Chromatography Basics 2021

| Title | 2020 |
© Yokogawa Corporation of America
Scott Eddleman / Tim Roth
January 21, 2021
Live Webinar
Gas Chromatography Basics

| Title | 2020 |
2
Presenters
Host
Cherlyn Marlow
Product Marketing Manager
P
r
e
s
e
n
t
e
r
s
Tim has worked with process analyzers over the past 40 years. He is a veteran
of the United States Air Force and earned his Associate degree in computer
engineering from the Milwaukee School of Engineering and Bachelor of
Science degree from Marquette University. In Tim’s current role, he is actively
involved with the application and sale of both liquid and gas phase analytical
analyzers used across a broad spectrum of markets and applications.
Scott Eddleman has over 19 year of experience in process analyzer project
execution with responsibilities including but not limited to testing/QC to
the fabrication and engineering design. Scott has spent the last 19 years
with Yokogawa system integration group and he is currently one of our
Analytical Technical Sales Managers focusing on GC and System
Integration.
Scott Eddleman
Analytical Technical Sales
936-520-1854
Scott.Eddleman@yokogawa.com
Tim Roth
414-350-4202
tim.roth@yokogawa.com

| Title | 2020 |

| Title | 2020 |
Bottle of Black Ink
Chromatography: High School Science Experiment
 Dipped a piece of absorbent paper into Black Ink
 The ink wicked up the paper forming various color
bands
 The color bands were from the various pigments in
the ink absorbing onto the paper at different rates
 This showed that a mixture of compounds could be
separated by differences in how fast they moved
through the media
 Chromatography was originally invented for the dye
industry

| Title | 2020 |
Basic Chromatograph System
Process
Line
Cal
Bottle
Sample System
Carrier
Bottle
Probe
By-Pass
Filter
By-Pass Return
Slip Stream
Carrier Gas
Calibration Gas
GC Oven
Control Electronics
Detector Vent
Reference Vent
Injection Valve
Separation
Columns
Detector
Measurement Results
Maintenance Data
Atmos
Vent
User
Interface
Heater

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Functions Of The Analytical Oven
 Inject a sample onto the separation columns
 Separate the sample into individual compounds
 Detect concentration of individual compounds

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Types Of Sample Injection Valves
 Rotary Valve
 Sliding Plate
 Diaphragm Valve
 Liquid Sample Injection Valve Valve Off
Sample In
Carrier In
Sample Loop
Sample Out
To Columns
Valve On
Rotary Valve Operation

| Title | 2020 |
Separation Columns
 Long tubing filled with grains of sand with a chemical coating on the grains
 Sample is pushed through the tube by an inert carrier gas
 If a mixture of compounds move through the column, they separate due to
differences in chemical properties
 Separation by boiling point differences
 Separation by polarity differences
 Separation by molecular size
Carrier Gas
Pushing Chemical
Of Interest Column Tubing
Hot Oven

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Column Separation Of 3 Compounds
Methane
Ethane
Propane
One at a time, each component leaves the Column and
heads to the Detector for measurement

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Column Types
 Packed – 1/8” O.D.
 Micropacked - 1/16” O.D.
 PLOT - Porous Layer Open Tubular
 SCOT - Support Coated Open Tubular
 WCOT - Wall Coated Open Tubular
 FSOT - Fused Silica Open Tubular
(Capillary)
 0.53 mm Mega Bore
 0.32 mm Wide Bore
 0.10 mm Narrow Bore
Fused Silica Capillary Column
Packed Columns

| Title | 2020 |
Column Switching Techniques
 To speed up analysis times, multiple columns are used to
separate out the component of interest
 A number of techniques have been developed to speed up
the analysis
 Backflush to Vent
 Backflush to Detector
 Heart Cut
 Trap Bypass
 Multiple techniques might be used in the same analyzer for
complex situations

| Title | 2020 |
Vent
Carrier
Column Switching — Backflush To Vent
Column 1 Column 2
Sample
Inject Sample Backflush Mode
DET
SV
Carrier
Goal of Backflushing is to only separate the
components of interest to minimize the cycle time

| Title | 2020 |
Types Of Detectors Available
1 PPM 10 PPM 100 PPM 1000 PPM 1 Mole % 100 Mole %
Thermal Conductivity Detector (TCD)
Flame Ionization Detector (FID)
Flame Photometric Detector (FPD)

| Title | 2020 |
Thermal Conductivity Detector (TCD)
 Measures the thermal conductivity
difference between sample and
reference gas
 Results in difference in resistance on
one side of the electronics
 Universal detector
 All compounds have a thermal
conductivity
 Sensitivity down to ~5 ppm Output
Power
Supply
Sampl
e
Sampl
e
Reference
Reference
Vent Vent
From
Column
From
Reference
Output

| Title | 2020 |
Flame Ionization Detector (FID)
 Hydrocarbons form ions when burned in
a flame
 If a voltage is applied to the flame tip,
current will flow to a collector above the
flame when hydrocarbons present
 The more sample present, the bigger the
value
 Sensitivity down to ppb levels
 Only works for hydrocarbons
 No Sulfurs, H2O, O2, etc.
From
Columns
Air
H2
Bias
Voltage
Collector
Voltage
Igniter

| Title | 2020 |
Flame Photometric Detector (FPD)
 Flame turns yellow when sulfur
compounds are present
 The more sulfur present, the more yellow
 Sensitivity down to ppb levels
 Only works for sulfurs
 H2S, COS, CS2
 Mercaptans
 Thiophenes
 Etc.
From
Columns
Air
H2
Photo
Multiplier
Tube
Igniter

| Title | 2020 |
Typical Chromatogram (Natural Gas)

| Title | 2020 |
Peak Integration
Residence Time
Integration
On
Baseline
Time
Integration
Off
Retention Time identifies which component is which
Area under the peak determines concentration

| Title | 2020 |
Some Rules-Of-Thumb: Typical Analysis Times
 Simple straight chain hydrocarbons:
 2 minutes + 1 minute per measured compound
 Simple aromatics:
 6 minutes + 1 minute per measured compound

| Title | 2020 |
Some Rules-Of-Thumb: Weight % Vs. Mole %
 GC’s inherently generate results in mole %
 Liquid volume % available on liquid injections
 Weight % only possible with complete analysis
 Long analysis time
 Increase in analyzer complexity

| Title | 2020 |
Some Rules-Of-Thumb: What Makes A GC Complex
 More than three measured compounds
 Multiple measurement ranges
 Multiple detectors
 More than three process streams

| Title | 2020 |
Basic Chromatograph System: Sample System
Process
Line
Cal
Bottle
Sample System
Carrier
Bottle
Probe
By-Pass
Filter
By-Pass Return
Slip Stream
Carrier Gas
Calibration Gas
GC Oven
Control Electronics
Detector Vent
Reference Vent
Injection Valve
Separation
Columns
Detector
Measurement Results
Maintenance Data
Atmos
Vent
User
Interface
Heater

| Title | 2020 |
Principles Of GC Sample Conditioning
 Take a representative sample
 Transport the sample in a controlled & timely
manner
 Condition the sample for optimum analysis
 Provide sample stream switching and calibration
 Accommodate sample return or venting systems
 Accomplish above without excessive maintenance
and service attention

| Title | 2020 |
Purpose of Sample Extraction Probes
 Used to get a more representative sample due to
higher flow rates away from the walls
 Eliminates wall contaminates, particulates, etc.
 First stage of filtration

| Title | 2020 |
Typical Sample System Flow Diagram
Why so many valves to
stream switch you ask?

| Title | 2020 |
Multistream Sample Systems
Simple 3-way valve risks cross stream
contamination
Stream 1 Stream 2
To GC Sample Valve
Solenoid valve
starts to leak
Which leads to uncertainty in measurement

| Title | 2020 |
Double Block & Bleed Stream Switching
Stream 1 Stream 2
To GC Sample Valve
Atmospheric Vent Solenoid valve
starts to leak
Solenoid valve
starts to leak too
Eliminates Risk Of Cross Stream Contamination
Solenoid valve
starts to leak too

| Title | 2020 |
Information Needed For Proper Design
 Total stream composition (normal & upset )
 Sample point temperature and pressure as well as
sample return pressure
 Data on corrosive chemicals and particles
 Distance between probe and sample system

| Title | 2020 |
29
Conclusion and Wrap-up

| Title | 2020 |
Yokogawa’s OpreX™ Analyzer System Solutions
30
1
2
3
4
5
EXECUTE
SUPPORT
IMPLEMENT
STRATEGIZE PLAN
COMMUNICATION
TIME MANAGEMENT
SCHEDULING
BUDGETING
IMPLEMENT: INSTALLATION, FAT/SAT, etc…
From discussing application data, FAT results, and performance
goals to analyzing work orders, job scopes, drawings, and materials
to be used to optimize the installation sequence is just another day
in the office.
STRATEGIZE: FEED STUDIES
Front End Engineering and Design Capabilities (FEED & Feasibility)
studies provide you with Project Risk Reduction, Lower Project Costs
and More Owner Influence when EPCs are involved.
PLAN: DETAIL ENGINEERING & DESIGN
In-House Detailed design, fabrication, testing & Project Execution,
meeting an array of environmental, safety and local code
considerations (TDLR, ISO9000, NFPA, NEC, UL, etc.
EXECUTE: BUILT TO SPEC
Longest operating analytical system integrator in the world
providing customized solutions for any Process on any Analyzer
and any Where
SUPPORT: SITE SERVICES
From initial field audits, start-up, and commission to
troubleshooting and maintenance, We have the experience and
resources to work with you during all phases of your project.
https://web-material3.yokogawa.com/Process_Analyzers_Integration_Services_BU.us.pdf

| Title | 2020 |
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31
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| Title | 2020 |
OPEN DISCUSSION
32
Tim Roth
414-350-4202
Tim.roth@yokogawa.com
Scott Eddleman
936-520-1854
Scott.Eddleman@yokogawa.com

| Title | 2020 |
33
Q&A
Select and send all questions to “Panelist” now so that
we can address these
Questions
If you have any questions for this Webinar topic, please
send them to webinars@us.yokogawa.com

| Title | 2020 |
The names of corporations, organizations, products and logos herein are either registered trademarks or
trademarks of Yokogawa Electric Corporation and their respective holders.
Thank you for attending
34

Chromatography Basics 2021

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