Enhanced Detection Capabilities in Speciation Analysis Using a Highly Sensitive ICP-MS. Peio RISS ICP-MS Application Specialist.

Transcription

1 Enhanced Detection Capabilities in Speciation Analysis Using a Highly Sensitive ICP-MS Peio RISS ICP-MS Application Specialist aurora Elite

2 Bruker ICP-MS aurora series

3 The aurora series design All-digital Detection System Minimizes excited neutrals and other interferences prior to entering the quadrupole mass analyzer Lowest possible backgrounds CRI Interface Industry leading sensitivity Better detection limits 6 separate Patented Technologies Interlaced Coils Curved fringe rods 90 degree Ion Mirror Optics

4 The Ion Mirror Design Ion Mirror focuses all analyte ions into the mass analyzer, irrespective of the energy spread Unwanted particles neutrals, droplets, dust particles removed through Ion Mirror field by turbo pump 90 º Reflecting 3D Ion Mirror

5 NORMAL vs. HIGH sensitivity mode defocusing / focusing the ion beam o o o NORMAL Focus point lifted up Ion beam diffused - 3 mm focus achieved Sensitivity attenuated - 10x o o o HIGH Focus point within quad acceptance aperture 1 mm focus achieved Sensitivity - maximum 3mm focus 1mm focus

6 Control of the Ion Beam position Computer modeling X-Y position control Simulated initial Ion MS beam 5mm in diameter containing: 9 Be ~ 0.5eV 115 In ~ 2eV 232 Th ~ 5eV Freedom to move the ion beam focus in all 3 dimensions. Full 3D control!

7 Summary aurora Elite Significantly Improved Performance The aurora Elite ICP-MS now offers over 1,500,000 cps/ppb sensitivity at 115 In Precise and accurate quantification at single digit ppt concentration levels Shorter integration times Unmatched Gigahertz sensitivity for hyphenated techniques such as LA- ICP-MS or LC-ICP-MS

8 Bruker Advance Analytical LC for ICP-MS Separation Module Minimized System Volumes Improves Throughput Binary, high pressure mixing, solvent delivery system Unique 60 µl mixer/pressure transducer/purge valve Flow rates from µl/min UHPLC version to 15,000 psi (HPLC version to 8,000 psi) Optional UHPLC loading pump for On-Line Extraction (OLE) Internal multi-channel vacuum degasser Thermostatically-controlled column oven (30 90 C) Instrument control integrated with Bruker Compass software

9 Bruker Advance Analytical LC for ICP-MS Autosampler Based on Industry Standard CTC Platform Variable injection volume from µl (optional µl) Six sample tray capacity (54-vial trays and/or 96/384-well plates) Cool Stack sample temperature controlled from 4 40 C UHPLC injection valve rated to 15,000 psi Injection volume RSD better than 0.25% Dynamic liquid wash reduces carryover < 0.005% Optional On-Line sample Extraction (OLE) increases flexibility

10 Addition of Nitrogen to the Plasma : Nitrox 500 Numerous studies reported in the past on: increasing analyte ionization reducing matrix effects By adding Other gases to the Ar plasma Adding reagents to solutions With the aim of improving detection limits By increasing sensitivity Reducing interferences Especially for As and Se

11 Benefits of Nitrogen Addition Improves As and Se sensitivity 3-4 fold ppt As, Se Lower argon and matrix based polyatomic interferences observed Improves plasma robustness cps As75 Se78 Lower oxides (CeO/Ce ~ 0.5% ) Minimal gas flow required N 2 (ml/min) ~40-60mL/min N 2 added to auxiliary gas line Simple setup and optimize

12 Brooks Rand Labs Interlaboratory study : As in Food and Juice Matrices White Rice Brown Rice Kelp powder Apple juice Parameters Total Arsenic Inorganic As AsIII AsV MMA DMA MS Sample preparation White Rice, Brown Rice, Kelp powder : Microwave digestion Apple juice : 5-fold dilution

13 Automatic optimization MS

14 Advance HPLC conditions Parameter Column Value PRP-X100 Injection volume 50 µl Flow rate 1 ml/min Column temperature 40 C Mobile Phase A Mobile Phase B 12.5 mm Ammonium Carbonate, 1% Methanol 60 mm Ammonium Carbonate, 1% Methanol MS

15 aurora Elite setup Parameter Value Introduction system Standard Ion optics mode High sensitivity Plasma flow 15 L/min Auxiliary flow 1.5 L/min Nitrox 500 N2 flow 60 ml/min Acquisition mode Time-Resolved Dwell time 500 ms MS

16 aurora Elite Advance performance MS Chromatogram of a solution containing 1 µg/l of five As species

17 Brooks Rand Labs Interlaboratory study : As in food and Juice AsB AsIII DMA MMA MS AsV Calibrations ranging from 0.1 to 5 µg/l R2> LODs ranging from 2 to 5 ng/l

18 Brooks Rand Labs Interlaboratory study : As in food and Juice Sample Species Mean value Measured value Z-Score Total As AsIII White Rice Brown Rice AsV Insufficient data DMA Insufficient data <1 Insufficient data MMA Insufficient data <1 Insufficient data Total As AsIII MS AsV Insufficient data DMA Insufficient data <1 Insufficient data MMA Insufficient data <1 Insufficient data

19 Brooks Rand Labs Interlaboratory study : As in food and Juice Sample Species Mean value Measured value Z-Score Total As AsIII Insufficient data Kelp powder Apple Juice AsV DMA Insufficient data <1 Insufficient data MMA Insufficient data <1 Insufficient data Total As AsIII MS AsV DMA Insufficient data <0.02 Insufficient data MMA Insufficient data <0.02 Insufficient data

20 THANK YOU FOR YOUR ATTENTION Poster WP36 Wednesday 3pm Andrew Toms, Peio Riss, Meike Hamester Workshop WS209 Wednesday 5.10pm Meike Hamester Improving Analysis of Large Isotope Ratios Using High Sensitivity ICP-MS