Fast Analysis of Extended Natural Gas

using the New Transportable INFICON

Micro GC Fusion

Debbie Hutt

PITTCON 2013– Philadelphia, Pa

Wednesday March 20th, 2012

Copyright © 2013

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Syracuse, NY, USA

325

employees

394

employees

Cologne, Germany

Balzers, Liechtenstein

180

employees

Shanghai, China

• World wide, publically traded company with offices in 14 countries

• 900 employees

• Over 20 years of experience with designing and manufacturing GC and

GC/MS instrumentation

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Outline

Natural gas application information

The Micro GC Fusion for natural gas

analysis

Industry standard information

Future application development

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Natural Gas Application Information

Natural gas composition analysis is critical for :

• Producers

• Gatherers

• Gas distribution companies

• Gas utility companies

• Gas engine and appliance manufacturers

• Independent testing laboratories

Natural gas contains a large percentage of methane (CH4), and smaller

amounts of fixed gases, and light hydrocarbons

Often, it is desirable to analyze C6 to C12 components in order to obtain

more information about the gas sample

Liquefied petroleum or liquid propane (LP) gas and butane/air mixes can

be run using the same method as natural gas

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Natural Gas Analysis Scenarios

Scenario 1

• Wellhead analysis

• Gas and electricity supplied externally via a truck

• Wide BTU range gas

Scenario 2

• Gas appliance or engine development

• Gas and electricity supplied in a laboratory

• Natural gas, LPG, butane/air mixes

Scenario 3

• Gas utility company - leak detection

• Gas and electricity supplied in a laboratory

• Natural gas, landfill gas, transformer fault, cable burn

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Natural Gas Physical Properties

Due to variations in natural gas composition, it is important to measure

physical properties, especially for custody transfer situations

• A small change in value can have a significant financial impact

Physical properties of interest include:

Heating Value (BTU/ft3)

The amount of heat released during the

combustion of a specified amount of a substance

Relative Density/Specific Gravity

The ratio of the density of a substance to the density

of water

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Typical Natural Gas Composition

Component Heating Value

(BTU/ft3)

Wellhead % City gas (pipeline) %

Nitrogen (N2) 0 <10 < 2

CO2 0 <10 < 1-2

Methane (C1) 1010 70-90 93-96

Ethane (C2) 1770 <10 < 1

Propane (C3) 2516 <10 < 0.5

Isobutane (C4) 3252 <2 < 0.5

n-Butane (C4) 3262 <2 < 0.5

Isopentane (C5) 4001 <2 < 0.5

n-Pentane (C5) 4009 <2 < 0.5

Hexanes Plus (C6+) 5126 <2 < 0.2

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Micro GC Fusion Configuration and Method

Configuration

Column stationary phases 15 m RT-Q-BOND, 15 m Rxi-1

Injectors Variable volume

Detector MEMS TCD

Carrier gas pressure 50 psi

Carrier gas consumption 0.5 to 1.5 mL/min per channel

Dynamic Range 106

Method

RT-Q-BOND temperature ramp 80

C (10s hold, 0.35

C/s)150

C

Rxi-1 temperature ramp 80

C (90s hold, 1.7

C/s)250

C

Injector temperature 90

C

Column head pressure 30 psi

Objective: Elute C4 to C12 hydrocarbons on the Rxi-1 column in under 3 minutes

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Temperature Programming

Preliminary Fusion data was acquired on:

• 15 m RT-Q-BOND for N2, CO2, C1-C4 components

• 15 m Rxi-1 column for C4 to C8 components

Extended component analysis allows for more accurate heating value

and other physical property calculations

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Effect of C6-C12 on Heating Value

Compound Heating Value (BTU/Ft3) Gas 1 Mol% Gas 2 Mol %

N2 0 1.525 1.515

CO2 0 1.206 1.199

Methane 1010 88.67 89.12

Ethane 1770 2.994 3.048

Propane 2516 2.006 2.020

isobutane 3252 1.004 1.000

n-butane 3262 0.996 0.999

isopentane 4001 0.300 0.300

n-pentane 4009 0.300 0.300

n-C6 4756 0.603 0.293

n-C7 5503 0.320 0.167

n-C8 6249 0.056 0.028

n-C9 6996 0.019 0.007

n-C10 7742 0.003 0.001

n-C11 8489 0.0003 (3 ppm) 0.0001 (1 ppm)

n-C12 9236 0.00009 (0.9 ppm) 0.00004 (0.4 ppm)

Total Mol% 100 100

Heating Value (Ideal) - 14.696 psi, 60

C 1140 BTU/ft3 1120 BTU/ft3

Heating Value (Real) - 14.696 psi, 60

C 1143 BTU/ft3 1123 BTU/ft3

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Micro GC Fusion Natural Gas 2-Channel

C8s C7s C6s

n-p

en

tan

e

iso

pe

nta

ne

n-b

uta

ne

iso

bu

tan

e

15 m Rxi-1 80

C (90s hold, 1.7

C/s)250

C

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15 m RT-Q-BOND 80

C (10s hold, 0.35

C/s)150

C

pro

pa

ne

iso

bu

tan

e

n-b

uta

ne

eth

an

e

CO

2

me

tha

ne

N2

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Extended Natural Gas Analysis

The Rxi-1 Channel can be used to analyze an extended range of

hydrocarbons

C8s

C7s

C6s

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Isothermal vs. Temperature Programming

Isothermal run

• C4 and C5 hydrocarbons elute late on the RT-Q-BOND

• Potential for carry over

• Extended run times

• Allow 2-4 minutes to clear the column

Temperature programmed run

• C4 and C5 hydrocarbons elute earlier on the RT-Q-BOND

• C6-C8 compounds elute earlier on the Rxi-1

• Ensures a clean column

• Minimizes time between runs

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Component 120

C Isothermal

RT (s)

Temperature

Programming RT (s)

nC6 77 69

nC7 116 85

nC8 N/A 110

Example: Rxi-1

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Cycle Time

With temperature programming, the columns must be heated and

cooled quickly

The Micro GC Fusion cycle time is minimized so that more samples can

be run in a timely fashion

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Industry Standard GC Methods for Natural Gas

Gas Processors Association (GPA) 2145-09

Gas Processors Association (GPA) 2261

Gas Processors Association (GPA) 2172

Gas Processors Association (GPA) 2286 (Extended)

Gas Processors Association (GPA) TP-17

American Society of Testing and Materials (ASTM) D3588

International Standards Organization (ISO) 6976

Repeatability (r)

• Difference in measurement for repeat analysis of same sample on

same instrument (same method) by same operator

• Used to check the instrument

• Measure of precision

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Natural Gas GPA 2261 Repeatability

Component Value (%) r range (%)

Nitrogen 2.485 2.435 - 2.535

Methane 89.468 89.23– 89.65

Component GPA 2261 Repeatability

(r) +/- %

Nitrogen (N2) 2

CO2 3

Methane (C1) 0.2

Ethane (C2) 1

Propane (C3) 1

Isobutane (C4) 2

n-Butane (C4) 2

Isopentane (C5) 3

n-Pentane (C5) 3

Hexanes Plus (C6+) 10

Example:

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Future Application Development

Optimize natural gas analysis to analyze up to C12

• Rxi-1 column length

• Shorten column from 15 m to 5 or 10 m to increase run speed and improve peak shape

• Rxi-1 column film thickness

• Reduce film thickness from 2 µm to 1.2 µm

• Fixed volume injector to minimize matrix effects

• Industry standard repeatability testing

• Integrated sample conditioning

Heated regulator (100-110

C)

Pressure reducer

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Visit booth #1015

or

Visit our website www.INFICON.com

for more information

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