PAMS AutoGC€¦ · Temperatures Transfer line 200 ºC Valve 150 ºC Tube 0 ºC Trap –low -30 ºC...
Transcript of PAMS AutoGC€¦ · Temperatures Transfer line 200 ºC Valve 150 ºC Tube 0 ºC Trap –low -30 ºC...
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September 26, 2018TCEQ Operator Training 1
PAMS
AutoGC
Operator Training
Heath [email protected]
Orsat, LLC
www.orsat.com
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AUTOGC SYSTEM OVERVIEW
AutoGC Overview of VOC Analysis
Description of Equipment Functionality
Overview
Air System
Thermal Desorber Method
Gas Chromatographic Method
Chromatographic Data System
Analytical Method
Collection using Sequences
Data Processing and File management
OPERATOR ACTIVITIES
Building Sequences
EZ Sequence sequence generator
Initiation of sequences
Modifying sequences
Calibration
Merlin MicroScience Dilution System
Site Spreadsheet
Optimizing Methods
Updating retention times
Using Overlay Chromatograms
2018 TCEQ Operator Training
September 26, 2018TCEQ Operator Training 2
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PerkinElmer AutoGC System
September 26, 2018TCEQ Operator Training 3
Totalchrom
Data System
NCI 902 Inte
rface
Turbomatrix
Thermal Desorber
Clarus Gas
Chromatograph
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PerkinElmer AutoGC System
September 26, 2018TCEQ Operator Training 4
DVI
TD
DVINafion
Ballast
Tank to backup air cylinder
Zero Air
Purifier
Flow meter
In Line Regulator
Ballast
Tank
TOC Gas
Generator
Compressor
Auto Drain
GC
Diluter
AutoGC Air SystemHC Free Zero Air
for FIDs
HC Free & Dry (-50º DP)
Zero Air for Pelier Cooler
and Nafion Drier
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Temperatures
Transfer line 200 ºC
Valve 150 ºC
Tube 0 ºC
Trap – low -30 ºC
Trap – high 325 ºC
Rate 40 ºC/min
Times
Cycle 60 min.
Sampling 40 min.
Trap Hold 6 min.
Desorb 1 min.
Purge 1 min.
Options
Mode Online
Outlet split checked
Inlet split unchecked
Heated purge unchecked
Cycles 99
Pneumatics
Outlet split 1.0 – 3.0 mL/min.
Desorb vent ~ 10.0 mL/min.
Column 40.5 – 43.5 psig.
Pump 10-15 mL/min.
Inlet split N/A
Other
Nafion flow 0.15 – 0.30 Lpm.
AutoGC Methods - Turbomatrix
September 26, 2018TCEQ Operator Training 5
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Oven Temperature Profile
Initial Temperature 45 ºC
Initial time 15 min.
Ramp rate 1 5 ºC /min.
Temperature 1 170 ºC
Hold time 1 0 min.
Ramp rate 2 15 ºC /min.
Temperature 2 200 ºC
Final hold time 6 min.
Configuration
Valve 2 initial Off
Events
Valve 2 on 0.1 min.
Valve 2 off 8.0 – 13.0 min.
FID Parameters
Temperature 250 ºC
mV signal 0.12 – 0.40 mV
Attenuation x1
Range x1
Output Integrator
Offset 5.0 mV
Filter 200 ms
Flows and Pressures
Carrier pressure 12-18 psig.
FID air flow 350 – 400 mL/min.
FID H2 flow 35-40 mL/min.
Preset Air regulator 50-80 psig.
AutoGC Methods – Clarus Gas Chromatograph
September 26, 2018TCEQ Operator Training 6
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SYSTEMS WITH NCI902 INTERFACE
Totalchrom only collects signals from each FID
Cut-time is set only from the GC
Instrument method contains relay events to control sample type
X-sample.mth - ambient sample collection
X-cal.mth - collects diluted standard from blender
X-blank.mth – collects only diluent from blender
X-lcs.mth – collects static dilution LCS
X-rts.mth – collects full 40 min. sample from RTS can
X-spike.mth – collects 2 min. from RTS can and 38 min. of diluent from blender
SYSTEMS WITH INTEGRAL INTERFACE
Totalchrom controls all setpoints in Clarus GC for temperatures and flows
Totalchrom controls the cut-time in the method.
Totalchrom controls relay events to control samples selected
X-sample.mth - ambient sample collection
X-cal.mth - collects diluted standard from blender
X-blank.mth – collects only diluent from blender
X-lcs.mth – collects static dilution LCS
X-rts.mth – collects full 40 min. sample from RTS can
X-spike.mth – collects 2 min. from RTS can and 38 min. of diluent from blender
AutoGC Methods – Totalchrom Instrument Methods
September 26, 2018TCEQ Operator Training 7
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PLOT METHOD
Controls peak detection and
integration of all PAMS targets in the
PLOT column chromatogram
Detector signal = FID A
All components must go through the
BP1 column first
Last target component on the PLOT
column determines the cut-time on
the GC (2-methyl-1-pentene or 1-
hexane)
BP1 METHOD
Controls peak detection and
integration of all PAMS targets in the
BP1 column chromatogram
Detector signal = FID B
Connects to the Deans switch and
flows first to the PLOT column and
then to a deactivated restrictor after
the Deans switch time.
After Deans switch first peak to elute
from the BP1 column is n-Hexane
AutoGC Methods – Totalchrom Process Methods
September 26, 2018TCEQ Operator Training 8
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AutoGC Overlapping Sample Collection and Analysis
September 26, 2018TCEQ Operator Training 9
0 10 20 30 40 50 60
0 10 20 30 40 50 60
Collect Sample
Desorb
Heat Trap & Hold
Recycle to -30 degrees
Turbomatrix
System Ready
Start Analysis
Recycle
Gas Chromatograph
System Ready
Collecting Data
Process Data
Data System
0 10 20 30 40
48
48
40
101
7
1
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Sample Collection and Analysis
September 26, 2018TCEQ Operator Training 10
Sample Collection
Sample AnalysisFID A
FID B
FID A
FID B
BP1 Column
PLOT Column
Restrictor
Outlet Split
Nafion® Drier
Sample Pump
Trap
Weak Strong
C2 C3–C10
Collection Desorption
Trap Heat
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Sequences are used to automate sample collection
Allows for repeated unattended sample analysis
Specifies necessary instrument file for each hour
Applies processing method to each raw signal collection
Generates results files and ASCII text report files
EZ Sequence Visual Basic program
To generate a sequence which schedules daily check samples and weekly QC samples
Provides descriptive information of the collection hour for each sample
Generates unique filename based on site, sample type, month, day and hour of sample collection
September 26, 2018TCEQ Operator Training 11
AutoGC Totalchrom Sequences
ABSK25A.rst
hourday
month
Sample type
ColumnSite
Site designation: up to 3 alpha-numeric characters
Column: B = BP1; P = PLOT
Sample type: S = ambient; C = CVS; B = Blank; E = LCS; Q = RTS; D = MDL; M = multipoint
Month: A = Jan; B = Feb ….. L = Dec
Day: day-of-month
Hour: A = 00, B = 01, C = 03 …. X = 23
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Building Sequences
AutoGC EZ Sequence
September 26, 2018TCEQ Operator Training 12
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Building Sequences
September 26, 2018TCEQ Operator Training 13
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Building Sequences
September 26, 2018TCEQ Operator Training 14
This import sequence is
properly configured for
the necessary 2-channel
operations
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Save and Load Sequence
September 26, 2018TCEQ Operator Training 15
To Load Sequence:
• Find the row for the
starting sample hour
• Use Setup from the TC
Navigator
• Enter the sequence
filename and row to
start
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Setting Up the Sequence to Run
September 26, 2018TCEQ Operator Training 16
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Setting Up the Sequence to Run
September 26, 2018TCEQ Operator Training 17
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Setting Up the Sequence to Run
September 26, 2018TCEQ Operator Training 18
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Instrument Loading Sequence into GC Memory – Setting Up
September 26, 2018TCEQ Operator Training 19
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Details: Clarus GC Integral Interface vs. NCI902 A/D Interface
September 26, 2018TCEQ Operator Training 20
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Modifying the Active Sequence
September 26, 2018TCEQ Operator Training 21
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Modifying the Active Sequence
September 26, 2018TCEQ Operator Training 22
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Modifying Sequences
September 26, 2018TCEQ Operator Training 23
To Modify a sequence:
• Instrument Method
• Sample Name
• File Name
For both Channels
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Modifying Sequences
September 26, 2018TCEQ Operator Training 24
The same process is used
to schedule Calibration
curves. Calibrations are
run manually by changing
the setpoints on the
dilution system after the
sequence has been setup.
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Modifying Sequences
September 26, 2018TCEQ Operator Training 25
Audit samples or
additional retention time
check samples can be
scheduled to run when
needed.
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Modifying Sequences
September 26, 2018TCEQ Operator Training 26
After saving the
modified sequence the
system prompts for the
next starting row to
resume.
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Resetting the Sequence row
September 26, 2018TCEQ Operator Training 27
If your system gets off-
time, you can reset the
sequence by simply
using pause and resume
to choose a different
row.
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Calibration Curves
September 26, 2018TCEQ Operator Training 28
Automatic introduction of QC
samples
Dynamically diluted check
standard
Analytical blank
Manual dilution of multipoint
calibration curve
Dilution from 100 ppbv or 1
ppmv multi-component standard
Merlin MicroScience Dilution System
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Calibration Curves – MMSD Spreadsheet
September 26, 2018TCEQ Operator Training 29
The Blender Spreadsheet
is a useful tool for
tracking system
performance and
documenting calibration
curves. This workbook is
protected and highly
linked.
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Calibration Curves – MMSD Spreadsheet
September 26, 2018TCEQ Operator Training 30
The current CVS Standard
is entered into the CVS
Worksheet. This allows
operators to enter the
measured concentrations
from their nightly check
samples and see the
recoveries.
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Calibration Curves – MMSD Spreadsheet
September 26, 2018TCEQ Operator Training 31
The LCS Statically diluted
second source standard
concentrations and
dilution factor will be
entered on the LCS
worksheet for tracking
LCS recoveries.
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Calibration Curves – MMSD Spreadsheet
September 26, 2018TCEQ Operator Training 32
A worksheet is also
provided for calculating
weekly precision checks.
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Calibration Curves – MMSD Spreadsheet
September 26, 2018TCEQ Operator Training 33
The Blender Ratios worksheet shows the calibrated flows and allows operators to
enter pressures and see resulting flow rates. It also has a section for recording
annual flow checks.
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Calibration Curves – MMSD Spreadsheet
September 26, 2018TCEQ Operator Training 34
The Curve worksheet shows the pressures and resulting blend ratios used for the calibration
curve. Operators must change pressure settings for each sample collection and record the
resulting area counts for propane and benzene.
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INSTRUMENT METHODS
A single method for control of the gas
chromatographic parameters
Includes temperatures and pressures
as well as valve event for Deans switch
Includes relay events to control
samples collected on the Turbomatrix
All instrument methods are designed
to be exactly the same except for
valving required to change sample
types
PROCESS METHODS
A single method for each signal, 2
methods for each sample collection
Contains all targets and their expected
retention times for identification
Contains response factor to be used to
quantitate all identified targets.
Also contains noise and area thresholds
and bunching factors used to facilitate
accurate peak identification
Totalchrom Methods – Dual Channel Methods
September 26, 2018TCEQ Operator Training 36
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Totalchrom Methods
September 26, 2018TCEQ Operator Training 37
Instrument Methods
and Process Methods
are the same, but are
used differently
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Instrument Methods – xx-Sample.mth
September 26, 2018TCEQ Operator Training 38
Methods which are
designated as
Instrument methods in
the sequence will
control the instrument
parameters.
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Instrument Methods – xx-Sample.mth
September 26, 2018TCEQ Operator Training 39
There is no carrier
designated in the
Instrument Methods
since the carrier flow
is being supplied by
the Turbomatrix
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Instrument Methods – xx-Sample.mth
September 26, 2018TCEQ Operator Training 40
The Aux 2 carrier is
used to supply the
mid-point pressure
used by the Dean’s
switch.
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Instrument Methods – xx-Sample.mth
September 26, 2018TCEQ Operator Training 41
Detector settings are
the same for both
channels
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Instrument Methods – xx-Sample.mth
September 26, 2018TCEQ Operator Training 42
Instrument Methods
also contain the relay
events necessary to
determine which
sample is being
collected by the
Turbomatrix. This
means there must be a
different Instrument
method for each
sample type.
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Instrument Methods – xx-Sample.mth
September 26, 2018TCEQ Operator Training 43
There should be
nothing entered into
the component list on
any instrument
method
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Process Methods – xx-PLOT.mth
September 26, 2018TCEQ Operator Training 44
Process Methods contain
only the information
necessary for peak
identification and
quantitation. There is
one Process method for
each detector
signal/column.
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Process Methods – xx-PLOT.mth
September 26, 2018TCEQ Operator Training 45
You can review the
Method Summary or
the Component List by
selecting which
window is shown.
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Process Methods – xx-PLOT.mth
September 26, 2018TCEQ Operator Training 46
All the information for
the components in the
PLOT chromatogram can
be reviewed here,
however optimization is
more easily accomplished
graphically.
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Process Methods – xx-PLOT.mth
September 26, 2018TCEQ Operator Training 47
The Instrument section
of the method has
default values that are
not used when the
method is designated
in the sequence as a
process method.
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Process Methods – xx-PLOT.mth
September 26, 2018TCEQ Operator Training 48
Process parameters
such as integration
events can be reviewed
and defaults changed
globally. However,
optimization is better
done in Graphic Editor.
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Process Methods – xx-PLOT.mth
September 26, 2018TCEQ Operator Training 49
The user programs tab is
used to designate the
use of a user program
like mmove to be
executed at the end of
a chromatographic run.
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Process Methods – xx-PLOT.mth
September 26, 2018TCEQ Operator Training 50
While most
optimization occurs in
the Graphic Editor,
calibration information
must be entered
directly into the
method.
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Process Methods – xx-PLOT.mth
September 26, 2018TCEQ Operator Training 51
Once the response
factor is determined
when running a
calibration curve it
must be entered in the
global information to
be used for all
unidentified peaks.
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Process Methods – xx-PLOT.mth
September 26, 2018TCEQ Operator Training 52
Since the system uses
a carbon response
factor for all
components it also
must be entered
directly into each
method.
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Process Methods – xx-PLOT.mth
September 26, 2018TCEQ Operator Training 53
You can review the
parameters for
each component by
double clicking on
any one in the list.
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Process Methods – xx-BP1.mth
September 26, 2018TCEQ Operator Training 54
The BP1 Method is
setup the same as the
PLOT but with a
different component
list.
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Process Methods – xx-PLOT.mth
September 26, 2018TCEQ Operator Training 55
The Mmove user
program is initiated
from the BP1 method
at the end of the
analysis. Mmove
makes copies of the
ASCII text file and
moves them to the
polling directory
hourly. It also archives
the daily data.
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Modifying Methods
September 26, 2018TCEQ Operator Training 56
Method are protected
from editing by CAMS
locks when the system
is running. To modify
methods these CAMS
locks must be
removed.
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Modifying Methods
September 26, 2018TCEQ Operator Training 57
Remove CAMS locks by
deleting the methods
from the CAMS
Administration list.
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Modifying Methods
September 26, 2018TCEQ Operator Training 58
Once the methods are
removed from the list
you may edit them
without interruption.
This applies to Process
methods. Removing
locks from instrument
methods or sequences
could result in errors.
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Modifying Methods
September 26, 2018TCEQ Operator Training 59
Edit Methods using the
Build Method icon in
the Totalchrom
Navigator.
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Modifying Methods
September 26, 2018TCEQ Operator Training 60
If you do not see your
method in the recently
edited method list you
may use Load method
stored on disk to
browse to the
D:\TC\xx-meth
directory where all
your active methods
should be.
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Calibration Curves – Updating Process Methods for RF
September 26, 2018TCEQ Operator Training 61
When calibration curves
are run and new
Response Factors (RF)
are calculated they must
be entered into the
methods. This is done
from the Components
drop-down menu. RFs
are entered in the Global
Information and in the
Change Calibration Info
sections of the method.
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Modifying Methods – Updating Process Methods for RF
September 26, 2018TCEQ Operator Training 62
In the Global
Information section of
the method the
response factor is used
to calculate the
concentration of all
unidentified peaks on
each column.
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Modifying Methods – Updating Process Methods for RF
September 26, 2018TCEQ Operator Training 63
To change the response
factor for all target
compounds the new RF
must be entered using
the Change calibration
type check box and
entering the new RG
under use calibration
factor. Both the
change calibration
information and global
information must be
updated each time the
RF changes.
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Optimizing Methods for Peak Identification
September 26, 2018TCEQ Operator Training 64
Many factors can cause
peaks to be incorrectly
identified. Operators
must review
chromatograms often
to insure all targets
are being identified
correctly. Occasionally
method must be
“optimized” and
retention time
windows adjusted.
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Optimizing Methods for Peak Identification
September 26, 2018TCEQ Operator Training 65
After removing CAMS
locks and opening the
method use the Other
Graphic Editor to
graphically adjust
retention time
windows in each
method.
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Optimizing Methods for Peak Identification
September 26, 2018TCEQ Operator Training 66
The weekly RTS check is
a good place to start
since all the target
compounds will be in
this sample.
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Optimizing Methods for Peak Identification
September 26, 2018TCEQ Operator Training 67
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Optimizing Methods for Peak Identification
September 26, 2018TCEQ Operator Training 68
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Optimizing Methods for Peak Identification
September 26, 2018TCEQ Operator Training 70
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Optimizing Methods for Peak Identification
September 26, 2018TCEQ Operator Training 71
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Optimizing Methods for Peak Identification
September 26, 2018TCEQ Operator Training 72
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Optimizing Methods for Peak Identification
September 26, 2018TCEQ Operator Training 73
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Optimizing Methods for Peak Identification
September 26, 2018TCEQ Operator Training 74
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Optimizing Methods for Peak Identification
September 26, 2018TCEQ Operator Training 75
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Optimizing Methods for Peak Identification
September 26, 2018TCEQ Operator Training 76
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Optimizing Methods for Peak Identification
September 26, 2018TCEQ Operator Training 77
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Optimizing Methods for Peak Identification
September 26, 2018TCEQ Operator Training 78
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Optimizing Methods for Peak Identification
September 26, 2018TCEQ Operator Training 79
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Optimizing Methods for Peak Identification
September 26, 2018TCEQ Operator Training 80
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Optimizing Methods for Peak Identification
September 26, 2018TCEQ Operator Training 81
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Optimizing Methods for Peak Identification
September 26, 2018TCEQ Operator Training 82
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Optimizing Methods for Peak Identification
September 26, 2018TCEQ Operator Training 83
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Optimizing Methods for Peak Identification
September 26, 2018TCEQ Operator Training 84
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Optimizing Methods for Peak Identification
September 26, 2018TCEQ Operator Training 85
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September 26, 2018TCEQ Operator Training 86
Analytical Tools and Software to Assess Site Performance
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Site Reports (Orsat)
Rhone
Remote Connection/Site Visit
MAX - Merlin AutoGC Xplorer
Totalchrom Software – Overlaying Chromatograms
September 26, 2018TCEQ Operator Training 87
Analytical Tools and Software to Assess Site Performance:
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E:\Operator presentation\18_09_18_a_clinton.xls
September 26, 2018TCEQ Operator Training 88
Analytical Tools and Software to Assess Site Performance:
Site Reports
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September 26, 2018TCEQ Operator Training 89
Analytical Tools and Software to Assess Site Performance:
Rhone - Resources
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September 26, 2018TCEQ Operator Training 90
Analytical Tools and Software to Assess Site Performance:
Rhone – QC Report
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September 26, 2018TCEQ Operator Training 91
Analytical Tools and Software to Assess Site Performance:
Rhone – Monthly Report by Site
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TotalChrom Details: view sequence file,
current row, sample date and hour
D: Current folder – RST files, TXO files, TDS
D: Archive folder – Weekend files: LCS, RTS
spike, CVS, blanks, Daily Zip files
Site Visit: Instrument displays for splash
screens(power failures), TD event log,
equipment, support gas, and QC standards
for pressure/flow measurements
September 26, 2018TCEQ Operator Training 92
Analytical Tools and Software to Assess Site Performance:
Remote connection/Site Visit
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http://prod.orsatmax.com/login
September 26, 2018TCEQ Operator Training 93
Analytical Tools and Software to Assess Site Performance:
MAX – Merlin AutoGC Xplorer
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Analytical Tools and Software to Assess Site Performance:
Chromatograms – Overlaying Chromatograms
September 26, 2018TCEQ Operator Training 94
The Chromatograms Icon
in the TC Navigator will
allow operators to overlay
multiple chromatograms.
This allows evaluation of
the amount of retention
time shifting is occurring
as well as facilitate
determining if peaks at
low concentrations are
being correctly identified.
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Analytical Tools and Software to Assess Site Performance:
Chromatograms – Overlaying Chromatograms
September 26, 2018TCEQ Operator Training 95
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Analytical Tools and Software to Assess Site Performance:
Chromatograms – Overlaying Chromatograms
September 26, 2018TCEQ Operator Training 96
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Analytical Tools and Software to Assess Site Performance:
Chromatograms – Overlaying Chromatograms
September 26, 2018TCEQ Operator Training 97
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Analytical Tools and Software to Assess Site Performance:
Chromatograms – Overlaying Chromatograms
September 26, 2018TCEQ Operator Training 98
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Analytical Tools and Software to Assess Site Performance:
Chromatograms – Overlaying Chromatograms
September 26, 2018TCEQ Operator Training 99
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Analytical Tools and Software to Assess Site Performance:
Chromatograms – Overlaying Chromatograms
September 26, 2018TCEQ Operator Training 100
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Analytical Tools and Software to Assess Site Performance:
Chromatograms – Overlaying Chromatograms
September 26, 2018TCEQ Operator Training 102
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Analytical Tools and Software to Assess Site Performance:
Chromatograms – Overlaying Chromatograms
September 26, 2018TCEQ Operator Training 103
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Analytical Tools and Software to Assess Site Performance:
Chromatograms – Overlaying Chromatograms
September 26, 2018TCEQ Operator Training 104
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Analytical Tools and Software to Assess Site Performance:
Chromatograms – Overlaying Chromatograms
September 26, 2018TCEQ Operator Training 105
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Analytical Tools and Software to Assess Site Performance:
Chromatograms – Overlaying Chromatograms
September 26, 2018TCEQ Operator Training 106
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Analytical Tools and Software to Assess Site Performance:
Chromatograms – Overlaying Chromatograms
September 26, 2018TCEQ Operator Training 107
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System Status
Binding the Instrument
Method Loss
Port Comm Error
Unknown Instrument/Reconfigure Steps
September 26, 2018TCEQ Operator Training 108
Clarus GC Integral Interface: Understanding the TotalChrom
Software Appearance and Common Software Errors
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September 26, 2018TCEQ Operator Training 109
Clarus GC Integral Interface: System Status Ready
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September 26, 2018TCEQ Operator Training 110
Clarus GC Integral Interface: System Status Ready
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Clarus GC Integral Interface: Binding the Instrument
September 26, 2018TCEQ Operator Training 111
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Clarus GC Integral Interface: Port Comm Error
September 26, 2018TCEQ Operator Training 112
Ensure the GC interface cable is connected.
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Clarus GC Integral Interface: Method and Sequence Loss
September 26, 2018TCEQ Operator Training 113
Due to power outages.
System will continue to run without
the sequence but will not create any
data files.
Reloading the sequence is necessary.
(Approximately 6 minutes to load)
CMD: None, Not Ready, Ready, Run
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Clarus GC Integral Interface: Unknown Instrument/Reconfigure
September 26, 2018TCEQ Operator Training 114
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Clarus GC Integral Interface: Unknown Instrument/Reconfigure
September 26, 2018TCEQ Operator Training 115
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Clarus GC Integral Interface: Unknown Instrument/Reconfigure
September 26, 2018TCEQ Operator Training 116
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Clarus GC Integral Interface: Unknown Instrument/Reconfigure
September 26, 2018TCEQ Operator Training 117
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Clarus GC Integral Interface: Unknown Instrument/Reconfigure
September 26, 2018TCEQ Operator Training 118
Continue to select Yes and OK to each
command prompt until reconfiguration is
complete.
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Clarus GC Integral Interface: Unknown Instrument/Reconfigure
September 26, 2018TCEQ Operator Training 119
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Clarus GC Integral Interface: Unknown Instrument/Reconfigure
September 26, 2018TCEQ Operator Training 120
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Clarus GC Integral Interface: Unknown Instrument/Reconfigure
September 26, 2018TCEQ Operator Training 121
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Questions?
Concerns?
Feed Back?
Thank you all for your time and attention. Good luck!
September 26, 2018TCEQ Operator Training 122
Heath Hinojosa
Environmental Field Service Engineer
281.797.2291
Orsat, LLC
www.orsat.com