Fully Automated Total Metals and Elemental Speciation Single Platform Introduction System for ICP‐MS
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Elemental Scientific ICP | ICPMS | AA Fully Automated Total Metals and Elemental Speciation Single Platform Introduction System for ICP‐MS C. Derrick Quarles Jr., Ph.D. Sr. Scientist & LC Automation Product Manager Elemental Scientific, Inc. ‐ Atlanta (ESI HQ are located in Omaha, NE) Elemental Scientific, Inc. (ESI) Elemental Scientific, Inc. Omaha, NE, USA © 2019 Elemental Scientific History of Company © 2019 Elemental Scientific Elemental Scientific ICP | ICPMS | AA FAST ‐ “Automated Sample Introduction” What is FAST? © 2019 Elemental Scientific Faster Analysis = More Productive Traditional Autosampler = 5 min per sample ICP-MS Method = 50 s 4 min 10 s = sample flush, read delay, wash Traditional Autosampler = 288 samples in 24 h FAST Autosampler = 1 min 30 sec per sample ICP-MS Method = 50 s 40 s = sample flush, read delay, wash Reduction of 200 s per sample FAST Autosampler = 1200 samples in 24 h Assuming you run samples 24 h straight 1200 vs 288 = 417% More Productive with FAST © 2019 Elemental Scientific Elemental Scientific ICP | ICPMS | AA prepFAST ‐ “Automated Inline Autodilution System” © 2019 Elemental Scientific prepFAST – Inline Dilution © 2019 Elemental Scientific prepFAST – Inline Dilution © 2019 Elemental Scientific Conventional Calibration vs prepFAST Autocalibration © 2019 Elemental Scientific Sample Outside of Calibration Curve Load Sample ICP/ICPMS SOFTWARE Autodilute QC Dilution and Analyze PASS Correction QC Report Data FAIL Re-queue with Intelligent Dilution INTELLIGENT DILUTION © 2019 Elemental Scientific Elemental Scientific ICP | ICPMS | AA prepFAST IC ‐ “Automated Elemental Speciation and Total Metals” © 2019 Elemental Scientific Instrumentation HPLC + ICP-MS prepFAST M5 for Total Metal Analysis prepFAST IC for Speciation and Total Metal Analysis © 2019 Elemental Scientific prepFAST IC Features . Completely metal-free liquid and sample flow path from pump to nebulizer. Compatible with acids and organic solvents. Contamination free. Inline autodilution and autocalibration functions. Ability to operate in total metals or chromatography mode with a single instrument. No instrument modifications required to switch from total metals to speciation. Syringe-driven, post-column standard addition, dilution, or derivatization. © 2019 Elemental Scientific prepFAST IC – Total Metals and Speciation Speciation Mode Total Metals Mode 12000 ~ 25 uL Injection 60000 1.5 mL Dilution Loop 10000 50000 8000 40000 6000 30000 4000 20000 Intensity (a.u.) Intensity 2000 10000 Intensity @ m/z = 75 (cps) @ m/z Intensity 0 0 0 25 50 75 100 125 0 100 200 300 TIme (s) Time (s) © 2019 Elemental Scientific prepFAST IC – Total Metals and Speciation Autosampler Location Dilution Factor Sample Action 1 1 Blank - Total Metals Total Metals 2 50 Standard 1 Total Metals 2 25 Standard 2 Total Metals 2 10 Standard 3 Total Metals 2 5 Standard 4 Total Metals 2 1 Standard 5 Total Metals 101 10 Sample 1 Total Metals Total Metals 240 10 Sample 100 Total Metals 10 1 Dummy Sample Prime for Speciation Method 3 1 Blank - Speciation Speciation 4 100 Standard 1 Speciation 4 20 Standard 2 Speciation 4 10 Standard 3 Speciation 4 5 Standard 4 Speciation 4 2 Standard 5 Speciation 101 10 Sample 1 Speciation Speciation 240 10 Sample 100 Speciation 9 1 Dummy Sample Prime for Total Metals © 2019 Elemental Scientific prepFAST IC – Total Metals and Speciation Autosampler Location Dilution Factor Sample Action 1 1 Blank - Total Metals Total Metals 2 50 Standard 1 Total Metals 2 25 Standard 2 Total Metals 2 10 Standard 3 Total Metals 2 5 Standard 4 Total Metals 2 1 Standard 5 Total Metals 101 10 Sample 1 Total Metals Total Metals 240 10 Sample 100 Total Metals 10 1 Dummy Sample Prime for Speciation Method 3 1 Blank - Speciation Speciation 4 100 Standard 1 Speciation 4 20 Standard 2 Speciation 4 10 Standard 3 Speciation 4 5 Standard 4 Speciation 4 2 Standard 5 Speciation 301 10 Sample 1 Speciation Speciation 350 10 Sample 50 Speciation 9 1 Dummy Sample Prime for Total Metals © 2019 Elemental Scientific prepFAST IC‐HP prepFAST IC prepFAST IC-HP 45000 1 ppb 60000 5 ppb 1 ppb 40000 10 ppb 5 ppb 50000 10 ppb As(V) 25 ppb As(V) 35000 25 ppb 30000 40000 25000 30000 20000 As(III) As(III) 15000 20000 MMA DMA MMA DMA AsB = Arsenobetaine 10000 = 75 (cps) @ m/z Intensity Intensity @ m/z = 75 (cps) @ m/z Intensity AsB AsB 10000 DMA = Dimethylarsinic acid AsC AsC AsC = Arsenocholine 5000 MMA = Monomethylarsonic acid 0 0 0 50 100 150 200 250 300 0 50 100 150 200 250 300 Time (s) TIme (s) © 2019 Elemental Scientific © 2019 Elemental Scientific © 2019 Elemental Scientific Sample Uptake © 2019 Elemental Scientific Sample Uptake ‐ Speciation Mode © 2019 Elemental Scientific Arsenic Speciation 50000 1Standard ppb 1 As (V) 5Standard ppb 2 45000 10Standard ppb 3 25Standard ppb 4 40000 35000 30000 25000 As (III) 20000 MMA 15000 DMA Intensity @ m/z = 75 (cps) @ m/z Intensity 10000 AsB AsC 5000 0 0 20406080100120 TIme (s) AsB = Arsenobetaine AsB As III DMA AsC MMA As V DMA = Dimethylarsinic acid AsC = Arsenocholine LOD (ppt) 1.7 0.6 0.7 0.8 1.0 0.3 MMA = Monomethylarsonic acid © 2019 Elemental Scientific Inline Dilution Eliminates Species Interconversion Manual Dilution Inline Dilution 30X Manual DF 30X Inline DF 1 (Urine Spiked with 10 ppb As III): 29 (DI H2O) Urine Spiked with 10 ppb As III 2500 3000 As III As III 2000 2500 0h 0h 2000 1500 1500 1000 1000 Intensity @ m/z = 75 (cps) =75 m/z Intensity @ 500 Intensity @ m/z = 75 (cps) =75 m/z Intensity @ 500 0 0 0 50 100 150 200 250 300 0 50 100 150 200 250 300 Time (s) Time (s) C D Quarles Jr., P Sullivan, M P Field, S Smith, D R Wiederin, JAAS, 2018, 33, 745-751. © 2019 Elemental Scientific Inline Dilution Eliminates Species Interconversion Manual Dilution Inline Dilution 30X Manual DF 30X Inline DF 1 (Urine Spiked with 10 ppb As III): 29 (DI H2O) Urine Spiked with 10 ppb As III 2500 3000 As III As III 2000 2500 1h 1h 2000 1500 1500 1000 1000 Intensity @ m/z = 75 (cps) =75 m/z Intensity @ 500 Intensity @ m/z = 75 (cps) =75 m/z Intensity @ 500 0 0 0 50 100 150 200 250 300 0 50 100 150 200 250 300 Time (s) Time (s) C D Quarles Jr., P Sullivan, M P Field, S Smith, D R Wiederin, JAAS, 2018, 33, 745-751. © 2019 Elemental Scientific Inline Dilution Eliminates Species Interconversion Manual Dilution Inline Dilution 30X Manual DF 30X Inline DF 1 (Urine Spiked with 10 ppb As III): 29 (DI H2O) Urine Spiked with 10 ppb As III 2500 3000 As III As III 2000 2500 3h 3h 2000 1500 1500 1000 1000 Intensity @ m/z = 75 (cps) =75 m/z Intensity @ 500 Intensity @ m/z = 75 (cps) =75 m/z Intensity @ 500 0 0 0 50 100 150 200 250 300 0 50 100 150 200 250 300 Time (s) Time (s) C D Quarles Jr., P Sullivan, M P Field, S Smith, D R Wiederin, JAAS, 2018, 33, 745-751. © 2019 Elemental Scientific Inline Dilution Eliminates Species Interconversion Manual Dilution Inline Dilution 30X Manual DF 30X Inline DF 1 (Urine Spiked with 10 ppb As III): 29 (DI H2O) Urine Spiked with 10 ppb As III 2500 3000 As III As III 2000 2500 6h 6h 2000 1500 1500 1000 1000 Intensity @ m/z = 75 (cps) =75 m/z Intensity @ 500 Intensity @ m/z = 75 (cps) =75 m/z Intensity @ 500 0 0 0 50 100 150 200 250 300 0 50 100 150 200 250 300 Time (s) Time (s) C D Quarles Jr., P Sullivan, M P Field, S Smith, D R Wiederin, JAAS, 2018, 33, 745-751. © 2019 Elemental Scientific Inline Dilution Eliminates Species Interconversion Manual Dilution Inline Dilution 30X Manual DF 30X Inline DF 1 (Urine Spiked with 10 ppb As III): 29 (DI H2O) Urine Spiked with 10 ppb As III 2500 3000 As III As III 2000 2500 12h 12h 2000 1500 1500 1000 1000 Intensity @ m/z = 75 (cps) =75 m/z Intensity @ 500 Intensity @ m/z = 75 (cps) =75 m/z Intensity @ 500 0 0 0 50 100 150 200 250 300 0 50 100 150 200 250 300 Time (s) Time (s) C D Quarles Jr., P Sullivan, M P Field, S Smith, D R Wiederin, JAAS, 2018, 33, 745-751. © 2019 Elemental Scientific Inline Dilution Eliminates Species Interconversion Manual Dilution Inline Dilution 30X Manual DF 30X Inline DF 1 (Urine Spiked with 10 ppb As III): 29 (DI H2O) Urine Spiked with 10 ppb As III 2500 3000 As III As III 2000 2500 24h 24h 2000 1500 As V 1500 As V 1000 1000 Intensity @ m/z = 75 (cps) =75 m/z Intensity @ 500 Intensity @ m/z = 75 (cps) =75 m/z Intensity @ 500 0 0 0 50 100 150 200 250 300 0 50 100 150 200 250 300 Time (s) Time (s) C D Quarles Jr., P Sullivan, M P Field, S Smith, D R Wiederin, JAAS, 2018, 33, 745-751. © 2019 Elemental Scientific Manual Dilution vs Inline Dilution ‐ Summary 150 Manual Dilution 10 ppb As III Spiked Urine Samples Inline Autodilution Manual Dilution Time (h) As III % As V % As III + As V 125 0 100.0 0.0 100.0 100 1 95.7 0.0 95.7 3 92.8 0.2 93.0 75 6 91.3 1.6 92.9 50 12 78.5 12.0 90.6 % of As III Species 24 61.9 21.4 83.4 25 10 ppb As III Spiked Urine Samples Inline Autodilution Time (h) As III % As V % As III + As V 0 01361224 0 100.0 0.0 100.0 Time (h) 1 102.8 0.0 102.8 50 3 105.2 0.0 105.2 Manual Dilution Inline Autodilution 6 106.4 0.0 106.4 40 12 95.1 0.5 95.6 24 102.9 1.3 104.2 30 As III % = (x h As III / 0 h As III) * 100 As V % = (x h As V / 0 h As III) * 100 20 As III + As V = As III % + As V % As III to As V 10 % of As Species Converting from 0 01361224 Time (h) © 2019 Elemental Scientific Elemental Scientific ICP | ICPMS | AA Chromium Speciation and Total Metals Environment Application & Validation Study prepFAST IC + ICP‐MS © 2019 Elemental Scientific ESI & Eurofins Publication: Chromium Speciation C D Quarles Jr., M Szoltysik, P Sullivan, M Reijnen, JAAS, 2019.