Sensitivity: Large Sample Volume Splitless

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Sensitivity Large Sample Volume Splitless
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Speed Sensitivity in a NEW way!

• Think about extremes!

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A breakthrough technique for ULTRA sales

• Large volume techniques OC and PTV
• Overcoming SSL limitations for LV CSR
• When, why, and what of LVSL
• Practical aspects of LVSL injection
• Understanding how LVSL
• Some fundamentals of operation
• Competition
• Conclusions

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Large Sample Volume Injection

• Increased sensitivity
• Simplified sample preparation procedures
• cost reduction
• Better use of the sample material
• Lower amount of both solvent and sample used

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Large Sample Volume Injection

• Large Volume On-Column Injection
• suitable for volatile solute
• few operating parameters to be set
• sensitive to contaminants

• PTV Solvent Split Injection
• robust to contaminants
• difficult for volatile solutes
• several operating parameters to be set

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And with the SSL?

• Sample volume is limited to a few microliters
• The vaporizing chamber must be sufficiently large
  to house the whole sample vapour.
• The vaporizing chamber cannot be enlarged beyond
  a given size.

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SSL Overcoming of Sample Volume Limitation

• Slow injection?
• Introducing liquid at a rate that vapours can be
  immediately transferred to the column.
• Evaporation inside the needle
• DISCRIMINATION OF HIGH BOILING SOLUTES
• Concurrent Solvent Recondensation (CSR)
• Solvent recondenses into a column at the same
  rate as produced by sample evaporation.

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When and why LVSL injection?

• 1uL injection
• Initial Oven T. 60C

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When and why LVSL injection?

• WHEN USE LVSL
• Whenever you use the SSL injector the Worlds
  most used injector
• When you need more sensitivity than standard
  just inject more in the SSL injector!!
• WHY USE LVSL
• Simple to operate
• Performs on standard SSL injector
• NO impact on method validation!!!

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LVSL what do you need ?
New Proprietory DPFC with septum purge closure
capability. Forward pressure regulation
with sensor on the purge line and low dead volume
connections/tubes between valves and injector.
Will be the new standard for 250 1000 Kpa DPFC.
Software assist A simple dedicated parameter
selection program (separate from Chromcard)
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LVSL how do you install it?
CSR Large Volume Splitless GC Setup and Injection
Press-fit
Analytical column
Pre-column
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LVSL What else do you have to change?
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30uL injection for 30 times more sensitivity!

• No difference in method setup!!
• No method revalidation due to h/w differences!!

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CSR Large Volume Splitless InjectionSteps of
the Process

• Injection with liquid band formation
• Auto pressure surge
• Concurrent solvent recondensation into the
  precolumn
• Sample transfer
• Solvent evaporation in the precolumn

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Concurrent Solvent Recondensation (LVSL)
Bottom of the liner

• Restricted Evaporation Rate
• Injection with Liquid Band Formation
• Evaporation from a single droplet
• Increased Transfer Rate
• Solvent recondensation into a precolumn generates
  a strong suction effect

Solvent vapour
Liquid sample
Glass wool
High flow
Recondensed solvent
Precolumn
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Concurrent Solvent Recondensation
Transfer occurs concurrently with solvent
evaporation

• The vapour volume no longer limits the injection
  volume

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Step 3 visual difference with without CSR

• 35 uL Hexane injection
• BT 69C

• 65C starting temp
• Solvent recondensation
• Strong suction effect -fast pressure
  equilibration

• 100C starting temp
• No solvent recondensation,
• No suction effect - long time for pressure
  equilibration

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Concurrent Solvent Recondensation

• Injection of 30 ul of a hexane solution of
  n-alkanes
• Vapour volume 7.2 ml (300C and 50 kPa)
• Liner volume 1.6 ml

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Linearity from 5 to 50 ul
Precolumn 5 m x 0.32 mm id deactivated (Mega)
Column RTX1 15 m x 0.32 mm id, 0.5 um
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Injection Conditions
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Recoveries

• Better than those obtained with conventional SL!

Peak area normalized on C20 ratios calculated on
1 ul OC injection
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Analysis of PAHs with GC-MS
25 ul PAHs mix, 20 ppb in hexane Precolumn 5 m x
0.32 mm id Column RTX5 30 m x 0.25 mm id
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Analysis of PAHs with GC-MS
25 ul, 6 consecutive injections
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Analysis of OPPs with GC-FPD
40 ul OPPs mix, 12 ppb each in hexane Precolumn
5 m x 0.32 mm id Column 15 m x 0.32 mm id, RTX1
0.50 um
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Analysis of OPPs with GC-FPD
40 ul, 6 consecutive injections
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Competition NO COMPETITORS!!!

• Thermo is in dominant position competition is
  trying to defuse the bomb. We are in the position
  to put pressure

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Competition NO COMPETITORS!!!

• Lets crush them!!!

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Some Takeaways to keep in mind

• SSL INJECTORS ARE NO LONGER ALL THE SAME!!
• Ours is different in its substance
• TO USE WHENEVER THERE IS SSL INJECTOR
• Basic option and add-on kit (as seen in video!!)
• EASY TO PERFORM AND EXCELLENT RESULTS
• No specific expertise, total recovery and No
  discrimination
• NO REQUIREMENT FOR METHOD REVALIDATION
• NO COMPETITION
• Only Trace GC Ultra has Large Volume SL
• Only Trace GC Ultra has suitable pneumatics
• PROPRIETARY!!
• WE ARE THE FIRST LETS CAPITALISE!!!

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Some Takeaways to keep in mind

• SSL INJECTORS ARE NO LONGER ALL THE SAME!!
• Ours is different in its substance
• TO USE WHENEVER THERE IS SSL INJECTOR
• Basic option and add-on kit (as seen in video!!)
• EASY TO PERFORM AND EXCELLENT RESULTS
• No specific expertise, total recovery and No
  discrimination
• NO REQUIREMENT FOR METHOD REVALIDATION
• NO COMPETITION
• Only Trace GC Ultra has Large Volume SL
• Only Trace GC Ultra has suitable pneumatics
• PROPRIETARY!!
• WE ARE THE FIRST LETS CAPITALISE!!!