United States
Environmental Protection
Agency
Environmental Monitoring and Support EPA-600/4-79-067
Laboratory October 1979
Cincinnati OH 45268
Research and Development
&EPA
User's Guide for the
Gas Chromatography
Automation System
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RESEARCH REPORTING SERIES
Research reports of the Office ot Research and Development, US. Environmental
Protection Agency, have been grouped into nine series These nine broad cate-
gories were established to facilitate further development and application of en-
vironmental technology Elimination of traditional grouping was consciously
planned to foster technology transfer and a maximum interface in related fields.
The nine series are:
1. Environmental Health Effects Research
2 Environmental Protection Technology
3 Ecological Research
4. Environmental Monitoring
5. Socioeconomic Environmental Studies
6. Scientific and Technical Assessment Reports (STAR)
7. Interagency Energy-Environment Research and Development
8. "Special" Reports
9. Miscellaneous Reports
This report has been assigned to the ENVIRONMENTAL MONITORING series.
This series describes research conducted to develop new or improved methods
and instrumentation for the identification and quantification of environmental
pollutants at the lowest conceivably significant concentrations. It also includes
studies to determine the ambient concentrations of pollutants in the environment
and/or the variance of pollutants as a function of time or meteorological factors.
This document is available to the public through the National Technical Informa-
tion Service, Springfield, Virginia 22161.
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EPA-600/4-79-067
October 1979
USER'S GUIDE FOR THE
GAS CHROMATOGRAPHY AUTOMATION SYSTEM
by
Jonathan E. Kopke
Southwestern Ohio Regional Computer Center
University of Cincinnati
Cincinnati, Ohio 45220
Contract No. GS-05S-10458
Project Officer
John M. Teuschler
Physical and Chemical Methods Branch
Environmental Monitoring and Support Laboratory
Cincinnati, Ohio 45268
ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
CINCINNATI, OHIO 45268
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DISCLAIMER
This report has been reviewed by the Environmental Monitoring and Support
Laboratory - Cincinnati, U.S. Environmental Protection Agency, and approved
for publication. Approval does not signify that the contents necessarily re-
flect the views and policies of the U.S. Environmental Protection Agency, nor
does mention of trade names or commercial products constitute endorsement or
recommendation for use.
11
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FOREWORD
Environmental measurements are required to determine the quality of
ambient waters and the character of waste effluents. The Environmental
Monitoring and Support Laboratory - Cincinnati, conducts research to:
+ Develop and evaluate techniques to measure the presence and
concentration of physical, chemical, and radiological pollutants in
water, wastewater, bottom sediments, and solid waste.
+ Investigate methods for the concentration, recovery, and
identification of viruses, bacteria and other microbiological
organisms in water; and to determine the responses of aquatic
organisms to water quality.
+ Develop and operate an Agency-wide quality assurance program to
assure standardization and quality control of systems for
monitoring water and wastewater.
+ Develop and operate a computerized system for instrument automation
leading to improved data collection, analysis, and quality control.
This report was developed in the Advanced Instrumentation Section of the
Environmental Monitoring and Support Laboratory in the interest of advancing
laboratory techniques and quality control through computerization.
Dwight G. Ballinger
Di rector
Environmental Montioring and Support
Laboratory - Cincinnati
111
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ABSTRACT
This document contains a user's guide and a system manager's guide for
the Gas Chromatography Automation System of the EPA Laboratory Automation
Project.
The Gas Chromatography Automation System accepts reports from a Varian
220L Chromatography Data System, and it uses the data from these reports to
perform multi-point calibration, calculation of concentrations,
identification of compounds, calculation of relative retention times, and
calculation of EPA standard quality control statistics. The system also has
the capability to transfer the results to EPA's sample file control system.
This report was submitted in partial fulfillment of Task No. 79-219 by
the Southwestern Ohio Regional Computer Center of the University of
Cincinnati. It covers work done between January 10, 1979 and May 4, 1979.
IV
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CONTENTS
Foreword i i i
Abstract iv
1. Introduction 1
2. Using the Varian with this System 2
3. Signing on to the System 4
4. General Principles of the System 6
5. Method Interactions 8
Generating a New Method 8
Modifying a Method 9
Deleting an Existing Method 10
Displaying an Existing Method 10
6. Concentration Pattern Interactions 11
Creating a New Concentration Pattern 11
Deleting a Concentration Pattern 11
Displaying a Concentration Pattern 11
Listing the Concentration Patterns 11
7. Calibration 13
8. Calibration Curve Plotting 17
9. Injection Listing 19
10. Proce ss i ng 21
11. Qua! i ty Control 23
Control Standards 23
Spiked Samples 23
Duplicate Samples 24
Surrogate Spikes 24
12. Replicate Statistics 26
13. Dissimilar Analysis Confirmation 27
14. Sample File Control 28
Appendices
A. Commonly Used CAS Registry Numbers 30
B. Notes to the System Manager 35
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SECTION 1
INTRODUCTION
The Gas Chromatography Automation System (6CAS) is an elaborate exten-
sion of the Varian 220L Chromatography Data System. In this arrangement,
you will use the Varian to control your instrument and to collect data. The
data will be automatically transferred to the GCAS, and you will be able to
perform several types of multi-point calibrations, plot your calibration
curves, calculate concentrations, perform EPA standard quality control
calculations, calculate replicate statistics, perform dissimilar analysis
confirmations, and report your results to the Sample File Control System.
The GCAS is designed to be as self-explanatory and mistake-proof as
possible. The questions it asks are clear and complete. If you give an
unreasonable answer to a question, the GCAS will tell you so, and it will
ask you the same question again. Furthermore, no matter what mistake you
may make, the GCAS will not allow you to destroy any data that it received
from the Varian. Therefore, if you make a serious mistake, you can always
start over with no harm done. Feel free to experiment with the GCAS.
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SECTION 2
USING THE VARIAN WITH THIS SYSTEM
It is never necessary to work with both the Varian and the 6CAS at the
same time. Rather, you will operate the Varian according to its normal
procedures and then use the 6CAS for processing the data which the Varian
has collected. There are, however, a few points to keep in mind while you
are using the Varian.
First, your Varian method number will also be your method number in the
GCAS. You will have to cooperate with other users so that you will not try
to use someone else's method number. The computers cannot enforce this
cooperation.
When you create a method in the Varian, you have to provide an
identifier for each compound or group of co-eluting compounds. The GCAS
will not accept any identifier containing a comma. An identifier may be any
series of up to eight characters or spaces, but since the identifiers will
be used throughout the GCAS, you will want to pick memorable ones. For
example, your identifier for bromoform might be "CHBR3" or perhaps
"BROMFORM." There will not be any problem if two methods happen to use the
same identifier for different compounds, nor if two methods happen to have
different identifiers for the same compound. The only restrictions are that
within a single method, every identifier must be unique, and that in
different methods which are to be used for dissimilar analysis confirmation,
the identifiers of interest must be exactly the same.
The title which you give to a Varian report will be carried into the
GCAS for your reference. The only restrictions on specifying a title are
that the title cannot consist of more than thirty characters and spaces, and
it cannot contain a comma. Typical titles might be "THIRD STANDARD - 20UG/L
EACH" or "SAMPLE 46 SPIKED 10UG/L EACH."
The transfer of data from the Varian to the GCAS is done automatically
by a special microcomputer. All you need to do is specify that your reports
be printed on your own Varian terminal and one of the Varian terminals which
have been connected to the microcomputer. Ask the Varian system manager
which terminal(s) you should specify.
When your Varian report reaches the GCAS, it will be assigned an injec-
tion ID number which you will need to know in order to use the data. Since
the injection ID numbering scheme is easily predictable, you will be able to
write down the ID number for each injection without having to sign on to the
GCAS. Injection ID numbers are of the form "IIMMDDSS", where "11" is your
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Varian instrument number, "MM" is the month, "DD" is the day of the month,
and "SS" is the sequence number for the particular instrument that day. For
example, the sixth injection into instrument number nine on April 23, would
be assigned injection ID number "09042306."
The GCAS automatically keeps track of the sequence number portion of
injection ID numbers, and it sets the sequence number for an instrument back
to "01" whenever the date of an injection is different from the date of the
previous injection into the same instrument. However, if you have a set of
injections which will take more than one calendar day to complete, and if
you want their sequence numbers to be one long series, you can prevent the
GCAS from changing the date in the ID numbers. This ability may be parti-
cularly useful to you if you have an autoinjector running unattended past
midnight. Simply put "DATEMMDD" in the "operator identification" field of
your Varian reports, where "MM" is the month, and "DD" is the day of the
month. For example, to freeze the date at April 23, you would put
"DATE0423" in the operator identification field. When you use this feature,
the GCAS will use the date you specify, and the sequence numbers will
continue to accumulate until you change the specified date. Obviously, it
is important to change that date before the sequence number reaches 100.
This entire feature is optional. If you do not want to use it, leave the
operator identification field blank (or use it for your own purposes, but do
not put the word "DATE" in it).
The GCAS will store data for at most 100 injections for each instru-
ment. When you have reached the limit of 100 extant injection ID numbers
for your instrument, the oldest injection data will be displaced by new data
on a "first in/first out" basis.
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SECTION 3
SIGNING ON TO THE SYSTEM
The Gas Chromatography Automation System is a set of twenty-two BASIC
programs which run in a Nova 840 minicomputer. To use the GCAS, you must
first sign on to the Nova. Make sure that you use a terminal which is
connected to the Nova and set for full duplex, no parity, and 300 baud (or
1200 baud, if allowed by the Nova system manager).
To get the attention of the Nova, press the ESCAPE key once. (Some
Tektronix terminals do not have an ESCAPE key. On such terminals, hold down
the CONTROL and SHIFT keys, and press the K key.) If the Nova system is
already servicing as many users as it can, it will respond with "ALL LINES
BUSY," but normally it will ask for your "ACCOUNT ID." Type the
four-character account ID that was assigned to you by the Nova system
manager. The four letters will not appear on your terminal as you type them.
Next, the Nova system will usually print some message of the day, and
then it will automatically transfer control to the GCAS. This protects the
integrity of the GCAS by making it impossible for any user to change the
programs or data files. If you want to write your own BASIC programs, you
will need to sign on to the Nova under a different account ID.
The GCAS will immediately ask you "WHICH MASTER OPTION DO YOU WANT TO
USE? (0-10, OR 'RETURN1 FOR HELP)". If you press the return key, the GCAS
will print a list of the master options and then ask you the question again,
as shown in Figure 1. If you select option 0 (zero, not the letter 0), the
GCAS will automatically sign you off from the Nova.
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THESE ARE THE MASTER OPTIONS:
0. SIGN OFF
1. METHOD INTERACTION
2. CONCENTRATION PATTERN INTERACTION
3. CALIBRATION
4. CALIBRATION CURVE PLOTTING
5. INJECTION LISTING
6. PROCESSING
7. QUALITY CONTROL
8. REPLICATE STATISTICS
9. DISSIMILAR ANALYSIS CONFIRMATION
10. SAMPLE FILE CONTROL
WHICH MASTER OPTION DO YOU WANT TO USE? (0-10, OR 'RETURN' FOR HELP)
Figure 1. The master options question,
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SECTION 4
GENERAL PRINCIPLES OF THE SYSTEM
There are several general principles for using the GCAS which apply to
all of its options. The first of these is that any time you answer a
question, you must follow your answer with a RETURN. If the GCAS asks you
to type a number, and you type a character that is not a number, the bell in
your terminal will ring, and a question mark will be printed. If this
happens, simply type the correct answer, and the GCAS will proceed.
If you make a typing error and notice it before you press RETURN, you
can correct it. Pressing the RUBOUT key (the DELETE key on some terminals)
will eliminate the last character typed. Typing a backslash (\) will
eliminate your entire entry.
Whenever you complete an option in the GCAS, you will be returned to the
question, "WHICH MASTER OPTION DO YOU WANT TO USE? (0-10, OR 'RETURN1 FOR
HELP)". Furthermore, at any point in the GCAS, if you press the ESCAPE key
(or the Tektronix CONTROL, SHIFT K), you will also be returned to this
master options question. You can use this escape feature to get out of a
situation where you have made a mistake or simply to cut short any process.
Pressing ESCAPE will not get you out of the GCAS. The only way to get out
of the GCAS is to select master option 0.
The first time in a session that you choose a master option other than
interacting with a method or performing a dissimilar analysis confirmation,
the GCAS will ask you for the number of the method you want to use. It will
continue to use the same method for the rest of the session, or until you
interact with a method or perform a dissimilar analysis confirmation. After
either of these two options, the GCAS will once again ask for your method
number.
It is never appropriate to type a comma in the GCAS. For example, to
enter the number one million, you must type "1000000". If you are typing
the name of a chemical compound which must have a comma in it, type a slash
(/) where you want a comma to appear. For example, you might type
"1/2/3-TRIMETHYLBENZENE", and the GCAS would change it to "1,2,3-TRI-
METHYLBENZENE". This cumbersome arrangement is necessary due to a limita-
tion of the BASIC language in the Nova. The slash technique has been
implemented only for the names of compounds.
When the GCAS asks you a question that can be answered by "Y" or "N"
(that is, yes or no), just pressing RETURN is the same as answering "N".
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At many points in the GCAS, the Nova will do thousands of operations for
every one that you do, while at the same time it is also servicing several
other users. Consequently, slight delays are perfectly normal. If the GCAS
appears to have stalled, wait at least two minutes before you give up and
press ESCAPE.
There is no limit to the number of people who can use the GCAS at one
time, as long as they all use their own data. No two people can ever use
the same method or injection data at the same time.
If you find any error in the GCAS, make a detailed record of what lead
up to it. Bring this to the attention of the Advanced Instrumentation
Section, and the problem will be corrected.
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SECTION 5
METHOD INTERACTIONS
To interact with a method, you must select master option 1. There are
four types of method interactions: 1) generate a new method, 2) modify an
existing method, 3) delete an existing method, and 4) display an existing
method.
GENERATING A NEW METHOD
To create a new method, the GCAS will ask you to type a lot of
information, but once you have established the method, you can use it
indefinitely. When the GCAS asks, "WHAT SHOULD BE THE NUMBER FOR THE NEW
METHOD?" you will probably want to use your Varian method number to avoid
confusion, but you may use any number between 1 and 9999 inclusive, as long
as the number is not already assigned to a different GCAS method.
You will next have to select the type of method. The choices are: 1)
internal standards (not implemented in Version I of the GCAS), 2) purge and
trap with external standards, 3) liquid/liquid extraction with external
standards, and 4) direct aqueous injection with external standards. Your
choice of method type will influence how the GCAS performs calibration and
concentration calculations.
Next, you must select the type of retention time calculations from
either 1) relative retention times, or 2) capacity ratios. If you select
relative retention times, you will also have to enter the identifier for the
compound to whose retention time all others are relative. Then during
processing, relative retention times for all of the peaks will be calculated
by the formula:
Rel. Retn. Time . Inference * 100'
If you choose capacity ratios instead of relative retention times, you will
have to enter your dead volume time in seconds. Then during processing,
capacity ratios for all peaks will be calculated by the formula:
Capacity Ratio - - 1.
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When you type the identifiers for the method, be sure to spell them
exactly the same way you did in the Varian. The identifiers do not have to
be in any particular order. When the GCAS asks "NUMBER OF COMPOUNDS? (1,
2, OR 3)" enter the number of co-eluting compounds which are associated with
the identifier. The names of compounds may contain up to forty characters.
The Chemical Abstracts Services (CAS) Registry numbers are required by
the GCAS only if you intend to send your results to the Sample File Control
System. If you do not need to use CAS numbers, simply press RETURN when the
GCAS asks "CAS NUMBER?" If you do type a CAS number, the GCAS will check it
for typing errors, but the GCAS cannot check whether you have typed the
correct CAS number for the compound named.
When you have entered all of the identifiers for your method, type the
word "END" as the next identifier. A method may not contain more than sixty
identifiers.
MODIFYING A METHOD
There are four types of method modification: 1) add an identifier, 2)
delete an identifier, 3) add another co-eluting compound to the list for an
identifier, and 4) change retention time data. If none of these features
will change what you need to change, you can delete the troublesome identi-
fier and then put it back in correctly as a new identifier, or you can
delete the entire method and start over.
Adding an Identifier
Adding extra identifiers is just like entering the identifiers when you
originally create a method. You may add as many as you need up to a total
of sixty. Type the word "END" as an identifier when you do not want to add
any more. When you add an identifier to a method, the GCAS will delete all
of the concentration patterns for that method, since they would no longer be
complete.
Deleting an Identifier
To delete an identifier for a method, you simply have to type it
correctly, and the GCAS will confirm that it has been deleted.
Adding Another Co-eluting Compound
If you discover that another compound is co-eluting with one of your
named compounds, you can add the name and CAS number of the additional
compound to the list of compounds associated with the established identi-
fier. No identifier can have more than three co-eluting compounds
associated with it.
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Changing Retention Time Data
If you use this feature, you will be able to answer the retention time
questions from the method generation process again, without deleting the
method.
DELETING AN EXISTING METHOD
To delete a method, you only need to type the method number, and the
GCAS will confirm that the method has been deleted. All of the concen-
tration patterns associated with a method will automatically be deleted also.
DISPLAYING AN EXISTING METHOD
To display a method, you must type the method number.
will print a method report, as shown in Figure 2.
Then the GCAS
M-E-T-H-O-D R-E-P-0-R-T
ANALYST: JOHN DOE
TYPE OF METHOD: PURGE AND TRAP
IDENTIFIER FOR RELATIVE RETENTION TIME REFERENCE
IDENTIFIER NAME OF COMPOUND
1. CHCL3 CHLOROFORM
2. CHBRCL2 BROMODICHLOROMETHANE
3. CHBR2CL DIBROMOCHLOROMETHANE
4. CHBR3 BROMOFORM
METHOD NUMBER: 8001
PEAK: CHCL3
CAS NUMBER
67-66-3
75-27-4
124-48-1
75-25-2
Figure 2. Typical method report.
10
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SECTION 6
CONCENTRATION PATTERN INTERACTIONS
A concentration pattern is a list of concentrations for the identifiers
in your method. Concentration patterns are used as the prepared concen-
trations of calibration standards and control standards and as the added
concentrations for spiked samples. There are four types of concentration
pattern interaction: 1) create a new concentration pattern, 2) delete an
existing pattern, 3) display an existing pattern, and 4) list the names of
the concentration patterns for your method.
CREATING A NEW CONCENTRATION PATTERN
To create a concentration pattern, you must first answer the question
"WHAT SHOULD BE THE LETTER NAME FOR THE NEW PATTERN? (A, B, C, ..., OR
Z)". You may use any letter of the alphabet for the name of a concentration
pattern, as long as the letter is not already assigned to an existing
pattern for your method. You will next need to choose the unit of concen-
tration from either 1) nanograms per microliter, or 2) micrograms per
liter. Then you will be asked to type the concentrations of all of the
identifiers in your method. You will need to create one concentration
pattern for each calibration standard, control standard, and spike that you
intend to use.
DELETING A CONCENTRATION PATTERN
To delete a concentration pattern, you must simply type the letter name
of the pattern, and the GCAS will confirm that the pattern has been deleted.
DISPLAYING A CONCENTRATION PATTERN
To display the contents of a concentration pattern, you must type the
letter name of the pattern, and the GCAS will print a concentration pattern
report, as shown in Figure 3.
LISTING THE CONCENTRATION PATTERNS
To have the GCAS print a list of concentration patterns for your method,
you do not need to do anything other than select this feature. A sample
concentration pattern list is shown in Figure 4.
11
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C-0-N-C-E-N-T-R-A-T-I-O-N P-A-T-T-E-R-N R-E-P-0-R-T
CONCENTRATION PATTERN: G METHOD NUMBER: 0200
IDENTIFIER
BZ
TOLU
ETBZ
P XYL
M XYL
0 XYL
IPBZ
STYRENE
NPBZ
T BBZ
SEC BBZ
124TMBZ
N BBZ
BZFURAN
CONCENTRATION
80.000
80.000
80.000
80.000
80.000
80.000
80.000
80.000
80.000
80.000
80.000
80.000
80.000
80.000
Figure 3. Typical concentration pattern report.
C-O-N-C-E-N-T-R-A-T-I-O-N P-A-T-T-E-R-N L-I-S-T
CONCENTRATION PATTERNS FOR METHOD 0200: A, B, C, D, E, F, G, H, I, J
Figure 4. Typical concentration pattern list.
12
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SECTION 7
CALIBRATION
When you choose master option 3, the GCAS will begin a calibration
procedure. In Version I of the GCAS, there are two calibration procedures,
one for external standards calibration using purge and trap processing, and
the other for external standards calibration using either liquid/liquid
extraction or direct aqueous injection. The GCAS will automatically use the
correct calibration procedure for your method, based on an answer you gave
to a question during method generation. The two calibration procedures will
be discussed together here since there is only one noticeable difference
between them.
As calibration begins, the GCAS asks "DO YOU WANT TO CALIBRATE ALL
IDENTIFIERS OF METHOD XXXX AT ONCE? (Y OR N)". If you answer "N", the GCAS
will ask, "DO YOU WANT TO CALIBRATE XXXXXXXX? (Y OR N)" for each identifier
of your method. This allows you to calibrate all of your identifiers at
once, and, in a second session, to recalibrate individual identifiers to
discard outliers.
The GCAS will then ask for the injection ID numbers for your calibration
standards, the concentrations patterns for your standards, and (for
liquid/liquid extraction and direct aqueous injection) the injection volumes
in microliters. Type "END" as an injection ID when you do not want to enter
any more standards information. The GCAS will accept up to 15 calibration
standards, including any replicates.
The GCAS will then give you the choice of four types of curve fitting:
1) linear regression, 2) quadratic regression, 3) linear interpolation
extended to the origin, and 4) linear regression forced through the origin.
Linear regression will find the equation of the straight line which most
nearly passes through all of your calibration points. The equation of the
line will be of the form
C = sA + t
where C is the concentration and A is peak area. You must use at least
three standards to perform linear regression, because fewer standards would
not be enough to prove that the response from your detector is linear. An
example of a linear regression is shown in Figure 5.
13
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Quadratic regression will find the equation of the parabola which most
nearly passes through the calibration points and which is of the form
C = rA2 + sA + t.
You must use at least four standards for this type of fit, because fewer
standards would not be enough to prove that the response from your detector
is parabolic. An example of a quadratic fit is shown in Figure 6.
Linear interpolation simply connects the calibration points with line
segments. A segment is also produced from the origin to the lowest
standard. Linear interpolation can be done with one or more standards.
Figure 7 shows a linear interpolation.
Linear regression forced through the origin finds the equation of the
line which passes through the origin and most nearly passes through all of
the calibration points. The equation is of the form
C = sA.
At least three standards are required for this type of fit. An example of a
forced-origin regression is shown in Figure 8.
14
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GAS CHROflATOGRAPHV AUTOMATION SVSTEH
C-A-L-1-B-R-A-T-I-O-N C-U-R-U-t
ANALVSTI T. BELLAR METHOD« 0801
IDENTIFIER! 1188CL4C DATE OF CALIBRATION! 06/06/79
TVPE OF FITI LINEAR REGRESSION FITTING ERRORS S.71X
77000
70000
£3000
P
E
A
1C
A
R
E
A
56000
49000
48000
35000
88000
81000
H000
7000
0
0.00 0.80 0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80 8.00 8.80
CONCENTRATION IN HICROGRAflS PER LITER
Figure 5. Typical linear regression calibration curve.
GAS CHROHATOCRAPHY AUTONATION SYSTEM
C-A-L-I-B-R-A-T-I-O-N C-U-R-U-E
ANALYST! T. BELLAR METHODI 0201
IDENTIFIER! 1188CL4C DATE OF CALIBRATION! 06/06/79
TVPE OF FITl QUADRATIC REGRESSION FITTING ERROR! 8.02*
7?eee I " 1 1 -r 1 1 1 r
70000 '
P
E
A
K
A
R
E
A
0.00 0.80 0.40 0.60 0.80 1.00 1.80 1.40 1.60 1.80 8.00 8.80
CONCENTRATION IN HICROGRANS PER LITER
Figure 6. Typical quadratic regression calibration curve.
15
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GAS CHROMATOGRAPHV AUTONATION SYSTEM
C-A-L-I-B-R-A-T-I-O-N C-U-R-0-E
ANALYSTl T. BELLAR METHOD! 0201
IDENTIFIER! 1122CL4C DATE OF CALIBRATION! 06/06/79
TYPE OF FITI LINEAR INTERPOLATION FITTING ERRORS O.OOK
770001 1 > 1 T- 1 1 1 r-
70000 -
p
E
A
K
A
R
E
A
e.ee 0.20 0.40 0.60 0.80 i.ee 1.20 1.40 1.60 i.so 2.00 2.20
CONCENTRATION IN HICROGRAHS PER LITER
Figure 7. Typical linear interpolation calibration curve.
GAS CHRONATOGRAPHV AUTOMATION SYSTEM
C-A-L-I-B-R-A-T-I-O-N C-U-R-U-E
ANALYSTS T. BELLAR METHOD! 0201
IDENTIFIERI 1122CL4C DATE OF CALIBRATION! 06/06/79
TYPE OF FIT! LINEAR REGRESSION THROUGH ORIGIN FITTING ERROR! 8.09*
77000
P
A
K
A
R
E
A
70000
63000
56000
49000
42000
35000
28000
21000
14000
7000
0.00 0.20 0.40 0.60 0.80 1.00 1.20 1.40 1.60 1.80 2.00 2.20
CONCENTRATION IN MICROGRAHS PER LITER
Figure 8. Typical forced origin calibration curve.
16
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SECTION 8
CALIBRATION CURVE PLOTTING
Calibration curve plotting can be done by selecting master option 4.
The GCAS must first ask you what type of terminal you are using, since the
plotting feature of this option was designed specially for either Tektronix
4000 Series terminals or Hewlett-Packard 2647 or 2648 terminals. However,
if you are not using one of these specific terminals, you can still get
useful information from this option.
After you have typed the identifier for which you want a calibration
curve plot, the GCAS will clear the screen and draw the picture, as shown in
Figures 5, 6, 7, and 8. When the picture is complete, the bell in your
terminal will be sounded five times to inform you that you may make a hard
copy. When you are ready to proceed, press RETURN, and the GCAS will clear
the screen and print a table of residuals as shown in Figure 9. If you are
not using a plotting terminal, the plotting feature will be skipped, but the
data shown in Figure 9 will be printed.
The GCAS provides a "fitting error" statistic to help you judge your
calibration curves. The fitting error is actually a percent, relative,
standard error of estimate (also known as the coefficient of variation). It
is calculated by the formula:
2
(Known Cone. - Calculated Cone.)
Number of Standards - 2
Mean Cone.
A fitting error of 0.0% indicates a perfect fit; that is, the curve
passes through all of the calibration points. Other fitting error values
are meaningful only in terms of comparison and experience. For example, in
Figures 5, 6, 7, and 8, the same points have been fit four different ways.
The fitting errors can be used comparatively to prove that linear regression
(5.71% fitting error) is a better fit than linear regression forced through
the origin (8.09% fitting error) but not as good as quadratic regression
(2.02% fitting error) for these specific points. Furthermore, experience
has shown that any curve having a fitting error greater than about 5.0% is
not good enough to use. Some analysts have been able to routinely get
fitting errors of about 2.0%.
Fitting errors cannot be used to judge linear interpolation, since by
definition interpolation always produces a fitting error of 0.0%, no matter
how poor the carve is.
17
-------
C-A-L-I-B-R-A-T-I-O-N D-A-T-A
ANALYST:
IDENTIFIER
T. BELLAR
: 1122CL4C
R-E-P-0-R-T
METHOD: 0201
TYPE OF FIT: LINEAR REGRESSION THROUGH
INJECTION
01030101
01030102
01030103
01030104
01030105
EQUATION:
ID PEAK AREA
76236
41738
16905
9779
4327
CONCENTRATION
DATE
ORIGIN
PREPARED CALCULATED
2.000
1.000
0.400
0.200
0.100
= +2.56E-05(A)
1.949
1.067
0.432
0.250
0.111
OF CALIBRATION:
FITTING ERROR
DIFFERENCE
+0.051
-0.067
-0.032
-0.050
-0.011
04/30/79
: 8.09%
Figure 9. Typical calibration data report.
18
-------
SECTION 9
INJECTION LISTING
If you get confused about your injection ID numbers, you can use master
option 5 to find out what ID number has been assigned to each injection.
There are three types of reports which this option can generate: 1) all
extant injection ID numbers from one instrument, 2) ID numbers for a
specific date from one instrument, and 3) the title of the Varian report for
any ID number from any instrument.
To get the first type of report, you only need to type your Varian
instrument number, and the GCAS will print a report such as that shown in
Figure 10. The injection ID numbers on this report are in reverse chrono-
logical order.
E-X-T-A-N-T I-N-J-E-C-T-I-O-N-S
INSTRUMENT
02060409
02060403
02053002
02052406
02052301
02052103
02050211
02050205
02050113
02050107
02050101
02043008
02043002
02042706
02042313
02042307
02042301
NUMBER: 02
02060408
02060402
02053001
02052405
02052205
02052102
02050210
02050204
02050112
02050106
02043013
02043007
02043001
02042705
02042312
02042306
02042014
02060407
02060401
02052502
02052404
02052204
02052101
02050209
02050203
02050111
02050105
02043012
02043006
02042710
02042704
02042311
02042305
02042013
02060406
02060103
02052501
02052403
02052203
02050301
02050208
02050202
02050110
02050104
02043011
02043005
02042709
02042703
02042310
02042304
02042012
R-E-P-0-R-T
ALL
02060405
02060102
02052408
02052402
02052202
02050213
02050207
02050201
02050109
02050103
02043010
02043004
02042708
02042702
02042309
02042303
INJECTIONS
02060404
02060101
02052407
02052401
02052201
02050212
02050206
02050114
02050108
02050102
02043009
02043003
02042707
02042701
02042308
02042302
Figure 10. Typical extant injections report.
19
-------
To get the second type of report, you need to also specify the month and
day of interest. The GCAS will produce a report similar to that shown in
Figure 11.
Figure 12 shows how to get the title of the Varian report associated
with an injection ID number. Figure 12 also shows the type of messages
which the GCAS will print if you try to use an injection whose Varian report
was faulty.
E-X-T-A-N-T I-N-J-E-C-T-I-O-N-S R-E-P-0-R-T
INSTRUMENT NUMBER: 02 MONTH: 06 DAY: 04
02060409 02060408 02060407 02060406 02060405 02060404
02060403 02060402 02060401
Figure 11. Typical extant injections report for one day.
WHAT ID? 02050102
FOR ID 02050102, THE REPORT TITLE IS '20/500 STD #10.'
DO YOU WANT TO PRINT THE TITLE FOR ANOTHER ID? (Y OR N) Y
WHAT ID? 01021902
01021902 CANNOT BE USED BECAUSE THE REPORT DID NOT HAVE A TOTAL AREA.
DO YOU WANT TO PRINT THE TITLE FOR ANOTHER ID? (Y OR N) Y
WHAT ID? 01022301
01022301 CANNOT BE USED BECAUSE THE REPORT WAS IN THE WRONG FORMAT.
DO YOU WANT TO PRINT THE TITLE FOR ANOTHER ID? (Y OR N) N
Figure 12. Typical reports of injection titles.
20
-------
SECTION 10
PROCESSING
Processing an injection involves calculating the concentration of every
identifier, calculating the relative retention time or capacity ratio for
every peak, looking up the full chemical name(s) and CAS Registry number(s)
for the identifiers that appear in the Varian report, and printing an
injection data processing report. Also, if there is any identifier in your
method which is not detected in the injection, the GCAS will add that
identifier to the data for the injection with a notation of "NOT DETECTED"*
Injections must be processed before they can be used for quality control
calculations, replicate statistics, or dissimilar analysis confirmation.
In Version I of the GCAS, there are three types of concentration calcu-
lations corresponding to three types of sample preparation: 1) purge and
trap,"2) liquid/liquid extraction, and 3) direct aqueous injection. The
GCAS will automatically use the correct algorithm, based on an answer you
gave to a question during method generation.
To initiate the processing routine you must choose master option 6. The
GCAS will always ask for the ID number of the injection to be processed. If
you are using direct aqueous injection, the GCAS will also ask for the
volume of the injection in microliters, and if you are using liquid/liquid
extraction, the GCAS will also ask for the volume of the extract in milli-
liters and the volume of the water extracted in liters.
The rest of the processing procedure is entirely automatic, although
somewhat time-consuming. A sample injection data processing report is shown
in Figure 13.
21
-------
PO
ro
GAS CHROMATOGRAPHY AUTOMATION SYSTEM
I-N-J-E-C-T-I-O-N D-A-T-A P-R-0-C-E-S-S-I-N-G R-E-P-0-R-T
ANALYST: JOHN DOE
METHOD NUMBER: 3001
METHOD TYPE: PURGE AND TRAP
INJECTION ID NUMBER: 13060603
REPORT TITLE: SAMPLE NO. 65487245
DATE: U 6/79
COMPOUND(S)
1. UNEXPLAINED PEAK
2. UNEXPLAINED PEAK
3. CHLOROFORM
4. BROMODICHLOROMETHANE
5. DIERONOCHLOROMETHANE
6. UNEXPLAINED PEAK
7. EROMOFORM
8. UNEXPLAINED PEAK
9. BROMOCHLOROMETHANE
C.A.S.
NUMBER
PEAK RETENTION RELATIVE
TYPE TIME RETENTION TIME
67-66-3
75-27-4
124-48-1
75-25-2
132
154
169
180
191
205
225
231
78.11
91.12
100.00
106.51
113.02
121.30
133.14
136.69
AREA OF
PEAK
970.0
1011.0
5538.0
6838.0
11426.0
1227.0
3048.0
1225.0
CONCENTRATION IN
MICROGRAMS/LITER
45.224
6.951
32.852
6.745
NOT DETECTED
Figure 13. Typical data processing report.
-------
SECTION 11
QUALITY CONTROL
The GCAS is capable of performing four types of quality control calcu-
lations: 1) control (check) standards, 2) spiked samples, 3) duplicate
samples, and 4) surrogate spikes. Before you begin to use any quality
control feature, you must create the necessary concentration patterns and
process the appropriate injections.
CONTROL STANDARDS
To get a control standard report like that shown in Figure 14, you only
need to type the injection ID number and the concentration pattern letter
for your control standard. The concentration pattern should contain the
prepared concentrations for all of the identifiers. The GCAS will allow you
to use the same concentration patterns for calibration standards and control
standards, or establish different concentration patterns for your control
standards. The percent recovery of control standards is calculated by the
formula:
Percent Recover, - »%£* ^cen'^Uon * «»
In the GCAS, it is allowable to process an injection, use it as a
control standard, decide to recalibrate, and use that same injection as a
calibration standard.
SPIKED SAMPLES
To get a spiked sample report like that in Figure 15, you must enter the
injection ID number for the unspiked sample, the concentration pattern for
the spike added values, and the injection ID number for the spiked sample.
The percent recovery of spikes is calculated by the formula:
Percent Recovery = Final Cone. - Prig. Cone.
percent Kecovery Added Cone.
23
-------
DUPLICATE SAMPLES
Figure 16 shows a typical duplicate samples report. To get such a
report, you only need to type the injection ID numbers of the two samples.
SURROGATE SPIKES
You must type the ID number for the injection containing a surrogate
spike, the identifier for the surrogate spike, and the prepared
concentration of the surrogate spike to get a report like that in Figure
17. Obviously, you must have calibrated for the surrogate spike compound to
make this feature work. The percent recovery of surrogate spikes is calcu-
lated by the formula:
Percent Recovery =
Calculated Cone.
Prepared Cone.
x 100.
C-O-N-T-R-O-L S-T-A-N-D-A-R-D R-E-P-0-R-T
INJECTION ID: 13060511 METHOD NUMBER: 8001
CONCENTRATION PATTERN: C
IDENTIFIER
CHCL3
CHBRCL2
CHBR2CL
CHBR3
CH2BRCL
PREPARED
CONCENTRATION
60.000
60.000
60.000
60.000
60.000
CONCENTRATIONS IN MICROGRAMS /LITER
MEASURED
CONCENTRATION
61.888
62.089
59.903
57.979
NOT DETECTED
PERCENT
RECOVERED
103.1%
103.5%
99.8%
96.6%
Figure 14. Typical control standard report.
24
-------
S-P-I-K-E-D S-A-M-P-L-E
INJECTION ID FOR SPIKE ORIGINAL: 13060521
CONCENTRATION PATTERN FOR SPIKE ADDED VALUE:
INJECTION ID FOR SPIKE FINAL: 13060522
CONCENTRATIONS IN MICROGRAMS/LITER
ORIGINAL ADDED
R-E-P-0-R-T
METHOD NUMBER: 8001
C
FINAL PERCENT
IDENTIFIER CONCENTRATION CONCENTRATION CONCENTRATION RECOVERED
CHCL3 61.888 60.000
CHBRCL2 62.089 60.000
CHBR2CL 59.903 60.000
CHBR3 57.979 60.000
117.913 93.4%
117.035 91.6%
115.615 92.9%
114.237 93.8%
CH2BRCL NOT DETECTED 60.000 NOT DETECTED
Figure 15. Typical spiked sample report.
D-U-P-L-I-C-A-T-E S-A-M-P-L-E-S R-E-P-0-R-T
INJECTION
INJECTION
ID FOR FIRST MEMBER: 13060527
METHOD NUMBER: 8001
ID FOR SECOND MEMBER: 13060528
CONCENTRATIONS IN MICROGRAMS/LITER
IDENTIFIER
CHCL3
CHBRCL2
CHBR2CL
CHBR3
CH2BRCL
FIRST
CONCENTRATION
59.668
14.726
49.693
8.412
NOT DETECTED
SECOND
CONCENTRATION
61.345
13.706
52.361
7.722
NOT DETECTED
ABSOLUTE
DIFFERENCE
-1.678
+1.020
-2.667
+0.691
Figure 16. Typical duplicate samples report.
S-U-R-R-O-G-A-T-E S-P-I-K-E
INJECTION ID: 13060532
PREPARED CONCENTRATION OF BROMOCHLOROMETHANE:
CALCULATED CONCENTRATION: 28.019
PERCENT RECOVERED: 93.4%
CONCENTRATIONS IN MICROGRAMS/LITER
R-E-P-0-R-T
METHOD NUMBER:
30.000
8001
Figure 17. Typical surrogate spike report.
25
-------
SECTION 12
REPLICATE STATISTICS
To use the replicate statistics option, you must select master option 8
and type the injection ID numbers for all of your replicate injections. You
may enter up to ten replicates. The GCAS will print a report like that
shown in Figure 18.
R-E-P-L-I-C-A-T-E S-T-A-T-I-S-T-I-C-S R-E-P-0-R-T
METHOD NUMBER: 8001
REPLICATE
IDENTIFIER
CHCL3
CHBRCL2
CHBR2CL
CHBR3
CH2BRCL
CONCENTRATIONS IN MICROGRAMS/LITER
INJECTION ID NUMBERS: 13060536, 13060537, 13060538, 13060539
AVERAGE
CONCENTRATION
22.138
23.923
22.055
17.690
STANDARD
DEVIATION
0.20
0.42
0.03
0.25
NUMBER OF
REPLICATES
4
4
4
4
0
Figure 18. Typical replicate statistics report.
26
-------
SECTION 13
DISSIMILIAR ANALYSIS CONFIRMATION
Master option 9 will allow you to perform a dissimilar analysis
confirmation. The GCAS will handle up to four different methods for this
feature. Also, to allow for Florisil Column Adsorption Chromatography
techniques, you are allowed to enter the injection ID numbers for up to four
injections for each method. Dissimilar analysis confirmation is performed
for only one identifier at a time.
After you have typed your method numbers, injection ID numbers, and
identifier of interest, the GCAS will print a report as shown in Figure 19.
D-I-S-S-I-M-I-L-A-R A-N-A-L-Y-S-I-S C-0-N-F-I-R-M-A-T-I-O-N
IDENTIFIER: CHBR2CL CONCENTRATIONS IN MICROGRAMS/LITER
METHOD INJECTION CALCULATED
NUMBER ID CONCENTRATION
8001 13060536 22.044
8001 13060537 22.073
8002 14060502 22.021
8002 14060503 22.081
Figure 19. Typical dissimilar analysis confirmation report.
27
-------
SECTION 14
SAMPLE FILE CONTROL
The basic plan of Sample File Control (SFC) is that when environmental
samples arrive in the laboratory, they will be logged into the SFC computer
and assigned SFC sample ID numbers. The computer will provide you with a
backlog sheet showing which samples need to be analyzed and what compounds
are to be measured. You will use the GCAS to calculate the concentrations
of the specified compounds, and then the GCAS wiTl enable you to create a
"run results file" which you can send back to SFC. SFC will report the
results to the requestor, and will provide you with control charts and a
historical record of your work.
To create an SFC run results file, you must use master option 10.
Although this option is no more difficult to use than the others, it must be
used very carefully since the GCAS cannot prevent you from sending erroneous
data to SFC, and since the only way to correct most mistakes is to start
over. If you press the ESCAPE key while you are using this option, you will
return to the master options questions, and your incomplete run results file
will be deleted.
When you begin to use this feature, you will be confronted with three
types of SFC interaction: 1) create a new run results file, 2) edit or
delete an existing run results file, or 3) send an existing run results file
to the SFC computer. To create a run results file, you will have to type
the parameter/method code (which can be found on your backlog sheet), the
measurement instrument ID, and your three initials. Then you can place
laboratory control standards data into the run results file by simply typing
the injection ID and concentration pattern letter for each standard. Since
laboratory control standards are not environmental samples, they do not have
SFC sample ID numbers. The SFC system distinguishes between laboratory
control standards and instrument check standards, and it has been decided
that for gas chromatography, instrument check standards will not be reported
to SFC.
Next, you will be able to report the measured concentrations for the
samples on your backlog sheet, along with associated QC results. For each
sample, you must type the SFC sample ID from the backlog sheet, the injec-
tion ID of the sample, the prepared concentration of any surrogate spike,
the injection ID's and concentration pattern letters of any spikes, and the
injection ID's of any duplicates.
28
-------
When you have finished the run results file, the name of that file will
be displayed. The name of a run results file is the parameter/method code
followed by a letter of the alphabet.
Finally, you will be asked again if you want to create, edit, or send
the run results file. You do not have to edit your run results file, but
you must send it to SFC. If you choose the editing feature, you will be
transferred to the RUNEDIT program of the SFC system. Similarity, if you
choose the sending feature, you will be transferred to the SFC program named
SEND. In both of these programs, you will need to know the name of your run
results file. After either of these two programs, you will be returned to
the beginning of the 6CAS. Check the SFC user's guide for instructions on
how to use RUNEDIT and SEND.
29
-------
APPENDIX A
COMMONLY USED CAS REGISTRY NUMBERS
TABLE A-l. The Forty-Six Compounds of the Base-Neutral Fraction
Compound Name
1,3-Di ch1orobenzene
1,4-Dichlorobenzene
1,2-Dichlorobenzene
Hexachloroethane
Bis(2-Ch1oroethyl) ether
Bis(2-Chloroisopropyl) ether
N-nitrosodi-n-propylamine
Isophorone
Nitrobenzene
Hexachlorobutadiene
1,2,4-Trichlorobenzene
Naphthalene
Bis(2-Chloroethoxy)methane
Hexachlorocyclopentadiene
2-Chloronaphthalene
Acenaphthylene
2,6-Dinitrotoluene
Acenaphthene
Dimethylphthalate
Fluorene
4-Chlorophenyl phenyl ether
2,4-Dinitrotoluene
1,2-Diphenylhydrazine
Diethylphthalate
N-Nitrosodiphenylamine
Hexachlorobenzene
4-Bromophenyl phenyl ether
Phenanthrene
Anthracene
Di-n-butylphthalate
Fluoranthene
Pyrene
Benzidine
Butylbenzylphthalate
Bis(2-ethylhexyl)phthalate
Chrysene
CAS Registry Number
541-
106-
95-
67-
111-
39638-
621-
78-
98-
87-
129-
91-
111-
77-
91-
208-
606-
83-
131-
86-
7005-
121-
122-
84-
86-
118-
101-
85-
120-
84-
106-
129-
98-
85-
117-
218-
73-1
46-7
50-1
72-1
44-4
32-9
64-7
59-1
59-1
68-3
82-1
10-3
91-1
47-4
58-7
96-8
20-2
32-9
11-3
73-7
72-3
14-2
66-7
66-2
30-6
74-1
55-3
01-8
12-7
74-2
44-0
00-0
87-5
68-7
81-7
01-9
(continued)
30
-------
TABLE A-l (continued)
Compound Name CAS Registry Number
Benzo(a)anthracene 56-55-3
Benzo(b)fluoranthene 205-99-2
Benzo(k)fluoranthene 207-08-9
3,3'-Dichlorobenzidine 91-94-1
Di-n-octylphthalate 117-84-0
Benzo(a)pyrene 50-32-8
Indeno(l,2,3-cd)pyrene 193-39-5
Dibenzo(a,h)anthracene 53-70-3
Benzo(g,h,i)perylene 191-24-2
Nitrosodimethylamine 62-75-9
31
-------
TABLE A-2. The Twenty-Six Compounds of the Pesticide Fraction
Compound Name CAS Registry Number
P-endosulfan
a-Benzenehexachloride
Y-Benzenehexach1 oride
3-Benzenehexachloride
Aldrin
Heptachlor
Heptachlor epoxide
S-endosulfan
Dieldrin
4,4'-DDE
4,4'-DDD
4,4'-DDT
Endrin
Endosulfane sulfate
5-Benzenehexach1 oride
Chlordane
Toxaphene
Aroclor-1242
Aroclor-1254
Aroclor-1221
Aroclor-1232
Aroclor-1248
Aroclor-1260
Aroclor-1016
2,3,7,8-Tetrachlorodibenzo-p-dioxin
Endrin Aldehyde
33213-65-9
319-84-6
58-89-9
319-85-7
309-00-2
76-44-8
1024-57-3
959-98-8
60-57-1
72-55-9
72-54-8
50-29-3
72-20-8
1031-07-8
319-86-8
57-74-9
8001-35-2
53469-21-9
11097-69-1
11104-28-2
11141-16-5
12672-29-6
11096-82-5
12674-11-2
1746-01-6
32
-------
TABLE A-3. The Thirty Compounds of the Purgeable Fraction and
Two Direct Aqueous Analytes
Compound Name CAS Registry Number
Acrolein 107-02-8
Acrylonitrile 107-13-1
Chloromethane 74-87-3
Dichlorodifluoromethane 75-71-8
Bromomethane 74-83-9
Vinyl chloride 75-01-4
Chloroethane 75-00-3
Methylene chloride 75-09-2
Trichlorofluoromethane 75-69-4
1,1-Dichloroethylene 75-35-4
1,1-Dichloroethane 75-34-3
Trans-l,2-Dichloroethylene 540-59-0
Chloroform 67-66-3
1,2-Dichloroethane 107-06-2
1,1,1-Trichloroethane 71-55-6
Carbon tetrachloride 56-23-5
Bromodichloromethane 75-27-4
Bis(chloromethyl)ether 542-88-1
1,2-Dichloropropane 78-87-5
Benzene 71-43-2
Trans-l,3,-Dichloropropene 542-75-6
Cis-l,3-Dichloropropene 542-75-6
Trichloroethylene 79-01-6
Dibromochloromethane 124-48-1
1,1,2-Trichloroethane 79-00-5
2-Chloroethyl vinyl ether 110-75-8
Bromoform 75-25-2
1,1,2,2-Tetrachloroethene 127-18-4
Toluene 108-88-3
1,1,2,2-Tetrachloroethane 79-34-5
Chlorobenzene 108-90-7
Ethyl Benzene 100-41-4
33
-------
TABLE A-4. The Eleven Compounds of the Acid Fraction
Compound Name CAS Registry Number
Phenol 108-95-2
2-Chlorophenol 95-57-8
2-Nitrophenol 88-75-5
2,4-Dimethylphenol 105-67-9
2,4-Dichlorophenol 120-83-2
p-chloro-m-cresol 59-50-7
2,4,6-Trichlorophenol 88-06-2
2,4-Dinitrophenol 51-28-5
4-Nitrophenol 100-02-7
4,6-Dinitro-o-cresol 534-52-1
Pentachlorophenol 87-86-5
34
-------
APPENDIX B
NOTES TO THE SYSTEM MANAGER
The Gas Chromatography Automation System consists of 22 programs and
potentially thousands of files, all in one directory. The system is
designed to automatically delete old data. The only attention that the GCAS
will need from the system manager will be to add new users and to clean up
after analysts who have stopped using the system. These notes provide the
information necessary for these functions.
ORGANIZATION OF THE DIRECTORY
The GCAS uses only one directory, namely DZO:GCAS60. This directory
must be INITed from the background CLI and never RELEASEd. If DZO:GCAS60 is
inadvertently released, and if any user signs off, all of the other users
will get UNKNOWN DIRECTORY SPECIFIER errors.
Each user has an account ID of four characters beginning with "GC" and
ending with the user's initials. The microcomputer, which the Nova
considers to be a user, has the account ID "MIKE". Figure 20 shows how
BASIC.ID must be organized for the GCAS.
To protect its integrity, the GCAS is designed to prevent any user from
reaching BASIC command level in the directory DZO:GCAS60. When any user
logs in, the program MESSAGE.JT is automatically run, as specified in
BASIC.ID. MESSAGE.JT must be located in the directory DZO:BASIC, and it
must contain the statement CHAIN "INITIALIZE", as shown in Figure 21. In
directory DZO:GCAS60, the program named INITIALIZE will chain into the GCAS,
as shown in Figure 22, but in other directories, INITIALIZE may be used to
start other programs.
An exception to the plan above is necessary to accommodate the micro-
computer which transmits data from the Varian to the Nova. Therefore,
BASIC.ID specifies a different login message, namely MICROLOGIN.JT, for the
account ID MIKE. MICROLOGIN.JT is shown in Figure 23. It must be located
in directory DZO:BASIC. There is one other account ID in BASIC.ID which
uses MICROLOGIN. This allows the programmer to get into DZO:GCAS60 at BASIC
command level for debugging purposes.
35
-------
FILE NAMES IN THE GCAS
File names in the GCAS adhere to the following conventions:
GCNN PROGRAM NAME, where NN is the program number.
GCTTTT METHOD FILE NAME, where TTTT is the method
number.
GCOTTTT TEMPORARY OUTPUT FILE NAME, where TTTT is
the method number.
GCOOOOII ID LIST FILE NAME, where II is the
instrument number.
GCTTTTOCC CONCENTRATION PATTERN FILE NAME, where TTTT
is the method number and CC is the position
of the concentration pattern letter name
in the alphabet.
GCIIMMDDSS INJECTION DATA FILE NAME, where II is the
instrument number, MM is the month, DD is
the day, and SS is the sequence number.
GCOOOOOOOO ARRIVAL FILE NAME.
-.RR SFC RUN RESULTS FILE NAME.
DELETING UNUSED FILES
If an analyst stops using a particular method or instrument, or stops
using the GCAS entirely, many useless files will remain in the system.
Deleting such files can easily be done with the background CLI. To get a
lineprinter listing of all existing method files and their date of last use,
use the CLI command.
LIST/A/L/0/S GC****-
The name of the person who generated a method can be found by using the
method display feature of the GCAS. If you decide to delete a method, you
should also delete all of the concentration patterns associated with that
method. This can be accomplished by the CLI command
DELETE GCTTTT. GCTTTTO**.
where TTTT is the method number.
Similarly, to get a lineprinter listing of all existing ID list files,
use the CLI command
LIST/A/L/0/S GCOOOO**.
36
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If you decide to delete an ID list file, you should also delete all of the
injection data files associated with that ID list file by using the CLI
command
DELETE GCOOOOII. GCII******.
where II is the instrument number.
Never release DZO:GCAS60 after using the background CLI.
GCTB/DZO:GCAS60/MESSAGE.JT
GCDF/DZO:GCAS60/MESSAGE.JT
GCLM/DZO:GCAS60/MESSAGE.JT
GCDM/DZO:GCAS60/MESSAGE.JT
GCBP/DZO:GCAS60/MESSAGE. JT
GCJK/DZO:GCAS60/MICROLOGIN.JT
MIKE/DZO:GCAS60/MICROLOGIN.JT
Figure 20. Required structure of BASIC.ID for the GCAS.
0010 REM
0020 REM + LOGIN MESSAGE
0030 REM 4- PROGRAM NAME: MESSAGE.JT
0040 REM + DO NOT DELETE!
0050 REM +=H-«+>H-'H--^'H-"H-'^-+"H--+"^-+-+
0060 REM
0078 PRINT
0080 PRINT " CALL 7314 TO REPORT ANY PROBLEM WITH THE SYSTEM."
0090 REM
0110 REM + THIS SECTION STARTS AUTOMATION SYSTEMS +
0120 ON ERR THEN GOTO 0140
0130 CHAIN "INITIALIZE"
0140 ON ERR THEN STOP
0150 REM
016,0 ESC
0170 NEW
Figure 21. Required features of MESSAGE.JT for the GCAS.
37
-------
0010 REM
0020 REM
0030 REM
0040 REM
0050 REM
0060 REM
0070 NOESC
0080 PRINT
0090 PRINT
0100 PRINT
0110 PRINT
0120 CHAIN
.=+=+=+=
+ GAS CHROMATOGRAPHY AUTOMATION SYSTEM
+ PROGRAM NAME: INITIALIZE
+ BY: J. KOPKE (SWORCC), JANUARY 25,
"G-A-S C-H-R-0-M-A-T-O-G-R-A-P-H-Y";
" A-U-T-0-M-A-T-I-O-N S-Y-S-T-E-M"
"GCOO" THEN GOTO 0100
1979
Figure 22. Kequired features of INITIALIZE for the GCAS.
0010 REM
0020 REM
0030 REM
0040 REM
0050 REM
0080 ESC
0090 NEW
+=+=H
=+
=+=+=+=+=+=+=f=+=H
+ LOGIN MESSAGE FOR MICROCOMPUTER
+ PROGRAM NAME: MICROLOGIN.JT
+ DO NOT DELETE!
+=+=+=+=H-=+=+=+=+=+=f=f=+=4-=+=+=+=+=+=+=H
Figure 23. Required features of MICROLOGIN.JT for the GCAS.
38
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TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing)
1. REPORT NO. 2
EPA-600/4-79-067
4. TITLE AND SUBTITLE
User's Guide for the Gas Chromatography Automatic
System
7. AUTHOR(S)
Jonathan E. Kopke
9. PERFORMING ORGANIZATION NAME AND ADDRESS
Southwestern Ohio Regional Computer Center
University of Cincinnati
Cincinnati , Ohio 45220
12. SPONSORING AGENCY NAME AND ADDRESS
Environmental Monitoring & Support Lab. - Cinn, OH
Office of Research and Development
U.S. Environmental Protection Agency
Cincinnati, OH 45268
15. SUPPLEMENTARY NOTES
3. RECIPIENT'S ACCESSION-NO.
5. REPORT DATE
n October 1979
6. PERFORMING ORGANIZATION CODE
8. PERFORMING ORGANIZATION REPORT NO.
10. PROGRAM ELEMENT NO.
11. CONTRACT/GRANT NO.
GS-05S-10458
13. TYPE OF REPORT AND PERIOD COVERED
14. SPONSORING AGENCY CODE
EPA/600/06
16. ABSTRACT
This document was written as a guide for users of the Advanced GC data
system (EPA-600/4-79-038).
The document contains the prescribed procedures for operating the advanced
GC system from a user's viewpoint. Also contained in the document is a description
of the system manager's duties and responsibilities in maintaining the GC system.
17. KEY WORDS AND DOCUMENT ANALYSIS
a. DESCRIPTORS b.lDENTIFI
Gas Chromatography
Calibrating
Quality Assurance
Computers
18. DISTRIBUTION STATEMENT 19. SECURI
,. r, L-, Uncla
Release to Public
r\CICOjC lAJ ruuiiv, 20. SECURI
Uncla
ERS/OPEN ENDED TERMS
TY CLASS (This Report)
ssified
TY CLASS (This page)
ssified
c. COS AT I Field/ Group
09/B
14/B
07/C
21. NO. OF PAGES
45
22. PRICE
EPA Form 2220-1 (9-73)
39
a u.s. OMCMUITiwmKomct an -657-146/5444
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