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Chemical Industry Standard of the People's Republic of China
HG2161—91
Tricyclazole Wettable Powder
Published on November 18, 1991
Ministry of Chemical Industry of the People's Republic of China
Implemented on May 1, 1992
Chemical Industry Standard of the People's Republic of China
Tricyclazole Wettable Powder
Subject Content and Scope of Application
HG2161—91
This standard specifies the technical conditions, inspection methods, inspection rules, and marking, packaging, transportation and storage requirements for 20% tricyclazole wettable powder.
This standard applies to tricyclazole wettable powder processed from tricyclazole technical with fillers and additives. Active ingredient: tricyclazole.
Chemical name, 5-methyl-1,2,4-triazolo-3,4-b)benzothiazole. Structural formula:
Molecular formula: C.HN.S
Relative molecular mass: 189.24 (1987 international relative atomic mass)2
Cited standards
GB1601
Determination method of hydrogen ion concentration of pesticides
GB1605
Sampling method of commercial pesticides
GB3796
6 General rules for pesticide packaging
GB5451
Determination method of wettability of pesticide wettable powders HG2-896 Determination method of fineness of pesticide powders 3 Technical requirements
3.1 Appearance: Grey or light yellow to brownish yellow loose powder. Tricyclazole wettable powder should also meet the following index requirements: 3.2
Tricyclazole content, %(m/m)
Fineness (through 45um sieve), %(m/m)Wetting time, min
Suspension rate, %(m/m)
Approved by the Ministry of Chemical Industry of the People's Republic of China on November 18, 1991>
20.0±:
Implementation on May 1, 1992
4 Inspection method
4.1 Determination of tricyclazole content
4.1.1 Summary of method
HG2161—91
The sample is extracted with chloroform and centrifuged. Tricyclazole is separated and quantified using a chromatographic column filled with SE-30/GasChromQ and n-tetracosane as the internal standard. 4.1.2 Reagents and solutions
Tricyclazole standard sample: known content, ≥99.0% (m/m); internal standard: n-tetracosane (no impurities interfering with analysis); chloroform (GB682);
Fixed liquid: SE-30
Carrier: GasChromQ or ChromosorbW-HP, 180~250um (60~80 mesh); internal standard solution: use chloroform to prepare a solution containing 12g of n-tetracosane. 4.1.3 Instruments
Gas chromatograph: hydrogen flame ionization detector; chromatographic column: glass column with a length of 1m and an inner diameter of 3mm, filled with 7% SE-30/GasChromQ (or ChromosorbW-HP), 180~250um filler;
Microinjector: 10uL;
Centrifuge: with 50mL centrifuge tube.
4.1.4 Operation steps
4.1.4.1 Preparation of chromatographic column
4.1.4.1.1 Coating of stationary liquid
Weigh about 0.28g SE-30 in a 250mL beaker, add about 25mL chloroform (it is appropriate for the solvent to just immerse the carrier), stir to completely dissolve it, pour about 4g of the weighed carrier into the above beaker at a time, shake it gently to mix it evenly, wait for it to dry slightly, pour it into culture III, place it under an infrared lamp, let the solvent evaporate to near dryness, and then place it in a 100℃ oven to dry for 2h. 4.1.4.1.2 Filling of chromatographic column
Connect a small glass funnel to the inlet end of the cleaned and dried chromatographic column, plug an appropriate amount of silanized glass wool at the outlet end and wrap it with clean gauze, and connect it to the vacuum pump with a clean rubber tube. Turn on the vacuum pump, pour the filler in from the funnel in batches, and tap the column wall continuously to make the filler fill the chromatographic column tightly and evenly, then insert a small ball of silanized glass wool into the column inlet and press it properly. 4.1.4.1.3 Aging of the chromatographic column
Connect the inlet of the chromatographic column to the vaporization chamber, and temporarily do not connect the outlet to the detector. Raise the temperature to 280℃ in stages at a nitrogen flow rate of about 15mL/min, and age at this temperature for at least 48h. After cooling, connect the column outlet to the detector. 4.1.4.2 Gas chromatography operating conditions
Temperature:
Column chamber 240℃;
Vaporization chamber 290℃;
Detector 290℃.
Gas flow rate:
Carrier gas (N2) 30mL/min;
Hydrogen 50mL/min;
Air 500mL/min.
Recorder paper speed: 4mm/min.
Injection volume
2uL.
Retention time:wwW.bzxz.Net
Tricyclazole about 3min;
Tetracosane about 6min.
HG2161—91
The above gas chromatography operating conditions are typical operating parameters. According to the characteristics of the instrument, the operating parameters can be appropriately adjusted to obtain the best effect.
Gas chromatogram of tricyclazole wettable powder
1-Tricyclazole; 2-n-tetracosane
4.1.4.3 Preparation of standard solution and test solution4.1.4.3.1 Standard solution
Weigh 0.125g (accurate to 0.0002g) of tricyclazole standard sample, place it in a 25mL volumetric flask, add 10mL of internal standard solution with a pipette, add chloroform to the scale, and shake well. 4.1.4.3.2 Test solution
Weigh a test sample containing about 0.125g of tricyclazole (accurate to 0.0002g) in a 50mL centrifuge tube, add 10mL of internal standard solution with a pipette, and then add 15mL of chloroform, shake well, centrifuge, and take the supernatant. 4.1.4.4 Determination
Under the selected chromatographic conditions, after the instrument is stable, repeatedly inject 2uL of tricyclazole standard solution until the change in the peak area ratio of tricyclazole to internal standard between two consecutive injections is less than 1%. Then analyze in the following order: a. Standard solution;
b. Sample solution;
c. Sample solution;
d. Standard solution.
4.1.4.5 Calculation
HG 216191
According to the chromatograms of the four injections a, b, c, and d, calculate the average value of the peak area ratio of tricyclazole to internal standard for injections a and d and injections b and c, respectively. The mass percentage content X1 of tricyclazole is calculated according to formula (1): ri.mP
Wherein: r1——the average value of the peak area ratio of tricyclazole to the internal standard in the two sample solutions of b and c; r2——the average value of the peak area ratio of tricyclazole to the internal standard in the two standard sample solutions of a and d; m1——the mass of the sample, g;
m2——the mass of the sample, g;
P——the percentage content of the standard sample, % (m/m). 4.1.5 Allowable difference
The difference between the results of the two parallel determinations of this standard shall not exceed 1.0%. 4.2 Determination of pH value
Determine according to the pH meter method in GB1601.
4.3 Determination of wetting time
Determine according to the method in GB5451.
4.4 Determination of fineness
Determine according to the method in HG2-896.
4.5 Determination of suspension rate
4.5.1 Summary of method
: (1)
Use standard hard water to prepare a suspension of known concentration. Under specified conditions, determine the content of tricyclazole in the bottom 1/10 of the suspension and calculate the suspension rate of the sample.
4.5.2 Reagents
Standard hard water, 342 ppm, prepared according to the provisions of GB5451. 4.5.3 Apparatus
Measuring cylinder with stopper: the distance between 0-250mL scale should be 20.0-21.5cm, the distance between 250mL scale and the bottom of the stopper should be 4-6cm;
Glass pipette: about 40cm long, inner diameter about 5mm, with a 2-3mm hole at one end, the other end of the tube connected to the corresponding suction source,
Glass constant temperature water bath: 30±1℃;
Stopwatch.
4.5.4 Determination steps
Weigh a liquid containing about 0.Place a 13g sample of tricyclazole in a 100mL beaker, add 510mL of standard hard water, swirl the beaker, and after the sample is self-wetted, add 50mL of standard hard water (30±1°C) while stirring, and place the suspension in a water bath at the same temperature for 13 minutes. Then wash it all into a 250mL stoppered cylinder with 30±1°C standard hard water, dilute to the scale, and cover the stopper. Invert the cylinder 30 times within 1 minute, then place it vertically in a constant temperature water bath without vibration, open the stopper, and place it for 30 minutes. Use a pipette to remove 9/10 (i.e. 225mL) of the suspension in 10 to 15 seconds. Do not shake or stir up the sediment in the cylinder, and ensure that the top of the pipette is always a few millimeters below the liquid surface. Use a long pipette to draw the remaining 1/10 (25 mL) of the suspension into a 50 mL centrifuge tube, rinse the bottom of the measuring cylinder with 10 mL of water three times (avoid washing the sticky materials on the upper wall of the measuring cylinder), and transfer them to the centrifuge tube. Use a pipette to add 10 mL of internal standard solution and 15 mL of chloroform. Stir well with a glass rod, centrifuge, take the organic phase, and determine the content of tricyclazole according to the steps specified in 4.1.4.4. 4.5.5 Calculation
First calculate the mass of tricyclazole in the remaining 1/10 suspension. The suspension rate X2 of tricyclazole wettable powder expressed as a mass percentage is calculated according to formula (2): X2=m1=m2x10x
Wherein: m1—the mass of tricyclazole in the sample used to prepare the suspension, g; m2—the mass of tricyclazole in the remaining 1/10 suspension in the measuring tube, g. 4.5.6 Allowable error
The difference between the results of two parallel determinations of this method should not exceed 5.0%. 5 Inspection rules
5.1 Tricyclazole wettable powder should be inspected by the quality supervision and inspection department of the manufacturer. The manufacturer should ensure that all tricyclazole wettable powders shipped out of the factory meet the requirements of this standard, and each batch of tricyclazole wettable powder shipped out of the factory should be accompanied by a quality certificate in a certain format. 5.2 The user has the right to inspect the quality of the received tricyclazole wettable powder in accordance with the provisions of this standard to see if it meets the requirements of this standard.
5.3 Sampling method: According to the sampling method of wettable powder in GB1605, mix the samples evenly and put them into two clean, dry glass bottles with ground stoppers. Paste labels on the bottles, indicate the manufacturer's name, product name, batch number, sampling date, and send one bottle to the quality supervision and inspection department for inspection. One bottle is sealed.
5.4 In the test results, if some indicators do not meet the requirements of this standard, re-samples should be taken from twice the amount of packaging for inspection. If only one indicator does not meet the requirements of this standard, the whole batch of tricyclazole wettable powder is unqualified. 5.5 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 according to the inspection method specified in this standard.
6 Marking, packaging, transportation and storage
6.1 The marking and packaging of tricyclazole wettable powder shall comply with the relevant provisions of GB3796. 6.2 Tricyclazole wettable powder is packed in 80g kraft paper bags, covered with sealed plastic film bags, with a net weight of 200g or 500g per bag. A certain number of small bags are tightly arranged in a calcium plastic box or iron barrel, with a net weight of no more than 25kg per box (barrel) (other forms of packaging can also be used according to user requirements).
6.3 During storage and transportation, it should be strictly protected from moisture and sunlight, and maintained in good ventilation. It should not be mixed with food, seeds and feed, and should avoid contact with the skin and inhalation through the mouth and nose.
6.4 The shelf life of this product is 2 years. During the shelf life, except for the suspension rate being allowed to drop to 65%, other indicators should still meet the standard requirements.
Additional remarks:
This standard is proposed by the Science and Technology Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard is drafted by the Shenyang Chemical Industry Research Institute and Hunan Pesticide Factory. The main drafters of this standard are Lou Shaowei, Gao Xiaohui, Xu Fan, Zou Boliang, Yao Jiaren and Wen Meirong.
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