Some standard content:
Professional Standard of the People's Republic of China
ZBG25010—90
Alachlor Technical
Published on April 11, 1990
Published by the Ministry of Chemical Industry of the People's Republic of China and implemented on January 1, 1991
Professional Standard of the People's Republic of China
Alachlor Technical
1 Subject Content and Scope of Application
ZBG25010—90
This standard specifies the technical indicators, test methods, test rules, and requirements for marking, packaging, transportation and storage of Alachlor Technical. This standard applies to Alachlor Technical synthesized by acylation and condensation process with 2,6-diethylaniline, polyoxymethylene and chloroacetyl chloride as the main raw materials.
Active ingredient: Alachlor
Chemical name: α-chloro-2',6'-diethyl-N-methoxymethylacetanilide C2He
Structural formula:
CH20CHs
Molecular formula: CuH20CINO2
Relative molecular mass: 269.77 (1987 international atomic weight)2
Cited standards
GB1600
GB1604
GB1605
GB3796
3 Technical requirements
Method for determination of moisture content in pesticides
Pesticide acceptance rules
Sampling method for commercial pesticides
General rules for pesticide packaging
3.1 Appearance: Brown or purple viscous liquid or semi-solid. Alachlor technical shall also meet the following index requirements: 3.2
%(m/m)
Indicator name
Alachlor content
Acidity (in HSO.)
Acetone insoluble matter\
Note: 1) is a random inspection item.
4 Inspection method
Determination of alachlor content
Superior grade
Approved by the Ministry of Chemical Industry of the People's Republic of China on April 11, 1990
First grade
Qualified product
Implemented on January 1, 1991
4.1.1 Method summary
ZBG25010—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.
Stationary liquid: SE-30;
Carrier: Chromosorb
W-HP180~250μm (6080 mesh);
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
Filling material;
Gas chromatograph: with hydrogen flame ionization detector; Chromatographic column: 1m long, 3mm inner diameter stainless steel column, filled with 5% SE-30/chromosorbW-HP
180~250μmbzxZ.net
Recorder or gas chromatography data processor; Micro-injector: 10μL.
4.1.4 Operation steps
4.1.4.1 Preparation of chromatographic column
Coating of stationary liquid: Weigh 0.5g SE-30 in a 200mL beaker, add about 50mL chloroform. Stir with a glass rod to completely dissolve SE-30, add about 10g carrier. Shake the beaker to completely immerse the carrier in the solution. Heat the beaker under an infrared lamp, and shake the beaker gently by hand from time to time until the solvent evaporates. Then place the beaker in an oven at 110°C for 1 hour, take it out and place it in a desiccator. b. Filling of the chromatographic column: Connect the inlet end of the column to a funnel, wrap the outlet end with clean gauze and connect it to the vacuum pump with a rubber tube. Turn on the vacuum pump, and pour the column filling material into the funnel in batches while tapping the column tube continuously until the filling material stops falling. 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 48 hours at a column temperature of 250°C. 4.1.4.2 Chromatographic operating conditions
Column chamber: 200°C;
Vaporization chamber: 220°C;
Detection chamber: 220°C.
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.
ZBG25010—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 1L 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 ratio. 3
4.1.5 Calculate
ZBG25010-90
the mass percentage of alachlor X1, according to formula (1): Xf =\2:mi ·P
wherein: n is the average value of the peak area ratio of alachlor to the internal standard in the standard solution; T2
is the average value of the peak area ratio of alachlor to the internal standard in the sample solution; the mass of the standard sample, g; the mass of the sample, 8; the mass percentage of the standard sample, %. 4.1.6 Allowable difference
The difference between the results of the two parallel determinations of this method should be within 1.5%. 4.2 Determination of moisture
Determine according to the Karl Fischer method in GB1600. 4.3 Determination of acidity
4.3.1 Reagents and solutions
Acetone (GB686): redistilled;
Sodium hydroxide (GB629) standard titration solution: c(NaOH)=0.02mol/Lc.
Buffer solution: Mix 100mL120g/L acetic acid solution and 100mL40g/L sodium hydroxide solution, and dilute to 1000mL with deionized water.
4.3.2 Instruments
pH meter: accurate to ±0.1pH, with temperature compensation or temperature correction chart; electromagnetic stirring;
c. Glass electrode: soak in distilled water for 24h before use, saturated calomel electrode. 4.3.3 Analysis steps
Use the above-mentioned electrode and pH meter to measure the pH of a mixture of 50 mL of redistilled acetone and 5 mL of buffer solution at 20°C. Weigh 10 g of the sample (accurate to 0.01 g) and put it into a 100 mL beaker, dissolve it with 50 mL of redistilled acetone, add 5 mL of distilled water, and mix well. Under the same conditions as above, titrate with sodium hydroxide standard titration solution to the pH value of the acetone-buffer solution mixture at 20°C, which is the end point.
4.3.4 Calculation
The acidity X2 of alachlor technical expressed as mass percentage is calculated according to formula (2): X: = 9-V×0. 049 × 100
Wherein: V—the volume of sodium hydroxide standard titration solution consumed by the titrated sample, mL; the actual concentration of the sodium hydroxide standard solution, mol/L; m
—the mass of the sample, g;
—the mass of sulfuric acid equivalent to 1.00 mL of sodium hydroxide standard titration solution [c(NaOH)=1.000 mol/L) expressed in grams.
4.4 Determination of acetone insoluble matter
4.4.1 Instruments and reagents
a.Glass crucible: G3;
Filter bottle: 500mL;
c. Acetone (GB686).
4.4.2 Analysis steps
ZBG25010—90
Weigh 10g sample (accurate to 0.1g) in a 200mL beaker, add 140mL acetone and stir until all solubles are dissolved, pour the solution into the G3 glass that has been weighed to a constant weight and filter. Wash the beaker with acetone 3 times (20mL each time), and pour the washing liquid into the filter. Bake in a 110℃ oven to a constant weight (accurate to 0.0002g). 4.4.3 Calculate the mass percentage of acetone insoluble matter Xs according to formula (3): Xs = m1 = m2 × 100
Wherein: m1—the mass of the crucible and acetone insoluble matter after constant weight, g; m2—the mass of the sand core after constant weight, g;
m—the mass of the sample, g.
5 Inspection rules
5.1 Alachlor technical should be inspected by the quality supervision and inspection department of the manufacturer. Acetone insoluble matter is a random inspection item, which should be inspected at least once a week. The manufacturer should ensure that all Alachlor technical products shipped from the factory meet the requirements of this standard, and each batch of Alachlor technical products shipped from the factory should be accompanied by a quality certificate. 5.2 The mass of each batch of Alachlor technical products should not exceed the capacity of the packaging storage tank. 5.3 The sampling method should be carried out in accordance with GB1605.
5.4 The user has the right to verify whether the received alachlor technical product meets the requirements of this standard in accordance with the provisions of the product standard. 5.5 In the test results, if some indicators do not meet the standards, samples should be taken from twice the number of packages for re-verification. If only one indicator does not meet the requirements, the whole batch of products will be unqualified. 5.6 When the supply and demand parties have disputes over product quality, they can be resolved through negotiation or the statutory inspection agency can 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 technical should comply with the relevant provisions of GB3796. 6.2 Alachlor technical is packaged in galvanized iron drums, and the net weight of each drum shall not exceed 200kg. Other forms of packaging can also be used according to the requirements of users.
6.3 During storage and transportation, strictly prevent moisture and sunlight, maintain good ventilation, do not mix with food, seeds, and feed, avoid contact with skin, and prevent inhalation through the mouth and nose.
Additional Notes:
This standard was proposed by the Department of Science and Technology of the Ministry of Chemical Industry. This standard is under the jurisdiction of Shenyang Institute of Chemical Industry. This standard was drafted by Shenyang Institute of Chemical Industry. The main drafters of this standard are Jiang Minyi, Yuan Chunfeng, Li Xiujie, Lu Zenan, and Xu Meiying. 5
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