high throughput automation for epa method 200.7 & 200

© Elemental Scientific | www.icpms.com | [email protected]

Elemental Scientific

Elemental ScientificICP | ICPMS | AA

High Throughput Automation for EPAMethod 200.7 & 200.8

Stephen J. Mangum Elemental Scientific

NEMC Conference 2021



• 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



SampleSense Enviro

• What is SampleSense Enviro?

• DXCi Intelligent Autosampler

• SampleSense FAST• Vacuum control valve

• Pergo Argon Humidifier



DXCi: The Intelligent Autocorrecting Autosampler



• 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



• 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



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



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



SampleSense Enviro Flow Diagram



Step 1:



Step 2:

When both sensors are triggered, vacuum valve closes and then sample valve switches to inject.



Step 3:



SampleSense Enviro Analytical Cycle



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



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



A Few Examples of Calibrations



Pergo ‐ Argon Humidifier

Benefits• Dissolves salt crystals at nebulizer tip

• Reduces long term drift• Improves stability• Improves detection limits



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



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)



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)



Benefits Summary



Questions??

SampleSense Enviro – provides fastest, most economical, most intelligent analysis

high throughput automation for epa method 200.7 & 200

Documents