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پاورپوینت کامل مالئیک اسید ۷۰ اسلاید در PowerPoint

اسلاید ۴: ۴ScopusISI web of knowledge1990-20089688Supercritical fluid78116Supercritical carbon dioxide3459Supercritical carbon dioxide AND Extraction48Supercritical carbon dioxide AND reactionPublications in the Field of SCF in Iran

اسلاید ۵: ۵Reactive Exns When the extracting solvents are apolar, their ability to extract the polar compounds such as organic acids, amino acids, and phenols is low. About 30 years ago extraction with the help of a chemical reaction or strong physical interaction between the extracting solvent and the sample was used to solve the problem in LLE.In this method usually a small amount of a reactant is added to the extracting solvent to:1) Increase solvent polarity2) Have specific interactions with analyte3) Increase the extraction selectivity

اسلاید ۶: ۶Applications of Reactive Extractions in LLE Systems 1) Separation and purification of heavy metal ions such as platinum, Ga (e.g. selective extraction of Ga from coal), etc using organic ligands or strong Lewis bases2)Extraction of organic compounds from aqueous solutions have also been extensively studied:a)Separation of amino acids using bis(2-ethylhexyl) phosphoric acids b) Separation of Penicillin using Amberlite LA-2Amberlite, LA-2 LIX 54-N

اسلاید ۷: ۷ Mechanisms of Reactive Extraction of Organic Acids Using Amines Four major mechanisms for extraction of organic acids with amines has been proposed:1- Ion exchange mechanism; in an aquous solution of an organic acid or its salt and extractant including an amineR4N+ A-org + HXaqR4N+ X-org + HAaq2- Ion-pair formation; when the basic power of the extracting amine is equal or higher than the anion to be extracted.RnNH(4 – n)org+ RnNH(3 – n)org + H+aq3- Hydrogen bonding formation4- Solvation mechanismRnNH+ (4 – n) org … A-orgRnNH+ (4 – n) org + A-aq RnNH+4-n A-org + HXaqRnNH+4-n X-org + HAaq

اسلاید ۸: ۸Reactive Extraction of Carboxylic Acids in a LLE system Organic extractants already used are divided into 3 major categories:1- Hydrocarbons and oxygen containing extractants.2- Solvents containing oxygen and phosphorous.3- High molecular weight aliphatic amines Use of amines in the reactive extraction is limited to tertiary amines with long alkyl chainprimary amines are water soluble secondary amines are changed into imines when distilled or their pH is changed dramatically for separation of amine from acid higher efficiencycheaper than organophosphorous solventsreversible reaction with carboxylic acidshigh selectivity

اسلاید ۹: ۹Experimental Section

اسلاید ۱۰: ۱۰CO2Schematic diagram of SFE system1st Time Reactive Exn of Carboxylic Acids Using SCF Saturated from TOA

اسلاید ۱۱: ۱۱PumpBPRPumpBPRSolventMicrosampling Method Used ab

اسلاید ۱۲: ۱۲GC was used for quantitation of the extracted MA & PA1. MA decomposes at 135 oC at the GC injection port2. TOA-acid ion-pair Boiling point is higher than the injection port temperature3. Direct determination of dicarboxylic acids needs very high polar columns. Normal columns leads to broadened and asymmetrical peaks which is not good for quantitative works.Therefore, the acids should be changed to compounds that could be easily separated

اسلاید ۱۳: ۱۳Determination of Extracted Samples via Derivatization Methanolic BH3Benzyl bromideAcetic anhydrideTFAA & butanol

اسلاید ۱۴: ۱۴ROH = ButanolButanoic Acid (Z)/Maleic Acid Dibutyl Ester

اسلاید ۱۵: ۱۵

اسلاید ۱۶: ۱۶Phthalic Acid Dibutyl Ester ROH = Butanol

اسلاید ۱۷: ۱۷

اسلاید ۱۸: ۱۸Carrier gas = N2OV-1, 15 m capillary columnInjection port temp. = 240 oCFID temp. = 250 oCTemp. program; 1min at 70 oC with the rate of 10 oC/min to 250 oC for 5 min

اسلاید ۱۹: ۱۹In 70 L glass capillary tubes.Three parameters affect the derivatization:1) The amount of derivatizing agent/g of sample2) Derivatization temperature3) Derivatization timeDerivatizationThese stages were optimized using the GC peak area of the reaction products to the IS (dibenzyl ether)

اسلاید ۲۰: ۲۰Effect of the Derivatization Reagent (TFAA) Volume (µL) on the Peak Area of Derivatized Maleic Acid (), and Phthalic Acid (), at 463 K and 20 min Reaction Time

اسلاید ۲۱: ۲۱Effect of the Derivatization Reaction Temperature on the Peak Area of Derivatized Maleic Acid (), and Phthalic Acid (), at 423 K.

اسلاید ۲۲: ۲۲Effect of Derivatization Reaction Time on the Peak Area of Derivatized Maleic Acid (), and Phthalic Acid () at 190 oC

اسلاید ۲۳: ۲۳The effect of TOA on the Maleic Acid Derivatization00.20.40.60.811.21.41.61.8200.20.40.60.811.2g TOA per 5mL solutePeak area maleic acid / Is

اسلاید ۲۴: ۲۴۰۰.۲۰.۴۰.۶۰.۸۱۱.۲۱.۴۱.۶۱.۸۲۰۰.۲۰.۴۰.۶۰.۸۱۱.۲g TOA per 5mL solutePeak area phthalic acid / IsThe effect of TOA on the Phthalic Acid Derivatization

اسلاید ۲۵: ۲۵Phthalic AcidCalibration Curve Maleic Acid Calibration Curve

اسلاید ۲۶: ۲۶Parameters Affecting the Exn of Maleic and Phthalic Acid

اسلاید ۲۷: ۲۷The Effect of Dispersing Agent Crushed Glass Increases the repeatability and Exn Yield Increases the Contact Surface of the Solvent and Sample Reduces ChannelingCrushed Glass/Sample = 70 %; Mesh 40-60, and MA/PA = 1

اسلاید ۲۸: ۲۸The Effect of Static Time The sample is kept in contact with the solvent The higher the static time the higher the interaction between scCO2 and the sample and the higher the exn efficiencyStatic time of 30 min was chosen

اسلاید ۲۹: ۲۹Ta