High-Speed Gas and Headspace Analysis for the Process-Line and Laboratory: SIFT- MS IFPAC 2017
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1 High-Speed Gas and Headspace Analysis for the Process-Line and Laboratory: SIFT- MS IFPAC 2017 Y.J. Mange D.B. Milligan V.S. Langford B.J. Prince M. Perkins C. Anderson T. Wilks
2 Who is using Syft Technologies Instruments?
3 Outline SIFT-MS: instant and comprehensive gas analysis Automation of SIFT-MS Case study: simple formaldehyde analysis
4 SIFT-MS: Instant and Comprehensive Gas Analysis
5 Finding the missing piece of the analytical puzzle Polar SIFT-MS Analytes of all polarities and MWs Da LC-MS Analytes of low to high polarity and MWs above 300 Da Polarity Matrix GC-MS Analytes of low to medium polarity Effects? and MWs 30-1,000 Da Nonpolar Low Molecular Weight High
6 SIFT-MS technology: Key benefits Rapid, no chromatography, no pre-concentration Analyze chemically diverse species in real-time Sensitive to pptv levels Designed for both technical and non-technical personnel Remote operation, support and troubleshooting
7 Key Benefit 1: SIFT-MS can measure most VOCs and inorganic gases hydrocarbons alkanes, alkenes, aromatics, monoterpenes oxygenates alcohols, aldehydes, ketones, esters, ethers, carboxylic acids, formaldehyde nitrogen compounds amines, amides, nitriles, nitrated organics sulfur compounds mercaptans, thioethers, carbonyl sulfide halogenated compounds inorganics aliphatic and aromatic fluorides, chlorides, bromides and iodides ammonia, hydrogen cyanide, hydrogen sulfide, nitrogen dioxide, phosphine, hydrogen chloride, hydrogen fluoride, carbon dioxide, sulfur dioxide, ozone
8 Concentration / ppbv Key Benefit 2: Extreme sensitivity and wide dynamic range benzene: 30 ppmv benzene: 15 ppbv >1,000 fold increase of benzene has no affect on 1,3-butadiene measurement pptv sensitivity 1,3-butadiene: 30 pptv Time / seconds
9 Key Benefit 3: Concentrations can be monitored in real time
10 SIFT-MS: How this soft chemical ionization technique works Multiple reagent ions Pure reagent ion delivery Ultra-soft sample ionization Mass spectrometer
11 SIFT-MS separates compounds through gas-phase ion-molecule chemistry Mechanism H 3 O + NO + O + 2 OH - O - O - 2 NO - 2 NO - 3 Proton transfer (PT) Electron transfer (ET) Dissociative ET Hydride abstraction Association Proton abstraction Electron attachment Associative detachment Displacement/Elimination
12 Separation through ion chemistry and mass spectrometry propanal vs acetone (M R = 58) O O + NO + HNO + m/z = 57 O.NO + + NO + m/z = 88 O + phosphine vs hydrogen sulfide (M R = 34) H 2 S + O - 2 O 2 + HS - m/z = 33 PH 3 + O - 2 X no reaction acetaldehyde vs hydrocarbons (M R = 44) C 2 H 4 O + O - O + C 2 H 4 O - m/z = 44 C 3 H 8 + O - C 3 H 7 + OH - m/z = 17
13 The Principles of SIFT-MS Automation
14 Why integrate autosamplers with SIFT-MS? Simplest way to leverage high sample throughput from the rapid analysis provided by SIFT-MS Even better repeatability and reproducibility Further reduce labor costs
15 The very different sample introduction needs of GC-MS and SIFT-MS Analytical Technique: Gas Chromatography SIFT-MS Compound separation principle: Selectivity improvement achieved by: Sensitivity (S/N) improvement via: Monitoring of dynamic processes? Summary: Chromatographic (resolved in time) Rapid sample injection (narrow peak width) Concentrating more analyte prior to injection Not possible Rapid sample injection, but Measurement Time >> Sample Introduction Time Mass spectrometric (very soft chemical ionization) Use of additional reagent/product ion pairs Increasing the dwell time for product ions Via continuous sample introduction Slow sample injection because Measurement Time = Sample Introduction Time
16 Sample injection and analysis requirements in graphical form
17 Syringe injection headspace autosamplers work best with SIFT-MS In syringe injection autosamplers, the headspace is extracted using a syringe. The syringe is then injected directly into the GC inlet. In GC applications, the injection speed is typically very fast to give the narrow peak shape required for good chromatographic resolution. For SIFT-MS, we usually require: larger headspace samples than GC a much slower injection speed to maximize selectivity and sensitivity. The Gerstel MPS autosamplers provide this capability.
18 Case Study: Simple Formaldehyde Analysis
19 Formaldehyde analysis by GC-FID or GC-PID minutes minutes
20 Formaldehyde analysis by GC-MS after derivatization Low 8.4 minutes
21 Formaldehyde analysis using HPLC-UV following DNPH derivatization
22 Direct formaldehyde analysis using SIFT-MS 200 ppbv standard in Tedlar bags by SIFT-MS Rep. [HCHO] / ppbv Mean 203 %RSD 2.6
23 Linear detection of formaldehyde using SIFT-MS ppm range ppb range Slope = R 2 = Slope = 1.02 R 2 = 0.998
24 Formaldehyde in candle flame combustion products. Sample vapor products into prefilled Tedlar bag. Measured formaldehyde concentration = 235 ppbv This analysis took less than a minute including sampling the candle flame!
25 Automating Tedlar bag analysis using an autosampler
26 C 1 C 6 saturated aldehydes automated SIFT-MS analysis Bag 1 Bag 2
27 Typical derivatization HPLC method
28 Run-time for a traditional HPLC analysis HPLC Method 12.5 minute runtime Derivatization steps 20 Samples 4½ hours
29 Run-time for a SIFT-MS analysis SIFT-MS Method 30 second runtime No derivatization steps 20 Samples Less than 10 minutes 25x faster!
30 Summary Fast analysis time and high sample throughput Measurement of chemically diverse species in a single analysis Designed for operation by technical and non-technical personnel Low operating costs, simple automation, and remote operation
31
32 Thank you for attending! Questions? syft.com
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