GAS CHROMATOGRAPHY

Group 3
Section Outline
About the apparatus
01 • Equipment’s Description
• Principles
• Parts and functions

How to use the apparatus

02 • Sample Preparations
• Equipment Operation / Sample Testing
• Data Reporting and Interpretation

Maintenance and Troubleshooting

03 • Calibration/Equipment Maintenance
• Troubleshooting

04 Reference
PERKIN
E L M E R
Clarus 580
Gas
Chromatography
I. ABOUT THE APPARATUS
All
About
The
Apparatus
Perkin Elmer Clarus® 580 GC
A fully automated gas chromatograph.
The system offers the capabilities
required for laboratories performing
large numbers of routine analyses as
well as those involved in research
and development.
The industry leading system that
makes it easy to query data, submit
samples and generate results with the
highest degree of confidence.
Principle
of the
apparatus
The basic principal of
gas chromatography
is that greater the
affinity of the
compound for the
stationary phase,
more the compound
will be retained by the
column and longer it
will be before it is
eluted and detected
 Parts and functions

Touch Screen Interface

• Makes method development easy by
providing immediate access to all method
parameters in any order.

• Wherein all instrument functions are set

up and monitored.
 Parts and functions

Oven
• The oven gives excellent temperature
control and fast cool-down times for
maximum productivity.

• All temperature and time functions are

microprocessor controlled and are shown
on the touch-screen display.
 Parts and functions

Autosampler
• A full range of pneumatic options provides
optimum performance with all types of
columns and detectors.
 Parts and functions

Pneumatics
• A full range of pneumatic options provides
optimum performance with all types of
columns and detectors.
 Parts and functions

Detectors
•A wide choice of detectors optimized
for sensitivity and selectivity is available
for use with the Clarus 500 GC.

•All built-in detectors include an automated

background compensation feature that
corrects for column bleed.
 Parts and functions

Injectors
• Supports a comprehensive array of
injectors that provides accuracy and
precision to all of your sampling
applications.
• The injector elements that appear on a
particular injector screen depend on the
injector type as well as selected
configuration options.
 Parts and functions

PreVent
• Time-saver mode prevents higher
boiling components or residues from
going through the column and the detector.

• PreVent enhanced large-volume injection

(ELVI) mode isolates the column and
detector from the effects of high levels of
solvent.
 II. HOW TO USE
THE APPARATUS
SAMPLE
FOR LIQUID SAMPLE PREPARATIONS:
ANALYTES/SAMPLES SUITABLE FOR GC:
PREPARATIONS
• Anthracene
Insert tip of Pasteur pipet into the liquid.
• Capillary
Benzene action will draw approximately 10 mg of liquid
• into
DDT/ the pipet Diphenyl Trichloroethane
Dichloro
• Rinse
Formicthe pipette into a vial using 1 mL of volatile solvent
Acid
• (NOTE:
Hexane sample solvent can be used are pentane,
• dichloromethane,
NTG ether, etc..)
• Insert the tip
Potassium of a pipet into this liquid
Chloride
• Rinse this into another vial using 1mL of same solvent
Pyridine
• Sample
Sodium is ready to be injected
acetate
• Sulfuric Acid
 For solid sample preparation
SAMPLE SAMPLE
PREPARATIONS PREPARATIONS
• Dissolve approximately 10 mg of compound in 1 mL
of a volatile solvent

• Insert the tip of a pipet into this liquid

• Rinse this into another vial using 1mL of same solvent

• Sample is ready to be injected

T O U C H
S C R E E N
N AV I G AT I O N EQUIPMENT
O P E R AT I O N S
 SETTING UP
DETECTORS

FLAME IONIZATION
ELECTRON CAPTURE DETECTORS
DETECTOR
SETUP SUMMARY
SETUP SUMMARY
1. Setthe
Vent theECD
air and hydrogen flows
outlet
2. Automatically
Adjust the make-upignite the
gas flame
flow
3. Manually ignite the flame
ELECTRON CAPTURE DETECTOR SETUP SUMMARY
SETUP SUMMARY 1. Leak test
1. Turn on the oven and detector heaters 2. Set the hydrogen flow
ELECTROLYTIC
2. Equalize the makeup and reference gas 3. Bake out the reactor
flows 4. Connect the reactor to the conductivity cell
CONDUCTIVITY
3. Enter the TCD bridge current 5. Adjust the solvent flow
DETECTORS
4. Balance the bridge 6. Set a timed event to vent the sample solvent
NITROGEN PHOSPHORUS DETECTOR

FLAME PHOTOMETRIC DETECTOR

Setup Summary
1. Configure the linearizer and signal filter
2. Set up the FPD temperature
3. Set the hydrogen flow and air flow for
PPC
4. Turn on the photomultiplier tube
5. Ignite the flame
PERKIN
SETUP SUMMARY ELMER
1. Turn on the oven and detector heaters
PHOTOIONIZATION
2. Adjust the make-up gas
3. Turn on the UV lamp
DETECTOR
4. Optimize the lamp intensity
DATA
RESULT
AND
INTER-
PRETATION
DATA
RESULT
AND
INTER-
PRETATION
III. MAINTENANCE
AND TROUBLESHOOTING
 Calibration Maintenance
CARRIER GAS GLOW SETTING
• Touch on “Tool” at right hand corner of
screen on instrument

• Select “Option Utilities”

• Touch on “Column Flow Calc.”

• Enter “Column length, diameter, flow &

column over temp.” it will display required
pressure to set by using carrier pressure
knob
 Calibration Maintenance
COLUMN OVER
TEMPERATURE CALIBRATION
• Wear goggle and gloves while handling
glass wool
• Insert calibrated digital thermometer from
topside by piercing glass wool.
• Set column oven temp on GC to 50, 100,
200& 250 degree Celcius.

• Allow to stabilize the set temp for 5 mins

& record temp on digital thermometer at
respective temperatures.
 Calibration Maintenance
DETECTOR CALIBRATION
• Attach
Injector Temp
stainless 180C
steel packed column 2 m Detector Temp 220C
length & 1/8 inch diameter w/ stationary
phase (10% C Flow
Columnar 20 M 80/100)
2.7ml/min Inventor Temp 110C

• 1% v/v Toluene solutionn in n-Hexane (isothermal)

Run time 5 mins
• Set chromatographic conditions
• Inject blank and then 6 injections of 1 %
Toluene solution in system
• Record chromatogram for all injections
• Calculate RSD for the area of 6 1%
Toluene injections
• RSD should not be MT 15%
 EQUIPMENT
MAINTENANCE
• Visual
Gas linesinspection for correct
and connections leak
installation,
tested. damage or risk.

•• Injector
Gas flowsstropped and cleaned, seal
measured
and liner checked, replaced in
•necessary.
Cooling fans, joints, and
connections checked, cleaned
• internally
Detector and
stripped and lubricate
externally, cleaned,
worn parts replaced,
where required.
voltage/resistance checked.
Trouble Check the power supply,
electrical connections, and the

Shooting signal connections.

Check the gas purity and the

gas flows.

Check the temperature setting.

Check the syringe condition and

the sample preparations.

Check the analytical conditions.

TROUBLESHOOTING
Troubleshooting
IV. REFERENCES
References
Reference #1
Ocw.mit.edu. (2019). [online] Available at:
https://ocw.mit.edu/courses/chemistry/5-301-chemistry-laboratory-
techniques-january-iap-2012/labs/MIT5_301IAP12_GC_Sample.pdf
[Accessed 10 Apr. 2019].

Reference #2
Barry E.F. & Grob, R.L. (2004). Modern Practice of Gas
Chromatography. John Wiley & Sons, Hoboken, NJ, 4th Edition

Reference #3
Choudhary , A. (___). Calibration of Gas Chromatography . Retrieved
from Pharmaceutical Guidelines:
https://www.pharmaguideline.com/2010/11/gc-calibration.html

Reference #4
Clarus 580 Gas Chromatograph. Retrieved from:
https://www.perkinelmer.com/lab-
solutions/resources/docs/GDE_Clarus500-580UserGuide.pdf
Thank You
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