Ed Connor, GC Product Specialist econnor@peakscientific.com Supplying your GC using Peak gas generators - safe, reliable and convenient Ed Connor, GC Product Specialist econnor@peakscientific.com Author: Ed Connor Date / Rev: 10/2015

Webinar Helium – current situation and outlook Helium conservation Nitrogen carrier gas Hydrogen carrier gas Why use a generator? Precision generators Application examples using Hydrogen and Nitrogen

Helium – present and outlook Price has almost doubled 2013-2015 Qatar I & II now operational Qatar III to open in 2018 Further increase in cost Priority for liquid helium users? Need to look for alternatives where possible

Helium conservation

Helium conservation Conserve helium for applications where its use is essential – where methods allow no alternative Look at hydrogen and nitrogen method compatibility Eg. ASTM D2887 - SIMDIS Hydrogen Nitrogen

Alternative carrier gases Nitrogen Hydrogen Relatively ‘slow’ ‘Fast’ analysis Uopt 8-14 cm/sec Uopt 38-48 cm/sec Cheap Produced by gas generators Gas generators Perceived danger

Nitrogen carrier gas With sufficient resolution – can afford to lose some plates Will result in loss of efficiency at higher velocity OK if there is enough separation between peaks Using N2 at same linear velocity as He will result in HETP increase by a factor of 2 Loss of efficiency by a factor of 2 only means loss of resolution by a factor of 1.4

Hydrogen carrier gas Hydrogen is already used for a number of GC detectors Improved effiency Peaks are 2x higher (sensitivity) Therefore need 50% of injected amount Lower maintenance Sample throughput can be increased 2x relative to helium

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Why use a generator?

Why use a generator?

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Precision Hydrogen Trace Suitable for GC Carrier Gas, detector gas or reaction gas 99.9999% purity Internal leak detection with automatic safety shutdown features Proven PEM technology for safe hydrogen generation Automatic water loading pump as standard Maintenance limited to changing a de-ionizer cartridge Short and easy start-up and shut-down procedures via touch screen Combine multiple units for higher flow requirements 3 year standard cell warranty

Precision Hydrogen - Safety Precision hydrogen generators have a number of safety features to ensure safe and reliable operation: On power-up the generator conducts an internal leaks check External leak detection Forced air ventilation to prevent build-up of H2/O2 in the case of an internal leak Over/under pressure monitoring Overpressure cell shutdown Audible/visual alarms

Precision Hydrogen - LEL Hydrogen is a flammable gas with a lower explosion level (LEL) of 4.1% A room measuring 5m x 5m x 2.5m contains 50m3 (50000L) LEL would be 2050L A large 50L cylinder contains around 9000L hydrogen Precision Hydrogen generator will produce up to 500cc/min To reach LEL with generator would take almost 3 days in a hermetically sealed room

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Precision Nitrogen Standard and Trace Nitrogen generators available 99.999% Purity achieved using PSA Nitrogen trace has CAT chamber to remove CH4 Hydrocarbons (as methane) <0.05 ppm

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Precision range Hydrogen, nitrogen and zero air in one modular stack

Revalidation steps Review your documentation to make sure that your methods allow the use of hydrogen or nitrogen carrier gas Check health and safety documentation Perform routine maintenance (liners, septa etc) Install new gas lines (SS or Cu) Install new traps (MSD) Use method translation software to establish correct method parameters for hydrogen or nitrogen carrier gas

Applications – FAMEs analysis Analysis of FAMEs 39 Component standard Customer changing from helium to hydrogen carrier gas for GC-FID Method revalidated to match linear velocity of hydrogen to original helium method Results showed that retention times of compounds were unchanged Hydrogen improved peak shape and s/n relative to helium 0.00 5.00 10.00 15.00 20.00 25.00 30.00 35.00 40.00 45.00 50.00 5000 10000 15000 20000 25000 30000 35000 40000 45000 50000 0.00 5.00 10.00 15.00 20.00 25.00 30.00 35.00 40.00 45.00 50.00 5000 10000 15000 20000 25000 30000 35000 40000 45000 50000 Helium Hydrogen

Applications – DHA analysis ASTM method D6729 Detailed hydrocarbon analysis using a 100m column Analysis time cut from 125 mins to 73 mins by using hydrogen carrier gas Critical separations achieved Relative amounts of PONA constituents not significantly different when using helium or hydrogen Helium Hydrogen

Applications – BAC analysis BAC standard mixture run using Nitrogen and Helium carrier gas Nitrogen used for Headspace, Carrier and FID make-up High linear velocity - >80 cm/s No significant difference in results with Nitrogen compared with helium

Applications – BAC analysis BAC standard mixture run using Nitrogen and Helium carrier gas Nitrogen used for Headspace, Carrier and FID make-up High linear velocity - >80 cm/s No significant difference in results with Nitrogen compared with helium

Applications – BAC analysis BAC standard mixture run using Nitrogen and Helium carrier gas Nitrogen used for Headspace, Carrier and FID make-up High linear velocity - >80 cm/s No significant difference in results with Nitrogen compared with helium

All application notes can be found: http://www.peakscientific.com/articles/

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