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Professional Standard of the People's Republic of China
ZBG25015-90
Trichlorobenzolidine 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
Trichlorobenzolidine technical
Subject content and scope of application
ZBG25015-90
This standard specifies the technical requirements, inspection methods, inspection rules, and packaging, marking, transportation and storage conditions of trichlorobenzolidine technical. This standard applies to trichlorobenzolidine technical prepared from trichlorobenzene, chlorosulfonic acid and monochlorobenzene as the main raw materials through acylation, condensation and refining. Active ingredient: Trichloroacetic acid
Chemical name: 2,4,45-Tetrachlorodiphenyl sulfoneMolecular formula: C12H.Cl,O2S
Structural formula:
Relative molecular mass: 356.06 (1987 international atomic weight) 2 Reference standards
GB1600
Method for determination of moisture content in pesticides
Sampling method for commercial pesticides
GB1605
GB3796
3 Technical requirements
General rules for pesticide packaging
3.1 Appearance: Light yellow or yellow fine granular solid. 3.2
The technical material of trichlorobenzamide shall also meet the following index requirements: Index name
Trichlorobenzamide content
Acidity (in HSO)
Test method
4.1 Determination of trichlorobenzamide contentbzxz.net
Approved by the Ministry of Chemical Industry of the People's Republic of China on April 11, 1990 S
Superior grade
%(m/m)
Implementation on January 1, 1991
4.1.1 Summary of method
ZBG25015-90
The sample was dissolved in chloroform and n-hexadecane was used as the internal standard. The trichlorobenzamide was separated and quantified on a SE-30 column using a gas chromatograph with a hydrogen flame ionization detector. 4.1.2 Reagents and solutions
Chloroform (GB682);
Trichlorobenzyl sulfone standard sample: known content; stationary phase: SE-30;
Carrier: Chromosorb
W-Hp180~250μm (60~80 days);
Internal standard: n-hexacosane;
Internal standard solution: weigh 0.480g of n-hexacosane (no impurities interfering with chromatographic analysis) in a 200mL volumetric flask, dissolve and dilute to the scale with chloroform, and shake well.
4.1.3 Instruments
Gas chromatograph: with hydrogen flame ionization detector; recorder or gas chromatography data processor; chromatographic column: 1m long, 3mm inner diameter stainless steel column; p180~250μm;
Column filling: 5%SE-30/ChromosorbW-Hpd.
Micro-injector: 10μL.
4.1.4 Preparation of chromatographic column
4.1.4.1 Coating of stationary liquid
Weigh 0.20g SE-30 stationary liquid into a 250mL beaker, add appropriate amount (about 22mL) of chloroform to completely dissolve it, pour in 4.0g of carrier, shake gently to mix evenly, and after the solution evaporates to nearly dry, place it in a 110℃ oven for 2h. 4.1.4.2 Filling of chromatographic column
Connect a small funnel to the inlet of the clean chromatographic column, plug the outlet with gauze, and connect it to the vacuum pump with a rubber tube. Turn on the vacuum pump, add the dried filler in batches from the funnel, and tap the tube wall continuously to make the filler fill the chromatographic column evenly and tightly, and plug the two ends of the column with silanized glass wool.
4.1.4.3 Aging of chromatographic column
Connect the inlet of the chromatographic column to the vaporization chamber of the chromatograph, and do not connect the outlet to the detector for the time being. At a carrier gas flow rate of 20mL/min, gradually increase the column temperature to 260℃ and age it at this temperature for at least 48h. 4.1.5 Chromatographic operating conditions
Column temperature: 230℃;
Detection temperature: 250℃;
Vaporization temperature: 250℃.
4.1.5.1 Gas flow rate
Carrier gas (nitrogen): 60mL/min;
Hydrogen: 36mL/min;
Air: 300mL/min;
Injection volume: 0.8uL.
Retention time
Trichlorobenzylsulfone is 7min;
N-hexacosane is 10.5min.
ZBG25015-90
Chromatographic separation diagram of trichlorobenzylsulfone
1-Solvent 2-Trichlorobenzylsulfone 3-N-hexacosane The above chromatographic conditions are typical operating parameters of the chromatograph. When using this standard, the above parameters can be appropriately adjusted according to different gas chromatographs in order to obtain the best results. 4.1.6 Determination steps
4.1.6.1 Preparation of standard solution
Weigh 0.1g (accurate to 0.0002g) of trichlorofenoxal standard sample into a 25mL stoppered glass bottle, accurately add 25mL of internal standard solution with a pipette, and shake well.
4.1.6.2 Preparation of sample solution
Weigh a sample containing about 0.1g (accurate to 0.0002g) of trichlorofenoxal into a 25mL stoppered glass bottle, accurately add 25mL of internal standard solution with a pipette, and shake well.
4.1.6.3 Determination of sample
Under the selected conditions, after the instrument is stable, use a microinjector to inject and analyze in the following order: standard solution, sample solution, sample solution, standard solution. The injection volume is 0.8μL. The difference between the peak area ratio of trichlorobenzol and internal standard in the two sample solutions and the two standard solutions before and after the sample, divided by the average value, should not be greater than 1.0%, otherwise the injection needs to be repeated. 4.1.6.4 Calculation
Calculate the peak area ratio of the two sample solutions and the two standard solutions before and after the sample, respectively, and the mass percentage of trichlorobenzol in the sample, X, according to formula (1):
Ti·m2·P
Where: --- the average value of the peak area ratio of trichlorobenzol and internal standard in the sample solution; 2 --- the average value of the peak area ratio of trichlorobenzol and internal standard in the standard solution; m
the mass of trichlorobenzol technical sample, g; --- the mass of trichlorobenzol standard sample, m2
ZBG25015-90
P --- the percentage of trichlorobenzol standard sample, %. 4.1.6.5 Allowable difference
The difference between two parallel measurements should not exceed 1.2%. 4.2 Determination of moisture
Determine according to the chemical titration method in GB1600. 4.3 Determination of acidity
4.3.1 Reagents and solutions
Acetone (GB686)
Standard sodium hydroxide titration solution: c(NaOH)=0.02mol/L: Bromocresol green-methyl red indicator: 3 parts of 1g/L bromocresol green ethanol solution and 1 part of 2g/L methyl red ethanol solution are mixed evenly. 4.3.2 Analysis steps
Weigh 2.0-2.3g (accurate to 0.0002g) of trichlorobenzyl sulfone technical sample and place it in a 250mL conical flask, add 90mL acetone and 10mL water, and shake well. Add 57 drops of indicator and titrate with sodium hydroxide standard solution until the solution turns bright green, which is the end point. 4.3.3 Calculation
The acidity X expressed as a mass percentage shall be calculated according to formula (2): (V2-V).cX0.049
Wherein: c——actual concentration of sodium hydroxide standard solution (4.3.1.2), mol/L; V——volume of sodium hydroxide standard solution consumed by titrating the sample, mL; Vr——volume of sodium hydroxide standard solution consumed by titrating the blank solution, mL; m——mass of the sample, g;
0.049——mass of sulfuric acid equivalent to 1.00mL sodium hydroxide standard solution [c(Na0H)=1.000mol/L] in grams. 5 Inspection rules
5.1 Trichlorobenzyl sulfone technical shall be inspected and qualified by the quality supervision and inspection department of the manufacturer according to this standard before it can be shipped out of the factory. 5.2 Each batch of sulfonamide technical materials shipped out of the factory should be accompanied by a quality certificate, which includes: manufacturer name, product name, batch number or production date, net weight and proof of product quality conforming to this standard and standard number. 5.3 The quantity of each batch of sulfonamide should not exceed the capacity of the refining tank. 5.4 The user has the right to inspect whether the quality of the sulfonamide technical materials received meets the requirements of this standard in accordance with the provisions of this standard. 5.5 The sampling method should be implemented in accordance with GB1605.
5.6 If any of the indicators in the test results do not meet the requirements of this standard, re-sample from twice the amount of packaging bags for re-testing. Even if only one indicator in the re-test results does not meet the requirements of this standard, the entire batch of trichlorocarbamide is unqualified. 5.7 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 storage
6.1 The marking and packaging of trichlorocarbamide technical shall comply with the relevant provisions of GB3796 General Rules for Pesticide Packaging. 6.2 Trichlorocarbamide technical shall be packaged in plastic woven bags lined with plastic bags, 40kg per bag; other forms of packaging may also be used according to user requirements.
6.3 During storage and transportation, it should be strictly protected from sunlight and rain, and maintained in good ventilation; avoid collision during transportation. It shall not be mixed with food, seeds, and feed, and avoid contact with skin.
Additional instructions:
This standard was proposed by the Science and Technology Department of the Ministry of Chemical Industry. ZBG25015—90
This standard is under the technical supervision of Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. This standard was drafted by Shenyang Chemical Industry Research Institute of the Ministry of Chemical Industry. The main drafters of this standard are Yuan Chunfeng, Jiang Minyi and Li Xiujie. 5
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