Aplikasi Operasi Dan Verifikasi GC (Day 2-3)

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Your platform to do GAS ANALYSIS in the work place®
GC APPLICATION, SENSOR,
VERIFICATION AND
TROUBLESHOOTING
PUBLIC TRAINING (DAY 2-3 )
MAY 29-31, 2018
HSE Institution Training Academy

Jadwal Acara
Day 1-2 Day 3
- Video - Video
- Dasar dasar Analisa Gas - Kalibrasi GC
- Prinsip Analisa Chromatography (liquid dan Gas) - Studi kasus peralatan gas chromatograph
- Konsep Capillary dan sensor gas Chromatography
- Pemilihan GC terkait parameter column
Day 2-3
- Video
- Aplikasi Capillary column dan packed column
- Quantitative dan Qualitative Analysis
- Aplikasi Gas Chromatograph di berbagai Industri
- Verifikasi dan validasi Analisa GC
- Troubleshooting dan Perawatan GC
2
Copyright © 2016 BMU. All rights reserved.
Troubleshooting

Troubleshooting Concepts
4
Peak shapes
5
asymmetric ratio or tailing factor
6
A normal distribution.
7
Band broadening.
8
plate number, N. The peak at x represents a nonretained
component like air or methane.
9
Two nearly resolved peaks illustrating the definition of
resolution, Rs.
10
Band broadening due to molecular diffusion.
11
Illustration of mass transfer in the mobile phase.
12
Illustration of eddy diffusion.
13
Effect of carrier gas.
14
Effect of Sample flow and pressure.
15
Inlets For Liquid Samples And Solutions
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support coated open tubular (SCOT)
and porous layer open tubular (PLOT) column.
17
Column Length Recommendations
18
Split Injection
Split injection is the oldest, simplest, and easiest injection technique to use.
The procedure involves injecting 1 μL of the sample by a standard syringe
into a heated injection port that contains a deactivated glass liner. The
sample is rapidly vaporized, and only a fraction, usually 1-2%, of the vapor
enters the column
19
Water on GC columns
20
No peaks, no gas flow
21
Tailing
22
Fronting
23
Small peaks on fronting or tailing of bigger
peaks
24
25
Double peaks, doubled peak tops
26
Missing or overlapping peaks, poor separation efficiency
27
Broad peaks
28
Cut tops of peaks, broad peaks
29
Strong noise, waves
30
Strong noise, waves (cont’)
31
Increasing baseline, at high temperature bleeding or noise
32
33
34
And many………more
PLEASE SEE AT GC REFERENCES
35
Detectors used in GC

Kind of Detectors
37
Classification of GC Detectors
38
Classification of GC Detectors
Effect of flow rate on peak sizes for the two types of detector:
(a) Concentration and (b) mass flow rate.
39
definition of response time
40
Effect of detector time constant on peak characteristics;
41
Flame Ionization Detector (FID)
The FlD is the most widely used GC detector, and is an
example of the ionization detectors invented specifically for
GC. The column effluent is burned in a small oxy-hydrogen
flame producing some ions in the process. These ions are
collected and form a small current that becomes the signal.
When no sample is being burned, there should be little
ionization, the small current (10-14 amp) arising from
impurities in the hydrogen and air supplies.
42
43
44
45
THERMAL CONDUCTIVITY DETECTOR (TCD)
The TCD is a differential detector that measures the

thermal conductivity of the analyte in carrier gas,
compared to the thermal conductivity of pure carrier gas.
In a conventional detector at least two cell cavities are
required, although a cell with four cavities is more
common.
The cavities are drilled into a metal block (usually
stainless steel) and each contains a resistance wire or
filament (so-called hot wires).
46
47
48
49
Electron Capture Detector (ECD)
The carrier gas used for the ECD can be very
pure nitrogen (as indicated in the mechanism
presented) or a mixture of 5% methane in
argon. When used with a capillary column some
make-up gas is usually needed, and it is
convenient to use inexpensive nitrogen as make-
up and helium as the carrier gas
50
Comparison of working ranges for common GC
detectors.
51
Qualitative And Quantitative
Analysis ..

Qualitative Analysis
chromatographic parameter used for qualitative

analysis is the retention volume or some closely
related parameter. However, since retention parameters
cannot confirm peak identity, it is common to couple a
mass spectrophotometer (MS) to the GC (GC-MS)
for qualitative analysis
53
Identification of unknown by retention times
UNKNOWN
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Simple trapping device for qualitative analysis.
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Relative (PID/FID) response for 15 hydrocarbons.
56
Quantitative Analysis
Statistics of Quantitative Calculations
57
Quantitative Analysis
Calibration with Internal Standard Calibration with Addition Standard
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Example of Quantitative Analysis
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Capillary Direct Interface
60
Instrumentation of GC

Gas chromatography (GC) chromatographic process
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GC separation of twelve C1 to C5 fatty acids.
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High Performance Liquid Chromatography (HPLC)
64
GC Instruments
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Gas filters required for a GC instrument with Flame
Ionization
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GC pneumatic controls
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Split/splitless inlet.
68
Dipole-dipole and dipole-induced dipole interactions
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GC temperature programming
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Detector:Flame ionization (FID) detector
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Data System
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Gas Chromatography Separation Mechanism
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The Distribution Coefficient (Partition Coefficient) (Kc)
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The Distribution Coefficient (Partition Coefficient) (Kc)
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Summary

The Principle
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78
The Capacity Factor
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The Porosity Factor
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The Peak Broadening Factor
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The resolution between 2 peaks
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Van Deemter Phenomena
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GC Setup
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Sample
Injection
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GC Column
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GC Detector
87
TCD
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FID
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MSD
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GC APPLICATION
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HPLC
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HPLC Setup
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HPLC Injector
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HPLC Column
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HPLC Detector
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HPLC
Application
97
HPLC
Application
98

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Your platform to do GAS ANALYSIS in the work place®

HSE Institution Training Academy

HSE Institution Training Academy

HSE Institution Training Academy

HSE Institution Training Academy

HSE Institution Training Academy

HSE Institution Training Academy

HSE Institution Training Academy

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PLEASE SEE AT GC REFERENCES

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HSE Institution Training Academy

HSE Institution Training Academy

HSE Institution Training Academy

HSE Institution Training Academy

HSE Institution Training Academy

HSE Institution Training Academy

HSE Institution Training Academy

HSE Institution Training Academy

HSE Institution Training Academy

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The TCD is a differential detector that measures the

HSE Institution Training Academy

HSE Institution Training Academy

HSE Institution Training Academy

HSE Institution Training Academy

HSE Institution Training Academy

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chromatographic parameter used for qualitative

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HSE Institution Training Academy

HSE Institution Training Academy

HSE Institution Training Academy

HSE Institution Training Academy

HSE Institution Training Academy

HSE Institution Training Academy

HSE Institution Training Academy

HSE Institution Training Academy