Introduction 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… 3
ICP-MS Advantages: Quantitative and semi-quantitative analysis Detection limits at or below ppt level for much of the periodic table 8 orders of magnitude analytical range High productivity Isotopic analysis 4 Inductively Coupled Plasma -Mass Spectrometry Producer: Thermo Scientific Type: X series Contact: Michèle Vanroelen
PerkinElmer, Inc 5 Remark: Method Detection Limit (MDL) is generally 2-10 times more than Instrumental Detection Limit (IDL) (PerkinElmer)
Principles 6 Argon Plasma Aerosol Solid Gas Atoms Ions RF Load Coils ICP Torch Schematic representation of a quadrupole ICP- MS (PerkinElmer) Ionization of atoms At certain time, only ions with one certain mass-to-charge ratio can pass through and be detected. mass spectrometer Cones
Influence 7 Matrix 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 HNO 3 ) for several elements present in 0.5 M H 2 SO 4 matrix as a function of the mass number of the nuclide. (Vanhaecke F., Vanhoe H., Dams R., Vandecasteele C., Talanta, 1992, 39)
Influence 8 Spectral interferences: interferences between ions with similar atomic mass. Remedy: (USGS) Use of HNO 3 Select isotopes ( 65 Cu instead of 63 Cu (ArNa + )) Mathematical correction Modify sample preparation
Influence 9 Cone 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 digestion 11 Three acids digestion 0.1 g finely ground sample added in Teflon beaker with heating on the bottom and lid on the top Three acids: -HNO 3 : oxidation, dissolving oxides and hydroxides -HClO 4 : oxidation, dissolving organics -HF: dissolving silicate are 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 HClO 4 ) are needed until the complete dissolution of sample. Caution: highly corrosive acids applied and protection needed
Sample digestion 12 Micro wave digestion: Acid digestion carried out in microwave transparent inert material vessels, where pressure is introduced High temperature ( °C) High digestion quality Reduced acid consumption Reduced digestion time (20-60 minutes)
Sample digestion 13 Lithium metaborate fusion digestion: Thoroughly mix 0.1 g finely ground sample with 1.0 g of lithium metaborate (LiBO 2 ) Put the mixture in a graphite crucible and insert crucible into an oven at 1000 °C for 15 minutes Pour the melt mixture into 100 ml 5 vol% nitric acid solution Stir at least 15 minutes until all solid dissolved then filtrate the solution for dilution and measurement
Sample preparation 14 Sample dilution: The digested solution normally need to be dilute Concentration not larger than 1000 ppb Concentration not lower than detection limit Normally 2 vol% HNO 3 is added Standard preparation: Chose concentration of elements according the element concentration in diluted sample Addition of internal standards (e.g. Be, Ga, In and Tl) 3 or 5 calibration points, including one blank
Atomic Absorption Spectroscopy AAS 15 (http://web.vscht.cz/poustkaj) Principle: absorption of EM-radiation characteristic for electron transition in the outer shell of an atom of an element.
AAS 16 Measurement of almost all metals, metalloids and some non-metals (B, Si, P) Sample: - Solution in diluted acids - Diluted biological fluids - Suspensions of solid samples (slurries) Flame AAS (in CIT): measurement of higher concentration ( ppm) – high temperature flame (N2O) Measurement time 3-10 seconds Contact: Michèle Vanroelen
FT-IR Fourier Transform InfraRed (with diamond ATR) 17 (Thermo Nicolet, co.) Principle: absorption of IR-radiation results in changes of vibrational energy of molecules.
FT-IR 18 Identification 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
PerkinElmer GC lab 19 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 lab 20 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
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 ) (not operational yet by the moment, part of RARE 3 project)
Contact Angle Analyzer 22 KRÜSS Dsa10-MK2 Contact: Bart Van der Bruggen )
Contact 23 ICP-MS AAS FT-IR PerkinElmer GC lab Mercury Analyzer Contact Angle Analyzer Michèle Vanroelen Christine Wouters Tom Van Gerven ) Bart Van der Bruggen )