ministry of Chemical Industry of the People's Republic of China
Professional Standard of the People's Republic of China
Alachlor EC
Subject Content and Scope of Application
ZBG25011—90
This standard specifies the technical indicators, inspection methods, inspection rules, and requirements for marking, packaging, transportation and storage of alachlor EC. This standard applies to alachlor EC prepared from alachlor technical with suitable emulsifiers and solvents. Active ingredient: Alachlor
Chemical name: α-chloro-2,6'-diethyl-N-methoxymethylacetanilide C2Hg
Structural formula:
CH20CH
Molecular formula: CuH20CINO2
Relative molecular mass: 269.77 (International atomic weight in 1987) Reference standard
GB1600
GB1601
GB1 603
GB1604Www.bzxZ.net
GB1605
GB4838
3 Technical requirements
Method for determining moisture content of pesticides
Method for determining hydrogen ion concentration of pesticides
Method for determining stability of pesticide emulsions
Pesticide acceptance rules
Sampling methods for commercial pesticides
Emulsifiable concentrate pesticide packaging
3.1 Appearance: Brown or purple homogeneous liquid. 3.2 Alachlor emulsifiable concentrate shall also meet the following index requirements: Index
Alachlor content, % (m/m)
Water, % (m/m)
Emulsion stability (diluted 200 times)
Low temperature stability)
Hot storage stability 2)
Note: 1) and 2) are random inspection items.
Approved by the Ministry of Chemical Industry of the People’s Republic of China on April 11, 1990
Implementation on January 1, 1991
W.4 Test method
4.1 Determination of alachlor content
4.1.1 Summary of method
ZBG25011—90
The sample was dissolved in chloroform and determined by gas chromatography on a SE-30 column with di-n-pentyl phthalate as the internal standard. 4.1.2 Reagents and solutions
Chloroform (GB682);
Alachlor standard sample: known content:
Di-n-pentyl phthalate: identified by this method, no interfering impurities; c.
Fixed liquid: SE-30;
Carrier: Chromosorb W-HP180~250μm (60~80 mesh); e.
Internal standard solution: Weigh 3.2g of di-n-pentyl phthalate, place it in a 200mL volumetric flask, add chloroform to dissolve, dilute to the scale, and shake well.
4.1.3 Instruments
Gas chromatograph: with hydrogen flame ionization detector; a.
Filling material;
Chromatographic column: 1m long, 3mm inner diameter stainless steel column, filled with 5%SE-30/ChromosorbW-HP180~250μm recorder or gas chromatography data processor
d. Micro-injector: 10μL.
4.1.4 Operation steps
4.1.4.1 Preparation of chromatographic column
Coating of stationary liquid: Weigh 0.5gSE-30 in a 200mL beaker, add about 50mL of chloroform. Stir with a glass rod a.
to completely dissolve SE-30, add about 10g of carrier. Shake the beaker to completely immerse the carrier in the solution. Place the beaker under an infrared lamp to heat it, and shake the beaker gently by hand from time to time until the solvent evaporates and is almost dry. Then place the beaker in an oven at 110℃ for 1h, take it out and place it in a desiccator. Filling of the chromatographic column: Connect a funnel to the inlet end of the column, wrap the outlet end with 1,000 clean gauze and connect it to the vacuum pump with a rubber tube. Turn on the b.
vacuum pump, and pour the column filling material into the funnel in batches while tapping the column tube continuously until the filling material no longer drops. Remove the chromatographic column and plug a little silanized glass wool at both ends of the column. c. 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. Control the carrier gas flow rate to 10mL/min, and age for at least 48h at a column temperature of 250℃. 4.1.4.2 Chromatographic operating conditions
Column chamber: 200℃;
Vaporization chamber: 220℃,
Detection chamber: 220℃.
Gas flow rate
Carrier gas (N2): 40mL/min;
Hydrogen 33mL/min;
Air: 320mL/min
Injection volume: 1.0μL.
Retention time
Alachlor: about 4.5min;
Internal standard: about 9.5min.
W.bzsoso.cOmZBG25011—90
Gas chromatogram of Alachlor
1-Alachlor, 2 internal standard
The above gas chromatography conditions are typical operating parameters. Analysts can make appropriate adjustments to the operating parameters according to the characteristics of the instrument to obtain the best results.
4.1.4.3 Preparation of standard solution
Weigh 0.1g (accurate to 0.0002g) of alachlor standard sample, place it in a 10mL glass bottle with a ground stopper, accurately add 10mL of internal standard solution with a pipette, and shake well.
4.1.4.4 Preparation of sample solution
Weigh about 0.1g of emulsifiable concentrate sample containing alachlor (accurate to 0.0002g), place it in a 10mL glass bottle with a ground stopper, accurately add 10mL of internal standard solution with a pipette, and shake well. 4.1.4.5 Determination steps
Under the selected conditions, after the instrument is stable, first repeatedly inject 1μL of alachlor standard solution, and determine the response value ratio each time (alachlor peak area/internal standard peak area), until the relative deviation of the ratio of two consecutive response values is within 0.75%. Then, the samples are injected and analyzed in the following order: standard solution, sample solution, sample solution, standard solution. Calculate the average response value ratio r. 3
W4.1.5 Calculate
the mass percentage content X of alachlor according to the following formula: ZBG25011-90
T2·mi·P
ri·m2
Where: 1-the average value of the peak area ratio of alachlor to the internal standard in the standard solution; r2-the average value of the peak area ratio of alachlor to the internal standard in the sample solution; mi-the mass of the standard, g;
m2-the mass of the sample, g;
P-the mass percentage content of the standard, %. 4.1.6 Allowable difference
The difference between the results of the two parallel determinations of this method should be within 1.0%. 4.2 Determination of moisture
Determine according to the Karl Fischer method in GB1600. 4.3 pH value determination
Perform according to the pH meter method in GB1601.
4.4 Emulsion stability test
Perform according to GB1603.
4.5 Low temperature stability test
Take 50mL of sample in a 100mL beaker, put it in a refrigerator or ice water bath to maintain the temperature at 0±2℃, and leave it for 1h. Stir slowly with a glass rod from time to time to observe whether there is solid or oily precipitation. If there is no solid or oily precipitation, it is qualified. 4.6 Hot storage stability test
4.6.1 Instrument
a. Constant temperature box or constant temperature water bath: temperature control accuracy ±2℃ b. An: 50mL, long neck.
4.6.2 Analysis steps
Take 50mL of sample and inject it into a clean annulus (do not let the sample touch the neck of the annulus), and seal it with a gas lamp (avoid solvent evaporation when sealing). Seal at least two bottles of each sample and store them in a constant temperature box or constant temperature water bath at 54±2℃ for 14 days. Cool to room temperature and determine the alachlor content within 24 hours according to the method specified in Article 4.1. The relative decomposition rate is qualified if it is less than 6%. 5 Inspection rules
5.1 Alachlor EC products should be inspected by the quality supervision and inspection department of the manufacturer. Low temperature stability and heat storage stability are random inspection items, and random inspections are carried out at least once every three months. The manufacturer should ensure that all alachlor EC products leaving the factory meet the requirements of this standard, and each batch of alachlor EC leaving the factory should be accompanied by a quality certificate.
5.2 The quantity of each batch of alachlor EC products should not exceed the capacity of the packaging storage tank. 5.3 The sampling method shall be carried out in accordance with GB1605.
5.4 The user has the right to verify whether the alachlor EC products received meet the requirements of this standard in accordance with the provisions of the product standard. 5.5. If any index in the inspection result does not meet the standard, samples should be taken from twice the number of packages for re-inspection. If only one index does not meet the requirements in the re-inspection result, the whole batch of products shall be unqualified. 5.6. When the supply and demand parties have disputes over product quality, they can be resolved through negotiation or the legal inspection agency shall conduct arbitration analysis in accordance with the inspection methods specified in this standard.
6. Marking, packaging, transportation and purchase and storage
6.1. The marking and packaging of alachlor emulsifiable concentrate shall comply with the relevant provisions of GB4838. 4
WZBG25011—90
6.2. Alachlor emulsifiable concentrate is packaged in clean, dry brown glass bottles with inner and outer covers, with a net weight of 0.5kg or 1kg per bottle, and straw sleeves or corrugated paper are used as linings. They are tightly arranged in calcium plastic boxes or cartons, and the net weight of each box does not exceed 12kg. Other forms of packaging can also be used according to user requirements.
6.3 During storage and transportation, prevent moisture and sunlight, maintain good ventilation, do not mix with food, seeds, feed, avoid contact with skin, and prevent inhalation through the mouth.
6.4 The warranty period is 2 years. The content of alachlor shall not be less than 41.0% and the pH value shall not be less than 4 within 2 years. Additional remarks:
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry. This standard is under the jurisdiction of Shenyang Chemical Industry Research Institute. This standard is drafted by Shenyang Chemical Industry Research Institute. The main drafters of this standard are Jiang Minyi, Yuan Chunfeng, Li Xiujie, Lu Zenan, and Xu Meiying. 5
W.
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