analysis in process
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Analysis in ProcESS. Xuan Wang Department of Chemical Engineering Department of Metallurgy and Materials Engineering 23/01/2013. Table of content. Introduction ICP-MS Introduction Principles Influence Sample preparation AAS FT-IR PerkinElmer GC lab Mercury Analyzer - PowerPoint PPT PresentationTRANSCRIPT
Analysis in ProcESS
Analysis in ProcESSXuan Wang
Department of Chemical EngineeringDepartment of Metallurgy and Materials Engineering23/01/2013
Table of contentIntroductionICP-MSIntroductionPrinciplesInfluence Sample preparationAASFT-IRPerkinElmer GC labMercury AnalyzerContact Angle Analyzer
2Introduction ProcESS --- Process Engineering for Sustainable Systems
Research focuses on:
Process intensification
Solid waste treatment
Surface and interphase analysis
Advanced separation processes using membrane technology
Various analytical equipments:ICP-MS, AAS, FT-IR, GC, Mercury Analyzer, Contact Angle Analyzer
33ICP-MS
Advantages: Quantitative and semi-quantitative analysisDetection limits at or below ppt level for much of the periodic table8 orders of magnitude analytical range High productivityIsotopic analysis4Inductively Coupled Plasma Mass Spectrometry
Producer: Thermo Scientific Type: X seriesContact: Michle Vanroelen([email protected])
4
PerkinElmer, Inc5Remark: Method Detection Limit (MDL) is generally 2-10 times more thanInstrumental Detection Limit (IDL)(PerkinElmer)
Principles6Argon Plasma
AerosolSolidGasAtomsIonsRF Load CoilsICP TorchSchematic representation of a quadrupole ICP- MS (PerkinElmer)Ionization of atomsAt certain time, only ions with one certain mass-to-charge ratio can pass through and be detected.mass spectrometer ConesInfluence7Matrix effects: signal suppression or enhancement caused by overloading of plasma, cooling effects, changes of ionization, blockage of cones, change of ion sampling, etc. Remedy: internal standard (Be, Ga, In, Tl).
Residual signal (rlative to the signal in 0.14 M HNO3) for several elements present in 0.5 M H2SO4 matrix as a function of the mass number of the nuclide.
(Vanhaecke F., Vanhoe H., Dams R., Vandecasteele C., Talanta, 1992, 39)
Influence8Spectral interferences: interferences between ions with similar atomic mass. Remedy:
(USGS)Use of HNO3Select isotopes (65Cu instead of 63Cu (ArNa+))Mathematical correctionModify sample preparation Influence9Cone blockage The small orifice (~ 1mm) on the cones can be blocked if too much total dissolved solids (TDS) in the solution. This can cause decreased sensitivity and detection capability Remedy: diluted feeding solution (TDS no more than 0.2%)
Partially blocked orifice
(Kym Jarvis. Presentation for Nuclear Spectrometry Users Forum, May 2005) Sample preparation 10
PreparationSample digestionThree acids digestionMicrowave digestionLithium metaborate fusion digestion Sample dilutionStandard preparationSample digestion11Three acids digestion0.1 g finely ground sample added in Teflon beaker with heating on the bottom and lid on the topThree acids:HNO3: oxidation, dissolving oxides and hydroxidesHClO4: oxidation, dissolving organicsHF: dissolving silicateare added, 5 ml each, by sequential order until the previous one boiled down. If the sample is not completely dissolved, more cycles of the process (without HClO4) are needed until the complete dissolution of sample. Caution: highly corrosive acids applied and protection neededSample digestion12Micro wave digestion: Acid digestion carried out in microwave transparent inert material vessels, where pressure is introducedHigh temperature (260-300 C)High digestion qualityReduced acid consumptionReduced digestion time (20-60 minutes)
Sample digestion13Lithium metaborate fusion digestion:Thoroughly mix 0.1 g finely ground sample with 1.0 g of lithium metaborate (LiBO2)Put the mixture in a graphite crucible and insert crucible into an oven at 1000 C for 15 minutesPour the melt mixture into 100 ml 5 vol% nitric acid solutionStir at least 15 minutes until all solid dissolved then filtrate the solution for dilution and measurement
Sample preparation14Sample dilution:The digested solution normally need to be diluteConcentration not larger than 1000 ppbConcentration not lower than detection limitNormally 2 vol% HNO3 is added
Standard preparation:Chose concentration of elements according the element concentration in diluted sampleAddition of internal standards (e.g. Be, Ga, In and Tl)3 or 5 calibration points, including one blankAtomic Absorption SpectroscopyAAS15
(http://web.vscht.cz/poustkaj)Principle: absorption of EM-radiation characteristic for electron transition in the outer shell of an atom of an element. AAS16Measurement of almost all metals, metalloids and some non-metals (B, Si, P)Sample:Solution in diluted acidsDiluted biological fluidsSuspensions of solid samples (slurries)Flame AAS (in CIT): measurement of higher concentration (10-100 ppm) high temperature flame (N2O)Measurement time 3-10 secondsContact: Michle Vanroelen ([email protected])
FT-IRFourier Transform InfraRed (with diamond ATR)17
(Thermo Nicolet, co.)
Principle: absorption of IR-radiation results in changes of vibrational energy of molecules.FT-IR18Identification of unknown pure (organic) compounds
Identification of functional groups
Sample: liquid, solid (in solution), solid.
Fast measurement, in a matter of seconds
Less suited for quantitative analysis, detection limits around 2 %
Contact: Christine Wouters ([email protected] )
PerkinElmer GC lab19
GC-MS GasChromatograph Mass Spectrometry Analysis of PCBs, phenols, trizaines, organophosphorus and organochlorine pesticides, PAHs, mono-aromatic hydrocarbons.
GC-FID/ECD GasChromatograph Flame Ionization Detector and Electron Capture Detector Analysis of PCBs, phenols, organochlorine pesticides, mono-aromatic hydrocarbons, aspecific solvents, mineral oil, volatile organic acids.
PerkinElmer GC lab20
GC-FID GasChromatograph Flame Ionization Detector Analysis of phenols, mono-aromatic hydrocarbons, aspecific solvents, mineral oil, volatile organic acids.
GC-FID/NPD GasChromatograph Flame Ionization Detector and Nitrogen Phosphorus Detector Analysis of phenols, triazines, organophosphorus pesticides, mono-aromatic hydrocarbons, aspecific solvents, mineral oil, volatile organic acids.Contact: Christine Wouters ([email protected] )
Mercury analyzer
21 Design for all types of sample: Environmental samples (water, soil, plants, etc)-Human samples (hair, blood, urine, etc)
Vapour generation technique (remove most chemical interferences)
Atomic fluorescence spectrometry (mercury analysis down to ppt level)
Contact: Tom Van Gerven([email protected] )(not operational yet by the moment, part of RARE3 project)Contact Angle Analyzer
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KRSS Dsa10-MK2Contact: Bart Van der Bruggen ([email protected] )
Contact23ICP-MSAAS
FT-IRPerkinElmer GC lab
Mercury Analyzer
Contact Angle Analyzer
Michle Vanroelen([email protected])
Christine Wouters ([email protected] )Tom Van Gerven([email protected] )
Bart Van der Bruggen ([email protected] )24Many thanks!