advances in micro gas chromatography for fixed … hydrocarbon (c1 – c11) analysis column: rxi-1ms...

ADVANCES IN MICRO GAS CHROMATOGRAPHY FOR FIXED GASES AND LIGHT HYDROCARBON ANALYSIS ON A MICRO GC FUSION

Introduction

• Presented by Debbie Alcorn – Tuesday January 27, 2015

• History of the Micro GC

• 3000 Micro GC

• The Next Generation – Micro GC Fusion

• Micro GC Fusion Features

• Advances in Applications

• Future Developments

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INFICON Global Presence

900 employees; offices in 17 countries

3 INFICON Advances in Micro Gas Chromatography

Micro GC History

• The 3000 Micro Gas Chromatograph (GC) has over ten years of proven

excellent analytical performance

• Micro GC Fusion® expands the capability of the 3000 Micro GC

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2001

3000 Micro GC

Introduced

2013

Micro GC Fusion

Introduced

2010

INFICON Acquired

3000 Micro GC

3000 Micro GC

• Microelectromechanical systems (MEMS) based GC

• Isothermally heated capillary columns

• Micro Thermal Conductivity Detector (µTCD)

• Modular

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3000 Micro GC Applications

The Next Generation – Micro GC Fusion

• Micro GC Fusion builds on proven 3000

Micro GC technology • Utilizes the same MEMS injectors and TCD

• Traditional Micro GC technology is limited

due to: • Isothermal column temperature, leading to potential

carryover issues

• Ambient temperature effects

• Software and operating system compatibility

• Micro GC Fusion addresses these issues

using new technology

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Micro GC Fusion Features

• Temperature programmable columns

• Plug and play modules

• Integrated touch panel display

• Web-based user interface

• Wi-Fi capability

• Integrated sample conditioner

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Temperature Programming

• Fast temperature ramping based on resistive column heating technology

• Ability to ramp up to 300 ºC/min (5 ºC/sec)

• Column length dependent

• Ramping profile is independently optimized for each module

• Compared to one oven for multiple columns in a bench top GC

• Cool down time is optimized to achieve short cycle times

• 1-2 minutes, ramp and column length dependent

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Temperature Programming

• Benefits • Faster analysis of later eluting

compounds

• Improved peak shape and

height

• Improves sensitivity

• Rapid column cleaning

Specifications

Ramp rate Column length dependent, up to 300 ºC/min (5 ºC/sec)

Maximum Temperature Column phase dependent, 190°C to 300°C

Cooldown Column and method dependent, 1 to 2 minutes

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Isothermal vs. Temperature Programming

Isothermal

• Results in broad, late eluting peaks

Temperature programming

• Sharpens peak shape

• Shortens run time

• Improves sensitivity

Example – Propane

• Isothermal ~160 seconds

• Ramping ~50 seconds

• Improved peak shape and height

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Column: RT-Q-Bond

Isothermal column temperature: 55°C

Column: RT-Q-Bond

Temperature Ramp:

50°C(10s)90°C240°C, 2°C/s, 2.2°C/s

Isothermal vs. Temperature Programming

Isothermal – late eluting compounds may interfere with the next run

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Temperature Programming – elutes undesired peaks much faster to avoid carryover

INFICON Advances in Micro Gas Chromatography

Column: RT-Molsieve 5A

Isothermal column temperature: 100°C

Column: RT-Molsieve 5A

Temperature Ramp: 100°C(10s)200°C(2°C/s)

Plug and Play Modules

• Modules can be swapped out for easy maintenance or application

changes

• No “commissioning” or “decommissioning” modules

GC connector

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User Interface

• Web-based software eliminates operating system

compatibility issues

• License-free

• Works with any platform (Android, Apple, Windows)

• On-board hard drive stores hundreds of thousands of

runs

Internet Explorer

Version 10 and above

Mozilla

Firefox

Google

Chrome

Apple

Safari

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Micro GC Fusion Connectivity

• Micro GC Fusion can connect via Wi-Fi to: • Smart phones

• Tablets

• Computers with wireless cards

• Micro GC Fusion can be operated using the touch panel display to: • Run a method or sequence

• View analysis report

• View system status

• Micro GC Fusion can connect via Wi-Fi or LAN to computers for method development and advanced features

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Integrated Sample Conditioner

• An optional integrated sample conditioner can be configured

• The sample conditioner allows for:

• Reduction of sample pressures of up to 1000 psi down to 5-10 psi

• Filtering of particulates

• Heating the sample to 100 ºC

• A quick connect replaces the standard 1/16” inlet

• Can be controlled via the user interface

• No manual operation necessary

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Advances in Applications

• Temperature programming allows for expanded

application capability • Natural gas analysis on one module

• Extended natural gas analysis on two modules

• C2 analysis improvements

• Mud logging

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Natural Gas on One Module

• A single RT-Q-Bond module can be used for C1 to C8 Plus analysis

Column: RT-Q-Bond

Ramp: 60°C (hold 50s) -> 127°C (hold 10s) -> 220°C (hold 110s)

(2°C/s, 2.5°C/s)

N2

methane

CO2

ethane

propane

isobutane

n-butane

isopentane

n-pentane

hexanes

heptanes octanes plus

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Excellent Repeatability

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Extended Natural Gas

• An Rxi-1ms module can be added to conduct

extended hydrocarbon (C1 – C11) analysis

Column: Rxi-1ms

Ramp: 50°C 130°C280°C (2°C/s, 5°C/s) ~3 ppm

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Extended Natural Gas – C12 Analysis

• Rxi-1ms with temperature programming

• Straight chain hydrocarbons (C6 to C12) from a sample bag

overlaid with an extended natural gas calibration gas from a

cylinder

• Requires heated sample

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C2 Analysis

• A RT-U-Bond module is typically used to

analyze C2 compounds

• Temperature programming allows for

faster run time and improved peak shape

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Acetylene

Ethane

Ethylene

CO2

Column: RT-U-Bond

Isothermal Column Temperature: 50°C

Column: RT-U-Bond

Temperature Ramp:

50°C(30s)120°C, 3°C/s

Mud Logging

• Mud logging is the creation of detailed reports of a borehole on a

well site during active drilling

• Liquid, or “mud”, is used as the drilling fluid to bring gas, formation

fluids, and rock cuttings to the surface for analysis

• A mud log provides key geographical information, including lithology,

rate of penetration, and hydrocarbon content

• The concentration of compounds is critical and must be performed

on a continuous, 24-7 basis

• Two methods were developed:

• C1 to C5 in 30 seconds

• C1 to C8 in 60 seconds

• Still being optimized

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Mud Logging in 30 Seconds

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Column: RT-Q-Bond

Isothermal column temperature: 55°C

Mud Logging in 30 Seconds

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Column: Rxi-1ms

Isothermal column temperature: 90°C

Extended Mud Logging

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Column: RT-Q-Bond

Temperature Ramp:

55°C(15s hold)220°C(10s hold), 7°C/s

Extended Mud Logging

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Column: Rxi-1ms

Temperature Ramp:

75°C(9s hold)220°C(12s hold), 7°C/s

Future Developments

• Four module Micro GC Fusion expands application capability • Fixed gases, light hydrocarbons up to C12, and olefins

• Refinery gas analysis

• Reactor gas analysis

• Air analysis for natural gas

• Available in 2015

• Additional applications:

• Syngas, biogas

• Sulfur analysis - SO2, H2S

• Natural gas odorants - TBM and THT

• Dissolved gas analysis

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Conclusion

• Building on proven MEMS technology, Micro GC Fusion extends the

capability of the previous generation

• Using temperature programming, Micro GC Fusion extends

analytical capability

• Future development will include a four module instrument and

additional applications

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Questions?

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Visit our website www.INFICON.com for more information

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