The Bruker ICP-MS – a Versatile Tool for Sensitive and Interference Free Analysis of Different Matrices 1 08.04.2015 Applications for ICP-MS Environmental Waters Analysis • Drinking water • Effluents from industrial sites Sea Water Analysis • Most elements at ultra-trace levels Soil, Sediment and Land Site Contamination • Trace and toxic elements • Samples digested/leached in acids Agriculture and Food Food safety • Toxic elements Pb, Cd, Hg, Cr, As Plants, Herbs Fertilizer, Animal Feed Food, Fruits and Beverages • Toxic, essential and macrominerals • Meats, Crops, Milk, Tea, Wine, Juice 2 08.04.2015 Applications for ICP-MS Clinical research Bloods, Serums, Urine, Tissues • Complex matrix, viscous • High levels of C, S, P, Na, Mg, Fe, Cl Trace, Toxic and Nutritional Geochemical Applications Soils • As, Pb, Tl, Th, Cd, Cr • Digestion required • Se, Cu, Mn, Au, Pt • High TDS & matrix • I, Hg Rocks, Ceramics, Fly ash, Coal • Possibly crushed & fused • Al, Ca, Fe, K, Mg, Na, S, Cr, Cu, Ni, Pb, Zn Minerals and precious metals prospecting • Gold and the PGEs (Pt, Pd, Rh, Ru, Ir and Os) • Rare earth elements at trace levels 3 08.04.2015 Applications for ICP-MS Other Applications Industrial • Cement and building products Nuclear • Cooling water (10B/11B) • Isotope ratios Forensic • Gun powder residues Gold Characterization • Purity • Element fingerprinting to infer the origin of the material 4 08.04.2015 Diagram of ICP-MS Operations Sample Vacuum Detector Mass Analyser Data Process 5 08.04.2015 Ion Source ICP-MS Sample Preparation – Introduction Liquid samples • Viscous samples (dilute), run • Suspensions • dilute, run Powders and Solids filtrate/digest, run • digest (microwave), run P.G. A.G. Sample Flow N.G. P.G. – Plasma Gas S.G. A.G. – Auxiliary Gas N.G. – Nebulizer Gas S.G. – Sheath Gas To Waste 6 08.04.2015 High Performance Ion Optics 90 degree ion mirror • Increased efficiency and sensitivity • Reduced contamination • Improved long term signal stability • Simplified operation • Maintenance-free Curved entrance rods • Double off axis quadrupole • Removes excited neutrals before they reach the quadrupole • Lowest possible backgrounds • Better detection limits 7 Ion Optics – working principle Ions 7 Neutrals 6 Photons 4 1. Extract lens-1 2 5 2. Extract lens-2 3. Extract lens-3 4. Corner Lens 5. Mirror lens (L, R, B) 6. Entrance Lens 7. Entrance Plate 1 3 8 Bruker ICP-MS - Low Noise Quadrupol 1 1 Entrance lense 2 S-shaped pre-Quadrupol 3 3 MHz Quadrupol 2 3 Schematic of the Detector Operation Gain Control Quadrupole + ee- e- e- Signal Output Amplification Ion to eConversion Control Section The detector coverts ions into electrical pulses. Adjustment of voltage applied to control dynode provides attenuation of final output signal. 10 9 Orders Linear Dynamic Range 1 GHz 1000000000 Ca-Conc. 100000000 10000000 1 MHz 1000000 100000 10000 K-ConC. U - 1 ppb 1000 100 Cd - Limit TVO 5 ppb 10 1 Normal-sensitivityMode 10 ppt 100 ppt 1 ppb 10 ppb 100 ppb 1 ppm 10 ppm 100 ppm 0.1 % 1 % Interference Management The CRI Technology 12 Spectral Interferences in ICP-MS CRI reduce/remove common plasma based interferences Element Isotope Calcium 40Ca 40Ar+ Vanadium 51V 16O35Cl+ Chromium 52Cr 40Ar12C+ Iron 56Fe 40Ar16O+ Arsenic 75As 40Ar35Cl+ Selenium 78Se 40Ar38Ar+ 80Se 40Ar40Ar+ 13 Interfering ion CRI – Collision Reaction Interface • Operates on the plasma, NOT the ion beam • Uses similar chemistry to collision cells, but under very different conditions of temperature and pressure 14 CRI Simple and Effective Simple collision and reaction gases (He and H2) are injected into the plasma as it passes through the cones… Interferences are attenuated, allowing lower detection limits and better accuracy for ‘difficult’ elements. e.g. As, Se, V, Cr, Ca, Fe, etc. 15 New and Improved CRI II Universal Mode • CRI in ‘All He mode’ for all elements • Faster and simpler methodology Caters to future USEPA 200.8 requirements Nitrox 500 for online addition of N2 improves As & Se detection limits Multi-mode • Using optimal CRI conditions for more complex matrices (H2, He) • Clinical, semi-conductor, geochemical, etc… 16 Fe-analysis in Ca-matrix with CRI - H2 CaO (and ArO) interference on Fe Bruker Quantum, ICP-MS Software • • Integrated LC-ICP-MS Integratede LA-ICP-MS Aerosol dilution Minimizes sample preparation by extending matrix tolerance of ICP-MS • For samples containing 0.2 to 4% Total Dissolved Solids Eg. seawater contains ~3.5% TDS • Inline dilution via detuning of nebulizer efficiency & sheath gas dilution effect • Achieve 10-fold dilution without additional sample prep • Suitable for seawater, metals and mining, high TDS effluents 19 Auto-optimization of Aerosol Dilution Two dilution settings • Low dilution 5-fold dilution Samples with ~1-2% TDS Metals and mining, effluents • High dilution 10-fold dilution Samples with ~2-4% TDS Seawater 5-fold reduction in oxide interferences Rare Earths 20 08.04.2015 Typical Analysis Settings More efficient nebulization 0.8-1.1 L/min 0.1-0.3 L/min Low gas dilution 21 Aerosol Dilution Settings Less efficient nebulization 0.1-0.3 L/min 0.8-1.1 L/min High gas dilution Followed by automatic optimization of ion optic settings 22 08.04.2015 Seawater Analysis using Aerosol Dilution % Recovery of 10ug/L multi-element spiked into undiluted seawater 100% 0% % Recovery 23 56Fe 75As 78Se 52Cr 59Co 68Zn 114Cd Pb 105% 109% 99% 109% 92% 95% 110% 101% 08.04.2015 New! Nitrox 500 Gas Accessory Add N2 or O2 online to auxiliary gas 0-500 mL/min, computer controlled N2 for improved sensitivity and reduced interferences on As & Se • 3-4 times sensitivity improvement • lower DL’s for enviro applications Effects of Nitrogen Addition 2500 2000 1500 1000 O2 for organic solvents • petrochemical applications 24 500 0 N2 OFF N2 ON As75 Se78 Summary Unmatched Sensitivity All-digital Detection System • Only detector to offer 109 working range in pulsecounting (digital) mode. • High efficiency ion mirror • Excellent detection limits • Attractive to laser ablation and niche application markets Simplified Interference Management • No cross-calibration of digital-analog modes required Low Maintenance Design • Innovative Collision-Reaction Interface (CRI) • Hollow ion mirror design requires no cleaning • Removes interferences at plasma interface, not the ion beam • No need for additional cleaning / replace of interference management technology • Simplified setup and maintenance 25 08.04.2015 www.bruker.com 26 08.04.2015 For research use only. Not for use in diagnostic procedures.