Some standard content:
UDC632.95
National Standard of the People's Republic of China
GB12685—90
Tricyclazole technical
1990-12-30 Issued
State Administration of Technical Supervision
1991-12-01 Implementation
National Standard of the People's Republic of China
Tricyclazoletechnical
Subject content and scope of application
GB12685—90
This standard specifies the technical conditions, inspection methods, inspection rules, and marking, packaging, transportation and storage requirements for tricyclazole technical. This standard applies to tricyclazole technical.
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 (according to the international atomic weight in 1987) 2 Reference standards
GB1605
Sampling method for commercial pesticides
GB3796
6 General rules for pesticide packaging
3 Technical requirements
3.1 Appearance: Gray or light yellow to brown powder, without visible foreign impurities. Tricyclazole technical shall also meet the following index requirements: 3.2
go(m/m)
Indicator name
Tricyclazole content
Heating loss
Acidity (in terms of H,SO)
Test method
4.1 Determination of tricyclazole content
4.1.1 Summary of method
Approved by the State Bureau of Technical Supervision on December 30, 1990 as superior product
Qualified product
Implementation on December 1, 1991
GB12685—90
The sample is dissolved in chloroform, and n-tetracosane is used as the internal standard. The tricyclazole is separated and quantified using a chromatographic column filled with SE-30/GaschromQ.
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);
Stationary liquid: SE-30:
Carrier: GaschromQ or chromosorbW-HP, 180~250μm (60~80 mesh); internal standard solution: use chloroform to prepare a solution containing 12g/L 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), 180~250μm filler;
Microinjector: 10μL.
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 into a 250mL beaker, add about 25mL chloroform (it is advisable that the solvent just immerses the carrier), stir to completely dissolve it, pour about 4 weighed carriers into the above beaker at a time, shake gently to mix evenly; after it is slightly dry, pour it into a culture dish, 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 the outlet end with an appropriate amount of silanized glass wool and wrap it with clean gauze, and connect it to the vacuum pump with a clean rubber tube. Turn on the vacuum pump and pour the filler in batches from the funnel while tapping the column wall continuously to fill the column tightly and evenly. Then insert a small ball of silanized glass wool into the column inlet and compress it appropriately. 4.1.4.1.3 Aging of the chromatographic column
Connect the column inlet to the vaporization chamber, and temporarily do not connect the outlet to the detector. Raise the temperature to 280°C 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: 2μL; bzxZ.net
Retention time:
Tricyclazole about 3min,
Tetracosane about 6min.
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.
4.1.4.3 Preparation of standard solution and test solution 4.1.4.3.1 Standard solution
GB12685--90
Gas chromatogram of tricyclazole original drug
1-Tricyclazole; 2-n-tetracosane
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 25mL volumetric flask, add 10mL of internal standard solution with a pipette, dilute to the scale with chloroform, and shake well (filter if necessary). 4.1.4.4 Determination
Under the selected chromatographic conditions, after the instrument is stable, repeat the injection of 2 times 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 perform the injection analysis in the following order: a. Standard solution;
b. Sample solution;
c. Sample solution;
d. Standard solution.
4.1.4.5 Calculation
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 X of tricyclazole is calculated according to formula (1): im.p
GB12685-90
Wherein: yuan——the average value of the peak area ratio of tricyclazole to internal standard substance in the two sample solutions of b and c; r2——the average value of the peak area ratio of tricyclazole to internal standard substance in the two standard sample solutions of a and d; mi
-the mass of the sample, g;
-the mass of the standard, g;
-the percentage content of the standard, % (m/m).
4.1.5 Allowable difference
The difference between the results of the two parallel determinations of this standard shall not exceed 1.5%. 4.2 Determination of heating loss
Weigh 10g of the sample (accurate to 0.001g) in a weighing bottle (30mm high, 65mm inner diameter) that has been dried to constant weight, lay it flat, and place it in an oven and bake it to constant weight at 100±2℃.
The heating loss X expressed as a mass percentage is calculated according to formula (2): Xz= m1=m2 × 100
Wherein: mi-
The mass of the weighing bottle and the sample before drying, g; the mass of the weighing bottle and the sample after drying to constant weight, m; the mass of the weighed sample,.
4.3 Determination of acidity
4.3.1 Reagents and solutions
Acetone (GB686);
(2)
Buffer solution: Mix 100mL120g/L acetic acid solution and 100mL40g/L sodium hydroxide solution, and dilute to 1000mL with deionized water;
Sodium hydroxide (GB629) standard titration solution, c(NaOH)=0.02mol/L. 4.3.2 Instruments
pH meter: accurate to ±0.1pH, should have temperature compensation or temperature correction chart; electromagnetic stirrer;
Glass electrode: should be soaked in water for 24h before use; saturated calomel electrode.
4.3.3 Analysis steps
a. Using the above electrodes and pH meter, measure the pH value of a mixture of 100mL acetone and 10mL buffer solution at 20℃. b. Weigh 1g of sample (accurate to 0.001g) and put it into a 200mL beaker, use 100mL acetone solution, add 10mL water, and titrate with sodium hydroxide standard titration solution to the pH value of the acetone-buffer solution mixture at 20℃ as the endpoint. 4.3.4 Calculation
The acidity X of tricyclazole technical expressed as mass percentage is calculated according to formula (3): Xs = °.VX 0. 049
Wherein: c——actual concentration of sodium hydroxide standard titration solution, mol/L; X100
V——volume of sodium hydroxide standard titration solution consumed by the titrated sample, mL; -mass of the sample, g;
-mass of sulfuric acid in grams equivalent to 1.00mL sodium hydroxide standard titration solution [c(NaOH)=1.000mol/L].
5 Inspection rules
GB 12685-90
5.1 Tricyclazole technical shall be inspected by the quality supervision and inspection department of the manufacturer. The manufacturer shall ensure that all tricyclazole technical shipped out of the factory meets the requirements of this standard. Each batch of tricyclazole technical shipped out of the factory shall 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 technical in accordance with the provisions of this standard to see if it meets the requirements of this standard. 5.3 Sampling method: In accordance with the technical sampling method in GB1605, mix the samples evenly and put them into two clean, dry glass bottles with ground stoppers. Label the bottles with the manufacturer's name, product name, batch number and sampling date. One bottle is sent to the quality supervision and inspection department for inspection and the other bottle is sealed.
5.4 If any index in the inspection results does not meet the requirements of this standard, re-sampling from twice the amount of packaging should be conducted. If only one index does not meet the requirements of this standard, the whole batch of tricyclazole technical is unqualified. 5.5 When the supply and demand parties have a dispute over quality, it can be resolved through negotiation between the two parties, 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 technical shall comply with the relevant provisions of GB3796. 6.2 Tricyclazole technical shall be packaged in woven bags lined with plastic bags, with the net weight of each bag not exceeding 50kg (other forms of packaging may also be used according to user requirements).
6.3 During storage and transportation, it shall be strictly protected from moisture and sunlight, and maintained with good ventilation; it shall not be mixed with food, seeds and feed, and shall avoid contact with the skin and inhalation of isoflurane through the mouth.
Additional notes:
This standard was proposed by the Ministry of Chemical Industry of the People's Republic of China and is under the jurisdiction of the Shenyang Research Institute of Chemical Industry of the Ministry of Chemical Industry. This standard was drafted by the Shenyang Research Institute of Chemical Industry and Hunan Pesticide Factory. The main drafters of this standard are Lou Shaowei, Gao Xiaohui, Xu Fan, Zou Boliang, Yao Jiaren and Wen Meirong. 5
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