Excellence in Analytical Chemistry

Elan
Elan 6000
6000 // 6100
6100 /9000
/9000
Daily
Daily Optimisation
Optimisation

Refer to Elan 6000 Inductively Coupled Plasma Mass Spectrometer

Hardware and Software Guides
 Optimisation Schedule

• Daily Maintenance and Startup

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• Introduction of Optimising Solution

• X-Y Alignment

• Lens Optimisation

• Nebuliser Optimisation

• Autolens Calibration

• Daily Performance Check

• Re-introduction of Carrier Solution

 Daily Maintenance and Startup

• Check Pressures / Levels

Excellence in Analytical Chemistry

– Argon tank and pressure (51 +/- 1 psi)
– Chiller pressure and temperature (55 psi / 18C)
– Vacuum pump oil level and colour
– Waste and solution container levels
– Base vacuum pressure (plasma off)
• Check Sample Introduction System
– Clean or change cones
– Inspect Injector, Support adapter, Torch, and Coil. Clean /
replace if necessary
– Inspect all Pump Tubing and replace if necessary
• Startup
– Start plasma
– Start FIAS via Run Current Step in Device Control window
– Allow at least 20 minutes for plasma to stabilise
 Introduction of Optimising
Solution

• Bypass Carrier Solution Intake

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– Disconnect carrier solution tubing from black/black/black tubing
– Connect capillary tubing to end of black/black/black tubing
• Aspiration of Optimising Solution
– Obtain bottle of fresh Optimising solution (< 1 month old)
containing 10 ppb of Mg, Cu, Cd, Pb, Sc, Rh, Ce, Tb, Ba, Ge,
Be, Co, In, U, Tl in 2% Nitric acid
– Aspirate the solution via the capillary tubing
– Ensure solution stream to spray chamber is without bubbles
 X-Y Alignment

• Open X-Y Workspace

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– Menu Window Submenu Close All
– Menu File Submenu Open Workspace
– Select FIAS-XY
• Realtime Display
– Select Signal Display in Realtime window
– Select Options
– Enter max counts in Max cps or counts
– Enter max time in End Time (sec)
• Analyse Solution
– Read 10 ppb solution via Analyse Sample in Sample window
 X-Y Alignment cont…

• Adjust X and Y Alignment Knobs

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– Open instrument cover
– Watching signal display (fig.1), turn X alignment knob (futherest
from front) slowly clockwise then anti-clockwise until max Rh
intensity position reached
– Repeat for the Y alignment knob (closest to front)
– Repeat the X and Y alignment again
– Close instrument cover
X-Y Alignment cont…

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Fig.1 Signal display
 Lens Optimisation

• Optimisation Window

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– Auto Optimise tab and select Lens Voltage
– Change Start Value and End Value if necessary
– Optimise then Menu File Submenu Save
• Interactive Window
– A smooth curve with a defined peak should be displayed (fig.3)
– Optimum lens voltage setting is highlighted on curve
– Reduce Start Value if peak appears to the left of window
– Increase Start Value if peak appears to the right of window
– Re-optimise as above if peak was outside window
Lens Optimisation cont…

Excellence in Analytical Chemistry

Fig.3 Intensity vs Lens Voltage
 Nebulizer Optimisation

• Open NebLens Workspace

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– Menu Window Submenu Close All
– Menu File Submenu Open Workspace
– Select NebLens
• Optimisation Window
– Auto Optimise tab and select Nebulizer Gas Flow
– Get Analyte and select Rh 102.905
– Change Start Value and End Value if necessary
– Optimise then Menu File Submenu Save
• Interactive Window
– A smooth curve with a defined peak should be displayed (fig.2)
– Optimum nebuliser setting is highlighted on curve
– Reduce Start Value if peak appears to the left of window
– Increase Start Value if peak appears to the right of window
– Re-optimise as above if peak was outside window
Nebulizer Optimisation cont…

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Fig.2 Intensity vs Nebuliser Gas Flow
 Autolens Calibration

• Open AutoLens Workspace

– Menu Window Submenu Close All

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– Menu File Submenu Open Workspace
– Select AutoLens
• Optimisation Window
– Auto Lens tab
– Change Start Value and End Value if necessary
– Clear Calibration then Get Analyte List
– Calibrate then Menu File Submenu Save
• Interactive Window
– Analytes then <- Add All
– Lens vs Mass graph should have positive slope and pass close
to or through 3 points (fig.4)
– Be, Co, and In curves should be smooth with a definite peak
 Autolens Calibration cont…

• Interactive Window cont…

Excellence in Analytical Chemistry

– Reduce Start Value if any peak appears to the left of its window
– Increase Start Value if any peak appears to the right of its
window
– Re-calibrate as before if any peak was outside its window
Autolens Calibration cont…

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Fig.4 Autolens display
 Daily Performance Check

• Open Daily Performance Workspace

– Menu Window Submenu Close All

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– Menu File Submenu Open Workspace
– Select Daily Performance
• Optimisation Window
– Manual Adjust tab
– Select Nebulizer Gas Flow and reduce setting
• Samples Window
– Analyse Sample
• Report View Window
– Check that CeO/Ce % is < 3.0% (fig.5). If not reduce nebulizer
gas flow and re-analyse as above
Daily Performance Check cont…

Excellence in Analytical Chemistry

Fig.5 Daily Performance display
Daily Performance Check cont…

• Report View Window cont…

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– Check that RSD% for 24Mg 103Rh 208Pb are < or equal to 2%. If
not go to Method window, change Sweeps/Reading to 60, and
re-analyse
– Record values for neb flow, lens voltage, 24Mg 103Rh 208Pb
sensitivity, CeO/Ce %, Ba++/Ba %, Background, 9Be 59Co 115In
DAC values
• Save Final Settings
– Select Optimisation window
– Menu File Submenu Save
 Re-introduction of Carrier
Solution

• Re-connect Carrier Solution Intake

Excellence in Analytical Chemistry

– Disconnect capillary tubing from black/black/black tubing
– Re-connect carrier solution tubing to end of black/black/black
tubing