超临界萃取系统应用于环境分析的简介

1,Applied Separations was started in 1987 In 1992, Applied Separations entered into a CRADA with the U.S. Department of Agriculture to develop a low-cost supercritical fluid extraction instrument that overcomes many of the shortcomings of the instruments currently in the marketplace. The culmination of this effort, two years later, was the Spe-edSFE.,Copyright 2010 Applied Separations, Inc. All Rights Reserved.,2,What is aSupercritical Fluid?,3,Phase Diagram,Solid,Liquid,Gas,Temperature / C,SupercriticalFluid,31 Tc,Pressure / Atm,Pc 73,CO2,Supercritical Point,4,Physical Properties of Liquids, Gases and Supercritical Fluids,5,Supercritical Fluid (SCF),Density to dissolvePermeability,Not a gas Not a liquidBut with the advantages of both!,6,Critical Conditions of Various Solvents,7,Carbon Dioxide,Safe, environmentally friendlyInexpensive, readily availableNo residueMild ConditionsTunable,CO2 is the gas most commonly used as a supercritical fluid.,CO2 is:,8,Tunable,?,9,SuperCriticalFluid,Solid,Liquid,Increasing the pressure increases the density and makes the supercritical CO2 simulate greater polarity.,Gas,Carbon Dioxide,Pressure,Polar,Non Polar,Hexane,Methanol,Ethyl Acetate,a Tunable Solvent,a Tunable Solvent,10,One “solvent” has.,Solubility characteristics of many,11,12,Discussion,Where supercritical fluid are used todayStandard Supercritical Fluid systems from Applied SeparationsCustom SFE systems,13,Uses forSupercritical Fluids Today,14,Uses of Supercritical Fluids,Analytical SFEProcess development SFE,15,Uses of Supercritical Fluids,Environmental Natural ProductsPharmaceuticals and BiotechnologyFoodSpecialty Chemicals and PolymersTextilesElectronics Cleaning Analytical,16,Uses of Supercritical Fluids,Natural ProductsEthical and herbal medicinesFragrances and pigmentsNo solvent residueFractionationPharmaceuticals and BiotechnologyEthanol/Solvent removal Aerosols and particle sizing and morphologyCell lysing,17,Uses of Supercritical Fluids,FoodNo solvent residuesProcess ImprovementsFlavors and FragrancesPesticide RemovalResidual ExtractionRejuvenationSpecialties,18,Uses of Supercritical Fluids,ElectronicsElimination of chlorinated solventsOptical fiberIC processesPhotoresist developersCleaningMachine partsMedical DevicesDry cleaning,19,Uses of Supercritical Fluids,Specialty Chemicals and Polymers Impurity removalCFC productionMetal coatingsAerogelOil refining and productionTextilesImpregnation/dyeingSizing and finishing,20,Uses of Supercritical Fluids,Analytical TestingDrugs of AbuseSealed PackagingFoodCapsulesWeapons and ExplosivesTerrorist,21,Uses of Supercritical Fluids,Environmental-The EPA draft method 3560/8440 for the analysis of total petroleum hydrocarbons (TPH) in soil using SFE has been published.,22,Uses of Supercritical Fluids,Table 49 Representative Applications of Off-Line SFE for Quantitative Analysis,23,Discussion,Where supercritical fluid are used todayStandard Supercritical Fluid systems from Applied SeparationsConsiderations for analytical systems,24,Conception to Production,Analytical,Production,Pilot Plant,Applied Separations Supercritical Fluid Extraction Systems,Pilot Plant,25,Supercritical Fluid Extraction Instruments and Systems,Spe-ed SFEAnalytical instrument series “oven based”HelixBench top pilot plantMatrixMultipurpose, movable pilot system2Tech-L/SMultipurpose, movable pilot/small production system,26,Supercritical Fluid Extraction Instruments and Systems,Spe-ed SFEAnalytical instrument series “oven based”Vessels are heated by placing them in an ovenMaximum versatilityMany different sizes of vessels can be used Cost savingsNo need to purchase any additional SFE instruments,27,Supercritical Fluid Extraction Instruments and Systems,Spe-ed SFEAnalytical instrument series,28,Supercritical Fluid Extraction Instruments and Systems,Spe-ed SFE Analytical InstrumentsSpe-ed SFE-2General applicationsSpe-ed SFE-4General applicationsSpe-ed SFE-NPSpecifically designed for natural products Spe-ed SFE-15000Higher pressure applications,29,Applied Separations Spe-ed SFE Analytical Instrument,3 ModulesPumpOvenCollection and control,30,Spe-ed SFE,CO2 Pump Module,Modifier Pump Module,SPE,Neat,Micrometering Valves,Oven Module,ExtractorVessels,Carbon Dioxide,Air source,31,Applied Separations Spe-ed SFE Analytical Instruments,Pump ModuleReliable air driven pump10,000 psi (680 Bar)25 mL/min flow rate,32,Applied Separations Spe-ed SFE Analytical Instruments,Oven Module250o CVessels: Size: 5mL to 2 LitersQuantity: 2 4Parallel Processing,33,Applied Separations Spe-ed SFE Analytical Instruments,ControlHeated micrometering valveFlow meterCollectionNeatLiquid trapSPE,34,Important Parameters of an SFE System,PressureTemperatureFlow RateExtraction Vessel CapacityCollection CapabilitySafety,35,Pressure Considerations,Some analytes are soluble only at high pressures,36,Triglyceride / Natural Oils Solubility Curves,Dont leave potential extracts in the vessel,37,Important Parameters of an SFE System,PressureTemperature,38,Temperature,Increased solubility,39,Solubilities* Increase with Temperature,Units,*Anthracene,40,Temperature,Increased solubilityKineticsHigh temperature can increase rate of desorbtion of bound compounds from matrix making them available for solublization,41,SFE Extraction Efficiencies of PCBs in River Sediment (SRM 1939),PCB Congeners,% Recovery,350 atm,42,SFE Extraction Efficiencies of PCBs in River Sediment (SRM 1939),PCB Congeners,% Recovery,650 atm,43,Important Parameters of an SFE System,PressureTemperatureFlow Rate,44,Flow Rate,Reduces time necessary to do extraction,45,Importance of Flow Rate,Effect of SFE flow-rate on the extraction of motor oil from soil,Extraction time (min),% Recovery,340 atm at 80 C. EPA Method 3560. Extraction efficiency 100% = 4 hours Soxhlet using trichlorotrifluoroethane,*,46,Flow Rate,Reduces time necessary to do extractionAnalytes with low solubility may be extracted without modifiers,47,Paradox: Polar Compound Soluble in Non-Polar Solvent SFE Recovery of Nitrosamines from Fortified All-Meat Frankfurters,48,High Solubility,Samplewith Analyte,Solvent,49,High Solubility,Samplewithout Analyte,Analyte Dissolved in Solvent,50,Low Solubility,Samplewith Analyte,Solvent,51,Low Solubility,Samplewithout Analyte,Analyte Dissolved in Solvent,52,Low Solubility - CO2,Samplewith Analyte,Solvent - CO2,53,Low Solubility - CO2,Samplewithout Analyte,Analyte Dissolved in CO2,54,Auto Concentrating,Samplewithout Analyte,Ambient CO2,55,Important Parameters of an SFE System,PressureTemperatureFlow RateExtraction Vessel Capacity,56,Extraction Vessel Size,Variety of larger size vesselsAnalytical to production2.5 ml to 2 litersLower concentration feedstocks,57,Important Parameters of an SFE System,PressureTemperatureFlow RateExtraction Vessel CapacityCollection Capability,58,Collection,Several Means of CollectionNeatDissolving into SolventDisposable solid supportInert materialActive sorbent - SPE,59,60,Important Parameters of an SFE System,PressureTemperatureFlow RateExtraction Vessel CapacityCollection CapabilitySafety,61,Safety Measures,PassiveAudible AlarmVisual Blinking LightActiveAutomatic Air Relief ValveRupture Disc,62,Discussion,What is a supercritical fluidWhy sell supercritical fluid extractionDescription of the analytical Spe-ed SFEOther SFE Systems,63,Supercritical Fluid Extraction Instruments and Systems,Spe-ed SFEAnalytical instrument seriesHelix pilot plant on the bench topMatrixMultipurpose, movable pilot system2Tech-L/SMultipurpose, movable pilot/small production system,64,Helix,Fits on a lab bench500ml extractor300ml cyclonic separator50 ml/min pumpPressurized solvent extractionFragrance extraction packageParticle generation packageAerogel dryingData logging,65,2Tech-L/S-2,Multipurpose, movable pilot/small production system,Solids extractionLiquid extractionCounter-currentLiquid batchCounter-current absorptionSchematic following control panelRecycle CO2Automation interface,66,2Tech-L/S System Specifications,Vessel size:2 or 5 liter Pressure:680 barTemp:150CPump CO2:300 g/minCC Vessel:2 liter Liquid feed:130 g/minCross over networkRecycle CO2 Automation interface,67,Discussion,Where supercritical fluid are used todayStandard Supercritical Fluid systems from Applied SeparationsConsiderations for analytical systemsCustom SFE systems,68,Custom Supercritical Fluid Systems,Applied Separations manufactures systems5 liters to 5,000 litersTo machine specs or to process specsAutomated or manual,Applied Separations will work with you!,69,If youre not thinking SFE,Youre not thinking,70,71,72,73,METHOD 8270C SEMIVOLATILE ORGANIC COMPOUNDS BY GAS CHROMATOGRAPHY/MASS SPECTROMETRY (GC/MS),74,Table 51 Effect of Temperature on Percent Recoveries of PAHs from a Railroad Soil Using Pure CO 2 Compared with Thermal Desorption Under Nitrogen,Supercritical fluid extraction recoveries at