GC Training Course

GAS
CHROMATOGRAPH
TRAINING COURSE
Applies to both
Daniel Danalyzer Gas Chromatograph
Rosemount Analytical Gas Chromatograph
Part Number 3-9000-301

Revision F
JULY 2006
GAS CHROMATOGRAPH TRAINING MANUAL JU L 2006
GAS CHROMATOGRAPH
TRAINING MANUAL
NOTICE
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EMERSON LOGO IS A TRADEMARK AND SERVICE MARK OF EMERSON ELECTRIC CO.
COPYRIGHT © 2006
BY DANIEL MEASUREMENT AND CONTROL, INC.,
HOUSTON, TEXAS,
U.S.A.
All rights reserved. No part of this work may be reproduced or

copied in any form or by any means - graphic, electronic, or
mechanical — without first receiving the written permission of
Daniel Measurement and Control, Inc. Houston, Texas, U.S.A.
PREFACE i
JU L 2006 GAS CHROMATOGRAPH TRAINING MANUAL
WARRANTY
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ii PREFACE
DATE:________________
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description of what you expect from this course.
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PREFACE iii
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iv PREFACE
TABLE OF CONTENTS
COURSE OUTLINE
CHROMATOGRAPHIC TRAINING OUTLINE . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
CHROMATOGRAPHIC THEORY
INTRODUCTION TO GAS CHROMATOGRAPHY . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5

HISTORY . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
BASIC PRINCIPLES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
CHROMATOGRAPHIC COLUMN . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
Solid Support . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
Stationary Phase . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
Column Temperature . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
Carrier Gas . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
Flow Rate Through the Column . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 23
Detectors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
Flame Ionization Detector (FID) (Figure 15) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
Thermal Conductivity (TC) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
Signal Attentuation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
SAMPLE INJECTION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32
DATA PROCESSING AND PRESENTATION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
Qualitative Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
Quantitative Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
SUMMARY . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
MAINTENANCE PRACTICES
MAINTENANCE CHECKLIST . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
TROUBLESHOOTING CHECKLIST . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
FUNCTION CODE DICTIONARY . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
DEW POINT OF VAPOR SAMPLES (Vapor Pressure of Components) . . . . . . . . . . . . . . . . . 43
VAPOR PRESSURE OF COMPONENTS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
THERMAL CONDUCTIVITY EXAMPLES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 45
TABLE OF CONTENTS v
SAMPLE SYSTEM
Genie® Supreme™ Model 120 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47

Genie® Probe™ Regulator . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
Temperature Compensated Regulator . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51
Purge Times for Various Sample Line Sizes . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53
SUGGESTED TEST EQUIPMENT
Alltech Digital Flow Check™ Flowmeters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57

Fluke 50 Series II Thermometers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 58
APPENDIX
Appendix A - Component Data Tables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-1
COURSE EVALUATION
Analyzer Course Evaluation
vi TABLE OF CONTENTS
CHROMATOGRAPHIC TRAINING OUTLINE

(Day 1 - 4 hours)
I. INTRODUCTION
A. Interviews
1. Evaluation of Students' level of experience, technical background,
and specific expectations for training
B. Chromatographic Equipment
1. Introduction to major parts, components, peripherals and functions
performed
II. THEORY OF OPERATION
A. Detector
B. Column Theory - Applied Chemistry
C. Chromatographic Principles
1. Carrier Gas(es)
2. Temperature Control
(Day 2- 8 hours)
III. DOCUMENTATION
A. Drawings
B. Specifications
C. Parameter Sheets
D. Chromatograms
E. Reference Manual
COURSE OUTLINE 1
IV. OPERATION (Hands-on)
A. Operational Modes
1. Keyboard Procedures
2. Prompts
B. Cold Start Programming of Model 2350A

1. Explanation of Prompts
C. Obtaining a Configuration Report
D. Editing the Program
E. Calibrating the Unit
F. Obtaining Accurate Analysis Reports
V. CALCULATIONS
A. Gas Chromatograph Calculations
VI. ALARMS
A. Functions of LED(s)
B. Alarm Conditions
C. Troubleshooting Using Alarms
2 TRAINING COURSE
(Days 3 and 4)
VII. HANDS-ON EXERCISES
A. Advanced Programming/Editing Exercises
VIII. MAINTENANCE
A. Routine Checks
B. Pre-Amp Balance
C. Gas Chromatograph Bench Calibration
D. Carrier Flow Measurement
E. Oven Temperature Calibration
F. Valve Overhaul
(Day 5 - 4 hours)
IX. TROUBLESHOOTING
A. Problem Diagnosis and Repair
COURSE OUTLINE 3
4 TRAINING COURSE
INTRODUCTION TO GAS CHROMATOGRAPHY

HISTORY
Chromatography was first employed in 1905 to separate mixtures of gases and vapors. The
following year, Tswett1 obtained discrete colored bands of plant pigments on a chromatographic
column. He coined the term "chromatography" (color writing) which in the light of present methods
is a misnomer.
Based on the work of the Englishmen Martin and Synge for which they were later awarded the Nobel
Prize, James and Martin introduced gas-liquid chromatography in 1952.
The sensitivity, speed, accuracy, and simplicity of this method for the separation, identification, and
measurement of volatile compounds has resulted in a phenomenal growth.
Gas chromatographs were available commercially about 1955. In this relatively short time, this
technique has become by far the most widely used analysis method in the world.
BASIC PRINCIPLES
Gas chromatography employs elements for injecting a sample, separating the components of the
sample and for identifying and measuring the separated components. It is used to analyze gases,
liquids, and solids in their vapor phase.
1. Tswett, M., Ber. deut. botan. Ges. 24, 316, 384 (1906)
CHROMATOGRAPHIC THEORY 5
The analysis method is a batch type procedure. Discrete samples are injected separately. For best
results, the sample should be injected as quickly as possible.
Figure 1 shows the basic functional elements of a chromatograph.
Figure 1
6 TRAINING COURSE
The elements making up the system are:
• Carrier gas system - for transporting the component through the column at a constant
flow rate.
• Sampling apparatus - for measuring and injecting the sample into the carrier gas ahead
of the column.
• Chromatographic column - for separating the sample into individual components.
• Temperature-controlled chamber - housing at least the column and usually the

detector.
• Detector - for detecting the eluted components in the carrier gas.
• Integrator/controller - to measure components' concentration.
Although the fundamental principles are the same, the physical differences between laboratory and
process chromatographs are extensive. We shall discuss the common fundamental principles first
and the aspects peculiar to the process analyzer later.
We shall now discuss briefly the elements of the chromatograph in the order of their importance.
CHROMATOGRAPHIC COLUMN
The heart of the chromatograph is the column. It is here that the components in the sample are
separated so they may be identified and measured. The column is a length of tubing (1/16" - 1/4"
diameter up to 30 feet long) packed with particles.
Gas chromatography is a technique for separating volatile substances by flowing a gas stream over
a stationary phase. The column packing forms the stationary phase.
If the stationary phase is the particle, we speak of gas solid chromatography (GSC) and the
separation of the sample components is achieved by selective adsorption of the components on the
surface of the particles.
If the stationary phase is a liquid coating on the particle, we speak of gas liquid chromatography
(GLC) and the separation of the sample components is the result of the partitioning of each
component between its vapor phase and a non-volatile solvent (stationary phase) which is coated on
the inert particles (solid support).
The solvent (stationary phase) retains the sample components, according to their distribution
(Partition) coefficients, until they form separate bands in the carrier gas. These component bands
leave the column in the gas stream and are recorded as a function of time by the detector and
recording system. Figure 2 illustrates the formation of a chromatogram, the record showing three
peaks at the right of the diagram.
8 TRAINING COURSE
The following paragraphs will attempt to elaborate on the mechanism by which the separation of the
gaseous components in a sample is achieved.
Figure 2
First perhaps, a crude analogy will be helpful. Refer to Figure 3. Imagine the sketch represents the
following situation.
Figure 3
A groups of animals, elephants, deer, and foxes, are peacefully at home in a large area at the left
bounded by sheer rock walls, when a large grass fire whipped by winds blowing from left to right
bears down upon them and stampedes them toward the densely forested, but more restricted area at
the center of the diagram. Here, as indicated, the trees are closely spaced and the ground is muddy.
The large and heavy elephants encounter considerable difficulty in penetrating and passing through
the restricted area. The smaller and lighter deer encounter less difficulty and the small, light and
agile foxes even less trouble. So as all three are kept under pressure by the fire to keep moving to
the right, the foxes move through the restricted area fastest, the deer next, and finally the elephants
bring up the rear. The conditions as stated have served to separate the animals into three distinct
groups and as they emerge into the free world at the right, we can easily identify each group as well
as count them. If we should make a chart or graph of the animals as they emerge as a function of
time, we would have the equivalent of a chromatogram.
10 TRAINING COURSE
In Figure 4, we can easily relate some of the basic elements of a chromatogram to the drama just
played by the animals.
Figure 4
Getting a little closer to reality, the actual mechanism leading to the separation may be described as
follows:
A few micro liters of the sample to be analyzed is injected into a flowing stream of inert carrier gas
that is being swept through the column under carefully regulated conditions. During the transit of
the sample through the packed column, its components become separated according to their
distribution (partition) coefficients.
Consider the situation of Figure 5.
Figure 5
A closed container is partially filled with a solvent A. When solute B in the form of a gas is
introduced in a small amount above the liquid, an equilibrium will be quickly reached between the
fraction of B remaining in the vapor state and the fraction that goes into solution in liquid A.
At a particular temperature the ratio of the amount of solute per unit volume of liquid phase to the
amount of solute per unit volume of gaseous phase is a constant, or:
C liq
K(t) = S)))) distribution (partition) coefficient
C gas
12 TRAINING COURSE
If some of the gas should be removed from the space above the liquid, some of the gas dissolved in
the liquid will come out of the solution in order to maintain K constant.
Imagine now that Figure 6 is a magnified particle of support material in the column coated with the
liquid (stationary) phase and that this particle in the column is near the entrance of the column.
Figure 6
As the sample being swept through first encounters this particle, a fraction of each component in it
will be dissolved in the stationary phase according to its distribution coefficient. As the carrier
continues to sweep by the particle, the least soluble components will leave the stationary phase first
in their attempt to maintain the value of their distribution coefficient. Therefore, as they sweep
through the column, the components with the lower distribution coefficients will emerge first and
those with the highest coefficients last.
The value of K is high when most of a substance is retained in the liquid phase. This means the
substance moves slowly down the column because only a small fraction will be in the carrier gas at
any given time. Thus, separation between two components is possible, if their distribution
coefficients are dissimilar.
The time that elapses between the start of the analysis and the formation of the peak maxima
corresponding to each component in the sample is called "retention time" for the respective peak
(Figure 7).
Figure 7
14 TRAINING COURSE
Under fixed conditions, retention times are highly reproducible and hence, are used to identify the
sample components.
Factors that affect retention time are:
• Change column temperature - an increase in column temperature up to the stated safe

maximum for the stationary phase in use will result in decreased retention times and a faster
analysis.
• Amount of stationary phase impregnated on the support material - an increase

in the amount of stationary phase will increase retention times, (Figure 8).
• Volume flow rate of the carrier gas - an increase in flow rate will decrease retention
times.
• Length of the column - an increase in length will increase retention times and resolution
(Figure 9).
Factors that affect the ability of column to efficiently separate the components in a mixture:
• solid support
• type and amount of liquid (stationary) phase
• method of packing
• length and temperature of the column
• size and composition of the sample
• mode of injection of the sample
• type and rate of flow of the carrier
Figure 8
16 TRAINING COURSE
Figure 9
Solid Support
As stated previously, the solid support should expose a very large area of the stationary phase to the
sample in order that gas-liquid equilibrium may be achieved rapidly.
A good packing material should have a specific area of 2 or 5 meters2/gram (very porous) and
uniform particle size.
Each 100 parts by weight of the support material should have from 5 to 30 parts of the stationary
phase absorbed upon it.
Optimum Solid Support characteristics may be summarized as follows:
• Large specific surface area.
• A porous structure with uniform pore diameter in the range of 10 microns or less (.1mm).
• Inertness - a minimum of chemical and absorptive interaction with the sample.
• Regularly shaped particles - uniform in size for efficient packing.
• Mechanical strength. Should not crush on handling.
• Not affected physically at the operating temperature of the column.
Diatomaceous earth, teflon, crushed firebrick, and celite are often used as support materials.
18 TRAINING COURSE
Stationary Phase
Good solvent efficiency results in greater separation of peaks (greater ratios of retention times) or
better resolution, (Figure 10).
Figure 10
Resolution refers to the true separation of two consecutive peaks. It relates to the narrowness of
peaks and the separation between maxima (Figure 11).
Figure 11
As a general rule, the liquid (stationary) phase should be as similar in chemical class to the
components of a mixture to be separated as possible. There should be no possibility of reactivity
between the chemical groups of the stationary phase and those in the components of the analytical
mixture.
20 TRAINING COURSE
One of the major advantages of GC over the distillation is the ability to use solvents selected to
provide the best separation of the components in the sample. Thus components with same boiling
point which are impossible to separate by distillation may be separated on a GC.
There are several interaction forces which can aid in the GC separation. These are atomic and
molecular forces of various types. Without attempting to describe or explain them individually, it
may be said that their combined effects are expressed by the partition coefficient K.
Liquid phase requirements may be summarized as follows:
• Good absolute for sample components - if solubility is low, components elute rapidly, and
separation is poor.
• Good differential solvent for sample components.
• Non-volatile - vapor pressure .01 to .1mm at operating temperature for reasonable column
life.
• Thermally stable.
• Chemically inert toward the solutes of interest at column temperature.
Column Temperature
The partition coefficient K decreases with increasing temperature. The fraction of the solute in the
gas phase will increase with rising temperature and hence, the elution time will decrease, which also
decreases the width of the peaks. This results in decreased separation since it is the liquid phase
which performs the separation. So, to achieve better separation, lower temperatures should be used,
but this will result in longer analysis times (Figure 12).
Figure 12
22 TRAINING COURSE
Carrier Gas
A high pressure gas cylinder serves as the source of carrier gas. A pressure regulator is used to
assure a uniform pressure to the column inlet and thereby a constant rate of gas flow. At a given
temperature, this constant rate of gas flow will elute components at a characteristic time (the
retention time).
Commonly used gases are hydrogen, helium and nitrogen. The carrier gas should be:
• Inert to avoid interaction with the sample or solvent

• Able to minimize gaseous diffusion
• Readily available, pure
• Inexpensive
• Suitable for the detector used.
Flow Rate Through the Column
Column efficiency depends upon choosing the proper linear gas velocity.
The optimum flow rate can be easily determined experimentally by making a simple van Deemter
plot of HETP vs. linear gas velocity. HETP means Height Equivalent of a Theoretical Plate. Plates
as referred to in the term are somewhat analogous to those in a distillation column.
The number of theoretical plates (N) in a column are determined from a chromatogram as indicated
below (Figure 13).
Figure 13
The Height Equivalent of a Theoretical Plate is then simply the length of the column divided by N.
HETP = L/N
The most efficient flow rate is the one giving the minimum value of HETP. In other words, it is the
flow rate permitting the use of the shortest or most efficient column, for L = HETP x N. Where
HETP is minimum, so also will be L (Figure 14).
Figure 14
24 TRAINING COURSE
From the foregoing, it is apparent that a great many things affect the efficiency of a chromatographic
column. Its ability to produce sharp, well separated peaks in the chromatogram in the minimum
amount of time is a function of:
• Length, solid support and stationary phase.

• Temperature
• Carrier gas flow rate.
Detectors
After a chromatographic column has successfully separated the components in a sample, the problem
of detecting the components in the carrier gas for purposes of identification and quantitative
measurement remains.
To solve this problem, several different types of detectors have been devised. The detectors most
commonly used can be separated into two categories — concentration and mass flow rate.
The concentration detectors sense a bulk property, e.g. thermal conductivity, of both the carrier gas
and component. Thus, there must be a great difference in the value of this property between the
carrier gas and the sample components. An example of this type is the thermal conductivity detector.
Helium as a carrier gas has high thermal conductivity. Sample components have low thermal
conductivity. The change in thermal conductivity of the gas within a detector indicates the presence
of a component.
The mass flow rate detectors sense a specific property of the sample components and not of the
carrier gas. For example, in the flame ionization detector, the hydrogen flame ionizes the sample
components but not the carrier gas. Thus, the response is proportional only to the flow rate of
component molecules as they are ionized in the flame.
The chromatogram produced by a detector consists of a series of peaks, each of which corresponds
to a different component. The area under each peak is proportional to the total mass of that
component. Hence, the chromatographer may calculate weight percent compositions from area ratios
on the chromatogram. With thermal conductivity detectors, the peak area is inversely proportional
to carrier gas flow rate, so the flow rate must be kept constant for accurate quantitative analysis.
For detectors responding to mass flow rate, such as flame ionization detectors, the peak area is
independent of carrier gas flow rate.
Generally speaking, the usefulness of a detector regardless of the type, may be evaluated in terms
of the following characteristics:
• Selectivity
• Sensitivity
• Response
• Noise
• Linear Range
Secondly, to these things, it should be simple, rugged and relatively insensitive to changes in flow
rate and temperature.
The Flame Ionization and Thermal Conductivity detectors will now be discussed in more detail as
examples of the two types.
Flame Ionization Detector (FID) (Figure 15)
Ionization detectors operate on the principle that the electrical conductivity of a gas is directly
proportional to the concentration of charged particles within the gas. In the FID, effluent gas from
the column is mixed with hydrogen and burned in air or oxygen. Ions formed in the flame enter the
electrode gap which causes current to flow across the gap and through a series resistor. The resulting
voltage drop can then be amplified and recorded. The background current due to the carrier is
normally canceled out so that the effects of the sample components only are recorded.
The flame detector responds to all but a relatively short list of compounds (inorganics) which include
water, carbon disulphide, and also air. The lack of response to air and water make the FID especially
suitable for the analysis of air pollutants or aqueous samples.
26 TRAINING COURSE
FID performance depends on the proper choice of auxiliary gas (hydrogen and oxygen) flow rates.
Sensitivity and stability are affected and such detectors should be calibrated to determine the flow
rate that gives the best response.
Figure 15
Thermal Conductivity (TC)
Since the Gas Chromatograph (GC) uses a TC detector, the following paragraphs will elaborate on
this method of measurement.
The TC detector is widely used primarily because it responds to all types of compounds and can
sense trace concentrations as well as very high concentrations.
The TC detector operates on the principle that a hot body will lose heat at a rate proportional to the
composition of the surrounding gas. The rate of heat loss is then used as a measure of gas
composition.
The detector usually takes the form of a Wheatstone Bridge where the four arms of the bridge are
made of very fine wires or filaments of platinum or a tungsten alloy. The bridge current from a well-
regulated power supply is high enough to heat the bridge filaments to several hundred degrees
fahrenheit. The bridge wires are mounted on suitable supports and inserted in cavities in a small cell
block which are interconnected by passages through which the sample and the reference gases are
passed. Such an arrangement minimizes the effect of temperature and flow disturbances (Figure
16).
Figure 16
28 TRAINING COURSE
Most systems use four wire bridges where two legs are exposed to the sample and two to the
reference material. In some cases, two wire bridges are used and then only one heat sensitive
element responds to the sample and one to the reference.
When sample molecules mixed with the carrier (reference) gas pass by one pair of the bridge
elements, the rate of heat loss from the elements will be reduced and their resistance will increase,
thereby unbalancing the bridge. This bridge unbalance is usually impressed across an attenuator
network where either all, or some known fraction of it is applied to the input of a recorder and the
peak recorded.
The principle of operation is that the ability to conduct heat from a filament is a function of the
molecular weight of the gas surrounding it.
Figure 17 illustrates an arrangement for producing a chromatogram with a TC detector and an auto
ranging amplifier.
Figure 17
30 TRAINING COURSE
The four temperature elements of the thermal conductivity bridge are R1, R2, R3, R4. These four
elements are constructed to be as nearly identical as possible and they are mounted in the cavities
of the cell block to provide as nearly identical thermal environments as possible. The reasons for
matching elements and environments are to make the unit as insensitive to operating and
environmental changes as possible. A balanced Wheatstone Bridge tends to be self-regulating.
Elements R1 and R3 are mounted in the cell cavity through which pure carrier gas will pass and
elements R2 and R4 will be exposed to the effluent gas from the column. Electrical adjustments M
and N are provided for bridge balance and bridge current adjustment respectively.
Chromatogram baseline reference is obtained by passing pure carrier gas through both passage ways
in the cell simultaneously.
Signal Attenuation
Most detectors are shunted with an attenuator so that signal input to the recorder will result in a
readable peak even though there may be a very large differences in the absolute value of the bridge
output signals for different sample components. For example, the sample being analyzed may
consist of three principle components as follows: Component A 90%, Component B 9.9%, and
Component C .1%. In order that Component C produce a good measurable chromatogram peak
height, say of at least 10% of full scale on the recorder, the attenuator switch S is set to apply the full
bridge unbalance voltage to the recorder input terminals.
Now, peak B passes through the detector and in order to prevent this peak height from exceeding the
full scale span of the recorder, the attenuator must be reset so that only a known fraction of the
bridge output for this peak is applied to the recorder input. As Component A comes through, in all
probability, the attenuator will have to be reset again to accommodate the very large bridge output
it will produce.
The attenuator switch may be manually operated based on known sample composition or from
observation of peak heights as they are being recorded, or its manipulation may be programmed into
an automatic system that will initiate many other operations such as column switching, purging,
backflushing the system, etc., which are a part of overall system operation.
It may be noted here that this is a very demanding application for conventional analog recorders.
This is true for four principle reasons.
• To the recorder, the attenuator is a signal source with widely varying internal resistance.
This may affect measurement sensitivity unless the recorder input impedance is made quite
high.
• Narrow recorder spans of one mv or less are needed to record the peaks of trace components.
This demands high measurement sensitivity.
• High recorder pen speeds, one second for full scale travel or faster are required to record the
tops of the high peaks without attenuation. This requires high servo power.
• Good input filtering is needed to minimize the effects of transverse stray voltages which may
originate in the bridge power supply, for example, and which otherwise might affect the
performance of the recorder.
For a more complete discussion of the recorder in the chromatograph, the reader is referred to: The
Chromatography Slave - The Recorder, by Rob B. Bonsall, Lab and Test Markets, Honeywell Inc.,
Fort Washington, Pennsylvania.
SAMPLE INJECTION
The size and mode of injection of the sample is very important in the design of a good
chromatograph.
Since retention time identifies the components in the sample, the time of sample injection should be
established accurately.
The rate of sample injection should be rapid so that the total sample may be considered to have been
introduced into the system at one time and not spread out over an extended period. The width of the
narrowest peak in a chromatogram can never be less than the time required to introduce the sample.
The size of the sample should be small. This permits equilibrium to be reached rapidly between the
sample and the stationary phase in the column. In laboratory chromatographs liquid sample injection
is frequently done with a suitably prepared microliter syringe. With it a few microliters (1 to 5) are
quickly injected into the carrier gas system at the input end of the column. Not only must the
injection time be short, but the sample size must be known and reproducible so that repeat runs and
check runs may be reliably compared.
32 TRAINING COURSE
For gas sample injection, very precise and elaborate sample injection valves, as well as gas tight
syringes, are used for introducing samples.
Reproducibility of sample size is of the order of .5% with valves, whereas about 2% reproducibility
is typical with syringes.
DATA PROCESSING AND PRESENTATION
In gas chromatography, data processing and presentation involves the methods used in handling the
detector output to provide identification and amount of each of the sample components. These are,
respectively, qualitative analysis and quantitative analysis. The various techniques utilized to
accomplish qualitative and quantitative analysis will now be discussed.
Qualitative Analysis
Gas chromatography has a fantastic ability to separate components. One of the problems associated
with the technique is to positively identify all of the separated peaks emerging from the column.
Ability to identify peaks has not progressed as fast as ability to produce them.
The literature describes several methods for identifying sample components from their
chromatograms and most deal with retention data in various ways. Identification is based on
comparison of the retention time of the unknown component with that obtained from a known
compound analyzed under identical conditions. With constant carrier gas flow rate and constant
column temperature, retention time is peculiar to the compound for a given column. With well
designed equipment, retention data are quite reproducible. Confirmation of identifications where
retention data is difficult to interpret may be made using infrared, mass spectrographic, magnetic
resonance or other methods.
Quantitative Analysis
Component concentration is determined from peak heights or area or from other measurements
directly related to peak area.
High accuracies can be obtained providing the proper techniques are employed. Relating to accuracy
is the care with which the analyst recognizes and accounts for the many sources of error present in
the analyzing system. Some of these error sources are:
1. Does the sampling device and your sampling technique actually take the sample you wish
to analyze?
2. Does it actually put the sample into the chromatograph and without any changes in its
composition?
3. Is any of the sample absorbed or decomposed in the system?
4. Does the detector respond properly and consistently? Is it stable and sensitive?
5. Does the recorder have the capabilities to faithfully record the output of the detector in the
face of the conditions as listed previously?
6. Is the method selected for measuring and/or calculating peak area valid?
If these questions have been adequately considered and their effects taken into consideration, then
the relative areas of the peaks are a good measure of the composition of the sample.
Some of the ways (with advantages and disadvantages) of relating peak shape to sample
concentration are:
1. Peak height; peak heights may be affected by sample size as well as baseline drift.
2. Planimetry; peak area measured with a hand planimeter. Time consuming and subject to
individual variations.
3. Height x width at half height. This assumes symmetrical peaks of triangular shape and
reasonable width. Technique is rapid and simple (Figure 18).
.
Figure 18
34 TRAINING COURSE
4. Triangulation; height measured from the baseline to the intersection of two tangents (Figure
19).
Figure 19
5. Cutting and weighing paper; peaks are actually cut out of paper and weighed. Accurate, but
very time consuming and chromatogram is destroyed.
6. Integration
a. Ball and disc integrator driven directly from the recorder with "counts" being
recorded as the pen in recording a peak deviates from the baseline.
b. Electronic; where chromatographic input signal is fed into a voltage to frequency

converter. When the device senses the peak, pulses from the V-F converter are
totalized and printed out as a measure of peak area.
The relative percentages of each component in a mixture of components may be determined by

comparing the peak area for the component to the sum of the peak areas for all the components:
Area Peak A
Area Percentage = S)))))))))))) x 100
Area all Peaks
36 TRAINING COURSE
SUMMARY
Because of somewhat complicated effects that changes in the operating variables have on qualitative
and quantitative aspects of the data, an outline of these effects is given as follows. Please note that
these are the normally expected effects for the respective changes. Under certain conditions this may
not be valid, but those conditions would be considered abnormal. Also note that if the entire
chromatogram was properly processed by a computer, many of these changes would have no effect
on achieving accurate qualitative and quantitative analysis. However, since the primary aim of this
introductory primer is process gas chromatography, the effect on "peak height" by changing variables
is emphasized.
A. At a constant retention time, the peak height of a component will change with a change in
any of the following:
1. Sample size (peak height is proportional to sample size)
a. By a change in sample volume caused by partial filling of volume by solid

contaminant or change in physical dimensions of volume.
b. By a change in sample volume pressure which means more molecules in the

same sample volume.
2. A detector bridge current in a TC detector which changes temperature and thus

response of filaments. (A 2-fold increase in current can result in an 8-fold increase
in peak height.)
3. Attenuation or gain setting on the bridge output.
4. Detector temperature.
B. Retention time of a component will change with a change in any of the following:
1. Carrier flow rate - increase in flow rate decreases retention time.
2. Column temperature - increase in temperature decreases retention time about 5%/oC.
3. A large increase in sample size will result in a noticeable increase in retention time.
4. A decrease in column liquid phase (caused by operating column over the temperature
limit) will result in decreased retention time.
5. Column contamination could result in increased or decreased retention times. In

GLC, if very high boiling liquid dissolves in the liquid phase, retention times could
increase. In GSC, water would absorb on molecular sieve, plugging adsorption sites
which would decrease retention times.
C. At constant carrier flow rate, peak height increases as retention time decreases.
D. In TC detectors, peak height (sensitivity) increases as carrier flow rate decreases. This is
caused by decrease in the specific heat effect and increase in gas diffusion of component
molecules to filament area.
38 TRAINING COURSE
MAINTENANCE CHECKLIST
Date Performed ___ /___ / ___
Sales Order No. ____________
BI-MONTHLY AS FOUND AS LEFT NOMINAL
HELIUM CARRIER
CYLINDER
Cylinder Pressure Reading (High) ____ psig ____ psig
Cylinder Pressure Outlet Reading ____ psig ____ psig 110-115 psig
CARRIER PRESSURE PANEL

REGULATOR* ____ psig N/A 90 psig
SAMPLE SYSTEM
Sample Line Pressure(s) (1)___ psig ____ psig 5-15 psig
(2)___ psig ____ psig 5-15 psig
(3)___ psig ____ psig 5-15 psig
(4)___ psig ____ psig 5-15 psig
(5)___ psig ____ psig 5-15 psig

Sample Flows (Rotameter) (1)___ cc/min ____ cc/min 40-60 cc
(2)___ cc/min ____ cc/min 40-60 cc
(3)___ cc/min ____ cc/min 40-60 cc
(4)___ cc/min ____ cc/min 40-60 cc
(5)___ cc/min ____ cc/min 40-60 cc

Calibration Gas
High Pressure Reading ____ psig ____ psig
Outlet Pressure Reading ____ psig ____ psig 5-15 psig
Flow (Rotameter) ____ cc/min ____ cc/min 40-60 cc/min
* Adjusting carrier pressure panel regulator will result in retention time changes. Do not adjust
without consulting Customer Service.
MAINTENANCE PRACTICES 39
Table 5-2. TROUBLESHOOTING CHECKLIST
AS FOUND AS LEFT NOMINAL
ANALYZER
Leak check with SNOOP® from

helium
bottle to analyzer regulator.

calibration standard to auto-
calibration solenoid.
Pre-amp balance voltage _____ mV _____ mV 0 ±0.5 mV

(see Section 5.5.6)
SAMPLE SYSTEM

sample
probe to sample solenoid
MODEL 500 INPUTS
GC GRI PAZ (12-bit AD) Value (12-bit AD) PAZ (16-bit AD) Value (16-bit AD)
1 0.0 to 0.0 600 to 800 0 to 4095 4800 to 6400 -32767 to 32767
2 0.8 to 1.1 600 to 800 0 to 4095 4800 to 6400 -32767 to 32767
3 0.8 to 1.1 600 to 800 0 to 4095 4800 to 6400 -32767 to 32767
4 0.8 to 1.1 1150 to 1500 0 to 4095 9200 to 12000 -32767 to 32767
40 TRAINING COURSE
Table 5-2. TROUBLESHOOTING CHECKLIST (Continued)

AS FOUND AS LEFT NOMINAL
ANALYZER POWER SUPPLY

(TB4 Terminals 24, (+20V) ___ Volts +20.0 ±.5V
25, 26)
( - 20V) ___ Volts -20.0 ±.5 V
(+20 V) ___ mV AC 0.0 ±40 mV
( - 20V) ___ mV AC 0.0 ±40 mV
CHROMATOGRAM
(SPECTRUM “ON”)
Check baseline
Check component values on report
Number of peaks
Retention times
Date and file
TEMPERATURE
(see Section 5.5.7)
Detector Temperature °C or °C or
Thermocouple Wire #1 (Type J) ____ mV ____ mV 78-83°C
Heater Block Temperature °C or °C or
Thermocouple Wire #2 (Type J) ____ mV ____ mV 78-83°C
MEASURE VENT FLOW

(see Section 5.5.8)
Analyzer Valve 3 ON ___ cc/min ____ cc/min 12-18 cc/min
Analyzer Valve 3 OFF ___ cc/min ____ cc/min
* Refer to System Operational Parameters
FUNCTION CODE DICTIONARY

GC CONTROLLER
F/C 1 F/C 2 F/C 4 F/C 8

2251 TERM # 29 31 33 35
TB4 TERM # 11 12 13 14
VALVE 1 ON 5 VDC 5 VDC 0 VDC 5 VDC
VALVE 1 OFF 0 5 0 5
VALVE 2 ON 5 0 0 5
VALVE 2 OFF 0 0 0 5
VALVE 3 ON 0 5 0 0
VALVE 3 OFF 5 0 0 0
VALVE 4 ON 5 5 5 5
VALVE 4 OFF 0 5 5 5
VALVE 5 ON 5 0 5 5
VALVE 5 OFF 0 0 5 5
STREAM 1 5 5 5 0
STREAM 2 0 5 5 0
STREAM 3 5 0 5 0
STREAM 4 0 0 5 0
STREAM 5 5 5 0 0
42 TRAINING COURSE
DEW POINT OF VAPOR SAMPLES
For multi component vapor mixtures, calculation of dew point can be performed according to the
following formula:
(P) (Y)
X = ————
VP
P = total pressure in PSIA

Y = MOL fraction of component
VP = vapor pressure of component
Step 1. Assume lowest temperature sample may be subjected to.
Step 2. Find the vapor pressure of each component at the above temperature.
Step 3. Assume highest pressure (P) sample may be subjected to.
Step 4. Calculate X for each component. If the sum of the X's for all the components equal
to 1.00 or more, there will be some dropout of liquid. If the sum of the X's for all
the components equal to 0.95 or less, the sample will remain vapor.
VAPOR PRESSURE (PSIA) OF

COMPONENTS AT VARIOUS TEMPERATURES IN oF
Component 0 oF 20 oF 40 oF 60 oF 80 oF 100 oF 120 oF -20 oF
N 2 and C 1 2500 3000 3500 4000 4500 5000 5600 2000
CO 2 305 425 575 675 1000 1200 1500 210
C2 225 300 400 505 650 800 1000 160
C3 38 55 79 109 149 190 250 25
C4 11.8 18 26 38 55 68 100 7.1
NC 4 7.4 12 18 27 39 54 74 4.6
NEO 2.5 4 6.5 10 15 20.5 30 1.8
IC 5 2.5 4 6.5 10 15 20.5 30 1.8
NC 5 1.7 2.95 4.55 7.25 11 16 23 1
1/2C 6 and 1/2C 7 .15 .29 .5 .9 1.5 2.5 3.9 <.1
C6 .4 .71 1.2 2 3.3 5 8 .15
C7 <.1 .18 .32 .58 1 1.6 2.6 <.1
44 TRAINING COURSE
THERMAL CONDUCTIVITY EXAMPLES
NAME SYMBOL THERMAL

CONDUCTIVITY AT
ZERO DEGREES C
Air 5.8
Hydrogen H2 39.6
Helium He 33.6
Nitrogen N2 5.7
Argon A 3.9
Carbon Dioxide CO2 3.4
Methane CH4 7.2
Propane C3H8 3.6
Acetylene C2H2 4.5
Benzene C6H6 2.2
Butane C4H10 3.2
Chloroform CHCL3 1.6
Freon 12 CL2CF2 2.0
(Dichlorodifluoromethane)
Methanol CH3OH 3.4
Acetone C3H6O 2.4
46 TRAINING COURSE
SAMPLE SYSTEM 47
48 TRAINING COURSE
SAMPLE SYSTEM 49
50 TRAINING COURSE
SAMPLE SYSTEM 51
52 TRAINING COURSE
PURGE TIMES FOR VARIOUS SAMPLE LINE SIZES

(Standard flow rate of 2,000 cu cm/min at 15 psig)
SIZE VOLUME PURGE TIME

(cm3/Ft) (per 100 ft)
TUBING
1/8 x 0.030 wall 0.65 3.9 sec
1/8 x 0.020 wall 1.1 6.6 sec
1/4 x 0.030 wall 5.5 33.0 sec
3/8 x 0.035 wall 14 1.4 min
½ x 0.035 wall 29 2.9 min
5/8 x 0.049 wall 43 4.3 min
3/4 x 0.049 wall 66 6.6 min
PIPE
1/8 Sch 40 11 1.1 min
1/4 Sch 40 21 2.1 min
3/8 Sch 40 38 3.8 min
½ Sch 40 60 6.0 min
3/4 Sch 40 105 10.5 min
1 Sch 40 170 17.0 min
SAMPLE SYSTEM 53
54 TRAINING COURSE
56 TRAINING COURSE
SUGGESTED TEST EQUIPMENT 57

Fluke 50 Series II Thermometers
58 TRAINING COURSE
APPENDIX A, COMPONENT DATA TABLE
A.1 COMPONENT DATA TABLE
This appendix provides a sample standard Component Data Table as well as a table of the
ISO-related components.
• Table A-1, Example Standard Component Data Table
• Figure A-1, ISO Component Data Table
All values depend on a base pressure of 14.73 PSIA and a base temperature of 60 oF
(15.56 oC).
BTU components reference GPA Standard 2145-03.

Note: * Denotes components that are assigned temporary I.D. Codes, starting with 150, as they are used.
COMPONENT DATA TABLE A-1

Table A-1. Example Standard Component Data Table
D aniel
C om ponent M ol R eid R el D ens R el D ens L b/gal GPM G ross D ry N et D ry AGA8 Sim
N am e Wt V apor G as L iquid F actor BTU BTU N o. 2251
I.D . N o.
Acetylene 26.04 0.0 0.8990 0.6150 0.0 0.0 1476.9 1426.5 4 22
Air 28.9625 0.0 0.87484 0.8748 7.2931 0.10489 0.0 0.0 26 26
Argon 39.95 0.0 1.3792 0.0 0.0 0.0 0.0 0.0 21 46
Ammonia 17.03 212.00 0.5880 0.6173 5.1500 0.0874 435.4 359.8 0 *
Benzene 78.11 3.2240 2.6969 0.8844 7.3730 0.2798 3750.5 3599.2 15 *
Butanes 58.123 62.084 2.0068 0.5735 4.7815 0.32117 3264.67 3012.45 12 33
Butene-1 56.11 63.050 1.9372 0.6013 5.0130 0.2956 3087.0 2885.4 12 28
Butenes 56.11 55.448 1.9372 0.6097 5.0833 0.2916 3077.4 2875.7 12 32
1,2-Butadiene 54.09 20.000 1.8676 0.6580 5.4860 0.2604 2946.7 2795.5 12 35
1,3-Butadiene 54.09 60.000 1.8676 0.6272 5.2290 0.2732 2886.6 2735.3 12 34
C 3+ 44.097 188.74 1.5226 0.50736 4.2305 0.27534 2522.02 2320.36 5 47
C 4+ 58.123 51.683 2.0068 0.58407 4.8696 0.31525 3269.94 3017.97 12 48
C 4=1 56.11 63.050 1.9372 0.6013 5.0130 0.2956 3087.0 2885.4 12 29
C 5+ 72.15 15.558 2.4912 0.63111 5.2618 0.36216 4018.97 3715.58 14 49
C 6+ 47/35/17 95.9577 3.0199 3.31319 0.67994 5.6689 0.44618 5288.73 4900.61 22 08
C 6+ 50/50/00 93.1905 3.2909 3.21765 0.6761 5.6369 0.43621 5141.17 4762.99 23 09
C 6+ G PA 2261-99 93.191 3.5166 3.2177 0.67557 5.6325 0.4626 5141.13 4762.99 24 10
C 6+ 57/28/14 94.1923 3.3740 3.25224 0.67706 5.6449 0.43986 5194.55 4812.81 25 11
C arbon M onoxide 28.01 0.0 0.9671 0.8010 6.6800 0.0 321.2 321.2 9 15
C arbon D ioxide 44.01 0.0 1.5196 0.82275 6.8596 0.16946 0.0 0.0 3 17
C IS-2-Butene 56.11 45.540 1.9372 0.6271 5.2280 0.2835 3079.3 2877.6 12 31
COS 60.08 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0 42
C S2 76.14 0.0 2.6298 0.0 0.0 0.0 1267.0 1267.0 0 41
C yclohexane 84.16 3.2640 2.9057 0.7834 6.5310 0.3403 4492.1 4189.4 15 *
C yclopentane 70.14 9.9140 2.4215 0.7504 6.2560 0.2961 3772.4 3520.2 14 0
D iisobutyl 114.23 1.1010 3.9439 0.6979 5.8190 0.5185 6247.9 5793.9 17 *
2,3-D imethbutan 86.18 7.4040 2.9753 0.6664 5.5560 0.4096 4756.0 4403.1 15 *
2,2-D imethpenta 100.21 3.4920 3.4596 0.6782 5.6540 0.4682 5494.6 5091.4 16 *
2,4-D imethpenta 100.21 3.2920 3.4596 0.6773 5.6470 0.4686 5499.4 5096.0 16 *
3,3-D imethpenta 100.2 2.7730 3.4596 0.6976 5.8160 0.4550 5501.5 5098.2 16 *
A-2 TRAINING COURSE

D aniel
I.D . N o.
Ethane 30.07 800.00 1.0382 0.35639 2.9714 0.26729 1773.79 1622.74 4 01
Ethyl alchohol 46.07 2.3000 1.5906 0.7940 6.6200 0.1839 1602.8 1451.5 0 *
Ethyl benzene 106.17 0.3710 3.6655 0.8718 7.2680 0.3858 5234.3 4982.0 17 *
Ethylene 28.054 850.0 0.9686 0.23569 1.965 0.37707 1604.1 1502.47 4 21
Ethylene O xide 44.05 0.0 1.4900 0.0 0.0 0.0 1459.4 1410.2 0 36
3-Ethyl pentane 100.21 2.0120 3.4596 0.7028 5.8590 0.4517 5513.4 5110.1 16 *
H2S 34.08 394.67 1.1767 0.80267 6.6922 0.134506 638.6 588.178 7 40
HC L 36.46 925.00 1.2588 0.8558 7.1350 0.1349 0.0 0.0 0 *
Helium 4.002602 0.0 0.1382 0.0 0.0 0.0 0.0 0.0 20 13
Hydrogen 2.02 0.0 0.0696 0.0700 0.0 0.0 325.00 274.4 8 12
i-Butane 58.123 72.484 2.0068 0.56293 4.6934 0.32709 3259.4 3006.94 11 03
i-Butene 56.11 63.400 1.9372 0.6004 5.0060 0.2960 3068.2 2866.5 12 27
i-Pentane 72.15 20.456 2.4912 0.62459 5.2074 0.36594 4010.2 3707.6 13 05
i-Propyl benzene 120.19 0.1880 4.1498 0.8663 7.2230 0.4396 5976.6 5674.0 18 *
i-O ctane 114.23 1.7080 3.9439 0.6962 5.8040 0.5199 6246.1 5792.2 17 *
M ethane 16.043 5000.0 0.55392 0.3 2.5 0.26412 1012.3 911.1 1 00
M ethyl alcohol 32.04 4.6300 1.1063 0.7960 6.6400 0.1275 868.7 767.9 0 *
M ethycyclo C 5 84.16 4.5030 2.9057 0.7536 6.2830 0.3538 4511.6 4209.1 15 *
M ethylcyclo C 6 98.19 1.6090 3.3900 0.7740 6.4530 0.4019 5228.0 4874.9 16 *
2-M ethylhexane 100.21 2.2710 3.4596 0.6830 5.6940 0.4647 5507.3 5104.0 16 *
3-M ethylhexane 100.21 2.1300 3.4596 0.6917 5.7670 0.4589 5511.3 5107.8 16 *
m-X ylene 106.17 0.3260 3.6655 0.8687 7.2430 0.3871 5219.9 4967.8 17 *
n-Butane 58.123 51.683 2.0068 0.58407 4.8690 0.31525 3269.94 3017.97 12 04
n-D ecane 142.285 0.05889 4.9127 0.73404 6.12 0.61405 7760.8 7206.63 19 *
n-Heptane 100.204 1.6203 3.4598 0.68817 5.7375 0.46128 5515.33 5111.8 16 45
n-Hexane 86.177 4.9614 2.9755 0.66403 5.5363 0.41114 4767.0 4414.18 15 39
n-N onane 128.258 0.1796 4.4284 0.72185 6.0183 0.56288 7012.386 6508.02 18 38
n-O ctane 114.231 0.5366 3.9441 0.70696 5.8942 0.51188 6263.26 5809.41 17 20
n-Pentane 72.15 15.558 2.4912 0.63111 5.2618 0.36216 4017.974 3715.58 14 06
N eohexane 86.18 9.8560 2.9753 0.6540 5.4530 0.4175 4747.2 4394.1 15 *
N eopentane 72.15 35.900 2.4911 0.5967 4.9750 0.3830 3993.9 3691.4 13 07
N itrogen 28.0134 0.0 0.96723 0.80938 6.7481 0.10965 0.0 0.0 2 14

D aniel
I.D . N o.
NO2 46.00 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0 19
NO 30.01 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0 *
N 2O 44.02 0.0 0.0 0.0 0.0 0.0 0.0 0.0 0 18
o-xylene 106.2 0.2640 3.6655 0.8848 7.3770 0.3801 5222.0 4969.7 17 *
O xygen 31.9988 0.0 1.1048 1.1421 9.5221 0.08876 0.0 0.0 10 16
1-Pentene 70.14 19.115 2.4215 0.6457 5.3830 0.3441 3835.4 3583.3 14 37
Propane 44.097 188.74 1.5226 0.50736 4.2301 0.27534 2522.02 2320.36 5 02
Propadiene 40.07 0.0 1.4110 0.0 0.0 0.0 2254.2 2254.2 5 24
Propylene 42.081 227.87 1.4529 0.52264 4.3574 0.25507 2339.1 2187.05 5 23
Propyne 40.07 0.0 1.4110 0.0 0.0 0.0 2246.2 2246.2 5 25
p-xylene 106.17 0.3420 3.6655 0.8657 7.2180 0.3885 5220.8 4968.6 17 *
Sulfur D ioxide 64.06 88.000 2.2117 1.3970 11.650 0.1453 0.0 0.0 3 43
Styrene 104.15 0.2400 3.5959 0.9110 7.5950 0.3622 5042.7 4841.0 17 *
Toluene 92.14 1.0320 3.1812 0.8718 7.2680 0.3348 4485.4 4283.5 16 *
Trans-2-Butene 56.11 49.800 1.9372 0.6100 5.0860 0.2914 3075.1 2873.4 12 30
Triptane 100.21 3.3740 3.4596 0.6946 5.7910 0.4571 5496.2 5093.0 16 *
W ater 18.0153 0.95028 0.62202 1.0000 8.3374 0.05707 50.4444 0.0 6 44
A-4 TRAINING COURSE

Figure A-1. ISO Component Data Table

Figure A-1. ISO Component Data Table (Continued)
A-6 TRAINING COURSE


A-8 TRAINING COURSE


A-10 TRAINING COURSE

ANALYZER COURSE EVALUATION
1. Date of Course ____________________________
2. Did you find the course worthwhile? Q yes Q no
3. Do you feel confident in the operation of

the Emerson Process Management GC? Q yes Q no
4. Please rate the course content: Sufficient Insufficient Too Much
A. Chromatographic Theory Q Q Q
B. Chemistry Q Q Q
C. Programming Q Q Q
D. Sample System Q Q Q
E. Sampling Q Q Q
F. Blueprint Reading Q Q Q
G. Total System Operation Q Q Q
5. Compare lecture time to “hands on” time: Q Balanced

Q Too much lecture
Q Too much “hands on”
6. Instructor Rating: Good Fair Poor
A. Subject Knowledge Q Q Q
B. Clarity of Presentation Q Q Q
C. Course Organization Q Q Q
D. Courtesy Q Q Q
Other Comments:
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
7. Course Material: Good Fair Poor
A. Manual Q Q Q
B. Drawings Q Q Q
Comments:
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
8. How could the course be improved?

_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
_____________________________________________________________________________
Name: (Optional): ______________________________________________________________

Company (Optional): ____________________________________________________________

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GAS

Part Number 3-9000-301

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CHROMATOGRAPHIC TRAINING OUTLINE . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

INTRODUCTION TO GAS CHROMATOGRAPHY . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5

Genie® Supreme™ Model 120 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 47

SUGGESTED TEST EQUIPMENT

Alltech Digital Flow Check™ Flowmeters . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57

Appendix A - Component Data Tables . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . A-1

Analyzer Course Evaluation

CHROMATOGRAPHIC TRAINING OUTLINE

II. THEORY OF OPERATION

B. Column Theory - Applied Chemistry

IV. OPERATION (Hands-on)

B. Cold Start Programming of Model 2350A

C. Obtaining a Configuration Report

D. Editing the Program

E. Calibrating the Unit

F. Obtaining Accurate Analysis Reports

A. Gas Chromatograph Calculations

C. Troubleshooting Using Alarms

VII. HANDS-ON EXERCISES

A. Advanced Programming/Editing Exercises

C. Gas Chromatograph Bench Calibration

D. Carrier Flow Measurement

E. Oven Temperature Calibration

A. Problem Diagnosis and Repair

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INTRODUCTION TO GAS CHROMATOGRAPHY

Figure 1 shows the basic functional elements of a chromatograph.

The elements making up the system are:

• Chromatographic column - for separating the sample into individual components.

• Temperature-controlled chamber - housing at least the column and usually the

• Detector - for detecting the eluted components in the carrier gas.

• Integrator/controller - to measure components' concentration.

Consider the situation of Figure 5.

Factors that affect retention time are:

• Change column temperature - an increase in column temperature up to the stated safe

• Amount of stationary phase impregnated on the support material - an increase

Optimum Solid Support characteristics may be summarized as follows:

• Large specific surface area.

• Inertness - a minimum of chemical and absorptive interaction with the sample.

• Regularly shaped particles - uniform in size for efficient packing.

• Mechanical strength. Should not crush on handling.

• Not affected physically at the operating temperature of the column.

Liquid phase requirements may be summarized as follows:

• Good differential solvent for sample components.

• Chemically inert toward the solutes of interest at column temperature.

• Inert to avoid interaction with the sample or solvent

Flow Rate Through the Column

• Length, solid support and stationary phase.

Flame Ionization Detector (FID) (Figure 15)

Thermal Conductivity (TC)

DATA PROCESSING AND PRESENTATION

3. Is any of the sample absorbed or decomposed in the system?

b. Electronic; where chromatographic input signal is fed into a voltage to frequency

The relative percentages of each component in a mixture of components may be determined by

1. Sample size (peak height is proportional to sample size)

a. By a change in sample volume caused by partial filling of volume by solid

b. By a change in sample volume pressure which means more molecules in the

2. A detector bridge current in a TC detector which changes temperature and thus

3. Attenuation or gain setting on the bridge output.

1. Carrier flow rate - increase in flow rate decreases retention time.

(4)_ psig __ psig 5-15 psig

(5)_ psig __ psig 5-15 psig

(5)_ cc/min __ cc/min 40-60 cc

Pre-amp balance voltage _ mV _ mV 0 ±0.5 mV