PAMS AutoGC€¦ · Temperatures Transfer line 200 ºC Valve 150 ºC Tube 0 ºC Trap –low -30 ºC...

September 26, 2018TCEQ Operator Training 1

AutoGC

Operator Training

Heath HinojosaHeath@orsat.com

Orsat, LLC

www.orsat.com

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

PerkinElmer AutoGC System

Totalchrom

Data System

NCI 902 Inte

Turbomatrix

Thermal Desorber

Clarus Gas

Chromatograph

PerkinElmer AutoGC System

DVINafion

Ballast

Tank to backup air cylinder

Zero Air

Purifier

Flow meter

In Line Regulator

Ballast

TOC Gas

Generator

Compressor

Auto Drain

Diluter

AutoGC Air SystemHC Free Zero Air

for FIDs

HC Free & Dry (-50º DP)

Zero Air for Pelier Cooler

and Nafion Drier

Temperatures

Transfer line 200 ºC

Valve 150 ºC

Tube 0 ºC

Trap – low -30 ºC

Trap – high 325 ºC

Rate 40 ºC/min

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

Nafion flow 0.15 – 0.30 Lpm.

AutoGC Methods - Turbomatrix

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

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

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

AutoGC Overlapping Sample Collection and Analysis

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

Sample Collection and Analysis

Sample Collection

Sample AnalysisFID A

BP1 Column

PLOT Column

Restrictor

Outlet Split

Nafion® Drier

Sample Pump

Weak Strong

C2 C3–C10

Collection Desorption

Trap Heat

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

AutoGC Totalchrom Sequences

ABSK25A.rst

hourday

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

Building Sequences

AutoGC EZ Sequence

Building Sequences

This import sequence is

properly configured for

the necessary 2-channel

operations

Save and Load Sequence

To Load Sequence:

• Find the row for the

starting sample hour

• Use Setup from the TC

Navigator

• Enter the sequence

filename and row to

Setting Up the Sequence to Run

Instrument Loading Sequence into GC Memory – Setting Up

Details: Clarus GC Integral Interface vs. NCI902 A/D Interface

Modifying the Active Sequence

Modifying Sequences

To Modify a sequence:

• Instrument Method

• Sample Name

• File Name

For both Channels

Modifying Sequences

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.

Modifying Sequences

Audit samples or

additional retention time

check samples can be

scheduled to run when

needed.

Modifying Sequences

After saving the

modified sequence the

system prompts for the

next starting row to

resume.

Resetting the Sequence row

If your system gets off-

time, you can reset the

sequence by simply

using pause and resume

to choose a different

Calibration Curves

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

Calibration Curves – MMSD Spreadsheet

The Blender Spreadsheet

is a useful tool for

tracking system

performance and

documenting calibration

curves. This workbook is

protected and highly

linked.

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.

The LCS Statically diluted

second source standard

concentrations and

dilution factor will be

entered on the LCS

worksheet for tracking

LCS recoveries.

A worksheet is also

provided for calculating

weekly precision checks.

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.

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.

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

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

Totalchrom Methods

Instrument Methods

and Process Methods

are the same, but are

used differently

Instrument Methods – xx-Sample.mth

Methods which are

designated as

Instrument methods in

the sequence will

control the instrument

parameters.

There is no carrier

designated in the

Instrument Methods

since the carrier flow

is being supplied by

the Turbomatrix

The Aux 2 carrier is

used to supply the

mid-point pressure

used by the Dean’s

switch.

Detector settings are

the same for both

channels

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.

There should be

nothing entered into

the component list on

any instrument

method

Process Methods – xx-PLOT.mth

Process Methods contain

only the information

necessary for peak

identification and

quantitation. There is

one Process method for

each detector

signal/column.

You can review the

Method Summary or

the Component List by

selecting which

window is shown.

All the information for

the components in the

PLOT chromatogram can

be reviewed here,

however optimization is

more easily accomplished

graphically.

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.

Process parameters

such as integration

events can be reviewed

and defaults changed

globally. However,

optimization is better

done in Graphic Editor.

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.

While most

optimization occurs in

the Graphic Editor,

calibration information

must be entered

directly into the

method.

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.

Since the system uses

a carbon response

factor for all

components it also

must be entered

directly into each

method.

You can review the

parameters for

each component by

double clicking on

any one in the list.

Process Methods – xx-BP1.mth

The BP1 Method is

setup the same as the

PLOT but with a

different component

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.

Modifying Methods

Method are protected

from editing by CAMS

locks when the system

is running. To modify

methods these CAMS

locks must be

removed.

Modifying Methods

Remove CAMS locks by

deleting the methods

from the CAMS

Administration list.

Modifying Methods

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.

Modifying Methods

Edit Methods using the

Build Method icon in

the Totalchrom

Navigator.

Modifying Methods

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.

Calibration Curves – Updating Process Methods for RF

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.

Modifying Methods – Updating Process Methods for RF

In the Global

Information section of

the method the

response factor is used

to calculate the

concentration of all

unidentified peaks on

each column.

Modifying Methods – Updating Process Methods for RF

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.

Optimizing Methods for Peak Identification

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.

After removing CAMS

locks and opening the

method use the Other

Graphic Editor to

graphically adjust

retention time

windows in each

method.

The weekly RTS check is

a good place to start

since all the target

compounds will be in

this sample.

Analytical Tools and Software to Assess Site Performance

Site Reports (Orsat)

Remote Connection/Site Visit

MAX - Merlin AutoGC Xplorer

Totalchrom Software – Overlaying Chromatograms

Analytical Tools and Software to Assess Site Performance:

E:\Operator presentation\18_09_18_a_clinton.xls

Site Reports

Rhone - Resources

Rhone – QC Report

Rhone – Monthly Report by Site

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

Remote connection/Site Visit

http://prod.orsatmax.com/login

MAX – Merlin AutoGC Xplorer

Chromatograms – Overlaying Chromatograms

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.

System Status

Binding the Instrument

Method Loss

Port Comm Error

Unknown Instrument/Reconfigure Steps

Clarus GC Integral Interface: Understanding the TotalChrom

Software Appearance and Common Software Errors

Clarus GC Integral Interface: System Status Ready

Clarus GC Integral Interface: Binding the Instrument

Clarus GC Integral Interface: Port Comm Error

Ensure the GC interface cable is connected.

Clarus GC Integral Interface: Method and Sequence Loss

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

Clarus GC Integral Interface: Unknown Instrument/Reconfigure

Continue to select Yes and OK to each

command prompt until reconfiguration is

complete.

Questions?

Concerns?

Feed Back?

Thank you all for your time and attention. Good luck!

Heath Hinojosa

Environmental Field Service Engineer

281.797.2291

Heath@orsat.com

Orsat, LLC

www.orsat.com

PAMS AutoGC€¦ · Temperatures Transfer line 200 ºC Valve 150 ºC Tube 0 ºC Trap –low -30 ºC...

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