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Elemental ScientificICP | ICPMS | AA
High Throughput Automation for EPAMethod 200.7 & 200.8
Stephen J. Mangum Elemental Scientific
NEMC Conference 2021
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Elemental Scientific
• SampleSense Enviro• Reduces EPA methods sample to sample time• Provides Quality Assurance for sample loading• Eliminates method timing• Eliminates loading variability due to sample viscosity
Improves Sample throughput without data compromise
New Automation Creating High Throughput
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SampleSense Enviro
• What is SampleSense Enviro?
• DXCi Intelligent Autosampler
• SampleSense FAST• Vacuum control valve
• Pergo Argon Humidifier
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DXCi: The Intelligent Autocorrecting Autosampler
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• Monitors autosampler probe position in 3 axes of motion
• Intelligently corrects the position
• Reports unmoved obstructions
• Eliminates analytical interruptions
• Available in 2DXCi, 4DXCi, 8DXCi, 14DXCi
• All SampleSense systems will include new DXCi
New DXCi Intelligent Position‐Correcting Autosampler
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• Optical sensors monitor for arrival of solution front at both entrance and exit.
• Solution arrival at both locations provides confirmation that sample loop is fully loaded
• Air bubbles during the sample loop loading are detected
SampleSense Valve – how does it work?
Exit Sample In
Sensors
SensorIndicators
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SampleSense Enviro: Optimized QC Workflow
• Intelligent Sample Loading Verification• SampleSense Enviro reports non‐sample events:
• Capped Sample Vials• Underfilled Sample Vials• Underfilled/Empty QC Standards
• Log of “Un‐Sensed” Samples is Generated
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Elemental Scientific
SampleSense Enviro: Low Sample Consumption
• Vacuum‐Control Valve:• Trapping valve minimizes sample consumption. • Automatically shutting off the vacuum to conserve valuable sample.
• SampleSense Enviro consumes < 2.5 mL of sample*.• The black line shows the original level of 6 mL sample • Post analysis, 3.5 mL of sample remains for a potential reanalysis.
* System using 1.5 mL loop size
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SampleSense Enviro Flow Diagram
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Step 2:
When both sensors are triggered, vacuum valve closes and then sample valve switches to inject.
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SampleSense Enviro Analytical Cycle
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Experimental: Instrument Setup & Method conditions
Method settings use standard analytical conditions(Analytes, replicates, sample flow, etc.)
Method uses 3 replicates Uses < 2.5 mL sample/injection Probe washout and loop rinse are part of FAST method
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Example ICP‐OES Time Savings (U.S. EPA Method 200.7)
Standard Valving System• 1:16 per sample
Sample Id Acquisition Time
Blank 8/22/2018 12:16:46 PMCal-1 8/22/2018 12:20:32 PMCal-2 8/22/2018 12:24:18 PMCal-3 8/22/2018 12:28:06 PMCal-4 8/22/2018 12:31:18 PMCal-5 8/22/2018 12:34:31 PM
Sample Id Acquisition Time
BLANK 8/22/2018 5:27:48 PMCal-1 8/22/2018 5:29:45 PMCal-2 8/22/2018 5:31:40 PMCal-3 8/22/2018 5:33:00 PMCal-4 8/22/2018 5:34:16 PMCal-5 8/22/2018 5:35:32 PM
Standard autosampler• 3:12 per sample
SampleSense Enviro System• 0:45 per sample
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A Few Examples of Calibrations
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Pergo ‐ Argon Humidifier
Benefits• Dissolves salt crystals at nebulizer tip
• Reduces long term drift• Improves stability• Improves detection limits
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Experimental: Calibration and Data
0.0%
20.0%
40.0%
60.0%
80.0%
100.0%
120.0%
140.0%
160.0%
180.0%
200.0%
1 9 11 13 15 17 19 21 23 25 27 29 31 33 35 37 39 41 43 45 47 49 51 53 55
% Recov
ery
Row Index Number
Y‐Axial
Sc‐Radial
Sc‐Axial
• Calibration for As 193
• IS plot over sample run
0.999997
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Internal Standard Recovery
60%
80%
100%
120%
0:00 0:28 0:57 1:26 1:55 2:24 2:52 3:21 3:50 4:19 4:48
IS Recov
ery
Time (hours)
Drift without pergo
Sc 45 (IS)(cps)
Ge 72 (IS)(cps)
In 115 (IS)(cps)
Ir 193 (IS)(cps)
Rh 103(cps)
Tb 159(cps)
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Internal Standard Recovery
60%
80%
100%
120%
0:00 0:28 0:57 1:26 1:55 2:24 2:52 3:21 3:50 4:19 4:48
IS Recov
ery
Time (hours)
Stable Signal with pergo
Sc 45 (IS)(cps)
Ge 72 (IS)(cps)
In 115 (IS)(cps)
Ir 193 (IS)(cps)
Rh 103(cps)
Tb 159(cps)
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Elemental Scientific
Questions??
SampleSense Enviro – provides fastest, most economical, most intelligent analysis
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