How can one determine the structure of Methyl 3, 3-Dimethylpet-4-ENOATE?

This article will tell how to determine the Methyl 3, 3-Dimethylpet-4-ENOATE in the air, aiming to provide reference and experimental support for researchers in the fields of chemistry and other fields.

Background: METHYL 3, 3-Dimethylpet-4-Enoate is a key intermediate of DV- chrysanthemine and Z-CIS- trifluorosamosamosamite. This can be used to synthesize many insecticides for hygiene and agricultural use. Therefore, the study of Methyl 3, 3-Dimethylpet-4-Enoate plays an important role in the production of pyreteloderbhees.

Testing:

Wang Xiao and others establish the monitoring and analysis method of Methyl 3, 3-DimetHylpet-4-Enoate in the air. The method is: METHYL 3, 3-Dimethylpet-4-ENOATE adsorb , acetone solving , GC-FID measurement , The legal quantity of external bids. The method is quantitatively quantitative. , High sensitivity , is easy to operate , Can meet the micro-amount Methyl 3, 3-Dimethylpet-4-ENOATE monitoring needs in the air. The specific analysis method is as follows:

( 1 ) Sample before processing

Drive the activated carbon and silicone sampling pipes that are rich in samples. Activated carbon bottle , 2ml acetone to silicone bottle , parsing time 20min, filter the solution to GC small bottle for chromatography for chromatography analyze.

( 2 ) Chromatography conditions

The column temperature is constant to 60 ℃, maintain time 6.5min, balance time 0.50min . The sample inlet mode is diversion , diversion ratio ratio ratio than 5: 1, diversion flow : 10.0ml/min; Total traffic : 14.3ml /min . Temperature : 250 ℃; pressure : 63.9kpa; The load is high -purity nitrogen ( purity > ; 99.999%) . The detector (FID): The temperature is 250 ℃, hydrogen flow 30.0 ml/min, air flow 400.0ml/min, < /SPAN> High pure nitrogen ( purity purity with a constant tail flowing flow is ( purity purity purity purity 99.9999%).

( 3 ) The preparation of standard solutions and drawing of standard curves

According to the density of Methyl 3, 3-Dimethylpet-4-Enoate 0.90mg/μL, Putting its pure standard products with carbonide into a reserve A (9.0 μg/μL) And reserve B (0.90 μg/μL) . Methyl 3,3-dimethylpet-4-enoate is used as 9.0 μg/μL and 90 μl . The reserve of a certain amount of Methyl 3, 3-Dimethylpet-4-ENOATE with a certain amount of carbon sulfide as the solvent , respectively. span> 1.8 , 5.4 , 9.0 , 18.0 and 54.0 μg/ml, The standard series , uses the concentration of the peak area as the vertical coordinates.

( 4 ) Adsorption efficiency experiment

Perform gas adsorption efficiency experiments and use simulated gas. The gas collection pump drives gas from 25 milliliter flow to the activated carbon attachment pipe or silicone adsorption pipe. The color tube is placed in the 50 ° C the constant temperature in the water bath. The exit is connected to the gas collection pump. Slowly add 10 micro -lift blank bidding standard solution through a trace injection, which contains 90 micropenyl benzoate. Under the influence of the gas collection pump, the gas in the tube will be rich to adsorption pipes. 5 gas lift gas is collected at the rate of 1.0 / at the rate of minutes, and then the standard substance is analyzed through the premium of carbonide or acetone to relieve the front and rear segments.

( 5 ) Experiment of absorbing efficiency

Place the activated carbon and silicone pipe particles in the brown suction bottle , use a trace syringe into the granules that are standardized in the solution bottle /span> Reserve B, contains METHYL 3, 3-Dimethylpet-4-Enoate 18 μg, span>, Place 20 min . Open the bottle cap and add carbonide 2ml in the active carbon bottle , acetone 2ml > 20min, Filter it in GC small bottle , determines its content through chromatography.

( 6 ) The breakdown volume Experiment

The breakdown volume actually measures the adsorption ability of adsorbent treatment to measure the substance , The content detected in the rear adsorb agent WB exceeds the previous paragraph WF 10%, , is considered to be a breakdown. In 50 ℃ 25 of the water bath ML The 500,1000,2 000 μl SPAN>), and the adsorption pipes connected to the sampler at the mouth of the color pipe to collect METHYL 3, 3-Dimethylpet-4-Enoate , 1.0 L/min Collection 5L . The above experiments were used to use silicone pipes and activated carbon pipes to analyze , chromatography, and the content of METHYL 3,3-dimethylpet-4-enoate (μg) wf and wb, < /span> For example, BV (WB/WF) ≥10%, believes that the current bid increase is the breakdown of the standard substance on the sampling tube.

The results are: 5L containing 90 μg Methyl 3, 3-Dimethylpet-4-Enoate simulation gas as experiments , adsorption efficiency is 82 %. Experiments 18 μg Methyl 3, 3-Dimethylpet-4-Enoate as experiments , suction efficiency is 94%, sample volume is 10L <10L < /span> , instrument minimum detection limit is about 0.02mg/m3 .

References:

[1] Xiao Guang Li Yingtang . The improvement of the synthesis process improvement process of triple fluorosamosamoshiculose acid products [j]. salt and chemical , 2010, 39 (04): 27-29. Doi: 10.16570/J.CNKI.ISSN1673-6850.2010.04.015

[2] Wang Xiao Zhou Xiaojun , Liu Ge et al. Methyl 3, 3-Dimethylpet-4-Enoate measurement method in the air span> [j]. Environment and occupational medicine , 2009, 26 (06): 617-619. Doi: 10.13213/j.cnki.jeom.2009.06.001

[3] METHYL 3, 3-Dimethylpet-4-Enoate . Jiangsu Province , Jiangsu Province Pesticide Research Institute Co., Ltd. , 2004-01-01. < /span>