H1187A Student

P Series Micro GC and Data
System Operation
Course Number H1187A
Student Manual
P Series Micro GC and Data
System Operation
Course Number H1187A
Student Manual
Manual Part Number H1187-90000

Printed in the USA September, 2000
Notice
The information contained in this document is subject to change without notice.
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including but not limited to the implied warranties of merchantability and fitness
for a particular purpose.
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incidental, or consequential damages in connection with the furnishing,
performance, or use of this material.
No part of this document may be photocopied or reproduced, or translated to
another program language without the prior written consent of Agilent
Technologies, Inc.
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 2000 by Agilent Technologies, Inc.

All rights reserved
Printed in the United States of America
ii
Table Of Contents
MODULE 1: BOOK INTRODUCTION 1
Using this Book 2
Module Descriptions 3
MODULE 2: INTRO TO AGILENT P-SERIES MICRO GC 7
Introduction to the Micro GC 8
Basic Gas Chromatography 9
Micro GC 11
Carrier gas and gas control 11
The injector 11
The separation system 12
Backflush Modules 12
Detection system 12
Data system 13
Separation Processes 15
Qualitative analysis 16
Quantitative analysis 16
Gases and Plumbing 21
Micro GC Hardware 25
P-Series Micro GCs 26
External Inputs/Outputs 27
Agilent M-Series Micro GCs 28
Laboratory Exercises 34
Lab 1: Hardware Familiarization and Set Up 35

Part 1: Identifying the Hardware 35
Part 2: Observe the Panels of the GC 35
Part 3: Connecting the Hardware Components 35
Lab 2: Filling the Internal Carrier Gas Cylinder 36

Filling the Carrier Gas Cylinder 36
Module 2 Review 37
iii
MODULE 3: EZCHROM INTRODUCTION 39
Introduction to EZChrom 40
Windows Compatibility 41
Software Installation 43
MTI GC Setup 49
MTI GC Verification 51
Data File Path 55
Initiating EZChrom 56
Instrument Menu 59
Method and Data Menus 60
Math Menu 61
Calib and Help 62
Lab Exercises 64
Lab Exercise 1: Starting Up the System 65

Part 1: Turning On the PC 65
Part 2: Loading the EZChrom Software 65
Part 3: Turning on the GC 65
Part 4: Running GC Setup 66
Part 5: Launching the EZChrom Software 66
Part 6: Using the GC Verification Tool 66
Lab Exercise 2: Introduction to Windows NT 67

Part 2: Working with Windows NT 67
Part 3: File Management in Explorer 70
Lab Exercise 3: Working with Windows NT 72

Part 1: Organizing and Customizing the Desktop 72
Part 2: Changing the Logon Password 75
Part 3: Configuring Printers 76
Part 4. Windows NT Routine Maintenance 76
Optional Lab Exercise 4: Intro to Windows 95 78

Part 2: Working with Windows 95 78
Part 3: File Management in Explorer 80
iv
Part 4: Viewing the Contents of a File. 82
Lab Exercise 5: Working with Windows 95 83

Part 1: Organizing and Customizing the Desktop 83
Part 2: Configuring Printers 86
Part 3. Windows 95 Routine Maintenance 86
Module 3 Review 90
MODULE 4: DATA ACQUISITION AND ANALYSIS 93
Data Acquisition and Analysis 94
Creating a Method 100
Collecting the Data 111
Data Analysis 114
Graphic Manipulation 115
Optimizing Timed Events 118
Lab Exercises 124
Lab 1: Air Analysis using the Molsieve/Poraplot U Backflush GC 125

Part 1:Building the Method (Non-Backflush) 125
Part 2: Building a Backflush Method 127
Part 3: Optimizing the Integration 131
Lab 2: Butane Analysis using the MolSieve/Poraplot U GC 132
Lab 3: Natural Gas Analysis using the OV1/Poraplot U GC 133
Module 4 Review 134
MODULE 5: INJECTORS 135
GC Injectors 136
GC Hardware 139
Injection Process 144
Injector Types 153
Theory of Injector Operation 159
v
Heated versus Unheated Injector 175
Column Flow Considerations 176
Lab Exercises 177
Lab: Setting Inlet Options 178

Part 1: MolSieve/Poraplot U Backflush GC 178
Part 2: OV1/Poraplot U Heated Injector GC 178
Module 5 Review 179
MODULE 6: COLUMNS 181
Columns 182
GC Hardware 183
Column Separation 188
Column Types 189
Fundamentals of Separation Theory 195
Typical Applications 211
Lab Exercises 225
Lab Exercise: Changing Column Parameters 226

Part 1: Varying the oven temperature and column flow rate 226
Part 2: Calculating the Column Efficiency 226
Part 3: Accessing the Micro GC website 226
Module 6 Review 227
MODULE 7: DETECTORS 229
Detectors 230
Setting Detector Parameters 234
Detector Response Characteristics 235
Thermal Conductivity Detection 238
Lab Exercises 244
Lab Exercise: Modify the Detector Sensitivity 245
vi
Module 7 Review 246
MODULE 8 CALIBRATION, SEQUENCES, AND REPORTING 247
Calibration, Sequences, Reporting 248
Qualitative Analysis 250
Quantitative Analysis 251
Calibration Procedure 259
Reporting 269
Sequences 273
BTU Reporting 275
Lab Exercises 277
Lab 1: Preparing Calibration Standards 278

Part 1: Preparing Standards 278
Part 2: Analyzing Standards 279
Part 3: Optimizing the Method 280
Lab 2: Creating a Multi-Level Calibration 282

Part 2: Editing the Peak Table 283
Part 3: Recalibrating 284
Part 4: Calculating Response Factor 285
Lab 3: Exploring Reporting Options 286

Part 1:Standard Report Formats 286
Part 2: Custom Reporting Options 287
Lab 4: BTU Reporting 288
Module 8 Review 289
MODULE 9: TROUBLESHOOTING 291
Troubleshooting 292
Common Problem Areas 293
Routine Troubleshooting 301
Monitoring Instrument Status 303
vii
Communication Error Numbers 304
GC Verification Tool 305
MTI GC Setup 308
Maintenance Procedures 310
Module Change Tool 311
Lab Exercises 312
Lab 1: Troubleshooting Problems 313

Part 1: Confirming Performance 313
Part 2: “De-bugging” your instrument 313
Lab 2: Final Exam 314

Part 1: “I’ve run the Instrument, But Can I Get the Right Answers?” 314
Part 2: Final Exam Answer Sheet 314
viii
MODULE 1: Book Introduction
This module describes the contents of this book. The sections are:
• Using this Book
• Module Descriptions
• Instructional Materials Required
1
Using this Book
Using this Book

This book Agilent P Series Micro GC and Data System Operation contains
nine modules covering topics relevant to the instruction of operation of the P
Series GC System. The course modules are:
• Module 1: Book Introduction
• Module 2: Introduction to Gas Chromatography and the HP P Series Micro
GC Hardware
• Module 3: EZChrom Introduction
• Module 4: Data Acquisition and Analysis
• Module 5: GC Inlets
• Module 6: GC Columns
• Module 7: GC Detector
• Module 8: Calibration, Sequences, and Reporting
• Module 9: Troubleshooting and Maintenance
This book is used for training classes designated to teach P Series MicroGC and
Data System Operation. Each module contains an explanatory section made up of
Power Point slides with student notes and a section of lab exercises.
2
Module Descriptions
Module Descriptions
Module 1: Book Introduction

Using this Book
Module Descriptions
Instructional Materials Required
Hardware required
GC Configuration 1:
P200 (Portable) Micro GC
MolSieve (10-meter)/Poraplot U (8-meter) for Air and Butane Analysis
Backflush option for the MolSieve module
GC Configuration 2:
P200 (Portable) Micro GC
OV1 (10-meter)/Poraplot U (8-meter) for Natural Gas Analysis
Heated Injector option
1 Sampling Conditioner
1 PC for each GC
Consumables
1 Liter and 3-Liter Tedlar Bags for each GC
Blending manifold
500 uL, 1 ml and 10 ml syringes
Samples
Room Air
Butane disposable lighter
Natural Gas (not calibration grade)
Stock standards, 1000 ppm of the following:
cis-1,2-Dichloroethene
Chloroform
Tertrachloroethene
High purity Nitrogen
Software Required
EZ Chrom Ver. 4.5
Microsoft Excel
3
Module Descriptions
Module 2: Introduction to Gas Chromatography and the HP P Series

Micro GC Hardware
Basic GC concepts and definitions
Major components of a GC
Considerations for Gases and Plumbing
Filling the Carrier gas cylinder
Reference for Module 2: GC User Manual, Chap. 2 & 3
Lab Exercises
Lab 1: Hardware Familiarization and Set UP
Lab 2: Filling the Carrier Gas Cylinder
Module 3: EZChrom Introduction

Compatibility to Windows
Loading the Software
Performing GC Setup and GC Verification
Introduction of the software Menu Items
Reference for Module 3: Software User Manual: Chap. 1 & 2
Lab Exercises
Lab 1: Starting up the System
Loading the EZ Chrom Software and GC Tools
Verifying Installation using MTI GC Setup, checking Instrument
Status, using the GC Verification Tool.
Lab 2: Introduction to Windows NT
Lab 3: Working with Windows NT
Lab 4: Introduction to Windows 95
Lab 5: Working with Windows 95
Module 4: Data Acquisition and Analysis

Creating a Method
Setting up Acquisition Parameters
Creating Data Subdirectories
Reference for Module 4: Software User Manual; Chap. 3 & 4 (p41)
Lab Exercises*
Lab 1: Air Analysis using the MolSieve/Poraplot U GC
4
Module Descriptions
Lab 2: Butane Analysis using the MoleSieve/Poraplot U GC

Lab 3: Natural Gas Analysis using the OV1/Poraplot U GC
* Students will swap instruments in order to perform all labs.
Module 5: Inlets and Injection Process

Purpose of Inlets
GC and Injector Hardware
Function of the Injector
Types of Injectors
Understanding the flow dynamics of the Injector
Reference for Module 5: GC User Manual; pages 11 & 63
Lab Exercises*
Lab: Setting Inlet Options
a. Vary Injection and Sample times
b. Optimize Back Flush time
* Students will swap instruments in order to perform the exercises.
Module 6: Columns
Micro GC Attributes
Column Types
Fundamentals of Separation Theory
Common Micro GC Applications
Reference for Module 6: GC User Manual; Chapter 5
Lab Exercises
Lab 1: Varying Temperature and Flow rate
Lab 2: Calculating Column Efficiency
Lab 3: View various applications from Micro GC Website.
Module 7: Detector
Fundamentals of the Thermal Conductivity Detector
Reference for Module 7: GC User Manual; Appendix A
Lab Exercises
Lab 1: Modifying the Detector Sensitivity
5
Module Descriptions
Module 8: Calibration, Sequences, and Reporting

Fundamentals of Calibration Theory
How to use the Calibration Menus
Single and Multi-Level External Standard Calibrations
Reporting Options
Automated Sequences
BTU Reporting
Reference for Module 8: Software User Manual; Chapter 7
Lab Exercises
Lab 1: Preparing Calibration Standards
Lab 2: Creating Multi-level Calibration
Lab 3:Exploring Report Options
Lab 4: BTU Reporting
Module 9: Troubleshooting and Maintenance

Routine troubleshooting and maintenance procedures
Learn how to use the Module Change Tool
Lab Exercises
Lab 1: Troubleshooting Problems
Lab 2: Final Exam
6
MODULE 2: Intro to Agilent P-Series
Micro GC
In this section you will learn:

• Basic Gas Chromatography concepts and definitions
• The major components of the gas chromatograph
• Considerations for use of gases and plumbing configuration
• Filling the Carrier Gas Cylinder
MODULE 2: Intro to Agilent P-Series Micro GC
Introduction to the Micro GC
Introduction to the Micro GC
Introduction to Gas Chromatography and

the Agilent P-Series Micro GC Hardware
• Basic gas chromatography: concepts and definitions

• Major components of the gas chromatograph
• Considerations for gases and plumbing configuration
• Filling the carrier gas cylinder
Figure 1
The purpose of this module is to introduce the basic concepts of Gas

Chromatography and the AGILENT Micro GC.
8
Basic Gas Chromatography
Typical Gas Chromatograph
Electrometer
Gas Trap Detector
Column
PC
Sample Vent
Carrier Gas
Figure 2
The main components of a gas chromatograph are shown above.

The next page reviews the definitions for these components.
9
Definitions
• Gases
Carrier Gas -- Pressurized gas used to transport the sample through
the system
• Sample Introduction
Introduces the sample to the carrier gas stream with minimal
disruption of the gas stream
• Column
Achieves separation of the components in the sample
• Detector
Recognizes and responds to sample components as they elute from
the column
• Data Acquisition
Converts the detector signal to a picture chromatogram and provides
manual or automated determination of the identity and amounts of the
sample components
Figure 3
The first major component of the GC is the carrier gas. A carrier gas supply is
always present and usually consists of helium, nitrogen, or argon. The function of
the carrier gas is to carry the sample through the system. The gas one chooses
depends on the specific application. The gases are commonly supplied by
compressed gas cylinders. Gas generators are also an option as a gas source for
bench top units.
The next major component part is the sample introduction process. It usually
consists of an injection port but can also include valves. The purpose of the inlet
is to introduce the sample into the carrier gas stream.
The next major component part is the column. The purpose of the column is to
provide the separation of the components in the sample mixture.
The Thermal Conductivity detector is a device that senses the presence of
components different from the carrier gas and converts the information to an
electrical signal.
The data acquisition device is a PC that uses software to convert the detector
signal to a peak chromatogram and report.
10
Micro GC
Micro GC
Micro GC Diagram
Pressure
Carrier In Regulator Sample Loop
Switching Valve
Pressure
Transducer
Sample In Vacuum
Pump Sample Vent
Out
Micro Injector
Analytical Column
Detector Detector Vent
Column Heater
Reference Column
Note: Backflush modules also have a PreColumn

4
Figure 4
Carrier gas and gas control

The first component of a Micro GC is the carrier gas or mobile phase. The carrier
gas is contained in a high pressure cylinder. A two-stage regulator is attached to
the cylinder to allow monitoring and regulation of pressure. It also enables you to
determine when replacement or refilling of the tank is necessary. An on/off valve
allows you to open the tank to let the carrier gas flow through the injector,
through the column and the detector then out through the instrument vents. The
most common carrier gas used is helium. Helium provides the required sensitivity
for most GC applications.
The injector
The second major component is the injector. The injector introduces a measured
amount of sample into the inlet of the analytical column. The Micro GC contains
a timed injector micro machined from a silicon wafer using manufacturing
techniques borrowed from the semiconductor industry. The injection sequence
begins when the carrier gas for the reference column flows through the injector.
11
Micro GC
Two flow restriction channels moderate the flow of carrier gas to both the
reference and analytical columns. To take a sample, the sample microvalve in the
injector opens allowing the internal vacuum pump to pull sample gas through the
sample loop and out the vent. The sample microvalve then closes, the vacuum
pump turns off and a switch valve connects to the outlet of the pressure regulator,
thereby pressurizing the sample loop. Because of the flow restriction channels, the
pressure in the sample loop is slightly higher than the pressure at the inlet of the
analytical column. Therefore, when the inject microvalve opens, the sample from
the loop flows into the channel leading to the analytical column. The amount of
sample injected depends on the length of time the inject microvalve is open. After
a user defined time (typically about 40 msec), the inject valve is closed and the
switch valve connects to the vacuum pump. The injected sample flows into the
analytical column, where the sample is separated into its components.
The separation system

The third component and the separation system is the column. The column tubing
is packed/coated with a chemical substance that attracts some of the sample
components more than others. As a result, components will separate as they pass
through the column. A wide selection of columns offers a wide selection of
selectivity. Although column length as well as tubing dimensions influence
separation, separation is primarily influenced by solubility. Because solubility is
affected by temperature, column temperature must be controlled.
Backflush Modules
A GC module with a precolumn backflush-to-vent configuration has two
columns—a short precolumn and a longer analytical column. The backflush valve
lies between the precolumn and the analytical column. The stationary phase and
length of the precolumn is chosen so that, at the operating temperature of the
columns, undesirable sample components that interfere with the analyses are
retained on the precolumn stationary phase. The sample components for
quantification have minimal affinity for the stationary phase of the precolumn,
and pass quickly through the precolumn. After the last sample component for
quantification exits the precolumn and enters the analytical column, the
backflush-to-vent valve located between the precolumn and the analytical column
opens. The carrier gas flow through the precolumn is reversed and backflushes the
undesirable sample components off the precolumn. The sample components for
quantification continue to flow through the analytical column for separation and
detection. At the end of the analytical run, the backflush GC module is fully
purged of all sample components and is ready for the next analysis.
Detection system
The fourth Micro GC component is a detector. A detector monitors the carrier gas
and senses a change in its composition when a component in the sample elutes
from the column. One of the most common, reliable and easy to use detectors is
12
Micro GC
the universal micro machined Solid State Detector (SSD). The SSD is a micro
machined version of the Thermal Conductivity Detector (TCD). The design of
this detector is derived from a Wheatstone Bridge, which is an electronic device
that compares the electrical resistance of two branches in a circuit. In an SSD,
pure carrier gas elutes from the analytical column and passes over two matched
filaments. The bridge compares their resistance against those of the reference
side. When both sides have pure carrier gas flowing over the filaments, the bridge
is balanced and the output is zeroed. When a component elutes, the thermal
conductivity on the sample side of the bridge changes. Therefore, the resistance of
the analytical side changes and the output indicates a peak is eluting. A regulated
power supply controls the voltage being fed to the filaments at a constant level.
The bridge also has a balance control and an autozero circuit to zero the detector
output between runs. The user can select high, medium or low sensitivity levels
which changes the gain level of the electronics. This is unlike standard TCDs
where sensitivity increases by increasing filament temperature and corresponds
with a decrease in detector life.
Data system
The final or fifth component of a Micro GC is the data system. The main purpose
of a gas chromatographic system is to generate both qualitative and quantitative
data. Data systems provide both a visual recording of the detector output and an
area count of the detector response. The detector response is used to identify the
sample composition and measure the amount of each component by comparing
the area counts of the sample to the analysis of a known calibration standard.
Computer based data systems can communicate with the analyzers. This added
versatility allows the analyst to store and set operating conditions for an analysis
in the computer, making the data system and the analyzer an integrated
instrument.
13
Micro GC
Micro GC Column
Analytical
Column
Reference
Column
Heater/
Shroud
Figure 5
Columns are 4 to 14 meters long and 0.15 to .5 mm in diameter. For the function
of the Thermal Conductivity detector, both a reference and analytical column is
used.
14
Separation Processes
Typical Chromatogram
Time scale in Seconds

not
Minutes!
Retention Time: Parameter used to identify a sample component

Peak Area: Parameter used to identify the quantity of the sample component
Figure 6
A typical chromatogram is shown. Retention times are used to identify the

components in a mixture by comparing peak times to known reference standard
peak times. If the times match, it is very likely that the components are the same.
Note the time scale is in seconds!
Peak areas are used to determine the amount of the components present. A
default Area% report calculates the relative area amounts of the detected peaks.
Standards of known amounts of the components can be used as reference in a
calibration procedure to produce other report options (External Standard,
Normalized %, or BTU).
A chromatogram is a plot of the detector response versus time. The plot begins as
you place the sample into the carrier gas stream and should continue until the last
component in the sample elutes. The chromatogram depicts each component as it
exits the column as a peak. It also shows the separation achieved for that
particular sample. Each peak is identified by its retention time and the length of
time that a component takes to travel through the column. If analysis conditions
(flow and temperature) are maintained constant, the chromatographic trace is very
reproducible and could be used for both qualitative and quantitative analysis.
15
Qualitative analysis
Qualitative analysis is designed to identify the components of a sample. Gas
chromatography is not an absolute qualitative tool and usually must rely on other
techniques for peak identification. However, a Micro GC containing two GC
modules can separate the components of a sample with two different stationary
phases, simultaneously. The result is peak identification and confirmation in a
single analysis. To analyze qualitatively, a calibration standard of known
composition must be analyzed first. Pure compounds elute at the same time under
exactly the same analytical conditions. If you match the calibration standard peaks
with those in your samples, you can be fairly sure that you have those compounds
in your sample.
Quantitative analysis
Quantitative analysis is designed to determine the amount or proportions of the
components of a sample based on the detector response. The detector response
(area or height) is proportional to the amount of a component in a sample.
However this response varies slightly with each component. Therefore, it is
necessary to experimentally determine the area (or height) concentration
relationship by running a calibration standard containing the components of
interest. The conditions in which the detector response for the calibration standard
must be the same as those in the unknown samples.
16
Model of the Chromatographic Process

Separation of compounds , and
Flow
A
Figure 7
The column is responsible for the separation of the components in the mixture.
At the time of entering the column, the components are in a homogeneous
mixture. As the components pass through the column, certain components have
more affinity for the material inside the column and thus are retained longer than
other components. The components separate based upon this differential
interaction with the column material. Those components eluting first have the
least affinity for the column material, and those eluting last have the most
interactions with the column.
There are many different types of columns available. One chooses the column
type relative to the type of components requiring separation.
Gas chromatography is an analytical technique used for the separation of the
sample components between two phases; a mobile phase (the carrier gas) and a
stationary phase (the column packing or coating). The separation begins when a
gaseous sample fills the sample loop of the injector. The sample is then injected
from the loop onto the column. Carrier gas (mobile phase) transports the sample
down the length of the column. Because the different components in a sample
have different affinities or solubility, each component spends different amounts of
time in the column packing/coating. When in the packing/coating, a component
does not progress down the column. When diffused out of the packing/coating,
they progress down the column at the same rate as the carrier gas. As a result, the
components spend different amounts of time in the two phases, separating as the
carrier gas moves them through the column.
17
Assume that a component takes 5 seconds to travel through an empty column at a

constant carrier gas flow rate. Now, fill or coat the tube with stationary phase in
which the component is soluble. The same component spends 50% of the time in
the stationary phase and 50% in the mobile phase. Therefore, the component
elutes in 7.5 seconds rather than 5 seconds. Assume that a second component also
emerges in 5 seconds when it travels through an empty column. However,
because of its different solubility or affinity, the second component spends 30%
of its time in the carrier gas and 70% of the time in the stationary phase. The
second component now emerges in 8.5 seconds when it travels through the
column. Therefore, the two components separate.
The Figure above shows; A) the initial mixture of three components, B)
separation of a components beginning to occur, C) Increasing separation of the
three components D) The first component (triangles) beginning to pass through
the detector.
As each component emerges from the column, a peak is drawn on the screen for
the detector response versus time plot.
18
How Separation Occurs
Chromatography is a separation method achieved by the

distribution of substances between two phases: a mobile phase and
a stationary phase.
Mobile Phase Stationary Phase

Gas Solid Chromatography (GSC) Gas Solid
Gas Liquid Chromatography (GLC) Gas Liquid
Figure 8
In gas chromatography there is a mobile phase, the carrier gas, and a stationary
phase, the column material. The stationary phase can be a solid material or a
liquid material (a very viscous liquid like a polymer).
19
Column Types
Open (Capillary)
Packed
Wall Coated
Open Tube
(WCOT)
Porous Layer Open Tube

Micro Packed (PLOT)
Micro
PLOT WCOT
Packed
Length 0.25 - 10 cm 4-8m 4 - 14 m
I.D. 0.5 mm 0.15 - 0.32 mm 0.1 - 0.32 mm
Figure 9
Traditional GC columns were metal or glass tubing packed with a solid material.
Micro GC’s are configured with capillary or open-tubular columns. Capillary
columns are made of fused silica glass in very narrow diameters with their inside
walls coated with a stationary phase of solid or liquid.
20
Gases and Plumbing
Gases and Plumbing
Carrier Gases
Gases must be: Using Compressed Gas Safely

– Inert
– Dry Obtain safety information from your
company's safety department or
– Pure
from your local gas supplier.
Helium is best for most applications.
10
Figure 10
The gases used should not be reactive with the sample components; therefore,
inert gases are used. Gas purity is an important consideration to avoid
background interference problems. The vendor for your gas cylinders or
compressors can provide the purity levels for the gas provided.
Safety considerations should be reviewed regularly and safety information can be

obtained from your supplier.
21
Gases and Plumbing
Tubing and Traps External to the GC
• GC grade copper or stainless steel tubing should be used

• Precondition the tubing with solvent flush and carrier
gas drying
• Filters need to be changed at the manufacturer's
recommended interval to prevent contamination
breakthrough (every 3 cylinders)
• All external fittings should be checked on a routine
basis for leaks (every 4 - 6 months)
11
Figure 11
Molecular Sieve traps are recommended for use on all gases. Additional traps
may also be required. Indicator traps for moisture are available. However, caution
should be used since today’s detectors are usually more sensitive to moisture
content than the color change of the indicator.
Plastic tubing should not be used, only copper or stainless steel. Prior to use, the
tubing should be flushed with a solvent like methanol and carrier gas dried.
Filters or traps should be changed regularly; a conservative recommendation is
every 3 cylinders (supply, not internal MicroGC cylinder).
Ambient temperature changes and vibration can cause fittings to leak over time
and thus should be leak checked regularly.
22
Gases and Plumbing
Gas Regulators and Flow Controllers
The carrier gas must be regulated to provide constant pressure as

well as a constant mass flow.
External Carrier Gas source:

Recommended Carrier Gas Line Pressure: 80 psi
Internal Carrier gas cylinder:
Maximum pressure: 1800 psig/12,405 KPa
Filling the P200 Internal Carrier Gas Cylinder Procedure:
P-Series Micro Gas Chromatograph User’s Manual pg. 22-25
12
Figure 12
Minimum line pressures should be used in order to insure accurate pressure and
flow control.
23
Gases and Plumbing
Sample Connections
• Internal Filters should be changed by

authorized personnel only
• External Sample Filter Kit (KIT-2052)
protects the internal filters
• Sample Flow Controller Module reduces
flow of high pressure samples
13
Figure 13
24
Micro GC Hardware
Micro GC Hardware
Micro GC System
14
Figure 14
The MicroGC system includes the GC, PC (desktop or laptop) and printer.
25
Micro GC Hardware
Micro GC Models
M - Series (64% of Users) P - Series (31% of Users)
Analyzers QUAD - Series
15
Figure 15
There are several MicroGC models available. For Information on the various
models, see the Agilent website: http://www.agilent.com
P-Series Micro GCs

The P Series micro GCs go where you need them to go when you need them to be
there. With their built-in refillable carrier gas cylinder and rechargeable battery
pack, the units are completely self-contained. Yet the unheated model weighs less
than 23 pounds and is smaller than a briefcase. Operating with a notebook
computer and Agilent's easy-to-use micro GC software, you have a complete
portable system.
You can configure the micro GCs with single or dual columns, and choose an
unheated or a heated model. The unheated model analyzes gases at ambient
temperature with boiling points up to 150° C, while the heated model analyzes
heated samples (to 110° C) with boiling points up to 220° C, plus samples
containing H2O vapor.
The P Series micro GCs are ideal for analyzing vent gas, aqueous and soil sample
headspace, landfill gas, furnace gas, and scrubber/charcoal bed efficiency as well
as performing leak detection, environmental screening, waste-water VOC
monitoring, and natural gas analysis.
26
Micro GC Hardware
Sampling
Unheated model: Analyze gas samples containing multiple compounds with
boiling points up to 150°C.
Heated model: Analyze gas samples containing multiple compounds with boiling
points up to 220°C.
Injection System
Silicon micro-machined injector
Manual or automatic injection
Internal sampling pump
Injection volumes: 4 µL fixed, 0.5 µL to 15 µL user-selectable
Input 1/16" bulkhead union with built-in 5-µm filter
Detector
Silicon micro machined thermal conductivity detector with 240 nL internal
volume
Minimum detectable quantity: 1 ppm for most compounds
Linear dynamic range: 105±5%, 106±10%
Repeatability: ±2% RSD at constant temperature and pressure
Column Heater Range

Unheated model: 30 °C to 180 °C isothermal operation
Heated model: 50 ºC to 180 ºC isothermal operation
Carrier Gas
Internal carrier gas supply: refillable 300 mL tank, 1800 psi certified for 40 hours
continuous operation.
External carrier gas supply: He, H2, N2, or Ar, 80 psi input to 1/8" Swagelok
fitting
Power
Unheated model: Internal 12 V rechargeable lead-acid battery or 12 VDC
6-8 hours/30 watts maximum.
Heated model: Internal 12 V rechargeable lead-acid battery or 12 VDC
4 hours/60 watts maximum.
External Inputs/Outputs
Analog output: 0 to ±1 VDC and 0 to ±10 VDC
27
Micro GC Hardware
GC ready out
GC start
External wait ready
External wait ready
RS-232 for instrument status, control and data
Environmental
Operating temperature range: 0 °C to 50 °C
Humidity range: 0 to 95%, non-condensing
Physical
Dimensions
Unheated model: 15 cm (6") x 36 cm (14") x 36 cm (14")
Heated model: 15 cm (6") x 36 cm (14") x 41 cm (16")
Weight
Unheated model: 10.4 kg (23 lb)
Heated model: 13.2 kg (29 lb)
Agilent M-Series Micro GCs

The M Series micro GCs can be configured with one or two independently
controlled modules, each containing an injector, analytical and reference columns,
column heater and universal micro solid-state detector. And you can control the
micro GC with a Windows-based software package with a full range of
chromatography processing and editing capabilities. So you can analyze a wide
range of compounds, confirm peak identifications and display your results in
seconds.
You can also choose from an unheated or a heated model. The unheated model
analyzes gases at ambient temperatures with boiling points up to 150° C, while
the heated model analyzes heated samples to 110 °C with boiling points up to 220
°C, plus samples containing H2O vapor.
Versatile
The M Series micro GCs are ideal for analyzing vent gas, aqueous and soil
sample headspace, landfill gas, natural gas and furnace gas, as well as performing
leak detection, environmental screening, storage tank analysis, well logging, and
waste-water VOC monitoring in the lab, field or on-line.
28
Micro GC Hardware
Front View - P200

Gas sample inlet
Power Carrier gas Serial Carrier

on/off gauge port on/off
16
Figure 16
Front panel
The front panel of the P200/P200H includes the following:
Carrier gas gauge

This gauge indicates the pressure in the P200/P200H internal carrier gas tank.
Power on/off
This button turns power on or off to the entire system including the detector
filaments. The green light on the button acts as an internal battery charge and
power cutoff circuitry indicator.
Caution! Do not power up the GC unless the carrier gas is on. The presence of air
inside the detector cell will cause a rapid rise in the filament temperature. This may result
in irreversible damage to the detector.
Serial port
The serial port of the front panel is the same as the serial port on the back panel of
the P200/ P200H. Two ports are available for convenience purposes. This serial
port is made through a female DB-9 connector, which conforms, to the RS-232
29
Micro GC Hardware
standard. Agilent has several types of cables available to correspond to different

PC connectors.
Serial Interface Cables

Signal name P200 pin # Cable CBL-1482 Cable CBL-
1010
from PC DB-9 male DB-25 female
DB-9 female
DCD 1–held true 8 1
RXD 2–TXD 3 2
TXD 3–RXD 2 3
DTR 4–ignored 20 4
SIG, Gnd 5– 7 5
DSR 6–held true 6 6
RTS 7– ignored 4 7
CTS 8– held 5 8
true
Gas sample inlet

The sample inlet, a 1/16 inch Swagelok® union containing a 10µ frit, is located in
the center of the upper edge on the P200H. The inlet on the unheated P200 is
located to the right of the front panel serial port. With either instrument, use a
compression fitting at this inlet to connect to a sample line. The inlet on the
P200H is heated electrically to 110ºC.
WARNING Contact with the gas sample inlet on the P200H after it has reached the set
temperature will cause burns.
Carrier on/off
This valve opens and closes the carrier flow from the internal tank to the system
at 80psi.
30
Micro GC Hardware
Back View - P200
Analog/control Sample Serial I/O Power

A&B Vent to GC 12 VDC
Cylinder
Fill Port
Carrier
Out
Col A Ref A Carrier In

Col A Ref A Col A
Vent Vent Col B
Pressure Vent Vent
Pressure
Controls
Controls
17
Figure 17
The back panel of the P200/P200H is split into two parts to correspond to two
separate compartments inside the unit.
Left back panel

The left back panel corresponds to the GC compartment that contains the GC
chassis, the two GC modules, the pneumatics and the controller board.
Power 12 VDC
A round black female connector allows you to plug the 12 VDC recharger to the
P200/P200H. If connecting to voltage greater than 115 volts, make sure the power
supply is for the correct line voltage. The 12 VDC power supply recharges the
sealed lead-acid battery inside the P200/P200H whenever the power switch is
turned off. For battery charging instruction, see Chapter 3 of the User’s Manual.
Whenever possible run your P200 with the 12 VDC power supply connected to
the power line. This prolongs the life of your internal battery and eliminates the
need to recharge it often. When the internal battery needs replacing, the
procedures, which should be followed, are covered in Chapter 7 of the User’s
Manual.
31
Micro GC Hardware
Serial I/O RS-232 connector

This connector enables control of the GC from a computer data system. Pin
assignments are the same as those described in Table 5 for the front connector.
Analog control (A & B)
The analog/control port enables the signal to be transmitted to data collecting or
instrument control devices. The analog connector provides pins that allow you to
control the Start function of the GC through analog signals. In addition, you can
take the analog output of channel A and B detectors to a third party data system.
Vents
The back panel of the P200 contains four color-coded vents for both column A
and column B (sample is red and reference is green) and a fifth sample vent
(white) coming from the sample pump. For protection and to avoid
contamination, the vents are closed using Luer-Lock plugs when the unit leaves
the factory.
WARNING The Luer-Lock plugs must be removed when the unit is operating. Save plugs
to use for long term storage.
Analog Control Pin Assignments

Pin number Description Pin number Description
1 Ready in 8 A-analog –10
volt
2 Start in 9 Digital
ground
3 Start out 10 Ready out 1
4 Start out 2 11 Ready out 2
5 B analog 1 12 Chassis
volt ground
6 B analog, 10 13 B analog
volt return
7 A analog, 1 14 Chassis
volt ground
15 A analog
return
Control A and B pressure controls
The two controls are used to set the column head pressure. This parameter setting
strongly influences the retention time and separation of the components being
analyzed. P200 instruments used for BTU analysis require the use of a flat blade
screwdriver to change the settings.
Caution Consult either the BTU or the EZChrom User’s guide for instructions on how to
set column head pressure.
32
Micro GC Hardware
Right panel
The right back panel corresponds to the compartment containing the internal
battery and the internal carrier gas cylinder.
Carrier gas jumper line

The jumper line brings the carrier gas from the internal gas cylinder (carrier out)
to the GC components (carrier in), injector, columns and detector of both
modules. If using an external carrier gas source, first turn off the internal carrier
gas main valve on the front panel, then disconnect the jumper at Carrier In and
connect the alternate carrier (regulated to 80 psi) to the inlet line.
Caution Make sure power is off before disconnecting the carrier gas jumper line.
Caution Your unit has been set for either hydrogen/helium or nitrogen/ argon as the
carrier gas. If argon or nitrogen is used, certain switch settings in the motherboard will
need to be changed to avoid damage to the detector filaments. See Chapter 6 of the
User’s Manual for instructions.
Auxiliary 12 VDC
The auxiliary 12 VDC allows you to run your P200/ P200H from any other 12
VDC power source such as a vehicle cigarette lighter plug.
1800 psi inlet

This inlet provided is used to recharge the P200/ P200H internal carrier cylinder.
Installations on how to perform these operations were covered in Chapter 2 of the
User’s Manual.
Carrier outlet
The carrier outlet on the right back panel connects a stainless steel jumper tube to
the carrier inlet on the back left panel. When the front panel carrier gas knob is
turned on, carrier gas is released through this outlet at 80 psi.
Carrier inlet
The carrier inlet on the left back panel connects to a stainless steel jumper tube to
the carrier outlet on the back right panel. When the front panel carrier gas knob is
turned on, carrier gas flows into the inlet at 80 psi.
33
Laboratory Exercises
Laboratory Exercises
Lab Exercises
• Lab 1-Hardware Familiarization and Set Up

• Lab 2- Filling the Internal Carrier Gas Cylinder
• Module Review
18
Figure 18
34
Lab 1: Hardware Familiarization and Set Up
Lab 1: Hardware Familiarization and Set Up

In this exercise you will:
• Identify the hardware components of the Micro GC system.
• Observe the front and back panels of the Micro GC.
• Connect the hardware components: GC, PC, and Printer.
Part 1: Identifying the Hardware

Referring to the notes in this module of the student manual identify the hardware
components that are available for use in this class.
Part 2: Observe the Panels of the GC

Referring to Chapter 3, Installation, of the P Series Micro Gas Chromatograph
User’s Manual, identify the features on the front and back panels.
Part 3: Connecting the Hardware Components

Using the cables available, connect the GC, PC, Printer, and power cords.
Do Not Power On the System at this Time!
35
Lab 2: Filling the Internal Carrier Gas Cylinder
Lab 2: Filling the Internal Carrier Gas Cylinder

• Fill the internal carrier gas cylinder of the Micro GC.
Filling the Carrier Gas Cylinder

Referring to Chapter 3, Installation, of the P Series Micro Gas Chromatograph
User’s Manual, pages 22-25, fill the internal carrier gas cylinder.
36
Module 2 Review
Module 2 Review
1) List the primary components necessary to operate the Micro GC system.
a)
b)
c)
d)
e)
f)
g)
h)
i)
j)
2) Where and how is the carrier gas attached to the GC?
3) Why should traps be used in the gas plumbing?
4) Carrier gas contamination will produce:

_______________________ ________________________
_______________________ ________________________
This will effect the instrument’s ______________________________.
37
Module 2 Review
5) What can be done to avoid carrier contamination?

a)
b)
|
c)
d)
6) Why is it important to turn on the carrier gas prior to powering on the GC?
7) The Regulator should be set at what pressure?
8) The pressure ranges of the GC can be found _________________.

The regulator pressure should always be set slightly higher
than_____________.
Over pressurizing the system can:
a)
b)
9) How long will the portable Micro GC operate using the internal carrier gas
cylinder?
10) How is power attached to the GC?
11) How is the computer attached to the GC?
38
Module 3: EzChrom Introduction

• The Compatibility of Windows
• How to Load EZ Chrom Software
• How to Load the GC Tools
• How to Verify Installation, Setup, and Status
• The Organization of the EZChrom Menus
Introduction to EZChrom
• Introduction to Windows
• Loading EZChrom Software
• Loading the GC Tools
• Verifying Installation, Setup, and Status
• Introduction to EZChrom Menu
Figure 19
The purpose of this module is to introduce the use of the EZChrom software.
40
Windows Compatibility
EZChrom Compatibility with Windows
EZChrom Windows Windows Windows For Windows Windows

Revision 3.0 3.1 WorkGroups 95 NT
3.1 X
3.3 X
3.5.8 X * X
4.x X * X
* EZChrom was created for the Win 3.1 platform and is compatible on the Win 95 platform, but not supported.
Figure 20
Various revisions of EZChrom have different compatibilities with the Windows

environment. This chart shows the relationships. Communication problems may
arise if one uses a combination that is not reflected on this chart.
Computer system requirements

12) Computer: Any Microsoft Windows 3.1 compatible system, minimum 20
MHz 386 processor.
13) System memory: Minimum 4 Mb of RAM.
14) Disk storage: 100 megabyte hard drive and 3.5 or 5.25 inch floppy drive
15) Ports: One free serial port (two serial ports if a serial mouse is used).
16) Operating System: MS-DOS ® version 5.0 or higher.
17) Video Monitor: Any Microsoft Windows 3.1, 100% compatible, including
EGA, VGA or SVGA.
18) Operating environment: Microsoft Windows Version 3.1.
41
19) Printer: Any Microsoft Windows 3.1, 100% compatible.
GC instrument requirements
Firmware version 17.4 or later.
42
Software Installation
Installing the Software
• Loading the EZChrom Software

– Procedure for installing the software:
– EZChrom Chromatography Data System
– User’s Manual, pages 8-13
• Loading the GC Tools

– Follow same procedure
Figure 21
The next few pages will show the screens encountered when loading the software.
43
Figure 22
Your GC is shipped with one diskette containing EZChrom 200/400. This

diskette contains the chromatography data system.
Installing EZChrom 200/400

• Make sure the computer is running Windows, and is at the Program Manager.
• Insert the EZChrom 200/400 diskette into the appropriate floppy drive.
• Click the left mouse button on File in the top menu bar; the File menu will
appear. Then click the left mouse button on Run.
• A command box will appear. In the command line:
• Type “a:\setup” if your installation disk is in drive A or “b:\setup” if your
installation is in drive B.
44
Figure 23
• The initializing window will appear. EZChrom 200/400 will automatically

load the software to C:\HP or C:\MTI if an older revision of software.
45
Creating a Shortcut in Windows 95
Figure 24
Program groups are automatically created in Win 3.1, Win forWG, and WinNT.
But icons must be created in Win95.
46
Creating a Shortcut in Windows 95
Figure 25
The shortcut can be dragged to the desktop.
47
Windows Explorer
Figure 26
This slide shows the path where the software modules are located.
48
MTI GC Setup
MTI GC Setup
MTI GC Setup
Figure 27
A second floppy disk containing the GC Setup software must also be loaded the
same way as the Operation software.
With the GC system hooked up and powered on, start the GC Setup program.
This will establish the communication between the GC and PC.
49
MTI GC Setup
MTI GC Setup
10
Figure 28
This slide shows the selection of the com port and the identification and
communication between the GC and PC.
50
MTI GC Verification
MTI GC Verification
MTI GC Verification
11
Figure 29
After loading software, it is good idea to run the GC Verification Tool.

Your AGILENT GC was shipped with an GC Tool diskette, which contains a
record of the proper instrument configuration (operational parameters) for your
particular GC and two GC Tools programs; GC Verification and GC Module
Change Tool.
GC Verification is automatically installed when you run SETUP.EXE from a GC
Tools diskette. At this time, the configuration record for your GC is also installed
in your PC. Since GC Verification relies upon the existence of the configuration
record, you should run SETUP.EXE on each computer that you will want to use
with a given GC.
You may install GC Verification on as many computers as you will use with your
AGILENT GC.
The GC Verification Tool is used to verify and/or restore your instrument
configuration record. You can use GC Verification at any time to verify that your
GC firmware is in proper working order, to restore its configuration parameters,
clear error conditions or recover a lost configuration record.
51
MTI GC Verification
You should run GC Verification whenever any of the following conditions

pertain:
• You have just unpacked a new chromatograph and want to verify that it is in
good condition.
• EZChrom, or other software, reports that the GC has an error condition.
• The main controller board is changed.
• The EPROM (U32) is changed.
• The GC configuration record is changed.
• The GC battery-backed RAM is zeroed or otherwise compromised.
GC Verification requires no specialized knowledge of a GC beyond its serial
number. It will “walk you through” whatever procedures you can perform to
establish and/or restore a proper configuration.
GC Verification only verifies that the embedded computer system firmware in
the GC is OK. It does not check the columns, or other chromatography apparatus,
nor does it perform any special hardware checks.
To start GC Verification, double-click upon the GC Verification icon (the one
with a green check mark on it) in the HP Program Group Window.
52
MTI GC Verification
MTI GC Verification
12
Figure 30
The first window you will see is the Introduction Window. In general, the GC
Verification windows will have three text items:
Explanation
A short explanation of the purpose or use of a particular window.
Request
If you are expected to do anything in particular, the Request item tells you
what the program wants you to do.
Question
If GC Verification needs any information from you, a Question item will pose
a question, which you answer by clicking a button in the window.
This window asks you to verify that anAgilentGC is connected to your computer.
Click [Yes] when you have connected your GC to the serial port of your
computer and are ready to proceed. If you click [Quit], GC Verification will
terminate. If you click [No], GC Verification Tool will tell you that it cannot
proceed without a GC.
53
MTI GC Verification
MTI GC Verification
13
Figure 31
Typical sessions
In general, there are two types of sessions you will encounter when you are using
GC Verification. If your GC is OK, there is a simple sequence of windows, which
will be displayed as the condition of the GC is verified. If there is a problem, there
are a large number of possible window display sequences, depending on the type
of problem, which has occurred.
What happens if your GC is OK?
Connect your GC and click [Yes]. GC Verification checks each serial port on
your computer system for an M200. During this time a window is displayed. If
anAgilentGC is found, the window displays its serial number in the Status box
and, when you click [OK], GC Verification proceeds with checking the GC.
In the figure above, the “180505” represents the serial number of the GC. Your
Status box should display the serial number of your particular GC.
If your GC is OK, the final window is shown indicating successful verification.
See the User’s Manual for the EZChrom for further explanations if your GC has problems
(pages 139-158).
54
Data File Path
Data File Path
Data File Path
14
Figure 32
In Explorer or File Manager, one can review the path for storage of data and
methods.
55
Initiating EZChrom
Initiating EZChrom
Initiate EZChrom
15
Figure 33
In the Windows Program Manager or from the Desktop in Windows95…

• Locate the EZChrom 200/400 icon in the HP group window. Double-click on
the EZChrom 200/400 icon.
• When EZChrom 200/400 begins, a confirmation “window” will appear. Press
<Enter> or use your mouse to click on [OK].
56
Initiating EZChrom
Initiate EZChrom
Example.1 data file

Example.met method file
is automatically
loaded.
16
Figure 34
EZChrom 200/400 will then proceed to open and draw the windows, which
comprise the data system. Two display windows (four display windows, one each
for Channels A, B, C, D will appear with EZChrom 400) will appear in EZChrom
200 (i.e., one each for Channels A and B).
At this time, a default method and data file named after your instrument serial
number will be recalled and displayed. When you access the window represented
in the Figure above, the method and file names will be replaced by the serial
number of your particular instrument (i.e., the method EXAMPLE.MET will read
XXXXX.MET and the file name EXAMPLE.1 will read XXXXX.1, where
XXXXX represents the serial number for your instrument).
57
Initiating EZChrom
Initiate EZChrom
In Win95 Must move menu bar and can size and position windows.
17
Figure 35
If using Windows95, one must manually resize and position the windows.
58
Instrument Menu
Instrument Menu
Instrument Menu
18
Figure 36
The instrument status can be determined by selecting the Instrument menu item
and then selecting Status. Parameters cannot be changed in this screen.
59
Method and Data Menus
19
Figure 37
The Method menu allows one to choose instrument and method parameters. We
will explore these options in detail in a later module.
60
Math Menu
Math Menu
Math Menu
20
Figure 38
Purpose
Subtracts a user-selected chromatogram from the currently displayed
chromatogram. After analyzing, the reports and graphical display are updated.
Syntax
• Select Math or type <Alt> T.
• Select Catalog, or enter a path and file name to select a chromatogram. This
chromatogram will be subtracted from the currently displayed data set.
• Select [OK] to initiate the subtraction.
Comments
This feature could allow subtraction of large solvent peaks allowing easy
identification and integration of low level, overlapping peaks.
61
Calib and Help
Calib and Help
Calib and Help
21
Figure 39
Purpose
Sets up EZChrom for a two channel calibration. It also provides the capability of
selecting a calibration level (from 1-8) for users who desire a multilevel
calibration.
Syntax
• Select Calib or type <Alt> C
• Enter a number between 1 and 8 to select a calibration level.
• Select [OK]. To stop a calibration prior to analysis, select [Cancel]
• Select Analyze. This will take the calculated peak areas and assign them to the
appropriate peak name and amount value.
62
Calib and Help
Comments
Calibration does not begin until data is actually collected or stored data is
analyzed. Level 1 is all that is required for normal use. Higher levels are used to
construct linear or nonlinear (point-to-point) calibration plots.
Help
Displays a screen showing the current version of EZChrom.
We will explore the calibration options in a later module.
63
Lab Exercises
Lab Exercises
Lab Exercises
• Lab Exercise 1: Starting up the System

– Loading EZChrom Software and GC Tools
– Verifying Installation
– GC Setup
– GC Status
– GC Verification Tool
• Lab Exercise 2: Introduction to WinNT
• Lab Exercise 3: Working with Win NT
• Lab Exercise 4: Introduction to Windows 95
• Lab Exercise 5: Working with Windows 95
• Module review
22
Figure 40
64
Lab Exercise 1: Starting Up the System

• Power-on the GC and PC system.
• Load the EZChrom Software and GC Tools Disk
• Verify the Installation using
o GC Setup
o GC Status
o GC Verification Tool
Part 1: Turning On the PC

1) Ask your Instructor how to turn on the model PC you are using. If the PC is
already on, ask your Instructor how to properly shut down the PC.
2) Turn on the PC and you should see a Windows session initiate. Observe the
boot up process of the PC.
3) The PC desktop appears and depending upon which Windows operating
system is used and how the desktop was saved, there may be some
variations.
Part 2: Loading the EZChrom Software

4) Follow the software installation procedures in the EZChrom
Chromatography Data System User’s Manual pages 8-11.
Note: Verify with your instructor as to where (the file path) the software should be
installed. Some PC’s may have dual operating systems; i.e. Windows for Workgroups
and Windows 95.
5) Repeat the procedure for loading the GC Tools Disk. Verify that the serial
number on the disk matches the serial number of the GC.
6) If working in Windows95, the procedure for creating desktop shortcuts can
be found in Lab Exercise 4.
Part 3: Turning on the GC

7) Verify that carrier gas is flowing through your GC. Ask your instructor if
you have any concerns.
8) Power on the GC.
65
Part 4: Running GC Setup

9) Launch the GC Setup program from the MTI or HP program group.
If an icon is not available, see your instructor. For example, if the PC was set
up with a dual operating system and you installed the software in a path other
than the default C:\HP or MTI, you may have to:
o Restart Computer into MS-DOS
o At C: Type “CD:\WFW311”
o At Prompt type “Win”
o Open EZChrom
10) Verify the instrument configuration.
Part 5: Launching the EZChrom Software

11) Select the EZChrom icon to start the software. See the comment above if the
icon is not present.
12) A default method is loaded. Select the Instrument menu item, and then
select Status to verify the instrument set points and status.
13) Verify the following:
o Each column has flow
o The temperature of the columns and detectors are not too high
o The detectors are on
o The detectors are stabilizing
o The inlet heaters are on
14) After reviewing the instrument parameters, close the EZChrom software.
Part 6: Using the GC Verification Tool

Referring to the EZChrom Chromatography Data System User’s Manual pages
132-158, perform the performance verification by using the GC Verification Tool.
If the system has problems, let your instructor know.
66
Lab Exercise 2: Introduction to Windows NT

In this exercise, you will:
• Initiate a Windows NT session.
• Identify components of a Windows session.
• Use a few of the Windows NT more common features.

1) Ask your Instructor how to turn on the model PC you are using.
2) Turn on the PC and you should see a Windows NT session initiate. Observe
the boot up process of the PC.
3) You are prompted to press the “Control, Alt, and Delete” keys on the
keyboard. You are then prompted to enter a password. On new computers a
label with the administrator’s password is on the CPU case. For example,
“3000hanover” is used as the factory default password. If this password has
been changed, the instructor will advise you as to the password to be used.
4) Windows NT is a secure operating system that requires the use of a
password at logon. Lab Exercise 4 will demonstrate how the password can
be changed.
5) The PC Desktop appears, and depending upon how the desktop was saved,
there may be some variations. You should see a Start button in the bottom
left corner of the screen. Additional icons are displayed on the desktop.
Part 2: Working with Windows NT

6) Use the mouse to point and click on the Start button. The folders associated
with Start are now on the screen. The next Figure shows an example of the
folders associated with Start.
67
7) Select the Programs folder from Start. Point and click on the Windows Help
icon. The Figure below shows the Contents tab. If you are unfamiliar with
Windows NT, examine the contents of the Help topics.
8) When you have examined the various Help topics, close out the window by
clicking on the “X” icon in the top right corner of the Help window.
9) Select the Start icon, then the Programs folder. Select Windows NT
Explorer. The Figure below shows an example of the Explorer program.
68
10) Note the directory structure of the hard drive. In the upper right hand corner
of the screen, there are three icons. Point to and click the window shaped
icon in the center.
What happened?
What's the function of the other two icons?
11) Re-start Explorer. Verify that the tool bar appears as shown in the Figure
above. If it does not, select “View”, “Toolbar” and it should appear. Do not
“click”, but place the cursor on the bottom right corner of the “down arrow”
in box that appears in the small window under the menu items. Text should
appear which identifies the function of that arrow. See Figure 2.4 for an
example. Continue to place the cursor at the bottom right of each of the
icons and observe the definition of the function of each icon.
69
Part 3: File Management in Explorer

Directory
A directory is a group of related files. The root directory is where the primary
applications are located.
12) If the C: drive is not already expanded to show all the subdirectories, point
and double click on the C: icon. Note the contents in the right window and
scroll though the files listed. Note the folders and files listed.
13) Point and Click on a folder to examine its contents.
Change Directory
Changing directories is a way of navigating through your computer’s files.
14) Scroll down and Point and Double-click on the Programs sub-directory.
Then select the Windows NT sub-directory.
15) Note the files and folders. Click on the “-“ box next to the open Windows
NT folder in the directory tree.
What happened?
MTI Directory
16) Scroll down to the MTI subdirectory and Double-click on it to open the
folder. Note the default subdirectories.
70
Backing up Files
It is important to regularly backup your important files. We will use a floppy disk
for backup, however there are several other alternatives.
17) Insert a blank floppy into the A: drive. In Explorer, scroll up to the 3 1/2
Floppy (A:) icon in the directory tree and click on it. If the floppy is not
formatted, you will be prompted to format the disk. Follow the prompts for
a Full format.
18) Creating a Folder – To create a new folder on the drive, Point and Click on
the File menu. Select New, then Folder. Type “Data Files” as the name of
the folder. Open the A: drive folder in the left window so that the “Data
files” folder is visible in the directory tree.
19) Copying files – Click on the View menu item in Explorer and verify that the
option “Details” is selected. Copy any file. Point and click on one of the
files. Press and hold the Ctrl key on the keyboard while pointing and
clicking on a second file. If all went well, both files would appear
highlighted in reverse video. Scroll up the left window until the A: drive
icon is visible. With both files highlighted, hold down the left mouse button
while clicking on one of the highlighted files and drag them to the “Data
Files” folder on the A: drive. Release the mouse button, and this should
copy the files to the A: Floppy.
20) Verify that these files were copied by selecting the A: floppy icon and
viewing its contents.
71
Lab Exercise 3: Working with Windows NT

• Learn how to organize and customize your desktop.
• Learn how to Change the Logon Password.
• Learn how to Configure Printers.
• Learn about Windows NT routine maintenance procedures.
Part 1: Organizing and Customizing the Desktop

Arranging the Icons
You should have the following icons displayed on the desktop:
o My Computer
o Network Neighborhood
o Recycle Bin Inbox
o The Internet
o The Microsoft Network
o My Briefcase
1) To arrange the icons on the desktop, simply click on and drag the icon to the
desired location on the desktop. Position the cursor anywhere on the desktop
that does not have an icon. Click the right mouse button. Select Arrange
Icons, then by Name.
What happened?
2) Position the cursor anywhere on the desktop that does not have an icon.
Click the right mouse button. Select Arrange Icons, then Auto Arrange.
Again, try to spread your work around the desktop.
What happened?
3) De-select the Auto Arrange feature.
Modify Display Properties

Click the right mouse button. Select Properties. You can customize your
desktop and window features including screen savers. The next figure shows
the Display Properties Screen.
Note: Do not use any screen savers other than the standard Windows NT options. Other
screen saver programs can utilize system resources and could crash
yourAgilentChemStation.
72
Using Shortcuts
5) To launch an application represented by an icon on the desktop, simply
double-click on it. Select the Recycle Bin icon and double-click on it. If
there are contents in the list, select File, and Empty Recycle Bin. When a
file is deleted it is not removed from the disk drive to free up space until the
Recycle Bin is emptied.
6) Right click on the Start button on the bottom left corner of the screen.
Notice that a short menu appears and one can start Explorer by selecting
Explore.
7) If you are not sure where a file is located you may search for it in Explorer
or you may right click on the Start button and select Find. Type
"Config.sys" in the Named: field. Select C: in the Look in: field. Click
Find Now or press Enter. The file location is indicated. To close the Find
window, click on the X icon located in the upper right hand corner.
Add a program to the Start or Programs menu

8) Click Start, and then point to Settings.
9) Click Taskbar, and then click the Start Menu Programs tab.
73
10) Click Add, and then click Browse.

11) Locate Explorer in WinNT in the C: drive, and then double-click it.
12) Click Next, and then double-click the Start menu.
13) Type the name that you want to see on the menu, and then click Finish. (If
Windows NT prompts you to choose an icon, click one, and then click
Finish).
14) Click on Start button and note Explorer listed at the top of the menu.
Tip
15) You can also add a program to the top of the Start menu by dragging the
program's icon to the Start button. Locate “Notepad” in WinNT.
16) Click and drag it down to the Start button at the bottom left of the screen.
Close out the open windows and click on the Start button to see Notepad
listed in the menu.
Creating Shortcuts
To put a shortcut on the desktop
17) Now go back to Explorer. Open Windows NT, then Accessories, then and
Pinball. Locate the file name “Pinball” with the file type “Application”.
Click on the file name and drag it to the desktop. (If your desktop is not
visible because Explorer is the full size of the screen, select the multiple
window icon in the top right corner of the screen.). An icon shortcut should
be created.
18) Double-click on the icon to start the game.
19) Now go back to Explorer. Select “Tools”, “Find”. Search for the Start
Menu in the WinNT directory. Locate the folder for MTI.
20) Select one of the programs in the right window. Right click on it and select
Create Shortcut. A second short cut is created. Click on it and drag it to the
desktop (If your desktop is not visible because Explorer is the full size of the
screen, select the multiple window icon in the top right corner of the screen.)
Keyboard Shortcuts
Menu items can be selected using keyboard operations rather than the mouse.
21) With Explorer open, Hold down the Alt key and press the “f” key on the
keyboard. Note that the File menu items appear. Menu items can be
selected and activated by typing the underlined character present in the menu
item name. If the menu is activated unintentionally with Alt, pressing Alt a
second time can turn it off again just.
22) Now select Alt “e” and note that the Edit Menu items appear. Using the
control key (Ctl) activates additional keyboard shortcuts. These are shown
74
next to the menu items: Ctl+X will activate the Cut feature, Ctl+C will
activate the Copy feature, etc.
Managing Multiple Windows

23) Start the following programs: Windows Explorer, Calculator, and
WordPad (Calculator and WordPad is in the Accessories folder).
24) To activate any of the three panels, click the mouse anywhere in the visible
portion of the window. Notice what happens to the title bars as you do this.
The "active" window will always have a unique title bar. Notice the Taskbar
at the bottom of the desktop.
25) When you maximize a window, you may cover other windows. An
important keyboard shortcut for manipulating windows is Alt-Esc (the Alt
and Esc keys pressed simultaneously), which changes the active window.
Try Alt-Esc to activate each of the windows on the screen, and notice that
this operation will reveal any windows hidden underneath other windows.
26) An alternate way to activate a window is Alt-Tab, which toggles among the
windows that are activated. Try Alt-Tab and notice the difference between
this and Alt-Esc.
27) Close all the opened applications.
Part 2: Changing the Logon Password

28) Select the Start button and the Help icon.
29) In the Index, type passwords and select Display.
30) Select Changing your Password, the Display.
31) With the Help window still open, follow the directions. Change the
password to “hp”. Note that the password is case sensitive.
Caution: Make sure that you document the new password.
75
Part 3: Configuring Printers

Configuring Printers
Printers are identified by the presence of "driver" files, commonly having the
.DRV extension. The drivers for printers (and plotters, if any) are generally
loaded during the software installation. If a new printer/plotter is to be added to
the system after software has been installed, the printer driver may be required to
be loaded from Windows 95 or from the device driver the diskette for the Printer.
The Control Panel can be used to select printers to be used by the ChemStation
or the Printer folder may be used.
32) Click Start, Settings, then and Printers. Select the Add Printer icon from
the choices.
33) The print wizard will guide you through the installation. If you want this to
be your default printer, select File then Set As Default.
Part 4. Windows NT Routine Maintenance

Backing up Files
In Lab 2, files were backed up onto a floppy disk. A routine procedure for
backing up files on floppy, tape, zip or jazz disk, server, etc. should be performed.
Individual lab resources and protocol will dictate what backup procedures should
occur. The critical ChemStation files that should be routinely backed up are the
data files, method files, sequence files, and macros. One should also backup paper
printouts of all methods and sequences.
Deleting Temp files

Temporary files can accumulate over time and affect the performance of the PC.
Occasionally, temporary files accumulate in the directory specified by the TEMP
environment variable. These files are generally left open when Windows is
abnormally terminated, for example, by powering your computer down without
closing Windows first. The temporary files are named ~XXXXXXX.TMP, where
XXXXXXX are characters and numbers produced by the program that created the
temporary file. To recover the temporary space, you should delete these files after
closing all currently running applications.
34) Open Explorer. In the C: directory tree, Scroll down to the Temp directory
and open it. Delete any files that are there (You may not be able to delete all
of the files if some of them are currently in use by Windows or a Windows
application).
Maintaining Windows NT File Systems

CHKDSK can be used for scanning and repairing FAT and NTFS volumes.
76
Never use Scandisk.exe or Defrag.exe on a WinNT 4.0 NTFS partition. If this is done,
one will have to re-format the hard drive and re-load WinNT.
Virus Scanning
McAfee virus scanner is provided in ChemStation bundles. Many different
utilities are available for virus scanning. You should run a disk scanning utility if
you download programs from the Internet or exchange programs through e-mail
or flexible disks.
The programs must be updated regularly to protect your system. McAfee provides
an update monthly on its web site.
77
Optional Lab Exercise 4: Intro to Windows 95

• Initiate a Windows 95 session.
• Identify components of a Windows session.
• Use a few of the Windows 95 more common features.

1) Ask your Instructor how to turn on the model PC you are using. If the PC is
already on, ask your Instructor how to properly shut down the PC.
2) Turn on the PC and you should see a Windows 95 session initiate. Observe
the boot up process of the PC.
3) The PC desktop appears and depending upon how the desktop was saved,
there may be some variations. You should see a Start button in the bottom
left corner of the screen. Additional icons are displayed on the desktop.
Part 2: Working with Windows 95

4) Use the mouse to point and click on the Start button.
The folders associated with Start are now on the screen. The next Figure shows
an example of the folders associated with Start.
78
5) Select the Programs folder from Start. Point and click on the Windows Help
icon.
The Figure below shows the Contents tab. If you are unfamiliar with Windows
95, examine the contents of the Help topics.
6) When you have examined the various Help topics, close out the window by
clicking on the “X” icon in the top right corner of the Help window.
7) Select the Start icon, then the Programs folder. Select Windows Explorer.
The Figure below shows an example of the Explorer program.
79
8) In the upper right hand corner of the screen, there are three icons. Point to
and click the window shaped icon in the center. What happened? What's
the function of the other two icons?
9) Re-start Explorer. Verify that the tool bar appears as shown in the next
Figure. If it does not, select “View”, “Toolbar” and it should appear. Do not
“click”, but place the cursor on the “down arrow” in box that appears in the
small window under the menu items. Text should appear which identifies the
function of that arrow. Continue to place the cursor over each of the icons
and observe the definition of the function of each icon.
Part 3: File Management in Explorer

Directory
A directory is a group of related files. The root directory is where the primary
applications are located.
10) If the C: drive is not already expanded to show all the subdirectories, point
and double click on the C: icon. Note the contents in the right window and
scroll though the files listed. Note the folders and files listed. Point and Click
on a folder to examine its contents.
What does the .exe extension on some files mean?
80
Change Directory
Changing directories is a way of navigating through your computer’s files.
11) Scroll down and Point and Double-click on the Windows sub-directory.
Note the files and folders. Click on the “-“ box next to the open Windows
folder in the directory tree.
What happened?
12) MTI - Scroll to the MTI subdirectory. Double-click on it to open the folder.
Note the default subdirectories under MTI.
Backing up Files
It is important to regularly backup your important files. We will use a floppy disk
for backup, however there are several other alternatives.
13) Insert a blank floppy into the A: drive. In Explorer, scroll up to the 3 1/2
Floppy (A:) icon in the directory tree and click on it. If the floppy is not
formatted, you will be prompted to format the disk. Follow the prompts for
a Full format.
14) Creating a Folder – To create a new folder on the drive, Point and Click on
the File menu. Select New, then Folder. Type “System Files” as the name
of the folder. Open the A: drive folder in the left window so that the “System
files” folder is visible in the directory tree.
15) Copying files – Click on the View menu item in Explorer and verify that the
option “Details” is selected. Point and double click on the C: drive icon.
Scroll down the directory in the right window and locate the file
AUTOEXEC.bat (MS DOS Batch File). Point and click on this file.
Scroll down and locate the file CONFIG.SYS. Press and hold the Ctrl key
on the keyboard while pointing and clicking on this file. If all went well,
both files would appear highlighted in reverse video. Scroll up the left
window until the A: drive icon is visible. With both files highlighted, hold
down the left mouse button while clicking on one of the highlighted files and
drag them to the “System Files” folder on the A: drive. Release the mouse
button, and this should copy the files to the A: Floppy.
16) Select the Windows folder in the C: directory tree, locate the Win.ini file in
the right window list. Copy it onto the A: floppy in the “System Files”
folder.
81
17) The three files that were copied are important to have backed. In the event of
an operational problem with your PC, these files may be useful in restoring
its operation. Verify that these files were copied by selecting the A: floppy
icon and viewing its contents.
Part 4: Viewing the Contents of a File.

Opening a File
18) Select the Windows sub-directory again, locate the Win.ini file and double-
click on it. It should have opened up the Word or Note Pad application and
listed the contents of the “Win.ini” file.
19) In Word or Note Pad, click on the File menu, and then select Open. In the
Look in: field, Locate and Select C: by clicking on the arrow. In the
Filename: field Type AUTOEXEC.BAT. Then select Open, You should
now be viewing the contents of this file.
Printing a File
20) In the File menu, select Print to get a hardcopy of the file.
82
Lab Exercise 5: Working with Windows 95

• Learn how to organize and customize your desktop.
• Learn how to Configure Printers.
• Learn about Windows 95 routine maintenance procedures.
Part 1: Organizing and Customizing the Desktop

Arranging the Icons
You should have the following icons displayed on the desktop:
o My Computer
o Network Neighborhood
o The Microsoft Network
o The Internet
o Recycle Bin
o Inbox
o My Briefcase
1) To arrange the icons on the desktop, simply click on and drag the icon to the
desired location on the desktop.
Click the right mouse button. Select Arrange Icons, then by Name.
What happened?
Click the right mouse button. Select Arrange Icons, then Auto Arrange.
Again, try to spread your work around the desktop.
What happened?
4) De-select the Auto Arrange feature.
Modify Display Properties

Click the right mouse button. Select Properties.
You can customize your desktop and window features including screen savers.
The next figure shows the Display Properties Screen.
Note: Do not use any screen savers other than the standard Windows 95 options. Other
screen saver programs can utilize system resources and could crash yourChemStation.
83
Using Shortcuts
To launch an application represented by an icon on the desktop, simply double-
click on it.
6) Select the Recycle Bin icon and double-click on it. If there are contents in
the list, select File, and Empty Recycle Bin. When a file is deleted it is not
removed from the disk drive to free up space until the Recycle Bin is
emptied.
7) Right click on the Start button on the bottom left corner of the screen.
Notice that a short menu appears and one can start Explorer by selecting
Explore.
8) If you are not sure where a file is located you may search for it in Explorer
or you may right click on the Start button and select Find. Type
"Config.sys" in the Named: field. Select C: in the Look in: field. Click
Find Now or press Enter. The file location is indicated. To close the Find
window, click on the X icon located in the upper right hand corner.
84
Creating Shortcuts
9) To create a shortcut to an application Launch Explorer. Go to the Windows
folder and find the Start Menu subdirectory. Open the Programs folder and
locate the Explorer program. Click on the Explorer item and drag it to the
Start Menu folder in the directory tree.
10) Now left click on the Start button and note where the Explorer short cut
appears. Double-click on the shortcut and note that a second Explorer is
launched. Close out that program.
11) Now go back to Explorer, Programs, and Start Menu. Locate the folder
for MTI EZChrom. Select EZChrom 200 in the right window. Right click
on EZChrom200 and select Create Shortcut. A second short cut is created.
Click on it and drag it to the desktop (If your desktop is not visible because
Explorer is the full size of the screen, select the multiple window icon in the
top right corner of the screen.)
Keyboard Shortcuts
12) Menu items can be selected using keyboard operations rather than the
mouse. With Explorer open, Hold down the Alt key and press the “f” key
on the keyboard. Note that the File menu items appear. Menu items can be
selected and activated by typing the underlined character present in the menu
item name. If the menu is activated unintentionally with Alt, pressing Alt a
second time can turn it off again just.
13) Now select Alt “e” and note that the Edit Menu items appear. Using the
control key (Ctl) activates additional keyboard shortcuts. These are shown
next to the menu items: Ctl+X will activate the Cut feature; Ctl+C will
activate the Copy feature, etc.
Managing Multiple Windows

14) Start the following programs: Windows Explorer, Calculator, and
WordPad (Calculator and WordPad are in the Accessories folder).
15) To activate any of the three panels, click the mouse anywhere in the visible
portion of the window. Notice what happens to the title bars as you do this.
The "active" window will always have a unique title bar. Notice the Taskbar
at the bottom of the desktop.
16) When you maximize a window, you may cover other windows. An
important keyboard shortcut for manipulating windows is Alt-Esc (the Alt
and Esc keys pressed simultaneously), which changes the active window.
Try Alt-Esc to activate each of the windows on the screen, and notice that
this operation will reveal any windows hidden underneath other windows.
85
17) An alternate way to activate a window is Alt-Tab, which toggles among the
windows that are activated. Try Alt-Tab and notice the difference between
this and Alt-Esc.
18) Close all the opened applications.
Part 2: Configuring Printers

Configuring Printers
Printers are identified by the presence of "driver" files, commonly having the
.DRV extension. The drivers for printers (and plotters, if any) are generally
loaded during the software installation. If a new printer/plotter is to be added to
the system after software has been installed, the printer driver may be required to
be loaded from Windows 95 or from the device driver the diskette for the Printer.
19) The Control Panel can be used to select printers to be used by the
ChemStation or the Printer folder may be used. Click Start, Settings, then
and Printers. Select the Add Printer icon from the choices. The print
wizard will guide you through the installation. If you want this to be your
default printer, select File then Set As Default.
Part 3. Windows 95 Routine Maintenance

Backing up Files
In Lab 1, files were backed up onto a floppy disk. A routine procedure for
backing up files on floppy, tape, zip or jazz disk, server, etc. should be performed.
Individual lab resources and protocol will dictate what backup procedures should
occur. The critical ChemStation files that should be routinely backed up are the
data files, method files, sequence files, and macros. One should also backup paper
printouts of all methods and sequences.
Deleting Temp files

Temporary files can accumulate over time and affect the performance of the PC.
Occasionally, temporary files accumulate in the directory specified by the TEMP
environment variable. These files are generally left open when Windows is
abnormally terminated, for example, by powering your computer down without
closing Windows first. The temporary files are named ~XXXXXXX.TMP, where
XXXXXXX are characters and numbers produced by the program that created the
temporary file. To recover the temporary space, you should delete these files
after closing all currently running applications.
20) Open Explorer. In the C: directory tree, Scroll down to the Temp directory
and open it. Delete any files that are there. Go to the Windows directory
and open the Temp folder. Delete any files that are there (You may not be
able to delete all of the files if some of them are currently in use by
Windows).
86
DEFRAG
Over time, as programs read from and write to a hard disk, information stored on
the disk can become fragmented – that is, files are stored in noncontiguous
sectors. Fragmentation does not affect the validity of the information – the files
are still complete when they are opened. But it takes much longer for the
computer to read and write fragmented files than it does for unfragmented files.
Never run a defragmentation while an application is open. Never interrupt a
defragmentation in progress.
21) Click the Start button, click Run, then type defrag. If you have difficulty
finding the defrag program, select right click on Start, then Find, and type in
defrag. When the file is found simply double click on the defrag.exe file to
start the program.
22) In the Select Drive dialog box, specify C: and then click OK. The Disk
Defragmenter displays a dialog box telling you whether defragmentation is
recommended for this disk or not. If this disk has low fragmentation, the
Disk Defragmenter will not recommend defragmentation.
23) Showing details while the Disk Defragmenter is running causes it to take
longer than it does when showing only summary information or running it
minimized. For quickest performance, minimize the Disk Fragmenter
window while the utility is running.
To see defragmentation information for a particular drive:
24) In My Computer, right click the drive’s icon (C:), and then click Properties
25) Click the Tools tab. The Tools properties dialog box shows the number of
days since the last complete defragmentation process ran on the drive. You
can also run Disk Defragmenter from this dialog box.
87
ScanDisk
SCANDISK can be used to correct errors in the file system by searching for lost
file fragments and allow re-allocation of fragments to the file system. ScanDisk is
a full-featured disk analysis and repair program. ScanDisk runs automatically
when you start Windows 95 Setup.
ScanDisk checks and fixes problems in the following areas on hard disk drives,
floppy disk drives, RAM drives, and memory cards.
• File Allocation Table (FAT)
• Long filenames
• File system structure (lost clusters, cross-linked files)
• Directory tree structure
• Physical surface of the drive (bad sectors)
To run ScanDisk click Start button, then Run, and type scandisk.
88
Many different utilities are available for virus scanning. You should run a disk
scanning utility if you download programs from the Internet or exchange
programs through e-mail or flexible disks.
89
Module 3 Review
Module 3 Review
1) When is it safe to turn on the GC?
a)
b)
c)
2) What Indicates that the GC and the Computer are communicating?
3) If the computer locks up at boot-up, what may be the cause?
4) What should be checked if there is no communication between the GC and

PC?
a)
b)
c)
d)
5) How does one determine the compatibility of the operating system and the
revision of software?
6) What should be checked once everything is running?

a)
b)
c)
d)
e)
90
Module 3 Review
7) Why is it important to know the path for data and method storage on the
hard drive?
91
Module 3 Review
92

• How to build a method for an Analysis
• How to collect data
• How to work with graphics functions
• How to optimize the integration
Data Acquisition and Analysis
• Building a method for an Analysis

• Collecting Data
• Optimizing the Integration
Figure 41
The purpose of this module is to demonstrate the steps in developing a method.
94
Data Acquisition Process
Setup Acquisition
Parameters
Integration
Optimization
Calibration Setup
Reporting Options
Figure 42
We will first look at the steps in the Data Acquisition process.
95
Steps In Performing An Analysis
• Open up a method
• Edit method to fit project needs
• Download the method to the GC
• Setup the run file pathways
• Run blanks to check baseline
• Analyze the Sample
Figure 43
These are the overall steps one performs in setting up a method.
96
Set Up A Directory For Saving Data
• Use File Manager or Explorer, create a subdirectory for storing

data files
• When Saving Data Files, select “Data”, “Save As”
• Type in the appropriate path (i.e. c:\data\Aug_27\Junk)
Figure 44
It is important to keep track of where the data is being stored.
97
What Are The Sampling Mechanisms?
• Direct sample stream

• Summa or Silco canister
• Tedlar Bag
• Syringe
Figure 45
There are several alternatives for collecting and injecting the gas sample into the
GC.
98
How do I know the GC is running a sample?
• The sample pump runs

• The run time displays
• The new chromatogram is processed and drawn to the screen
Figure 46
When starting a run, one should hear the sample pump, see the run time displayed
on the PC and see the chromatogram being drawn.
99
Creating a Method
Creating a Method
Sample Session for an Analysis
The following slides will review the major steps taken when
creating a method.
For Detailed Procedures see the EZChrom Chromatography Data System

User’s Manual Pages 30-41.
Figure 47
In the following slides, we will identify the specific steps in creating a method
using the EZChrom software.
100
Creating a Method
Create a New Method Nam

The default Example.met will be modified.
Select New Method Save Method with new name.
Note method name in title bar.
Figure 48
When starting the software for the first time, the Example.Met is loaded. One
should modify the parameters of this method and save the method with a new
name.
Prior to making any modifications to the method, select the Method menu, Save
Method As, and give the method a new name.
101
Creating a Method
Select Instrument Setup
Instrument settings from last stored method are displayed.

For definitions of the parameters, see pages 32 & 33 of User Manual.
Figure 49
The instrument parameters are changed in the Instrument Setup screens.

Note that there is a separate screen for each Channel available.
102
Creating a Method
Edit the Instrument Setup Parameters
Note: There are some operational considerations when using Backflush modules.
10
Figure 50
Edit the individual parameters as needed for each Channel.

After completing all of the changes, Remember to Save the Method.
Note for Backflush Units
Carrier gas pressure surges greater than 1.4 psig/sec may damage the analytical
columns.
It is critical in BFMs to set the column head pressure
knobs to deliver zero psig before startup.
If full pressure is applied to the BFM, the precolumn phase dislodges from the
column wall and flakes away causing a flow restriction. Flow restrictions are
known to change the retention times, peak elution, Backflush at Times and even
destroy the detector. Therefore, it is necessary to always back-out the column
head pressure knobs for BFMs before turning on the carrier gas.
To ensure the integrity of the analytical columns in BFMs, do not subject the
columns to pressure surges. Before connecting a BFM to carrier gas, set the
column head pressure knob to zero psig by turning the knob counter clockwise.
After the carrier gas is connected, slowly turn the knob clockwise to increase the
column head pressure to original operating condition. To view column head
pressure, open the Status window in EZChrom.
As standard practice with BFMs, the column head pressure should be set to zero
psig when finishing up for the day. To protect the GC, turn the detectors off and
103
Creating a Method
cool the columns to about 40°C. Then, turn the column head pressure knob
counter clockwise until the carrier gas is set to deliver zero psig. It will take about
10 minutes for the pressure in the columns to decline to below 5 psig.
Caution To protect the detectors, always turn the detectors off before decreasing
column head pressure to zero psig.
The manifold delivers a column head pressure of about zero when, looking down
the edge of the BFM GC back panel, the black knob is 3/8 inch from the manifold
stem. The manifold delivers a column head pressure of around 30 psig when the
black knob becomes difficult to adjust.
Eight steps to backflush method development

The manual M200 and P200 Series MicroGC Backflush-to-Vent Modules
presents an eight step guide for developing new methods for a GC module with
the precolumn backflush-to-vent configuration (i.e., Modules A, B, and C in the
standard BFM). Verify that the GC is ready for sample analysis and a sample
source is connected to the GC sample inlet before starting method development.
Consider using the Starter Method and the operating parameters used for the
Sample Run provided with your AGILENT GC as the starting point for method
development.
104
Creating a Method
Send the Revised Method to the GC
11
Figure 51
It is necessary to Send the Current Method from the PC to the GC in order for
the parameters to be recognized by the GC.
105
Creating a Method
Verify New Setpoints
Check the Instrument Status to verify that the new setpoints are being implemented.
12
Figure 52
Select Instrument Status in order to confirm the implementation of the new set
points. One can watch any temperature changes as the zones heat up or cool
down.
106
Creating a Method
View the Peak Table
For definitions of the parameters in the table see pages 35 -37 of the User’s Manual.
13
Figure 53
Purpose
Contains compound names and elution times, which allows EZChrom 200/400 to
properly identify and quantify integrated peaks. It also provides the option of
grouping multiple peaks, which elute in a user-specified window. User-defined
response factors can be defined and referenced here.
Syntax
Select Peak Table or type E.
Comments
In most cases, the only information that needs to be entered in this table is peak
names, concentration units and Level 1 Cal Amounts. Retention times can be
entered graphically. The Peak Table contains the following information:
Peak Name
In this portion of the table, the names of the compounds which are to be analyzed
are entered. The peak names are entered for each component by typing them in.
When an integrated peak falls in a defined retention time window, it is assigned
the name linked to that window.
Retention Time
This is the amount of time it takes for the apex of a named peak to elute from the
column. The retention time can be entered graphically or with the keyboard. (In
107
Creating a Method
the Calibration Setup table there is an option to update the retention time at the
end of a run. If this is selected and the retention time changes, then the retention
time and the retention time window will be updated).
Retention Time Window
If a peak apex lies within a defined region of time, even though the retention time
of the peak may not match the retention time listed, it will be identified as the
compound defined by the preset retention time window.
Concentration Unit (CU)
This is a text entry, which identifies the concentration units of the various
compounds. Any three character text entries are allowed. The unit is not a
conversion factor and has no mathematical significance. Each component may
have a different concentration unit. The concentration units are only used for
external standard reports.
Level 1 Cal Amount
This is the amount of a compound that the level one external calibration standard
contains. When a Level 1 calibration is run, the entered amounts are assigned to
the areas of any integrated peaks, which elute in the appropriate retention time
windows. Obviously, accurate calibration standards must be used and retention
time windows must be properly set for EZChrom 200/400 to accurately quantitate
real samples. EZChrom 200/400 can use up to eight levels of calibration but for
routine analysis one level is usually sufficient. Each level corresponds to a gas
standard concentration and a point on a calibration plot.
Relative Response Factor (RRF)
When an external standard is unavailable, an estimated response factor may be
specified. Enter a number, which will be multiplied by a calibrated response
factor.
Peak
This entry is used to reference the RRF discussed above to a particular peak in the
Peak Table. Choose a compound, which has a similar thermal conductivity to the
uncalibrated peak.
108
Creating a Method
Edit the Peak Table
MolSieve or OV1
column
PoraPlot U
Column
14
Figure 54
The peak table should be edited with information relevant to the analysis.
109
Creating a Method
Save the Method
Lock and unlock method
15
Figure 55
It is important to Save the Method whenever changes have been made.

Locking a Method protects it from being inadvertently modified. A locked
Method may be modified during a session, but these changes will not be stored at
the end of the session unless a password is given.
To Lock a Method: To Unlock a Locked Method:

1. Select Method. 1. Open the Method that is locked.
2. Select Open. 2. Select Unlock in the Method
menu.
3. Select the method that is to be locked 3. Enter the password.
4. Select Method 4. Changes in Method parameters will
now be accepted.
5. Select Lock.
6. Enter a password (maximum of eight
characters).
7. Save the Method, entering your
password at the prompt
110
Collecting the Data
Collecting the Data
Collecting the Data
16
Figure 56
To start a run, select the Start menu.

8) Enter a Run ID for the air sample, which is to be run. This may be a
maximum of eight characters with no DOS control characters. (See page 162
for a list of DOS illegal characters.)
9) Enter 1 for the Number of Runs.
10) Select the Save box by clicking on it. (If any other boxes are selected (as
evidenced by an X appearing in the box) you may deselect them by clicking
on them.)
11) Click on [Start] or press <Enter> to begin data acquisition.
After the RUN window disappears, the vacuum pump will start and run for the
amount of time you specified in the Instrument Settings window. A small amount
of sample is injected onto the sample columns, then EZChrom 200/400 proceeds
to draw the chromatograms for channels A and B. A run clock is provided at the
top of the channel A and B windows. This clock displays the real time of the
chromatographic analysis that has progressed through a run. It should count up to
the run time specified in the Instrument Settings window.
111
Collecting the Data
Typical Chromatograms
17
Figure 57
When the run is completed, the data is first stored on the hard drive in the default
directory c:\HP\ezchrom\200\chrom under the run ID that you provided. The data
set is then automatically analyzed using the default timed events provided with
the NEW method. At this point take the opportunity to carefully examine the
analyzed chromatograms using the zoom and unzoom techniques. During your
examination, keep in mind the following questions:
Have all of the peaks been detected?
Are the peaks correctly integrated?
In the next few slides we will review data analysis techniques used in order to be
able to answer “Yes” to the above questions.
112
Collecting the Data
Save the Data File
18
Figure 58
You may choose to save the data with another name or in a different file path.
113
Data Analysis
Data Analysis
Setup Acquisition
Parameters
Integration
Optimization
Calibration Setup
Reporting Options
19
Figure 59
We will now investigate the process for optimizing the graphics and integration.
114
Graphic Manipulation
Zoom Box
Press
Pressand
andHold theleft
Holdthe leftmouse
mousebutton
button
andat
and atthe
thesame
sametime
timedrag
dragthe
thecursor
cursor
totothe
theright
rightand
anddown
downtotoform
formaa
rectangular
rectangularbox
boxaround
aroundthe
theportion
portionyou
you
wish
wishtotozoom.
zoom.
More information on zooming, moving and sizing windows is on pages 18-21.
20
Figure 60
Press and hold the left mouse button and at the same time drag the
cursor to the right and down, just below the baseline. This should draw a
rectangular box around a portion of the chromatogram.
Release the mouse button. EZChrom 200/400 will now draw the area inside the
zoom box so that it fills the lower screen.
115
Vertical Lines
Use
Usethese
thesecursors
cursorsasasmobile
mobile
reference
referencepoints
pointstotoobserve
observepeak
peak
amplitude
amplitudeandandretention
retentiontimes.
times.
Click
Clickthe
theright
rightmouse
mousebutton
buttonand
and
scan
scanthe
thecursor
cursoracross
acrossthe
the
chromatogram
chromatogramand andsee
seethe
thetime
time
and
andamplitude
amplitudedisplayed.
displayed.
Click
Clickthe
theleft
leftmouse
mousebutton
buttontoto
freeze
freezethe
thefirst
firstvertical
verticalcursor.
cursor.
21
Figure 61
Use these cursors as mobile reference points to observe peak amplitude and
retention times. They are also extremely useful in simplifying the selection and
definition of integration parameters and in the peak identification routine.
• Place the single-headed arrow cursor in either the channel A or B lower
window.
• Click the right mouse button. A single vertical line should appear. When
the mouse is moved to the left or right, the vertical cursor should move
accordingly. When using a laptop computer, the mouse must be moved slowly
for the vertical line to remain visible.
• Scan the cursor across the chromatogram and observe the string of text in the
lower display window. You should see the time and amplitude vary. Dragging
the mouse to the right should result in a larger time value. (This is because
data is collected from time 0, left to right). The value of the amplitude is the
actual instrument output in microvolts at the displayed time.
• Click the left mouse button. This will freeze the first vertical cursor.
• Drag the mouse to the right. The frozen cursor should remain, while a second,
mobile cursor will appear. The values for time and amplitude now displayed
are in reference to the first vertical cursor. That is to
say, the first vertical cursor now has been assigned a time and amplitude value
of 0.
116
Using Two Vertical Lines
Drag
Dragthethemouse
mousetotothetheright.
right.AAsecond
second
mobile
mobilecursor
cursorwill
willappear.
appear.Values
Valuesfor
fortime
time
and
andamplitude
amplitudenownowsetsetininreference
referencetotothe
the
first
firstvertical
verticalcursor
cursor(first
(firstvertical
verticalcursor
cursor
values
valueshave
havebeen
beenset
settotozero).
zero).
Click
Clickon onthe
theright
rightcursor
cursortotofreeze
freezethe
the
second
secondvertical
verticalcursor.
cursor.
To
Toremove
removethethevertical
verticalcursor,
cursor,select
select
Display,
Display,Cursor.
Cursor.
22
Figure 62
• Click the right mouse button. This freezes the second vertical cursor. The
region between the two vertical cursors is called the selected region. Being
able to select specific regions in a chromatogram is essential in graphically
setting up peak identification tables and integration parameters.
• Click the right mouse button again. This unfreezes the second vertical cursor.
• Click the left mouse button. This will cause the two vertical cursors to merge
and be mobile.
• Click the right mouse button. This will freeze the single vertical cursor
remaining, while also reactivating the single headed cursor. The single
headed cursor may now be used in any of the ways previously described.
• To remove the vertical cursor from the screen, click on Display in the
appropriate channel A or B window, then click on CURSOR.
Practice selecting various portions of the chromatogram. At first you may find it
difficult to obtain the desired cursor in an appropriate frozen or unfrozen state.
Don’t get frustrated; after a short time the manipulation of the mouse clicks will
become habit.
117
Optimizing Timed Events
23
Figure 63
After carefully examining the analyzed chromatograms using the zoom and
unzoom techniques, answer the following questions.
Have all of the peaks been detected?

This is indicated by a baseline, set off by vertical hash marks, drawn under each
peak. Hash marks, which point upward, indicate the start of integration while
downward-pointing hash marks define the end of integration.
Are the peaks correctly integrated?

Even though a peak has been detected, perhaps only a small portion of the peak
was actually integrated. Conversely, an integrated region may include areas on
either side of a peak, which should not be integrated. Be careful to zoom closely
on the base of a peak to determine if it has been properly integrated. If the peak is
properly integrated, the upward-pointing hash mark will appear at the beginning
of the peak’s upward slope and the downward-pointing hash mark will appear
where the peak returns completely to the baseline.
118
If the answer to either of the questions was no, then the Timed Events tables
must be optimized in order for an accurate analysis to be made. It may be that
the default timed event parameters were sufficient to find and integrate the peaks
in such a simple application. In general, though, this will not be the case.
Optimizing timed events

A Timed Event is a resetting of any of 10 calculation variables (see the Events
menu) that are used to calculate the area under a peak. Any or all of these may be
adjusted at various time points along the chromatogram. The purpose for setting
Timed Events is to attain the best possible peak area integration.
In order for EZChrom 200/400 to perform an accurate analysis, it is essential that
the proper parameters and values be entered into the Timed Events tables. Tables
are provided for both channels because different columns will require different
parameters to properly identify and integrate individual peaks. The most accurate
way to build an optimized Timed Events table is to select regions of a real
chromatogram with the vertical cursors and then evaluate the region with one of
the four basic timed event parameters. EZChrom 200/400 then calculates the
correct value for the event over the selected region and, if desired, adds the event
with the calculated value to the Timed Events table.
119
Timed Events
INTG Off – Integration Off Min Area – Minimum Area
Turns Integration Off Defines the smallest integrated area that
for a specified period of time. should be identified as a peak. Allows small
Prevents integration over selected peaks or baseline defects to be ignored
regions during peak search.
SLPSEN - Slope Sensitivity BL AT - Baseline At

Defines the average slope Resets the peak search from a user-selected
of the baseline in micro volts per point.
unit of time.
BLV - Baseline Valley
FINE SLPSEN - Fine Slope Sensitivity Forces the integration baseline to be drawn
Defines the threshold for the second derivative of the detector to the lowest point in the valley between two
voltage. The second derivative is used in peak processing to peaks.
determine the peak start and stop.
BLH - Baseline Horizontal
PKWD - Peak Width Forces the baseline to be drawn horizontally
Used to set the data bunching rate. Peak width adjusts the from the start time selected until the stop
bunching of data points to optimize peak detection. This time selected.
mechanism, combined with slope sensitivity and fine slope
sensitivity, acts as a noise filter. TAN - Tangent Skim
Forces the baseline tangent from the start of
Invert - Allows the user to invert any portion of a overlapping peaks to their tails.
chromatogram.
24
Figure 64
This page shows the definition of the various timed events.
120
Common Timed Events
Optimize these events for integration

• Integrator Off
• SLPSEN
• Fine SLPSEN
• PKWD
Refer to pages 41 - 45 of the User’s Manual for procedures for using these events.
25
Figure 65
The most common events used are listed above.
121
Setting Retention Times Graphically
Tick marks indicate integration
See pages 46-48 for more information on

identifying peaks.
26
Figure 66
The next step in constructing a complete and optimized application-specific

method is to enter the retention times and retention time windows for each of the
compounds in the peak table. The most accurate way to do this is to graphically
select each peak in a real chromatogram with the vertical cursors.
• Place the vertical cursors around the first peak that elutes on channel A. You
may use the vertical hash marks as a guide in placing the vertical cursors.
• Select the Peak RT and RT Window command, which is found under
the Events menu for channel A. A window will appear which lists the
compounds you previously entered in the channel A Peak Table.
• Click on the compound name of the peak in the window. The compound name
will depend on the type of column you have in module A. Click on [Ok] or
double click on the highlighted peak name.
• Repeat the procedure for each successive peak in the channel A
chromatogram, choosing the appropriate name from the list.
• Repeat the procedure for the channel B chromatogram.
122
Verify Retention Times in Peak Table
27
Figure 67
• Select the Analyze command from the lower menu bar. EZChrom will
analyze the chromatogram according to the parameters just set. Zoom in
closely on each peak to assure that the entire peak is within its predetermined
hash marks. If the peak does not have an upward hash mark at its beginning
and a downward hash mark at its end, it has not been integrated.
• Open the External Standard reports for channels A and B by clicking on
Reports, then on External Standard (See Figure 33). They should display the
peak names in the order of elution time and have large amount values for all
of the peaks listed in the reports. This is because the method is not yet
calibrated.
• If any of the peaks in the report have an amount of zero, and has an
integration baseline drawn underneath it, the retention time has been
incorrectly set.
• The Peak Table entries are verified when all the names you have added to the
Peak Table are present in the External Standard report.
123
Lab Exercises
Lab Exercises
Lab Exercises
• Lab Exercise 1: Air Analysis using the MolSieve/Poraplot U

Backflush GC
• Lab Exercise 2: Butane Analysis using the MoleSieve/Poraplot
U BackflushGC
• Lab Exercise 3: Natural Gas Analysis using the OV1/Poraplot U
GC
• Module Review
Students should swap instruments in order to perform all labs.
28
Figure 68
124
Lab 1: Air Analysis using the Molsieve/Poraplot U Backflush GC
Lab 1: Air Analysis using the Molsieve/Poraplot U

Backflush GC
• Set up a method for the analysis of air.
• Perform an analysis.
• Optimize the integration.
Follow the procedures from the EZChrom Chromatography Data System User’s
Manual pages 30-50 on performing a Sample Session.
Refer to the M200 and P200 Series MicroGC Backflush-to-Vent Modules
Manual for considerations when using the Backflush modules.
Part 1:Building the Method (Non-Backflush)

Use the procedure below to build a non-calibrated Method for Air analysis.
Save the Method as “Air”
The first step in optimizing the performance of EZChrom is to build a good
Method. This Chapter 7 of the User’s Manual provides a step-by-step sequence,
which simplifies the Method construction procedure outlined in Chapter 4 of the
User’s Manual. The following is an outline of the procedure that should be
followed whenever a new application is to be run.
Detailed instructions follow the outline.
• Set up the instrument parameters.
• Fill out the Peak Table.
• Run the GC.
• Set up the Timed Events Table.
• Adjust the instrument parameters, and rerun the GC (This step is optional and
frequently unnecessary).
• Optimize the Timed Events Table.
• Set the peak retention times and retention time windows graphically.
• Calibrate and save the method.
The details of each of these steps are reviewed below.
To exit EZChrom 200/400 at any time, double click on the box above Method in
the main menu.
125
Steps for the method construction procedure

1) Open the Instrument Setup window and set the column temperature, run
time, inject time, and detector sensitivity to appropriate values.
For most applications, columns temperatures of between 50 and 80 degrees will
give acceptable peak resolution.
Start with the maximum run time (160 seconds) and later reset it to 10 seconds
longer than the tail of the last eluting peak. Use a value of 50 milliseconds for the
inject time, unless sample gas concentrations are in the high % range (in which
case use 20 milliseconds) or low ppm range (in which case use over 100
milliseconds).
For concentration levels between 10 and 100%, use Low sensitivity. For levels
from 500 ppm to 10 %, use Medium sensitivity. For levels less than 500 ppm,
use High sensitivity.
Set the column head pressures for the individual modules. Pressures of between
15 and 20 psi are reasonable in most applications for the majority of columns.
2) Open the Peak Table and enter the names of the compounds for which you
wish to screen. If you are unsure of which column is appropriate for analysis
of a given compound, ask your instructor. In the Level One Cal
Amount boxes, enter the concentrations of each compound in your first
external calibration gas standard.
3) Attach your sample or calibration gas to the sample inlet and run the GC.
As the data is being acquired, observe the number, resolution, and amplitude
of the peaks in the chromatogram.
4) Open the Timed Events tables (See Figure 49) and add a SLPSEN,
FINE SLPSEN, and INTG Off event to both the channel A and B tables.
The time parameter should be zero for all these events. The value for
the INTG Off event (in seconds) should be set to 1.5 seconds. This turns the
integration off during the first part of the acquisition, where baseline artifacts
are observed due to sample injection. The values for the SLPSEN and
FINE SLPSEN events are dictated by the detector sensitivity for a particular
channel. The most accurate way of setting SLPSEN and FINE SLPSEN is
graphically (see Chapter 5 of the User’s Manual).
The following table provides suggested initial values for SLPSEN and FINE
SLPSEN.
Sensitivity SLPSEN value FINE SLPSEN value
Low 10 5
Med 50 30
High 100 75
5) If necessary, adjust the instrument setup parameters and column pressures so
all of the desired peaks are well resolved and on scale. Detector saturation is
126
evidenced by the tops of peaks rising above the upper limits of the channel
window display. (See page 117 through page 120 respectively for
explanations of how to unzoom and how to adjust attenuation.) After
adjusting the instrument parameters, run the GC again. If the analysis is still
unsatisfactory, repeat this step. Be careful not to be fooled by the display.
Always set the display Attenuation to 2048, and Fully Unzoom the
lower display when checking for detector saturation.
6) Once the instrument settings have been optimized, the integration parameters
tables should be adjusted. During the course of completing Step 5, you may
have noticed that some of the peaks in the chromatogram were not
integrated, or were integrated incorrectly. To correct this deficiency, PKWD
events must be added to the Timed Events tables.
Observe the last analyzed dataset on the screen. Note the first peak, which is not
properly integrated (the calculated baseline does not extend from the true
beginning of the peak to its true end). Using a Vertical Cursor, determine
the time at which the missed peak begins to elute. Now, add a PKWD event, with
a value of 0.2, and a time slightly less (approximately 0.5 seconds) than the
beginning of the missed peak, to the appropriate Timed Events table.
After the PKWD event has been added, Reanalyze the data. The peak, which
was previously not integrated, should now be properly integrated. If it is not,
double the PKWD value to 0.4 and reanalyze. Eventually, the peak will be
successfully integrated. Repeat the above steps for both channels and all
subsequent peaks, which are still incorrectly integrated, remembering to double
the value for each successive PKWD.
At this time, you may also wish to extend the Intg Off event to include
solvent or composite peaks, which are not of interest.
7) Set the Retention Times and Retention Time Windows
graphically (as described in Chapter 4 of the User’s Manual) for all peaks of
interest in both channels. If you now reanalyze the data, the External
Standard report should display the names and area counts for all integrated
peaks in the chromatogram.
8) Select the Calib command from the lower menu bar and run the GC. Data
will be acquired, and a calibration will be done. Inspection of the External
Standard reports should show all compounds, which were in the calibration
gas, and at the correct concentrations. The Method is now complete. Save
the Method to the hard drive.
Part 2: Building a Backflush Method

Use the Eight steps listed below to build an uncalibrated Method for Air.
Save the Method as “AirBF”
127
Backflush
Pressure Reducing
Valve
Sample Flow Restriction
Flow Detector
During
Injection
Analytical
Carrier Gas Pre-Column Column
supply
ForeFlush
Valve Inject Valve
Sample Vacuum Sample Valve

Vent pump Sample In
Out
Stream
Sample Fixed Volume
Switching
Chamber Section
Valve
Schematic for Backflush GC module
Eight steps to backflush method development

Use this eight step guide for developing new methods for a GC module with the
precolumn backflush-to-vent configuration (i.e., Modules A, B, and C in the
standard BFM). Verify that the GC is ready for sample analysis and a sample
source is connected to the GC sample inlet before starting method development.
Consider using the Starter Method and the operating parameters used for the
Sample Run provided with your AGILENT GC as the starting point for method
development.
1) Set the column temperature and column head pressure as appropriate. See
your Instructor for guidance on the appropriate operating parameters for
your BFM.
2) Set the "B backflush At" time to a value likely to produce the desired
chromatogram. In the absence of more specific guidance, set the "Backflush
At" time to 10 seconds. As the "Backflush At" time is reduced, fewer
sample components exit the precolumn and pass into the analytical column
for separation, detection, and quantification. When modifying the
"Backflush At" time, begin by changing the time by ± 1 second, eventually
using ± 0.1 second increments to fine tune the "Backflush At" time. The
maximum "Backflush At" time is 25.5 seconds in 0.1 second
increments.
3) Set the sampling time to 15 seconds or longer so that the BFM receives a
sample with consistent composition to the GC analytical column. Use
shorter sampling time only if you obtain reliable results. Avoid sampling
times shorter than 5 seconds.
128
4) Set the run time to 160 seconds. Select a shorter run time if you are certain
that all of the sample components for quantification will be detected within
the shorter run time. A long run time facilitates the detection of carry-over
peaks and the passage of undesirable sample components from the
precolumn to the analytical column.
5) Analyze a sample. Determine if all the sample components for quantification
appear in the chromatogram. If all the sample components for quantification
are not detected, go to step 7.
6) Change the Method and BFM operating parameters to optimize the analysis.
Adjust the column temperature, column head pressure, or "Backflush At"
time to optimize the analysis. Potential improvements to the analysis
include: detecting all the sample components for quantification; reducing the
run time needed to get peaks for all the sample components for
quantification; improving peak separation; and reducing the "Backflush At"
time. In general, shorter "Backflush At" times and lower column head
pressures yield better chromatography. Increasing the column temperature
generally improves peak shape for the late-eluting peaks. On the downside,
increasing the column temperature can undesirably reduce the resolution of
the early-eluting peaks in the chromatogram.
a) If peaks for all the sample components for quantification appear in
the chromatogram, monitor the peak area of the last peak for
quantification. The "last peak for quantification" means the peak
with the longest "retention time" among the peaks used for
calculating sample results. If the size or shape of the last peak for
quantification causes inaccurate peak integration, then monitor the
peak area of another peak near the last peak. Reduce the
"Backflush At" time and rerun the sample. Compare the previous
run peak area for the monitored peak to the peak area in the rerun
of the sample. If the peak areas agree within 2%, then the shorter
"Backflush At" time is preferred. On the other hand, if the previous
run peak area of the monitored peak quantification is more than
2% greater than the peak area from the rerun then increase the
"Backflush At" time and rerun the sample. Make small adjustments
(tenths of a second) when you think you are close to the optimum
time, and larger adjustments (1 to 5 seconds) when you are far
from optimum time. Find the minimum "Backflush At" time that
delivers all the sample components for quantification to the
analytical column. Determine the value of this minimum
"Backflush At" time, and then add some time increment (e.g., 5%
to 10%) as a buffer against system variability. For example, if 3
seconds is the minimum time, select 3.3 seconds for the
"Backflush At" time. Remember that the "Backflush At" time has a
resolution of 0.1 second. Verify the repeatability of the GC with
the selected "Backflush At" time. Hewlett-Packard suggests
analyzing the same sample eight successive times. The peak area
129
RSD ("relative standard deviation") of the last five runs should be

below 2% for the last peak if the peak is adequately resolved. The
RSD will generally be below 1% for a well-resolved peak above
1000 ppm. If the RSD exceeds 2%, the "Backflush At" time may
be too short to reliably deliver all the sample components for
quantification to the analytical column. Increase the "Backflush
At" time, the column temperature, or the column head pressure and
repeat Steps 5 and 6. Look for carryover peaks. If carryover peaks
appear, go to Step 6b.
Carryover peaks (from previous samples) may not appear until
after the third run.
b) If carryover peaks appear, the selected "Backflush At" time is
insufficient to separate the sample components of interest from the
other components in the sample. Decrease the "Backflush At"
times a few tenths of a second or reduce the column temperature a
few degrees and then repeat Steps 5 and 6. The "time window"
between the minimum "Backflush At" time to pass all the sample
components for quantification and the "Backflush At" time that
allows undesirable sample components to enter the analytical
column widens as the column temperature decreases.
c) If all the sample components for quantification were successfully
detected, consider further adjustments of the method to optimize
the analysis. Decrease the run time, or increase the column
temperature or column head pressure. Increasing the column
temperature or increasing the column head pressure causes faster
elution of the sample components. Increasing the column head
pressure tends to reduce the minimum "Backflush At" time
required. Changes to the column temperature or the column head
pressure may require adjustment of the "Backflush At" time (by
repeating Steps 5 and 6).
7) If any sample component for quantification is not detected, increase the
column temperature, increase the column head pressure, or increase the
"Backflush At" time, then and repeat Steps 5 and 6. Try increasing
temperature by 5°C to 20°C, pressure 3 to 8 psig, or "Backflush At" time- 1
to 5 seconds.
If the chromatography achieved following Step 1 through Step 7 is not
satisfactory, the particular precolumn and analytical column combination in the
module may not suit the analysis attempted.
130
Part 3: Optimizing the Integration

• Verify that the data files are being saved where you want them saved.
• Optimize the timed events
• Set Retention times graphically
• Save the final method.
131
Lab 2: Butane Analysis using the MolSieve/Poraplot U GC
Lab 2: Butane Analysis using the

MolSieve/Poraplot U GC
Repeat the procedure in Lab 1 using the Butane sample.
Save the method as “Butane”.
132
Lab 3: Natural Gas Analysis using the OV1/Poraplot U GC
Lab 3: Natural Gas Analysis using the

OV1/Poraplot U GC
Build a method for the analysis of the Natural Gas sample.
Save the method as “Natgas”.
133
Module 4 Review
Module 4 Review
1. When do changes to the method become active on the GC?
2. How can samples be introduced into the GC?
3. Why is it important to know how to use the of the vertical line cursors?
4. Did the type of column effect the analysis results?
5. What is the critical operational consideration when working with Backflush

modules?
134
Module 5: Injectors

• Purpose of injectors
• How injectors work
Module 5: Injectors
GC Injectors
GC Injectors
GC Injectors
• Purpose of the Injector

• GC and Injector Hardware
• Function of the Injector
• Types of Injectors
• Understanding the Flow Dynamics of the Injector
Figure 69
The purpose of this module is to review the key considerations of the injectors.
136
Module 5: Injectors
GC Injectors
Injection Systems
Purpose:
To allow the insertion of a sample into the gas chromatograph in a
repeatable, reproducible manner. The sample should be representative of
the bulk, and unless specifically desired should be inserted without
chemical change.
Injection Types:
• Unheated - Variable (Timed)
• Unheated – Fixed
• Unheated Backflush
• Heated Variable (Timed)
• Heated Fixed
Figure 70
There are several types of injection systems available on the MicroGC.
137
Module 5: Injectors
GC Injectors
Injector Hardware
Dual Channel Single Channel
Figure 71
Two common types of instruments are the dual and single channel designs.
138
Module 5: Injectors
GC Hardware
GC Hardware
The Portable Gas Chromatograph
• Miniaturization of two key

components:
– Injector (About size of a quarter)
– Detector (About size of a dime)
• Analysis times measured in
seconds not minutes
• Via micro-machining in silicon
• Originally founded in 1981 by
scientists from Stanford
University
Figure 72
139
Module 5: Injectors
GC Hardware
Major Components
GC Channel or Module
Solid state injector Pneumatics

Silicon micro-machined injector either
unheated (ambient) or heated (< 90oC.)
Electronics
Column
Narrow bore capillary column
0.15 - 0.32mm I.D.
Isothermally heated (ambient to 180oC)
1 2
Thermal conductivity detector

Silicon micro-machined TCD
Figure 73
This schematic shows the dual channel GC with the injector pneumatics module
140
Module 5: Injectors
GC Hardware
GC Module
6“
Detector
Vents SSD
Heater
Control 4“
Carrier
Input &
Valve
Activation
Injector
Column Heater Column Spiral Analytical
and Reference Columns
Figure 74
This diagram shows the relative size and arrangement of the GC components.
Inside each module is a complete gas chromatograph consisting of a micro
injector, columns (analytical and reference), column oven, universal micro solid
state detector and heaters. The module can be easily exchanged. However,
individual components can only be exchanged at the factory.
Observe that each module has an outside label. This clearly identifies the column
type, length, heater scale and the offset. Scale and offset will be discussed later,
since they need to be considered or are important when exchanging modules.
141
Module 5: Injectors
GC Hardware
Gas Samples
• Gaseous samples only!

– has to be a gas at ambient temperature
– hydrocarbons = C6 or less; as major components (up to C12 @
low concentration)
– fixed gases (CO, CO2, H2, N2, O2)
• TCD only (with low ppm sensitivity)
– not selective
– not as sensitive as other detectors (FID, ECD, PID)
– up to 10x more sensitive than standard TCDs
• Carrier Gases Used
– He, H2, N2, Ar
– Source pressure 80 - 100 psi
Figure 75
The P200 carrier gas moves the sample through the column. The carrier gas
should be dry and of high purity. The thermal conductivity of your carrier gas
should differ from components you want to analyze. Because of its high thermal
conductivity, the best choice for most applications is helium. Choose a gas with a
purity of at least 99.995%. When analyzing low ppm of oxygen and nitrogen, the
helium should be at least 99.999% pure. If you are analyzing helium or hydrogen
in a sample, nitrogen or argon are good carrier gas selections.
Caution Your P200/ P200H is configured at the factory to use helium/ hydrogen or
nitrogen/ argon as the carrier gas. Use of another carrier gas generates filament
temperatures that are too high and that result in damage to the detector if run at the
standard voltage levels. The GC controller board will adjust the filament voltage when
using argon or nitrogen so that filament temperatures are comparable to those when
using helium. These adjustments are discussed in Chapter 6–Theory of Operation.
Caution Hewlett-Packard does not recommend using hydrogen in the internal tank of
the P200.
The use of a carrier gas other than helium or hydrogen pose problems that result
in a loss in sensitivity. This is caused by the following:
142
Module 5: Injectors
GC Hardware
• The reduced voltage results in approximately an eight fold reduction in

sensitivity.
• The similarity in thermal conductivity between the carrier and the component
being analyzed reduces the detector signal.
• The physical characteristics of the carrier (viscosity, etc.,) results in a loss of
column efficiency.
In addition, you may see negative peaks due to sample components with higher
thermal conductivities than the carrier gas. While the data system provides the
Invert Timed Event function, you may also use an invert circuit plug that converts
the analog signal for negative peaks to positive and vice versa. Both the voltage
adjustments and the installation of the detector invert circuit are discussed in
Chapter 5.
143
Module 5: Injectors
Injection Process
Injection Process
Schematic of Micro GC - Sampling
Pressure
Switching Valve
Pressure
Transducer
Sample In Vacuum
Pump Sample Vent
Out
Micro Injector Analytical Column
Column Heater
Reference Column
Figure 76
This schematic shows the flow of gases in the sampling process.
Carrier gas flow path

Located inside the left compartment (as you face the front of the P200) is the
internal carrier gas cylinder. The tank is filled at the carrier fill 1800 psi. The
carrier fill inlet contains a check valve to prevent overfilling. Pressure at the tank
can be monitored at a front panel gauge. An On/Off front panel knob opens and
closes the flow that comes from the pressure regulator that has been factory set to
80 psi. The carrier gas then travels towards the back of the unit to the carrier
outlet.
A stainless steel jumper tube takes the carrier to the carrier inlet on the back panel
of the P200. The carrier is split into two streams, each going to its own manifold
and pressure controller. From each manifold, the carrier gas continues to the
injector inside each module. The flow goes through the analytical and reference
columns, to the detector and out through the vents .
144
Module 5: Injectors
Injection Process
Pressure at the head of the column is monitored by a pressure transducer, which

generates an analog signal that is digitized at the controller board. The pressure is
displayed in EZChrom's Instrument Status window.
145
Module 5: Injectors
Injection Process
Schematic of Micro GC - Injection
Pressure
Switching Valve
Pressure
Transducer
Sample In Vacuum
Pump Sample Vent
Out
Micro Injector Analytical Column
Column Heater
Reference Column
Figure 77
This schematic shows the flow of gases in the injection process.

The gas sample enters the GC at the sample inlet. The connected sample, ranging
in pressure from 0 to 30 psi flows through two separate sample lines held together
by a two-holed ferrule. The sample flows to the sample micro valve at the
injector.
The instrument receives a signal from EZChrom to begin an analysis. The
vacuum pump activates and draws the sample through the now open sample
valve. The sample enters the sample loop and exits to vent until the user
selectable sample time is completed. The sample valve closes, the pump stops and
the loop pressurizes. The inject valve then opens for a user selectable inject time,
allowing sample to be swept onto the analytical column. The analytical and
reference column flow passes through a solid state detector and the flow exits at
the back of the unit through the vents.
146
Module 5: Injectors
Injection Process
Schematic for Backflush GC module
Pressure Reducing Backflush

Flow Restriction Valve
Sample
Flow Detector
During
Injection
Analytical
Carrier Gas Pre-Column Column
supply
ForeFlush
Valve Inject Valve
Sample Vacuum Sample Valve

Vent pump Sample In
Out
Stream
Sample Fixed Volume
Switching Chamber Section
Valve
10
Figure 78
This schematic shows the flow of gases for the backflush process.
A GC module with a pre-column backflush-to-vent configuration has two
columns—a short pre-column and a longer analytical column. The backflush
valve lies between the pre-column and the analytical column. The stationary
phase and length of the pre-column is chosen so that, at the operating temperature
of the columns, undesirable sample components that interfere with the analyses
are retained on the pre-column stationary phase. The sample components for
quantification have minimal affinity for the stationary phase of the pre-column,
and pass quickly through the pre-column. After the last sample component for
quantification exits the pre-column and enters the analytical column, the
backflush-to-vent valve located between the pre-column and the analytical
column opens. The carrier gas flow through the pre-column is reversed and back
flushes the undesirable sample components off the pre-column. The sample
components for quantification continue to flow through the analytical column for
separation and detection. At the end of the analytical run, the backflush GC
module is fully purged of all sample components and is ready for the next
analysis.
147
Module 5: Injectors
Injection Process
Theory of operation of the pre-column backflush-to-vent:

During sampling, the backflush and sample valves are open and the inject and
foreflush valves are closed. Sample gas is drawn into the GC by the pump or the
sample gas pressure. The sample gas fills the sample chamber in the injector. A
section of the sample chamber is a "fixed-volume" sample loop. The sample valve
closes, then the sample gas in the chamber is pressurized and the backflush valve
closes. Next, the inject valve and foreflush valve open. Carrier gas flows from the
opened foreflush valve into the sample chamber at one end of the fixed-volume
section of the sample chamber. The carrier gas from the foreflush valve forces the
sample gas from the fixed-volume section of the sample chamber through the
opened inject valve, and into the carrier gas flow to the pre-column and analytical
column.
The sample gas in the fixed-volume section passes through the inject valve and
injects in about 1 second. As the injected sample gas flows through the pre-
column, the sample components begin to separate spatially. The foreflush valve
and inject valve remain open until the sample components for quantification exit
the pre-column and enter the analytical column. At the "Backflush At" time, the
foreflush valve closes, the backflush valve opens, and the flow of carrier gas
through the pre-column reverses-or back flushes. All sample components
remaining on the pre-column ’backflush’ to the sample vent, while the sample
components for quantification continue to flow through the analytical column to
the detector.
The amount of sample gas injected depends on the volume of the fixed volume
section, and on the temperature and pressure of the sample gas in the fixed-
volume section at the moment sample injection begins (Ideal Gas Law: PV =
nRT).
Carrier gas pressure surges
WARNING Carrier gas pressure surges greater than 1.4 psig/sec may damage the
analytical columns.
It is critical in BFMs to set the column head pressure knobs to deliver zero
psig before startup
If full pressure is applied to the BFM, the pre-column phase dislodges from the
column wall and flakes away causing a flow restriction. Flow restrictions are
known to change the retention times, peak elution, Backflush at Times and even
destroy the detector. Therefore, it is necessary to always back-out the column
head pressure knobs for BFMs before turning on the carrier gas.
To ensure the integrity of the analytical columns in BFMs, do not subject the
columns to pressure surges. Before connecting a BFM to carrier gas, set the
column head pressure knob to zero psig by turning the knob counter clockwise.
After the carrier gas is connected, slowly turn the knob clockwise to increase the
148
Module 5: Injectors
Injection Process
column head pressure to original operating condition. To view column head

pressure, open the Status window in EZChrom.
Shutdown Procedure
As standard practice with BFMs, the column head pressure should be set to zero
psig when finishing up for the day. To protect the GC, turn the detectors off and
cool the columns to about 40°C. Then, turn the column head pressure knob
counter clockwise until the carrier gas is set to deliver zero psig. It will take about
10 minutes for the pressure in the columns to decline to below 5 psig.
Caution To protect the detectors, always turn the detectors off before decreasing
column head pressure to zero psig.
The manifold delivers a column head pressure of about zero when, looking down
the edge of the BFM GC back panel, the black knob is 3/8 inch from the manifold
stem. The manifold delivers a column head pressure of around 30 psig when the
black knob becomes difficult to adjust.
149
Module 5: Injectors
Injection Process
Event Sequence Matrix
Solenoid Valves Injector

M icro valves
M ode N .C . N .O . N .O . Sam ple vlv Inj vlv
Sw itch vlv Sam ple vlv Ins vlv
Sam ple C C O O C
Sam ple D w ell C O O C C
Com pression O O O C C
Sam ple Inj C O C C O
Solenoid valves: Normally Open (N.O.) Normally Closed (N.C.)
11
Figure 79
This chart shows the valve positions during the injection process.
150
Module 5: Injectors
Injection Process
How does the manifold connect to the injector?
Injsolenoid position
Sam ple solenoid

position To injectvalve (80 psi)
To sam ple valve (80 psi)
Sam ple out

Sw itch solenoid
position
Sam ple in
M anifold (includes
pressure regulator) Carriergas out
12
Figure 80
This diagram shows how the injection manifold is connected to the injector.
151
Module 5: Injectors
Injection Process
Injector Function
• Description of Timed Injector

• Injector Specifications
• Theory of Operation
• Response Vs. Injection Time
• Response Vs. Dwell Time
• Response Vs. Compression Time
• Flow Schematic
13
Figure 81
The injection parameters are set in the software.
152
Module 5: Injectors
Injector Types
Injector Types
Injector Types
Unheated - Variable (Timed) * 1-30 uL

Unheated - Fixed 1-30 uL
Unheated Backflush 1 uL
(Pre-column / Analytical column combination)
Molsieve 13X/Molsieve 5A 1 uL
Poraplot Q/ Poraplot U 1 uL
Al2O3/Al2O3 0.4 uL
OV-1 (no pre-column) 1 uL
Heated Variable (Timed) * 1-30 uL
Heated Fixed 1 uL
* ~ 9 uL contained within injector
14
Figure 82
There are several choices of injectors that can be used. The application
determines which injector is best.
153
Module 5: Injectors
Injector Types
Fixed vs. Variable Loop?
• Fixed (1uL)
– better repeatability
– less flexibility with unknown samples
– backflush available: 1 or 0.4uL (specifically for Alumina PLOT)
• Variable/Timed
– offers greater flexibility
– 30uL volume
15
Figure 83
The application will determine which option to choose.
154
Module 5: Injectors
Injector Types
Description of Variable/Timed Injector
Standard MTI Injector exists in

heated and non-heated versions.
Allows for varying volumes of

sample to be injected directly on
column.
Physical Dimensions
Length: 1.166 +/- 0.002 inches
Width: 0.920 +/- 0.002 inches
Thickness: 0.118 +/- 0.002 inches
Silicon Micro-machined
Injector
16
Figure 84
This picture shows the actual hardware of the injector and the micro channels
where the gases flow.
155
Module 5: Injectors
Injector Types
Micro-Injector
• Low dead volume (220 nL), reduces band broadening

• 5 ms diaphragm valves, repeatable and reliable (> 1.5e7 cycles)
• Internal sample loop (0.4, 1, 1-30 uL)
• Minimum external fittings and connections
• Low surface activity
• Sample Volume (+/- 0.853 ml)
– Volume on die in Sample Reservoir: 9.38 ml
– Volume in sample path to end of die: 24.78 ml
– Maximum injection volume possible: 31.75 ml
– Total volume to beginning of manifold: 47.45 ml
• Injection times can be varied between 10 to infinity in 10 ms
increments
17
Figure 85
The characteristics of the injector are listed.
156
Module 5: Injectors
Injector Types
Injector Restrictions
• Pressure Restrictions
– Maximum Column Head Pressure: 55 psi
– Maximum helium inlet pressure: 90 psi
– Maximum sample inlet pressure: 55 psi
• Temperature Restrictions
– Maximum injector temperature: 110°C
• Particulate Restrictions
– Maximum particulate diameter: Dp50 = 25 mm
18
Figure 86
There are operational restrictions in order to have the best performance and to
avoid problems.
157
Module 5: Injectors
Injector Types
Response Vs. Injection Time
70
Concentration (ppm) 65
60
Curve Fit Equation:
55 y = 10.494Ln(x) + 24.117
R = 0.99
50
45
10 20 30 40 50 60 70
Injection Time (ms)
19
Figure 87
This chart shows the relationship between injection time and concentration
detected. Doubling the injection time doubles the response only for the shorter
injection times. Therefore, there are minimal gains when using longer injection
times.
158
Module 5: Injectors
Theory of Injector Operation
Theory of Operation
• Flow Paths in the Injector:

– Two different types of flow channels on the injector die
– Carrier gas (Helium) flow channels
– Sample flow channels
• Sample is:
– Drawn by a vacuum pump into the sample reservoir
– Equilibrated towards atmospheric pressure in sample reservoir
– Compressed in sample reservoir by column head pressure
– Injected onto the head of the analytical column for analysis
• Types of Valves in the Timed Injector:
– Single Channel Valves - Sample Valve
– T Channel Valves - Injector
20
Figure 88
There are single channel and “T” channel valves.
159
Module 5: Injectors
Single Channel Valve
Single channel valves control gas flow in straight channels
VALVE
OPEN
Helium Under
Positive Pressure
VALVE
CLOSED
21
Figure 89
This diagram shows the schematic of the single channel valve.
160
Module 5: Injectors
T Channel Valves
T Channel valves control gas flow at intersecting channels
VALVE VALVE
OPEN CLOSED
Helium Under
Positive
Pressure
22
Figure 90
The next few diagrams show the function of the “T” Channel Valve.
161
Module 5: Injectors
T Channel Valves
When one end of the T channel is closed, the flow becomes unidirectional
VALVE Closed
OPEN End
Helium Under
Positive Pressure
23
Figure 91
162
Module 5: Injectors
Inject Position
Valve
Switching
Pre-column Analytical
Column
Carrier Gas
24
Figure 92
163
Module 5: Injectors
Valve Open
Valve
Switching
To Sample Sample In
Pump
To Analytical Column
25
Figure 93
164
Module 5: Injectors
Valve Closed
Valve
Switching
To Sample Sample In
Pump
To Analytical Column
26
Figure 94
165
Module 5: Injectors
Backflush (Analyze) Position
Valve
Switching
Pre-column Analytical
Column
Carrier Gas
27
Figure 95
166
Module 5: Injectors
Micro Injector - Detail
Sample Channel
Sample Inlet
Sample Valve
Sample Channel
Sample Inlet Channel
Column Inlet Channel
Injection Valve Reference Column Inlet

Carrier Inlet
28
Figure 96
This diagram identifies the various channels.
167
Module 5: Injectors
Switch Solenoid and Pump

• Switch Solenoid is external to the injector, and is shown
in the normally closed position
• Sample Chamber connects via a stainless steel tube to a
switch solenoid valve outside the injector
• Switch tube is always open from the die to the switch
solenoid prior to the Sample Vacuum Pump
• During Compression, the switch solenoid toggles to the
helium column head pressure
Switch Solenoid
Helium
at CHP
Open
End of
Sample
Chamber Vacuum
Pump
29
Figure 97
168
Module 5: Injectors
Sampling
Sample
Pump On
Sample
Valve Open
Sample
From
Bulkhead
Fitting
Injector Valve Helium To Analytical Column

Closed
30
Figure 98
The activites during sampling are shown.
169
Module 5: Injectors
Sample Dwell
Time of sample pressure

equilibration to atmospheric
pressure by releasing Sample
pressure via the Switch Pump
Off
Solenoid valve.
Sample Valve (SAMV) is Sample

closed and all other valves Valve
remain in the Sampling Closed
position.
Sample Pump is turned off.

Injector
Valve
Closed
31
Figure 99
The activities during sample dwell are shown.
170
Module 5: Injectors
Response Vs. Dwell Time
Chloroform, Detector 1 (Compression 500ms)
6000000
5000000
Area Response
4000000
5000000-6000000
4000000-5000000
3000000
3000000-4000000
2000000-3000000
2000000
500 1000000-2000000
400 0-1000000
1000000
300
Injection Time
0 200
0 100 200 300 100
400 500
Dwell Time
32
Figure 100
The dwell time must be optimized with respect to the injection time.
171
Module 5: Injectors
Sample Compression
Switch Solenoid opens to

column head pressure CHP
On
(helium carrier).
Column head pressure Sample

(helium carrier) compresses Valve
Closed
the gases contained in the
Sample Chamber.
Injector Valve To Column

Closed
33
Figure 101
The sample compression activities are shown.
172
Module 5: Injectors
Response Vs. Compression Tim

C h lo ro fo rm , D e te c to r 1 (D w e ll 5 0 0 m s )
6000000
5000000
4000000
Area Response
5 0 0 0 0 0 0 -6 0 0 0 0 0 0
3000000 4 0 0 0 0 0 0 -5 0 0 0 0 0 0
3 0 0 0 0 0 0 -4 0 0 0 0 0 0
2000000 2 0 0 0 0 0 0 -3 0 0 0 0 0 0
500 1 0 0 0 0 0 0 -2 0 0 0 0 0 0
400 0 -1 0 0 0 0 0 0
1000000
300
I n j e c ti o n T i m e
0 200
0 100 200 100
300 400
C o m p r e ssi o n T i m e 500
34
Figure 102
Compression time must be optimized with respect to the injection time.
173
Module 5: Injectors
Sample Injection
Inject Valve opens, initiating CHP

sample introduction onto the On
head of the analytical
column.
Sample
Valve
Closed
Injector Valve Sample Injected on

Open Column
35
Figure 103
The activities during injection are shown.
174
Module 5: Injectors
Heated versus Unheated Injector
Conc. Peak Area Peak Area % Change

Analyte
(ppm) Heater On Heater Off (Heater On)
Hexane 200 82,662 101,860 - 23.22%
Octane 200 108,425 118,740 - 9.51%
Nonane 200 118,395 95,07 + 19.70%
Undecane 200 131,098 45,956 + 64.95%
Dodecane 200 122,885 -------- --------
Benzene 500 347,429 400,020 - 15.14%
Toluene 500 379,614 398,706 - 5.03%
Ethyl Benzene 500 398,840 314,682 + 21.10%
p-xylene 500 372,981 275,828 + 26.05%
o-xylene 500 365,462 249,87 + 31.63%
1,3,5-trimethylbenzene 500 375,574 170,136 + 54.70%
1,2,4-trimethylbenzene 500 317,642 128,422 + 59.57%
Data from Paul Johnson
36
Figure 104
This chart shows the affect of using a heated versus unheated injector. Sensitivity
is not enhanced for all components when a heated injector is used.
One should determine the need for a heated injector based upon the type of
components analyzed.
175
Module 5: Injectors
Column Flow Considerations
Column Flow Considerations
0.100 mm ID Column Flow Considerations
0.10 I.D. mm Column

150
140 Inlet Pressure (PSI)
@ 2 mL/min Helium
Column Head Pressure [psi]
130
120
110
100 Inlet Pressure (PSI) @ 1 mL/min Helium
90
80 Inlet Pressure (PSI) @ 2 mL/min Hydrogen
70
60
50
Inlet Pressure (PSI) @ 1 mL/min Hydrogen
40
30
20
10
0
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15
Column Length [m]
37
Figure 105
Longer column require higher head pressures. Using hydrogen as the carrier
allows for the use of lower head pressures.
176
Module 5: Injectors
Lab Exercises
Lab Exercises
Lab Exercises
• Lab: Setting Inlet Options

– a. Vary the Injection and Sample Times
– b. Vary the Back Flush Time
• Module Review
Students should swap instruments in order to perform all labs.
38
Figure 106
177
Module 5: Injectors

In this lab exercise you will:
• Vary the Injection and Sample Times
• Vary the Back Flush Time
Part 1: MolSieve/Poraplot U Backflush GC

Your instructor will suggest the method and parameters to use.
Part 2: OV1/Poraplot U Heated Injector GC

Your instructor will suggest the method and parameters to use.
178
Module 5: Injectors
Module 5 Review
Module 5 Review
1) How does one determine the type of injector to use?
2) What critical operational steps should be taken when using backflush

modules in order to avoid damaging the system?
3) What injector parameters should be optimized for a method?
4) What are the advantages and disadvantages of using hydrogen as a carrier

gas?
179
Module 5: Injectors
Module 5 Review
180
Module 6: Columns
In this section you will learn about:

• Micro GC Attributes
• Column Types
• Fundamentals of Separation
• Calculating Column Efficiency and Resolution
• Understanding Column Selectivity
• Common Micro GC Applications
Module 6: Columns
Columns
Columns
Columns
• Micro GC Attributes
• Column Types
• Fundamentals of Separation Theory
• Calculating Column Efficiency and Resolution
• Understanding Column Selectivity
• Common Micro GC Applications
Figure 107
The purpose of this module is to review the key considerations of the columns.
182
Module 6: Columns
GC Hardware
GC Hardware
Major Components
Solid state injector
•Silicon micro-machined
injector either unheated
(ambient) or heated
o
(< 90 C.) Pneumatics
Column
•Narrow bore capillary column
• 0.15 - 0.32mm I.D. Electronics
•isothermally heated(ambient to 180oC.
1 2
Figure 108
This section focuses on the columns in the modules.
183
Module 6: Columns
GC Hardware
Key Attributes - Micro GC
Speed
• much shorter analysis time
– 21 minutes for typical Natural Gas Analysis: maximum number of
samples per day is 68
– 2.67 minutes for Micro GC Natural Gas Analysis: maximum
number of samples per day is 539
• increase sample throughput
• use less power and carrier gas
– Micro GC with TCD requires only 3 mL per minute of carrier gas
(Typical GC with TCD requires 30 mL per minute of carrier gas)
Size
• portability for performing measurements at place needed
Sensitivity
• perform TCD measurements with up to 10X lower detection
Figure 109
Micro GC offers many improvements over traditional GC.
184
GC.
Standard Deviation
Figure 110
M
et
h
0.0000
0.1000
0.2000
0.3000
0.4000
Et an 0.5000
0.6000
0.7000
0.8000
h e
Et an
h e
Pr yle
n
Pr opa e
op ne
Is yl
ob en
Repeatability
n- uta e
tr B n
an u e
s- tan
2
1- -B e
u
Is But te
ob e ne
ci u ne
s- ty
2 l
Is -B ene
op ut
n en ene
Comparable or better than traditional GC
1, -Pe tan
3
3- -B nta e
M u n
e t e
tr thy adi
an l- e
2- s 1- ne
M -2 B
et -P ut
hy en en
l e
2- 1-P -1- ten
M e Bu e
et nt t
ci hyl ene ene
s- -1
2- B
n- Pen ute
He te ne
xa ne
ne
[Mole %]
[Mole %]
Micro Std. Dev
Conventional GC,
4
Standard Deviation
The Micro GC technique is very repeatable and reliable compared to traditional
185
Module 6: Columns
GC Hardware
Module 6: Columns
GC Hardware
GC Module
6“
Detector
Vents SSD
Heater
Control 4“
Carrier
Input &
Valve
Activation
Injector
Column Heater Column Spiral
Analytical and Reference Columns
Figure 111
The function of the TCD requires the use of two columns, an analytical and
reference column.
186
Module 6: Columns
GC Hardware
Analytical Column
Analytical
Column
Reference
Column
Heater
Figure 112
The very small columns allow for the speed and sensitivity of the Micro GC
technique.
187
Module 6: Columns
Column Separation
Column Separation
Separation is a Partitioning Process
MOBILE STATIONARY
SAMPLE
PHASE PHASE
Figure 113
Samples contain a mixture of components, which require separation. The

separation is a partitioning process whereby the sample dynamically interacts with
a mobile phase and a stationary phase. In gas chromatography the mobile phase
is a gas, the carrier gas, and the stationary phase is a solid or viscous liquid, which
is part of the column structure.
As the sample is carried through the column by the carrier gas, the components
interact with the stationary phase. Separation occurs when components have
different degrees of interaction with the stationary phase, those interacting the
least elute first, and those interacting the most elute last.
188
Module 6: Columns
Column Types
Column Types
Column Types
Open (Capillary)
Packed
Wall Coated
Open Tube
(WCOT)
Porous Layer Open Tube)

Micro Packed
(PLOT)
Micro
PLOT WCOT
Packed
Length 0.25 - 10 cm 4-8m 4 - 14 m
I.D. 0.5 mm 0.15 - 0.32 mm 0.1 - 0.32 mm
Figure 114
There are two primary types of columns used in GC; traditional packed columns
and open tubular capillary columns. Packed columns are literally packed with a
material for adsorption or absorption and capillary columns have inside walls
coated with an adsorbing of absorbing material. Most applications today utilize
capillary type columns; however, there are some specific applications, especially
fixed gas analyses, where packed columns are still used.
The primary differences in packed and capillary columns are the materials of
construction, column length, and column inner diameter. Packed columns are
made of copper, stainless steel, or borosilicate glass. Capillary columns are made
of fused silica. Packed columns are much greater in diameter, typically 2- mm,
whereas capillary columns are 0.5 to .75 mm. Packed columns are usually about
0.5 to 10 meters long whereas capillary columns can be as long as 150 meters.
There are significant differences in column flow rate conditions for the two types
of columns.
Micro GC utilizes primarily the PLOT and WCOT columns.
189
Module 6: Columns
Column Types
Gas Solid Chromatography (GSC)
Micro-Packed Columns
Adsorbent Packing
Carrier Gas
Porous with large surface area
Capillary - Porous Layer Open Tubular (PLOT)
Separation by size/surface area Carrier Gas

differences
Figure 115
When the stationary phase is a solid material, the type of chromatography is

called Gas-Solid chromatography. In packed columns, the stationary phase is an
adsorbent, which fills the column. In capillary columns the adsorbent adheres to
the inside walls of the column leaving an open tube. These columns are called
PLOT (porous layer open tubular) columns.
This type of separation is commonly used for the analysis of permanent gases and
low molecular weight hydrocarbons.
Gas-solid chromatography represents about 10% of all the gas chromatographic
applications.
190
Module 6: Columns
Column Types
Gas Liquid Chromatography (GLC)
Capillary Columns
Wall Coated Open Tubular (WCOT)
Liquid Phase
Separation by partitioning or differential solubility in stationary phase.
Components are separated based on differences in polarity

(interaction of dipole forces).
10
Figure 116
When the stationary phase is a viscous liquid, usually a polymer, the type of
separation is called Gas-Liquid chromatography. This type of separation is used
for about 90% of all the gas chromatographic applications.
In packed columns, the liquid stationary phase is coated onto a solid support and
the resulting material is packed into the column.
In capillary columns, the liquid stationary phase is coated onto the inside walls of
the column.
191
Module 6: Columns
Column Types
Popular Micro GC Columns

Micro-Packed
Hay Sep A, 25cm x 0.5mm ID; 100/200 packed
• C1 to C3 hydrocarbons
• Available lengths: 25 and 60 cm
Plot
Molecular Sieve 5A* PLOT, 4M x 0.32mm ID; 30um
Molecular Sieve 5A* PLOT, 10M x 0.32mm ID; 30um
•Fixed gases (H2, O2, N2, CO, CH4)
•Susceptible to water contamination
PoraPak U & Q
•Suited for nitrogen methane separation and CO2 analysis
•Unusually prone to flaking
WCOT
OV-1, 4M x 0.15mm ID; 1.2 um GC User Manual
OV-1, 6M x 0.15mm ID; 1.2um Page 47 lists all of the
• Best for Non-polar hydrocarbons > C3 available columns.
• Available lengths: 4 to 14 meters
• Very stable, few problems encountered ,
• OV-1 is most popular column phase. * 5 Angstrom sieving material
11
Figure 117
The most popular types of used in Micro GC are listed above.
192
Module 6: Columns
Column Types
Considerations
Problems Associated with PLOT Columns

• Flaking
– inherent to the manufacture and design of the column
– enhanced if the column is depressurized rapidly
– disrupts the flow path to the detector, resulting in detector failure
• Deactivation
– columns become deactivated overtime
– can be overcome by reconditioning column for twelve hours
Column Can Morphology

• Column is wound into can manually
• Winding process disrupts packing material
• Purging column with pressurized gas will dislodge material
12
Figure 118
There are some considerations that are unique to Micro GC.
193
Module 6: Columns
Column Types
Column Connection
Column connected with zero-dead volume glass union.
PLOT columns union contains glass wool to filter out dislodged material.
13
Figure 119
It is very important to avoid any particulates in the system. Glass wool filters are
used to trap particulates.
194
Module 6: Columns
Flow A
14
Figure 120
This diagram shows a mixture of components as they pass through a column.

Separation results when the various types of components have different degrees of
interaction with the stationary phase.
In this example, the triangles have the least amount of interaction and elute first;
the circles have the most degree of interaction and elute last.
195
Module 6: Columns
Column Separation Characteristics

Efficiency: Ability of the column to produce sharp peaks
Resolution: Ability of the column to separate two peaks from each
other
Selectivity: Ability of the column to determine chemical and/or
physical difference in two peaks
GOOD GOOD
POOR POOR
15
Figure 121
When characterizing separation the terms efficiency, resolution and selectivity are
discussed. Good efficiency or sharp peaks often leads to good resolution,
however in the diagram above, the first is an example of good efficiency but poor
resolution and the second is an example of good resolution but poor efficiency.
Factors like column diameter, length, column flow rate, and oven temperature can
have an effect on efficiency and resolution.
Selectivity refers to the type of stationary phase in the column. One must assure
that the components of interest will have the ability to interact with the type of
stationary phase of the column.
196
Module 6: Columns
Basic Resolution Equation

Retention (Capacity)
Column Efficiency or Partitioning Selectivity
R = n k
α-1
4 1 + k α
Factors Affecting
Flowrate/ Linear Velocity Film Thickness Type of Stationary

Column Diameter Oven Temperature Phase
Column Length
Carrier Gas Molecular Wt.
16
Figure 122
The critical step in developing a method for GC is determining the resolution

required to effect the desired separation. The ability of the chromatographic
system to separate the “critical pair” is not only dependent upon their absolute
retention times, but also the sharpness of their respective peaks (that is, the
separation efficiency of the column).
Resolution is a complex interplay of the following chromatographic parameters:
efficiency, retention, and selectivity.
n = the column efficiency expressed as the theoretical plate number
k = the solute partition ratio
α = the selectivity factor

Actual column and GC parameters which we can control over have an effect on
the resolution. The slide shows the correlation of the operational parameters
affecting the various theoretical parameters of the Resolution Equation. From a
practical sense, we are often more comfortable focusing on the operational
parameters rather than the theory.
197
Module 6: Columns
Partitioning
Kd = Distribution Constant
17
Figure 123
Solute partitioning between two phases in a chromagraphic column can be

described as a dynamic equilibrium expressed by the partition coefficient, Kd.
198
Module 6: Columns
Partitioning Theory
Concentration in stationary phase

Kd =
Concentration in the vapor phase
mass stationary/vol stationary

Kd =
mass vapor/vol vapor
mass stationary vol vapor

Kd =
mass vapor vol stationary
retention time column morphology
18
Figure 124
The partition coefficient has thermodynamic significance and is specific for a

given component with respect to column temperature.
199
Module 6: Columns
Partition Ratio
mass stationary
= partition ratio
mass vapor
retention time
Partition ratio is the relative amounts of component in the vapor phase versus
the stationary phase. This ratio can be deduced by knowing retention times.
tr - tm
partition ratio = = k
tm
tm = retention time on an unretained peak
tr = retention time of the solute
19
Figure 125
The Partition Ratio, k, is a measure of the molar distribution of the component

between the liquid and gas phases. It is experimentally calculated from the ratio
of the time the component spent in the stationary phase relative to the time spent
in the gas phase.
200
Module 6: Columns
Temperature and Phase Ratio
Partition ratio (i.e., retention) is influenced by temperature and phase ratio (ß).
If ß then k or If ß then k
Phase ratio = relative amount of stationary phase to the radius of the column.
r
ß= 2df
r = radius of column
df = film thickness of column
20
Figure 126
The Partition Ratio is related to Kd by the phase ratio, Beta.

For a wall coated open tubular column of internal radius, r, the phase ratio is
inversely related to the stationary phase film thickness, df. Typical values for
capillary columns range from 50-500, with a larger values indicating thinner film.
201
Module 6: Columns
Choosing Columns
• The greater the film thickness for a given diameter column, the
more retained a compound is.
• As the diameter of a column increases for a given film
thickness, the less the retention.
• By knowing the phase ratio of a column, one can change from
one diameter column to another and always know what film
thickness is needed.
21
Figure 127
The bottom line is that when choosing and comparing columns, it helps to know
the phase ratio.
202
Module 6: Columns
Calculating Efficiency
Solute t R' 2
N(eff) = 5.545
Wh
Start t R ' = Retention Time
W h = width at half-height
N = effective theoretical plates
tR Time
Let's relate “n” to the length of the column.

n
Plates per meter (N) = or
L
L
Height equivalent to a theoretical plate (HETP) = Thus, the more efficient the column,
n
the bigger the "N”and the smaller the
"HETP"
22
Figure 128
The absolute retention time, the one printed on the report represents the total time
the component spends on the column from time of injection to time of detector.
Separation occurs because components spend different degrees of time in the
stationary phase. Therefore it would be useful to know how much time a
component interacts with the stationary phase as opposed to being in the mobile
phase.
The assumption is that at any given moment in time the component will be found
either in the stationary phase or traveling along with the carrier gas in the mobile
phase. Another assumption is that all components will spend the same amount of
time in the mobile phase and this time is directly related to the length of the
column. The amount of time spent in the mobile phase is equal to the time it
takes for a non-retained species to elute from the column. The assumption is that
there is no time spent in the stationary phase since there is no interaction with the
stationary phase. In many analyses the solvent has very little interaction with the
stationary phase, eluting first and very early in the analysis.
One can calculate the time spent in the stationary phase by subtracting the non-
retained species retention time from the reported retention time of a component.
This is known as the corrected retention time.
Separation Theory assumes that column is divided into a number of zones called
theoretical plates. A simplified definition would be to think of a theoretical plate,
203
Module 6: Columns
as each time there is an interaction between the component and the stationary
phase.
The number of theoretical plates can be calculated using the formula in the figure
on the previous page. The corrected retention time and the width of the peak is
substituted into the formula. One has a choice of which peak width to use, one at
the base of the peak, or one at the half-height. The constant 5.545 is related to the
use of the peak width at half-height.
The effective number of plates can then be related to the column length by
calculated the plates per meter or height equivalent to a theoretical plate (HETP).
The more efficient the column, the more plates per meter or the smaller the
HETP.
204
Module 6: Columns
Efficiency & Carrier Gas Linear Velocity
Efficiency is a function of
B +C µ
HETP = A +
µ
the carrier gas linear
velocity or flow rate.
The minimum of the curve

HETP
represents the smallest

MOLECULAR B { C RESISTANCE TO MASS TRANSFER
HETP (or largest plates per
DIFFUSION } meter) and thus the best
efficiency. "A" term is not
} A EDDY DIFFUSION present for capillary
columns.
µ ( opt µ)
Plot of HETP vs. linear velocity is know as the Van Deemter plot.
The linear velocity value at the minimum of the curve is the optimum value for achieving
the best efficiency.
23
Figure 129
The Van Deemter plot relates the linear velocity or flow rate to the column
efficiency. From the plot, one can determine what column flow rate or linear
velocity to us for an analysis to yield the sharpest peaks. In methods
development, one may want to spend some time generating a plot as a tool for
determining the column flow to use.
In the Van Deemter equation: A = eddy diffusion term
B = longitudinal or ordinary diffusion term
C = resistance to mass-transfer term
Since capillary columns have no packing material to cause obstruction to flow,
there is no eddy diffusion term. Therefore, the HETP is fundamentally lower than
for packed columns. The longitudinal diffusion term is related to the type of
carrier gas used. The smaller molecular weight gases, like hydrogen as compared
to nitrogen offer more diffusivity and thus reduce the value of “B”. The “C” term
accounts for the resistance to mass transfer in the liquid phase. An obvious way
of reducing this term is to reduce the liquid film thickness.
205
Module 6: Columns
Head Pressures and Flow Rates
Suggested Column Head Pressures
Column length Head pressure
4- 6 meters 15- 25 psi
8- 12 meters 25-30 psi

* rule of thumb; for every 2 meters
increase pressure by 5 psi
Measuring Column Flow Rate
1. Connect carrier gas

2. Make sure detector is off
3. Dial in desired column head pressure
4. Check for flow at the rear of the instrument
5. Turn detector on
6. Inject non-retained peak to establish linear velocity
7. Dial out pressure regulator before disconnecting carrier gas
24
Figure 130
Based upon the VanDeemter plot, the suggested column head pressure ranges
should produce the best efficiency.
206
Module 6: Columns
How To Improve Column Efficiency
1. Use smaller diameter column

Typical values of N based on column diameter:
Diameter (mm) Plates per Meter (N)

0.32 3100
0.25 3900
0.18 5150
2. Use a lower % or thinner film of stationary phase

3. Use smaller sample size
! Effective column efficiency is dependent upon good sample introduction technique.

Samples should be introduced in a tight, rapid plug to avoid band broadening.
25
Figure 131
When trying to optimize efficiency, one can try the above changes in order to
make improvements.
207
Module 6: Columns
Resolution
Resolution is a measure of the ability of a
column to separate two peaks.
RT = 4.41
Resolution is measured in terms of two
RT = 4.59
RT = 5.10
6.0E5 adjacent peaks which we want to separate.
Generally, the most difficult pair is chosen; if
these can be pulled apart successfully then
5.0E5
all of the others will be resolved as well.
4.0E5 1.18 ( RT - RT1 )

2
Abundance
R= (W + W )
3.0E5 1 2
2.0E5
R = 1.5 Means Baseline Separation
1.0E5
Doubling column length does not double resolution!
4 4.5 5 5.5 6
Time ( Min.)
The more efficient the column, the greater the chances of better resolution.
26
Figure 132
Resolution can also be calculated. The above diagram presents the formula using
retention times and peak widths of two adjacent peaks in question.
208
Module 6: Columns
Type of Carrier Gas Effect on Efficiency and

Resolution
HETP C17 at 175º C Helium

Nitrogen Hydrogen
(mm)
k' = 4.95 (58 cm/sec) (58 cm/sec) (58 cm/sec)
1.2 N2 WCOT Column
OV-101 0.4µ
1.0
25 m x 0.25 mm
He 15 m x 0.25 mm
.8
Glass WCOT
.6 SE - 52
H2
.4 Isothermal, 150º C
.2
10 20 30 40 50 60 70 80 90
R = 1.17 R = 1.37
Average Linear Velocity (cm/sec)
Efficiency curves for a 25 m x 0.25 mm id WCOT column Effect of carrier gas on the resolution of n-
with 0.4 um of OV-101. heptadecane and pristane.
27
Figure 133
The type of carrier gas used effects efficiency as already discussed in reference to
the Van Deemter plot. Using hydrogen allows for the use of faster flow rates or
linear velocity, which will result in shorter run times. However, if nitrogen is
used at the fast linear velocity of 58 cm/sec., resolution of the peaks is lost.
209
Module 6: Columns
Column Temperature Operation
• Isothermal Operation
– Oven is maintained at a constant temperature throughout the
analysis.
– Stop time is set with the initial time.
– Excessive broadening of later eluting peaks.
• Column Conditioning
– Mol Sieve 5A and Al oxide/KCL Plot columns become deactivated.
– Set Oven Temp to 180 degrees for min. 4 hours to overnight.
– Cleans out moisture and residues from column.
Caution! Not all columns can tolerate high temperatures!
28
Figure 134
Only Isothermal analyses are available in Micro GC. Traditional GC offers the
alternative of temperature programmed analyses.
Plot columns may require periodic reconditioning.
210
Module 6: Columns
Typical Applications
Enterprise Application Enterprise Type Application
Type
Chemical Monitor feedstocks,

analyze vent gases, Environmental Site assessment,
setup pilot plants etc. (Field) LUST, soil gases.
Non-regulated-Landfill
Natural Gas BTU content, detect gases, stack
leaks, analyze fixed emissions.
gases; sulfur gases Environmental VOC sample
(Lab) screening of soil and
Petroleum Refinery gas analysis, water
setup pilot plants, R&D Pharmaceutical Monitor VOCs in
gas analysis, wastewater waste water, fixed
analysis gases, fermentation
Refinery gas, light process monitoring.
hydrocarbons, fixed Residual solvents,
gases environmental
monitoring
Specialty gas product quality Automotive Test engine
companies emissions, monitor
fuel quality
29
Figure 135
This chart lists some typical applications for the Micro GC.
211
Module 6: Columns
Application Notes
Natural Gas Literature Refinery Gas Literature
See Agilent Web Site: www.agilent.com

Select: Products, GC, MicroGC, Reference Chromatograms and Conditions.
30
Figure 136
There are numerous published application notes available for commonly

performed applications.
212
Module 6: Columns
What is a Natural Gas?
Mixture of fixed gases and light hydrocarbons; generally <C12

Primary uses:
• heating fuel
• feedstock to petrochemical processes
• low emission vehicles
What is Btu Measurement?

o
Btu = British Thermal Unit amount of energy to heat 1 lb. of H20 1 F.
traditional measurement
Analytical determination of the energy content of the gas (caloric
content) hydrocarbon type and distribution is key
The higher the Btu value the greater the heat generation capability
per unit volume of gas
3
Emerging measurement standard = kilojoule/m
31
Figure 137
213
Module 6: Columns
Measurement of C1-C3
Houston, Texas
2
1 Nitrogen 0.717%
Natural Gas Sample
2 Methane 92.685% Taken on-line
1 1034 BTU
3 Carbon Dioxide 1.807%
4
4 Ethane 3.598%
3
5 Propane 0.808%
5
0 10 20 30 40 50 60 70 80 90 100110 120 130 140 150

Retention Time (Second)
32
Figure 138
214
Module 6: Columns
Measurement of C4-C9 Houston, Texas
1 i-Butane 0.094%
2
2 n-Butane 0.137%
1
3 i-Pentane 0.045%
4 n-Pentane 0.037%
3 4
5 Hexane 0.035%
3
6 Heptane 0.019%
4
7 Octane 0.008% 10 15 20
8 Nonane 0.010% Retention Time (Second)
5
Natural Gas Sample 6
7 8
Taken on-line
1034 BTU 10 20 30 40 50 60 70 80 90 100110120130140150
33
Figure 139
215
Module 6: Columns
Sulfur (Odorants) in Natural Gas
1 2&3
1. Composite
2. i-Pentane 1510 ppm
3. n-Pentane 1500 ppm
4. Hexane 500 ppm
5. Water
6. Heptane 200 ppm
7. 1-Propanethiol 150 ppm
8. 2-Propanethiol 120 ppm
4
9. 2-Me-2-propanethiol
100 ppm
5 6 78 9
0 20 40 60 80 100 120 140 160
34
Figure 140
216
Module 6: Columns
What is a Refinery Gas ?
Any petrochemical or petroleum refinery sample

stream that is primarily in a gas phase at approximate
ambient temperature and pressure….
Simple Compositions:
Fixed gases - H2, O2, N2, CO, CO2

Hydrocarbons - alkanes
Sources:
• Distillation
• Catalytic reforming
• Fractionating / separating units
35
Figure 141
217
Module 6: Columns
QRGA Pora PLOT U, 8m, 320um ID With

Backflush
36
Figure 142
218
Module 6: Columns
QRGA Pora PLOT

Hydrogen vs. Helium Carrier
37
Figure 143
219
Module 6: Columns
Complex Compositions
• Fixed gases - H2, O2, N2, CO, CO2

• Hydrocarbons - Alkanes, alkenes, alkynes, dienes
Sources
• Cracking catalysts
• Thermal cracking
• Fractionating units for cracking units
38
Figure 144
220
Module 6: Columns
QRGA Alumina Oxide PLOT

1. methane 12. cis-2-butene
2. ethane 13. neo-pentane
3. ethylene 14. cyclopentane Helium carrier,
4. propane 15. iso-pentane 1.6 mL/min.
5. propylene 16. n-pentane
6. acetylene 17. 1,3-butadiene
7. iso-butane 18. 3-methyl-1-butene
8. n-butane 19. trans-2-pentene
9. trans-2-butene 20. 1-pentene
10. 1-butene 21. cis-2-pentene
11. isobutylene
39
Figure 145
221
Module 6: Columns
QRGA Alumina Oxide PLOT
1. methane 12. cis-2-butene

2. ethane 13. neo-pentane Hydrogen carrier,
3. ethylene 14. cyclopentane
4. propane 15. iso-pentane 5.0 mL/min.
5. propylene 16. n-pentane
6. acetylene 17. 1,3-butadiene
7. iso-butane 18. 3-methyl-1-butene
8. n-butane 19. trans-2-pentene
9. trans-2-butene 20. 1-pentene
10. 1-butene 21. cis-2-pentene
11. isobutylene
40
Figure 146
222
Module 6: Columns
QRGA OV-1, 10m, 150um ID, 2.0um
1. methane/N2 8. neopentane
2. ethylene/ethane 9. iso-pentane
3. propane/propylene 10. 1-pentene Helium carrier
4. iso-butane 11. n-pentane
5. iso-butylene/1-butene 12. cis-2-pentene 0.47 mL/min.
6. 1-butene 13. cyclopentene
7. cis-2-butene 14. n-hexane
41
Figure 147
223
Module 6: Columns
QRGA OV-1, 10m, 150um ID, 2.0um
1. methane/N2 8. neopentane
2. ethylene/ethane 9. iso-pentane
3. propane/propylene 10. 1-pentene
4.
5.
iso-butane
iso-butylene/1-butene
11.
12.
n-pentane
cis-2-pentene
Hydrogen carrier
6.
7.
1-butene
cis-2-butene
13.
14.
cyclopentene
n-hexane
0.77 mL/min.
42
Figure 148
224
Module 6: Columns
Lab Exercises
Lab Exercises
Lab Exercises
• Lab Exercise 1: Vary the oven temperature and flow rate.

• Lab Exercise 2: Calculating Efficiency
• Lab Exercise 3: Column Selectivity: View various Application
Notes on the WWW site for the MicroGC
• Module Review
43
Figure 149
225
Module 6: Columns
Lab Exercise: Changing Column Parameters
Lab Exercise: Changing Column Parameters

In this lab exercise you will learn:
• The effect of using different oven temperatures and column flow rate
• How to calculate column efficiency
• How to access the Agilent Website for Application Notes
Part 1: Varying the oven temperature and column flow

rate
Your instructor will advise you as to which method you should use and suggest
temperature and flow rate settings to use. Save the results for use in the next part.
Part 2: Calculating the Column Efficiency

Referring to the formulas presented in this module, calculate the plates per meter
for the column are at least two different column flow rates used in part
Part 3: Accessing the Micro GC website

Your instructor will demonstrate the access of the website.
226
Module 6: Columns
Module 6 Review
Module 6 Review
1) Why would one routinely monitor the number of theoretical plates or plates
per meter for a column?
2) What is the relationship between column diameter and efficiency?
3) What is the usefulness of the Van-Deemter Plot?
4) When would it be critical to carefully maintain the optimum linear velocity?
5) Does the type of liquid phase effect the elution order of unsubstituted
aliphatic hydrocarbons (i.e., C-3 through C-8)?
6) What happens to the peak shape of later eluting peaks as the oven
temperature is reduced?
227
Module 6: Columns
Module 6 Review
228
Module 7: Detectors
In this section you will learn the:

• Fundamentals of Detector Performance
• Thermal Conductivity Detector Design
• Operational considerations of the TCD
Module 7: Detectors
Detectors
Detectors
Detectors
• Fundamentals of Detector Performance

• Thermal Conductivity Detector Design
• Operational considerations of the TCD
Figure 150
The purpose of this module is to review the key considerations of the detectors.
230
Module 7: Detectors
Detectors
The Micro GC
Solid state injector
•Silicon micro-machined
injector either unheated
(ambient) or heated Pneumatics
(< 90oC.)
Column
•Narrow bore capillary column
• 0.15 - 0.32mm I.D.
•isothermally heated(ambient to 180oC. Electronics
1 2
Figure 151
We will now focus on the detector part of the GC module.
231
Module 7: Detectors
Detectors
GC Detector - A Definition
A GC Detector is a device which senses the presence of a component

different from the carrier gas, and converts that information to an
electrical signal.
Thermal Conductivity Detector (TCD)
Figure 152
TCD
Filament temperature increases as analytes present in the carrier gas pass over it,
causing the resistance to increase.
232
Module 7: Detectors
Detectors
GC Module
6“
Detector
Vents SSD
Heater
Control 4“
Carrier
Input &
Valve
Activation
Injector
Column Heater Column Spiral
Analytical and Reference Columns
Figure 153
This diagram shows the position of the TCD relative to the column and injector.
233
Module 7: Detectors
Setting Detector Parameters
Figure 154
The detector parameters are set in this screen.
234
Module 7: Detectors
Detector Response Characteristics
Sensitivity: The response per amount of sample, that is,

the slope of the response/amount curve. The
minimum amount on the curve is defined as
the minimum detectable level (MDL).
Selectivity: A measure of which categories of compounds

will give a detector response.
Dynamic Range: The range of sample concentrations for which

the detector can provide accurate quantitation.
Figure 155
When optimizing performance of the detector, one must be aware of the

characteristics of Sensitivity, Selectivity, and Dynamic range. We will discuss
each of these characteristics in this section.
235
Module 7: Detectors
Increased Sensitivity With Capillary Columns
Packed Columns Capillary Columns
Area = 2600 Area = 2600

S/N = 5 Height = 10 S/N = 10
Height = 5
Noise = 1 Noise = 1
Sensitivity = Signal/Noise Ratio
Figure 156
One of the considerations for applications to be converted from packed columns

to capillary columns is the effective increase in detector sensitivity with capillary
columns. Capillary columns are more efficient, producing sharper peaks.
Detector sensitivity is defined in reference to the signal to noise ratio. The
component signal should be greater than the noise background signal.
The above example assumes that the amount of the component in each
chromatogram is the same, but the peak shape is much sharper with the capillary
column. Therefore, smaller levels can be detected if the peaks are sharper.
236
Module 7: Detectors
Dynamic Range
Dynamic range is a measure of response vs. Quantity
Response is the signal produced by the sample.
Dynamic Range
Response increases reproducibly with
Response increased quantity.
Quantity
Linear Dynamic Range

Response increases proportionally with
increased quantity.
Response
Quantity
Non-linear response, as long as it is reproducible, can be

dealt with using non-linear calibration techniques.
Figure 157
It is important to know the response characteristics of the detector. If one doubles

the concentration of a component, one hopes to see twice the area detected. This
is not always true with all detectors. It is best to use a detector for the analyses of
components, which fall within the linear response range of the response versus
quantity curve. However, through multi-level calibration procedures, one can
determine amounts for detector responses that are not linear.
237
Module 7: Detectors
Thermal Conductivity Detection
Thermal Conductivity Detector

The TCD is a nondestructive
concentration sensing detector.
A heated filament is cooled by the

flow of carrier gas.
FLOW
When the carrier gas is contaminated by

sample, the amount of cooling changes.
The difference in cooling is used to

generate the detector signal.
Figure 158
Using a Thermal Conductivity Detector

The TCD compares the thermal conductivity of two gas flows—pure carrier gas
(also called the reference gas) and carrier gas plus sample components (also called
column effluent).
This detector contains a filament that is heated electrically so that it is hotter than
the detector body.
When helium (or hydrogen) is used as carrier gas, the sample causes the thermal
conductivity to fall. If nitrogen is used, the thermal conductivity usually goes up
because most things are more conductive than nitrogen. The TCD does not
destroy the sample during the detection process.
238
Module 7: Detectors
Wheatstone Bridge
10
Figure 159
The universal micro Solid State Detector (SSD) is a four filament resistive
Wheatstone Bridge where two branches of a circuit are joined to compare
resistance. When pure carrier gas passes through both branches of the bridge, the
cooling effect on the filaments is the same and the bridge, which was initially
balanced, will stay balanced. When a component elutes from the column and
touches one set of filaments, the cooling effect on the one set of filaments will
change. With the change in temperature the resistance of the filaments will
change and the bridge will become unbalanced. The bridge will become balanced
again when pure carrier gas passes again through the filaments.
The sample effluent from the analytical column flows over two
filaments and the flow from the reference column flows over the other two
filaments. In addition, the jumper in the controller board controls the current to
the filaments. This current change is for applications using argon or nitrogen as a
carrier gas.
Caution: Using an incorrect jumper setting will damage the filaments.
An auto-zero voltage generated by a digital to analog converter (DAC) sums the

detector output signal. The DAC cancels the offset voltage of the bridge when no
sample is present. EZChrom 200 controls the sum of the signal and the
239
Module 7: Detectors
amplification by choosing Low, Medium or High sensitivity. This choice changes

the amplifier gain from 5, 50, and 500. Dividing the output by 10Ω through a
resistor creates a one-volt output. The front and back panel ports provide the full
detector output.
Our schematic shows the four matched filaments (R1, R1, S1, and S1). Two of
those filaments are exposed to the flow coming from the sample column, and two
are exposed to the flow coming from the reference column. Pin 1 and Pin 3 bring
out the detector signal, while Pin 4 and 2 bring in the regulated power supply
voltage to the filaments.
240
Module 7: Detectors
Solid State Detector
11
Figure 160
This diagram shows the actual detector schematic.
241
Module 7: Detectors
The Micro Detector
• 220 nL Internal Volume

– Low dead
– Narrow peaks Must use Pure Carrier Gas
– Low surface activity 99.9995%!
• 2,400 Å x 6 um filaments
– improves sensitivity
– Response time 1-5 ms
– “Hardened” filaments, resist O2, etc.
• Low, medium and high sensitivity settings
• Low power consumption
– GC with TCD can require as much as 1,000 Watts to operate
– Micro GC with TCD requires only 30 Watts to operate (non-heated
version only)
12
Figure 161
In traditional GC, the Thermal Conductivity is the least sensitive of the GC

detectors. The Micro detector has features that overcome this limitation. The
internal volume of the Micro TCD is a fraction of the internal volume of the 6890
TCD.
242
Module 7: Detectors
Thermal Conductivity
The ability of a substance to conduct heat from a warmer to a cooler surface.
Carrier Gas Thermal Molecular

Conductivity Weight
Hydrogen 41.6 2
Helium 34.8 4
Methane 7.2 16
Nitrogen 5.8 28
Argon 3.8 40
Pentane 3.1 72
Hexane 3.0 86
13
Figure 162
This table lists the relative thermal conductivity values for several gases. When
helium is used as a carrier gas, all components other than hydrogen have lower
thermal conductivity values. Therefore, the filament will heat up when the gas
stream is “contaminated” with sample effluent of any gas with a lower thermal
conductivity compared to helium. If hydrogen were present, the filament would
become cooler; therefore, a negative peak would result.
243
Module 7: Detectors
Lab Exercises
Lab Exercises
Lab Exercises
• Lab Exercise 1:Modify the Detector Sensitivity

• Module Review
14
Figure 163
244
Module 7: Detectors
Lab Exercise: Modify the Detector Sensitivity
Lab Exercise: Modify the Detector Sensitivity

In this lab exercise you will learn:
• How to change the detector sensitivity and compare the results.
Your instructor will advise you as to which method you should use. Analyze the
sample using all three sensitivity choices.
245
Module 7: Detectors
Module 7 Review
Module 7 Review
1) Why is it important to understand the relationship of thermal conductivity
values for various gases?
2) The TCD is known as a universal detector. Why?
3) What features of the Micro TCD makes it so sensitive compared to

traditional GC TCD’s?
4) Why is it important to use very pure carrier gas that is free of particulates?
246
Module 8 Calibration, Sequences, and
Reporting

• Fundamentals of Calibration Theory
• How to use the Calibration Menus
• Multilevel Calibration
• Reporting Options
• Automated Sequences
• BTU Reporting
247
Module 8 Calibration, Sequences, and Reporting
Calibration, Sequences, Reporting
• Quantification Theory
• Calibration Theory
• Calibration Menus
• Multi Level Calibration
• Reporting Options
• Automated Sequences
• BTU Reporting
Figure 164
The purpose of this module is to review the key considerations of calibration,

sequences, and reporting.
248
Setup Acquisition
Parameters
Integration
Optimization
Calibration Setup
Reporting Options
Figure 165
This section will focus on the setup for Calibrated methods.
249
Qualitative Analysis
Module 4 discussed:
• Create a Method (setting up instrument parameters)
• Fill out the Peak Table with expected peaks
• Run the Analysis
• Identify the Peaks
• Set up the Timed Events
• If necessary, adjust any GC parameters
• Optimize the Timed Events Table
• Set the peak retention times and retention time windows
graphically
Reference: User’s Manual HP EZChrom Chromatography Data System, pages 96-102.
Figure 166
In Module 4, Data Acquisition and Analysis, the steps for performing

uncalibrated analyses was reviewed.
250
Quantitative Analysis
What is Quantification?
Quantitative Analysis involves:

• Knowing the compound you are analyzing
• Establishing a Method for analysis
• Analyzing a sample or samples of known concentration
• Analyze the sample containing an unknown concentration
• Compare the response of the unknown sample response to the response of the
known concentration
OR
I’ve Run My Standards, What Do I Do With The Data?

• Integrate calibration samples
• Print out data
• Calculate response factors
• Enter calibration into method
Figure 167
After the peaks have been integrated and identified, the next step in the analysis is
quantification. Quantification uses peak area to determine the concentration of a
compound in a sample.
A quantitative analysis involves many steps, which are briefly summarized as
follows:
• Know the compound you are analyzing.
• Establish a method for analyzing samples containing this compound.
• Analyze a sample or samples containing a known concentration or
concentrations of the compound to obtain the response due to that
concentration. You may alternatively analyze a number of these samples with
different concentrations of the compounds of interest if your detector has a
non-linear response. This process is referred to as multi-level calibration.
• Analyze the sample containing an unknown concentration of the compound to
obtain the response due to the unknown concentration.
251
• Compare the response of the unknown concentration to the response of the

known concentration to determine how much of the compound is present.
To obtain a valid comparison for the unknown sample response to that of the
known sample, the data must be acquired and processed under identical
conditions
252
Quantification Calculations
Calibration is the process of relating a particular peak height or

area quantity with a component concentration or quantity.
EZChrom offers the following Calculation Procedures:

• Area Percent
• Normalization
• External Standard (ESTD)
Figure 168
EZChrom offers the above calculation procedures for determining the

concentration of each component present in a mixture. The calculations used to
determine the concentration of a compound in an unknown sample depend on the
type of quantification. Each calculation procedure uses the peak area for the
calculation and produces a different type of report.
253
Area Percent - Uncalibrated Procedure
Area Counts Area %
Nitrogen 318487 0.72

Methane 41170132 93.04
Analysis of a sample containing
CO2 802659 1.81 unknown amounts of nitrogen,
Ethane 1598210 3.61 methane, CO2, Ethane, and propane.
Propane 358909 0.81
44248397 99.99
1598210
Area % of Ethane = X 100 = 3.61
44248397
AREA (pk)
Σ AREA (pk)
Figure 169
Uncalibrated calculation procedures do not require a calibration table. The

Area% calculation procedure reports the area of each peak in the run as a
percentage of the total area of all peaks in a run. Area% does not require prior
calibration and does not depend upon the amount of sample injected within the
limits of the detector. No response factors are used. If all components respond
equally in the detector and are eluted, then the Area % provides a suitable
approximation of the relative amounts of components.
Area% is used routinely where qualitative results are of interest and to produce
information to create the calibration table required for other calculation
procedures.
The example above shows the analysis of several gases. The Area% is calculated
from the detected areas of the five peaks.
254
External Standard Calculation
Area Counts Area % Actual Amount Response

% Factor
Nitrogen 318487 0.72 1 1 / 318487 = 3.14 E-6

Methane 41170132 93.04 93 93 / 41170132 = 2.25 E-6
CO2 802659 1.81 2 2 / 802659 = 2.49 E-6
Ethane 1598210 3.61 3 3 / 1598210 = 1.87 E-6
Propane 358909 0.81 1 1 / 358909 = 2.78 E-6
44248397 99.99
Single point calibration of a standard sample containing known amounts of

nitrogen, methane, CO2, Ethane, and propane.
RESPONSE FACTOR = AMOUNT / AREA

AMOUNT OF UNKNOWN = AREA(pk) X RF(pk)
Response factor takes into account that equal amounts do not yield equal
detector response.
Figure 170
The ESTD procedure is the basic quantification procedure in which both

calibration and unknown samples are analyzed under the same conditions. The
results from the unknown sample are then compared with those of the calibration
sample to calculate the amount of the unknown.
The ESTD procedure uses absolute response factors. The response factors are
obtained from a calibration and then stored. In following sample runs, component
amounts are calculated by applying these response factors to the measured sample
amounts. One precaution that must be observed in this type of calculation is that
the sample injection size must be reproducible from run to run.
The absolute response factor for a sample component represents the amount of the
component divided by the measured area or height of the component’s peak in the
analysis of a calibration mixture. The absolute response factor corrects for
detector response to individual sample components.
In the example above, the actual amount of each of the components is shown.
The detected area count for each component is divided by the known amount to
determine the response factor.
The unknown concentration of the component is determined by multiplying the
detected area by the response factor.
255
Calibration Comparison
Area Percent
• No calibration mixture required
• For Accuracy: All peaks must elute and all peaks must be
detected.
External Standard
• Requires calibration mixture
• Not all peaks need elute or be detected
• Choose the components in the mixture to quantitate.
Normalization
RF (pk) X AREA (pk)
NORM % = X 100%
[RF (pk) X AREA (pk)]
Each peak in the mixture is calibrated.
Figure 171
In the Normalization method, response factors are applied to the peak areas (or
heights) to compensate for changes that occur in detector sensitivity for the
different sample components. The Norm% report is calculated the same way as
an ESTD report except that there is an additional step to calculate the relative
rather than absolute amounts of compounds.
The Norm% has the same disadvantages as the Area% report. Any changes that
affect the total peak area will affect the concentration calculation of each
individual peak. The Norm% report should only be used if all components of
interest are eluted/migrated and integrated. Excluding selected peaks from a
normalization report will change the reported results in the sample.
256
Single And Multi-Level Calibration

C
C A
C A
C A B
A B
B
B
1 0.5 1.5 1.5 1.0 2.0 2.0 1.5 3.0 3.0 2.0 4.0
LEVEL 1 LEVEL 2 LEVEL 3 LEVEL 4
SINGLE POINT FOR

COMPONENT A
AREA/HEIGHT
Level 4
Level 3
AREA/HEIGHT
Level 2
Level 1
Area
Response of
Unknown
CONCENTRATION CONCENTRATION
Calculated
Amount MULTI-LEVEL FOR
COMPONENT C
Figure 172
The above example shows the generation of single and multi-level calibration
curves. In the first diagram the results of four analyses are shown. Four
calibration standards of known amounts of three different components were
prepared and analyzed.
In the single point calibration, the area or height response for Component A in the
Level 1 calibration mixture is plotted versus the known concentration of
Component A. When a mixture containing an unknown amount of A is analyzed,
its area count is noted on the plot and its concentration is determined by the
extrapolation from the plot.
For the Multi-level calibration above, each of the area counts for the four different
concentrations of Component C is plotted versus their known amounts. When
complete one would have three calibration plots, one for each component.
Multilevel calibration is used when it is not sufficiently accurate to assume that a
component shows a linear response or to confirm linearity of the calibration
range. Each calibration level corresponds to a calibration sample with a particular
concentration of components. Calibration samples should be prepared so that the
concentration of each component varies across the range of concentrations
expected in the unknown samples. In this way it is possible to allow for a change
in detector response with concentration and calculate response factors
accordingly.
257
EZChrom 200/400 will handle calibrations with up to eight gas standard

concentration levels. Each calibration level corresponds to a point on a calibration
plot. Each component for a particular channel must be calibrated with the same
type of calibration method (i.e., point-to-point or linear). That means that if a
point-to-point calibration is used for one component, the same must be used for
all of the other components. However, the number of calibration levels may be
different for each component.
258
Calibration Procedure
Setting Up Multi-Level Calibrations
What Determines the Concentration Range?

– What range does the project require?
– What is the instrument detection limit?
– What is the upper range of the instrument?
What Do I Need to Make my Dilutions?
– Blending manifold
– 1 Liter and 3 Liter Tedlar Bags
– 500 uL, 1 ml and 10 ml syringe
– Stock standard
– High purity Nitrogen
Calibrated Standards can be purchased.
10
Figure 173
When setting a calibrated method it is necessary to obtain calibrated standards.

One can either prepare the standards or purchase them.
259
Calibrating with New Data
1. Obtain Calibration Gas Mixture

2. Run the Calibration Sample
3. In the Peak Table, identify the peaks
4. Set Pk RT and RT Windows
5. Complete the Peak Table
6. Data: Clear Statistics
7. Calibration Setup
8. Save the Method Calibrating with Previously Run Data
9. Start Analysis 1. Select and Open a data file
2. In the Peak Table, identify the peaks
3. Set Pk RT and RT Windows
4. Complete the Peak Table
5. Data: Clear Statistics
6. Calibration Setup
7. Save the Method
8. Calib
9. Analyze
11
Figure 174
One can create the calibrated method as the samples are analyzed, or sometimes it
is more convenient to collect the data and then do the data processing on the
previously collected data files.
260
Method Menu, Select Peak Table
For definitions of the parameters in the table see pages 35 -37 of the User’s Manual.
Figure 175
It is assumed that the method has been created and a peak table exists. The
integration parameters should have been optimized. Verify that all the pertinent
peaks in the analysis are listed in the table.
261
Calibration Set Up
13
Figure 176
In addition to allowing up to eight levels of calibration, EZChrom 200/400

software can calibrate either on peak height or peak area. Also, the calibration
plot can be either point-to-point or linear. For a linear plot, at least two levels of
calibration are required. When a new method is being built, EZChrom defaults to
a set of values for the Calibration Setup. In most cases the default values will
suffice. In certain cases, however, values other than the defaults may be
appropriate. To access and alter the Calibration Setup table:
• Select Method.
• Select Calibration Setup.
• Make any necessary changes in the table.
• Select OK to close the table.
The features available in the Calibration Setup table, and their default values are
described below:
Peak Attribute (Area or Height)

Determines whether the calibration and quantitation are to be based on peak
height or peak area. The default is Area.
262
Calibration Fit (Point or Linear)

Determines whether the calibration plot is to be based on a point-to-point plot or a
linear plot. The default is Point.
Number of Runs (A & B)

This corresponds to the number of calibration runs that will be performed at each
calibration level. The integrated areas for each peak are then averaged, and an
average response factor is generated. The default is One.
Begin Calibration at Run

This allows the instrument to stabilize before calibration. The default is One.
Uncalibrated Peaks RF
This option allows the assignment of a blanket response factor to all unidentified
peaks. This response factor is multiplied by the area of the unknown peaks to give
an amount value. The default is Zero.
Multiplication Factor
This is a multiplication factor that is applied to all quantitated peaks, both in
calibration standards, as well as, samples. This feature is useful when a
concentrator or dilutor is used in the sampling system. The default is One.
Update Retention Time After (Calib and/or Run)

This allows the user to update the retention times of the components listed in the
peak table after each calibration and/or run. The default is No.
263
Single Level Calibration
14
Figure 177
To enter the concentrations from your calibration standard gases into your Peak
Calibration Table:
• Select Method
• Select Peak Calibration.
• Select Channel A or B
• Enter the amount information for each level using Page Down as necessary.
The calibration amounts must be entered in order from least to most
concentrated. A level one calibration will require only one entry per
compound.
• To switch compounds, click on [Prev] or [Next].
• The area information can also be entered now, manually, or later while
performing a calibration on stored or newly acquired data.
• To plot the new calibration points, click on the Plot button. The slope of this
plot defines the response factor for that compound.
264
Calibrating the instrument

Once the Calibration Setup and Peak Calibration Tables have been completed, the
instrument is ready to be calibrated.
Calibration can be performed with stored data or during an acquisition sequence.
265
Multi-Level Calibration
15
Figure 178
Follow directions for Stored Calibration or Run Calibration, depending on which

option is preferred. Any combination of these options can also be performed.
Stored calibration
First, clear the statistics for a clean start.
• Select Data.
• Select Clear Statistics.
• Select [OK].
Now select the stored data file to use as a calibration standard.
• Select Data.
• Select Open.
• Enter the data file name manually, or double click on the data file name.
Now set up to calibrate.
• Select Calib.
• Enter the Calibration Level (The calibration level refers to which calibration
gas dataset is being analyzed: first, second, third, etc.).
266
• Select [OK].
To finish the calibration:
• Select Analyze.
• Repeat the preceding steps for each calibration gas standard dataset.
Run calibration
• Attach the first cal gas standard.
• Select Calib.
• Enter the Calibration Level.
• Select [OK].
• Start the GC.
Calibration will begin immediately. Prior to sampling, the EZChrom menu title
bar will display the following message:
Calibration level X – Runs left Y

Where:
X = the calibration level selected under Calib.
Y = the number of calibration runs entered in the Calibration Setup.
Repeat the preceding steps for each calibration gas standard.
It is critical to remember that the cal gases must be calibrated in order of
increasing concentrations. This is necessary, not only to match the previously
entered Calibration Amounts, but also to allow the plotting algorithm to function
properly (the plotting routine does not automatically sort area/amount pairs).
For multi-component cal gases, it may be impossible to calibrate all compounds
in order of least to most concentrated. In this case it will be necessary to manually
sort the area counts in the Peak Calibration table.
267
Calibrated Peak Table
Show peak table with response factors
Figure 179
Once the Calibration is set up, the Peak Table will list the response factors.
268
Reporting
Reporting
Setup Acquisition
Parameters
Integration
Optimization
Calibration Setup
Reporting Options
17
Figure 180
There are several reporting options available.
269
Reporting
Reporting
18
Figure 181
To print reports and/or chromatograms during an autorun sequence, the Print

Options table must be filled in. By checking the Print option in the Start window,
the selected material will be printed during the time between runs. Remember,
enough time must be allowed for the printing process to be completed prior to the
next run.
Caution Chromatograms generate many data points that occupy a lot of memory on
your storage media. If you are printing multiple chromatograms simultaneously, you may
overload the printer memory and lock up your system.
1. Select Method.
2. Select Print Options.
3. Check any of the reports you wish to print, at the completion of the analysis,
for both channels.
4. Select [OK]. Remember to check the Print box in the Start window
prior to beginning a run. The available options are:
Chromatogram (full scale and/or zoomed)
Hard copies of the chromatograms can be generated for channels A or B. If the
Zoomed option is selected, the zoomed chromatogram shown in the lower display
will be printed.
270
Reporting
Any or all of the three available reports (Area %, ESTD, or Norm) for channels A
and B can be printed between autoruns.
271
Reporting
Display Options
19
Figure 182
There are specific display options one can set.
272
Sequences
Sequences
Automated Sequences
Number of
Consecutive Runs
Type of File Options

DIF Save - saves external
standard report peak name and
amount information as ASCII
characters delimited by tabs
(EXCEL format). The filename
used is the Run ID followed by
the extension .DIF. Batch Processing for Reanalyzing Files
PRN Save - Saves peak name and amount information as ASCII characters delimited with quotes and
numbers delimited by commas (Lotus format). The filename used is the Run ID followed by the
extension .PRN.
Extended - Check if you would like to include area and RT in the saved information.
20
Figure 183
Running the GC and obtaining accurate results is a simple task once a good
Method has been developed.
• Select Start.
• A run window will appear which prompts for information regarding the
automated run sequence.
• In the Run ID space, enter a name for the data, which is to be collected and
stored. This may be a maximum of eight characters and DOS illegal
characters are forbidden.
• Specify the Number of Runs. If the number of runs is greater than one,
the run number is appended to the Run ID as a data file extension (for
example: run.1, run.2, etc.).
• Specify the Time Between Injections in seconds. Note what the
delay interval is between injections; make sure this interval is long enough to
accommodate the run time, time between runs, and any necessary printing
time.
273
Sequences
• Check if the data is to be Saved and/or Printed after each run. Make
sure that printing selections have been made in Print Options before
selecting Print here.
• Check if the data is to be output in a DIF or PRN format.
The DIF format saves external standard report peak name and amount information
as ASCII characters delimited by tabs (EXCEL format). The filename used is the
Run ID followed by the extension .DIF. The PRN format saves the peak name and
amount report information as ASCII characters delimited with quotes and
numbers delimited by commas (Lotus format). The filename used is the Run ID
followed by the extension .PRN.
Check Extended if you would like to include the area and retention time in the
information saved to DIF or PRN files.
Recall allows one to reprocess data.
274
BTU Reporting
BTU Reporting
BTU Reporting
BTU Software is required. A third window is available.
See the BTU Analyzer User Manual for additional information.
21
Figure 184
The BTU Analyzer and Chromatography Data System instrument is a complete

gas chromatography system designed for natural gas BTU analysis. The data
system has software with a special BTU Gas Analysis software module
enhancement. As a result, an easy to use dedicated natural gas analysis system has
been developed. This system's compatibility with Microsoft Windows™ 3.1 or
higher makes the operation extremely user friendly. With a simple click of a
mouse button, you can initiate data collection, save or retrieve data, or begin a
BTU analysis.
The system is factory calibrated and, in most cases, data collection requires
simply clicking on the Start command. This data system is designed for beginning
analysts and experts alike. It performs routine natural gas analysis with minimal
user input. But for complex samples that require special data treatment where the
factory preset conditions do not apply, a variety of menus and commands are
provided to customize the quantification and identification of gaseous
compounds. You can, at any time, close the BTU analysis module and revert your
system to a standard EZChrom Data System to handle your other gas analysis
needs.
275
BTU Reporting
Description of the BTU User’s Manual

This manual covers the operation of the BTU Analyzer and Data System. Begin
with Chapter 2 to learn how to install the hardware and software, refill the
internal carrier gas cylinder and check general operation of the system. Once
installation is complete, continue to
Chapter 3 for instructions on running a natural gas sample, generating data and
interpreting a BTU report.
Chapter 4 shows you how to calibrate your system using your own standard and
how to save the calibration factors of this new method for future analysis.
Chapter 5 deals with troubleshooting tips, instrument adjustments, and method
development.
Chapter 6 is a reference to all menus and commands of this program. This section
is encyclopedic in nature and is to be consulted when doubts arise about the
function of a specific menu or command.
Chapter 7 covers advanced skills such as data handling, transferring files, batch
reprocessing, and the formatting of data for spreadsheet programs. This section
also covers setting up your system, running multilevel calibrations and calibrating
with multiple gases.
Chapter 8 covers integration principles, calculation methods, peak identification
and BTU calculations. The Glossary contains technical terms used throughout this
manual.
276
Lab Exercises
Lab Exercises
Lab Exercises
• Lab Exercise 1: Preparing Calibration Standards

• Lab Exercise 2: Creating a Multi-Level Calibration
• Lab Exercise 3: Exploring Report Options
• Lab Exercise 4: BTU Reporting
• Module Review
22
Figure 185
277

• Obtain stock standards
• Meter N2 bags for dilutions
• Calculate dilutions
• Prepare standards
• Analyze standards
• Optimize instrument and Method.
Part 1: Preparing Standards

You will need the following:
• Blending manifold
• 1 Liter and 3 Liter Tedlar Bags
• 500 uL, 1 ml and 10 ml syringe
• Stock standard
1000 ppmv of the following:
a) cis-1,2-Dichloroethene
b) Chloroform
c) Tertrachloroethene
• High purity Nitrogen
1) Pick 5 levels which span the chosen concentration level.
Level 1. .
Level 2. .
Level 3. .
Level 4. .
Level 5. .
2) Make the dilutions using the following formula.
Concentration = Concentration
278
------------------ ------------------
Area Area
(Conc. of Stock X Volume Used)

---------------------------------------- = Conc. of Dilution
(Volume diluted into)
Level 1. . into .= .
Part 2: Analyzing Standards

3) Complete a Run Log
File Name Sample ID Time Init

1
2
3
4
5
6
7
8
9
10
4) Load the method to be used. Verify or set up the Peak Table with the
appropriate entries.
279
5) Verify the Instrument Parameters.

6) Select Start from the Menu bar to begin the analysis of the first, most dilute
standard.
Type in the Run ID and select Save for saving the data.
Part 3: Optimizing the Method

7) Review the results.
280
8) If necessary, optimize the instrument parameters.

9) If necessary, optimize the integration and graphics display parameters.
10) Resave the method if any changes were made.
281
Lab 2: Creating a Multi-Level Calibration

• Analyze all the calibration samples
• Print out data
• Calculate response factors
• Determine repeatability
• Enter calibration into method
The last step in building an optimized method is setting up a calibration.
Calibration generates response factors on a known calibration standard so you can
perform quantitative analysis on an unknown sample. When running your first
sample, the system reported the concentration and other values based on the
method that was set up. It is recommended that you recalibrate with your own
calibration standard at least once per week to ensure the validity of your analysis.
When you need to recalibrate with your own standard, you should begin by
checking that you are obtaining repeatable performance from your analyzer. This
is done by obtaining the relative standard deviation of at least five injections of
your calibration sample.
Caution It is imperative that the composition (i.e., analyte identification and

concentration) of the calibration standard closely resembles that of the gas sample. The
analyte concentrations in the calibration standard should cover the expected
concentration range in the gas sample.
The relative standard deviation (%SD) is:

%SD = (Standard Deviation/mean) × 100
When the RSD of the peaks are within 2.0%, you are ready to edit your
calibration table. If you experience problems of peak detection, incorrect results
or similar difficulties, you should carry out the steps in Troubleshooting, before
continuing with the system calibration.
Part 1: Determining repeatability
EZChrom provides you with a very fast way to verify the repeatability of
injections and the adequacy of your integration and peak identification
parameters. To obtain reports that will give you the %SD of multiple injections,
do the following:
Before collecting data that will be used to determine the RSD of the peaks, inject
a sample twice to remove any air that may be in the transfer lines.
282
1) At the EZChrom Main Menu Bar, click on Data and then select Clear
Statistics. Then click on [OK]. All previous results that have
accumulated in the statistics registers are cleared and you are ready to begin
your analysis.
2) Click on Start at the Main Menu Bar. Enter 5 or more for the Number of
runs in the Run window. Save the data. Analyze your calibration sample at
least five times.
Make sure the number of runs found in Calibration Setup under the
Method menu equal the number of runs found in the Run window from the Start
Menu.
3) Click on the {Start} button in the Run window or press <Enter> to
begin the series of 5 runs.
4) After the last analysis of the sequence, click on Reports and then choose
External Standard. Observe the Relative Standard Deviation values
reported (%RSD) for all the peaks. The % SD should be equal to or less than
2.0% for satisfactory quantification. You may have to enlarge the window or
scroll down to see all the peaks.
If some of the peaks in your calibration are not reported (0.00 amounts), go to
Chapter 5 Troubleshooting of the User manual. If all peaks are reported and the %
RSD of all peaks is equal to or less than 2.0%, you can continue with the editing
of the peak table.
Part 2: Editing the Peak Table

A new calibration can be executed simply by editing the current peak table
instead of creating a new file.
5) At the EZChrom Main Menu Bar, click on Method, then on Peak
Table.
6) Choose the appropriate channel. A peak table exists in the current method
which will include all the information on the compounds in the calibration
standard: the RT Time (retention times, the time it takes the compound to
elute from the columns), the RT window (retention time window), CU
(concentration unit header), BP (bunched peaks), Level 1 Cal Amount
(calibration amount), the RRF (relative response factor), and the Peak (peak
number).
7) The flashing vertical cursor which appears once you press the <Tab> key,
may be moved to the left or right inside a box, using the arrow keys. Type in
the known Level 1 calibration amount.
Caution Do not change anything other than Level 1 Cal Amount.
To edit: Press the <Backspace> key repeatedly until the entry is completely
deleted. To delete more easily, place the arrow cursor at the beginning or end of
the entry and double-click. You can also click and hold the left mouse button
283
while dragging the mouse so that the whole entry is blackened. Now press the
<Del> key to remove the entry or simply type the new entry.
8) Using the values determined for your new calibration standard, reenter the
concentration for all other components in the Peak Table. All text and
numbers in the cells, other than the values in the instrument status window,
may be edited in this way.
9) Enter a "Y" under the BP column for those components that elute in a
component window and that you want to group. Normally these are isomers
of a particular component. Grouping is set up for hexanes, heptanes, and
octanes to generate a composite C 6 + calibration amount. Your calibration
sample should only have one peak for each of those components. Your
unknown samples will be more complex.
10) Click on [OK] when finished.
Caution Do not attempt to change the retention times of your calibration table
manually.
It is easier to reset them graphically. This procedure is shown in Chapter 5 of the

EZChrom User’s Manual.
Part 3: Recalibrating
Once repeatability has been checked and found acceptable, your peak table has
been set up, and all peaks have been detected, run the calibration sample to obtain
new response factors through the following steps:
11) At the EZChrom main menu bar, click on Calib. You will access the
Calibration window. Enter 1 for the Calibration Level and click on [OK].
12) Connect your calibration standard to the flow controller. Make sure that the
transfer lines have been purged and your calibration sample is flowing into
the GC inlet.
13) Click on Start at the EZChrom Main Menu Bar. You will open the Run
ID window. Enter the number of runs (three runs are recommended), and
click on Save to store your runs.
14) Click on the [Start] button at the Run window or press <Enter>.
A ratio of areas to concentrations for your calibration standard (Response Factors)
are calculated for each component peak. These factors are used for the calculation
of your reports when unknown samples are analyzed.
15) Click on Method and Save As to store the new calibration in your
method file. The current method name is blackened and you must type a new
name to differentiate it from the existing one. Use the extension ".met" to
distinguish this file as a method file.
284
Caution If you click on Save instead of Save As, or if you store your new calibration
under the original filename, it will replace the original calibration with your new calibration.
16) Repeat the procedure for the remaining calibration 4 levels of standards.
Part 4: Calculating Response Factor

We can manually calculate the response factors and standard deviation and
compare them to those reported.
Reponse Factor = Area Counts / Concentration
Complete the table for one of the components.
Compound: _____________________________________
Area Counts detected Known Conc Response Factor

1.
2.
3.
4.
5.
Average Response Factor = __________________________
Standard Deviation = ________________________________
Percent RSD (Stand. Dev./Response Factor) = ____________________________
285
Lab 3: Exploring Reporting Options

• Explore various reporting and printing options.
Part 1:Standard Report Formats

Explore the various reporting and printing options available on the following
menu choices
286
Part 2: Custom Reporting Options

Explore various custom reporting options, including exporting to Excel.
287

Refer to the BTU Analyzer and Chromatography Data System User’s Manual
for the procedures for generating BTU reports.
288
Module 8 Review
Module 8 Review
1) Describe the steps needed to prepare a single level calibration table.
2) Describe the steps needed to prepare a multi level calibration table.
3) Explain the following Setting:

a. Retention Time Window:
b. Multiplication Factor
c. Uncalibrated Peaks RF
289
Module 8 Review
d. Update Retention Time After: Calib or Run
4) What concentration or amount values should your calibration standards

have in reference to your unknown sample concentrations or amounts?
5) How important is curve linearity in reference to calculated accuracy?
6) How does one know that the calculated result is accurate?
290
Module 9: Troubleshooting

• Routine troubleshooting and maintenance
• How to use the Module Change Tool
Troubleshooting
Troubleshooting
Troubleshooting
• Routine Troubleshooting and Maintenance

• Monitoring Status Screen
• Module Change Tool
Figure 186
The purpose of this section is to review fundamental troubleshooting and

maintenance procedures.
292
Common Problem Areas
• Sample line
• Chromatograph
• Computer
• Communications
Figure 187
We will review some common problem areas associated with the Micro GC.
293
Troubleshooting the Sampling Line
• Inlet pressure
• Temperature
• Clogged line
• High moisture
• Flow restrictions
• Pressure biasing
• Component failure
Figure 188
294
Troubleshooting the Chromatograph
Hardware
– Power supply
• No power
• fluctuations
– RF interference
– Module
– Detector
– Carrier gas
– Heated inlet
– Pump
– Solenoid valve
Figure 189
295
Troubleshooting the Software
• Sampling time
• Method Parameters
– Column temperature
– Injection time
– Run time
– Sensitivity
• File management
– Data file path
– Format
Figure 190
296
Troubleshooting the Chromatography
• No peaks
• Saturation
• Co-elution
• Carryover
• Baseline problems
• Retention time shift
• Out of calibration
• Negative peaks
• Integration parameters
Figure 191
297
Troubleshooting the Computer
• Cables
• Power
• Software conflicts
• GC setup
• Printing
• Lockups
Figure 192
298
Troubleshooting Communication Problems
• Phone line
• Modem
• Serial connection
• Communications software
Figure 193
299
Troubleshooting Strategies
Symptom Possible Solutions
Figure 194
300
Routine Troubleshooting
• Micro GC User’s Manual has Troubleshooting Tables on the

following:
– Chromatographic Problems
– Temperature Readout Problems
– Pressure Readout Problems
– Fuse Problems
– Output Problems
– Electric Problems
– Communication Problems
• Perform a Baseline Analysis
• Perform a Reproducibility Test
10
Figure 195
You should refer to the troubleshooting tables available in the User Manuals.
301
Common Inspection Points
1. Verify Flows
Check for reference and analytical column flow at vents on rear panel of GC
2. Verify Communication between GC & PC
Check for cable connections, Send/Receive Method to GC
3. Verify Pressure readings
Verify pressure readings are displayed on CRT
4. Verify Detector Autozero is within limits:
(±) 300 mv
5. Verify Detector noise is within acceptable limits:
2000µv within 2 second window.
6. Check All column heaters ramp to maximum in a timely manner:
CT max < 4 min
7. Check board configuration
Board can be configured in either the Ar mode or the He mode.
He mode with Ar carrier or Ar mode with He carrier is very bad,
will burn detector.
8. Zero inject baseline can show signs of micro-valve failure
11
Figure 196
This slide lists some specific inspection point values.
302
Monitoring Instrument Status
Monitoring Instrument Status
Monitor Instrument Status
12
Figure 197
One should routinely check the instrument status to verify the instrument set
points.
303
Communication Error Numbers
1 Receiving queue overflowed. There was either no room in the

input queue or a character was received after the end-of-file
character was received.
2 Character was not read from the hardware before the next
character arrived. The character was lost.
4 Hardware detected a parity error.
8 Hardware detected a framing condition.
16 Hardware detected a break condition.
32 CTS (clear-to-send) timeout.
64 DSR (data-set-ready) timeout.
13
Figure 198
There are some error codes associated with communication errors.
304
GC Verification Tool
14
Figure 199
In Module 3, we used the GC Verification Tool to verify software installation.

One can use the tool to troubleshoot possible corruption of the software.
305
MTI GC Verification
15
Figure 200
306
MTI GC Verification
See EZChrom User’s

Manual for failure
information.
16
Figure 201
307
MTI GC Setup
MTI GC Setup
MTI GC Setup
17
Figure 202
The GC Setup disk is supplied with each GC.
308
MTI GC Setup
MTI GC Setup
18
Figure 203
309
Maintenance Procedures
GC User’s Manual includes some procedures:

– Replacing the controller board
– Resetting Instrument Configuration
– Resetting Column Head Pressure Values
– Replacing a Module
– Replacing the Sampling Pump
– Replacing the Battery
19
Figure 204
There are some Maintenance procedures available in the User Manuals.
310
Module Change Tool
Module Change Tool
Module Change Tool
Installed during Setup.

Can run from Explorer.
See HP EZChrom User’s Manual

for more information using the
tool.
20
Figure 205
If one changes a GC module, the Module Change Tool must be used to

reconfigure the new module.
311
Lab Exercises
Lab Exercises
Module 9 Lab Exercises
• Lab Exercise 1: Troubleshooting Problems

• Lab Exercise 2: Final Exam
21
Figure 206
312

In this lab you will:
• Perform a baseline analysis
• Troubleshoot problems.
Part 1: Confirming Performance

1) Your instructor will tell you which method and sample to use.
2) Perform a “ blank”, baseline analysis. Save the print out of the
chromatogram and report.
3) Perform an analysis using the specified sample. Save the print out of the
chromatogram and report.
Part 2: “De-bugging” your instrument

4) Leave the room as your instructor “bugs” your instrument.
5) Determine the problem or problems.
6) Correct the problem(s).
7) Perform the “blank”, baseline analysis to confirm performance.
8) Perform the analysis on your sample to confirm performance.
313
Lab 2: Final Exam
Lab 2: Final Exam

• Analyze an Unknown sample.
Part 1: “I’ve run the Instrument, But Can I Get the Right
Answers?”
1) 1. Load your method.
2) 2. Run your unknown.
3) 3. Fill out your answer sheet.
4) 4. Take a deep breath, your done!
Part 2: Final Exam Answer Sheet

Compound Conc. (ppmv) Conc. (ppmv) % Dev
Found Actual
If you have an unknown, label as unknown.

Give the unknown an estimated concentration.
314

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P Series Micro GC and Data

Manual Part Number H1187-90000

Agilent Technologies, Inc

 2000 by Agilent Technologies, Inc.

MODULE 1: BOOK INTRODUCTION 1

Using this Book 2

MODULE 2: INTRO TO AGILENT P-SERIES MICRO GC 7

Introduction to the Micro GC 8

Basic Gas Chromatography 9

Gases and Plumbing 21

Lab 1: Hardware Familiarization and Set Up 35

Lab 2: Filling the Internal Carrier Gas Cylinder 36

Data File Path 55

Method and Data Menus 60

Calib and Help 62

Lab Exercise 1: Starting Up the System 65

Lab Exercise 2: Introduction to Windows NT 67

Lab Exercise 3: Working with Windows NT 72

Optional Lab Exercise 4: Intro to Windows 95 78

Lab Exercise 5: Working with Windows 95 83

MODULE 4: DATA ACQUISITION AND ANALYSIS 93

Data Acquisition and Analysis 94

Creating a Method 100

Collecting the Data 111

Data Analysis 114

Graphic Manipulation 115

Optimizing Timed Events 118

Lab Exercises 124

Lab 1: Air Analysis using the Molsieve/Poraplot U Backflush GC 125

Lab 2: Butane Analysis using the MolSieve/Poraplot U GC 132

Lab 3: Natural Gas Analysis using the OV1/Poraplot U GC 133

Module 4 Review 134

MODULE 5: INJECTORS 135

Injection Process 144

Injector Types 153

Theory of Injector Operation 159

Column Flow Considerations 176

Lab Exercises 177

Lab: Setting Inlet Options 178

Module 5 Review 179

MODULE 6: COLUMNS 181

Column Separation 188

Column Types 189

Fundamentals of Separation Theory 195

Typical Applications 211

Lab Exercises 225

Lab Exercise: Changing Column Parameters 226

Module 6 Review 227

MODULE 7: DETECTORS 229

Setting Detector Parameters 234

Detector Response Characteristics 235

Thermal Conductivity Detection 238

Lab Exercises 244

Lab Exercise: Modify the Detector Sensitivity 245

MODULE 8 CALIBRATION, SEQUENCES, AND REPORTING 247

Calibration, Sequences, Reporting 248

Qualitative Analysis 250

Quantitative Analysis 251

Calibration Procedure 259