:Analytical devices

.Measurement of Chemical quantities instead of physical quantities

Chemical components Physical components

Conductivity Level
PH Flow
Oxygen pressure
CO2 Temperature
CO Speed
Nitrogen
CnHm
…
:Common analytical parts

:All analytical devices have three main common parts

Sensor
Transmitter
Sampling system
 Process line

Sample probe

To LER

Sensor
Transmitter

Sample box
Sample line (1/2"-1/4" tube) Cable Cable
tube"1/4

Typical analyzer system

Sensor
Transmitter
sampling system

:sampling system contains three main parts

sample line
sample probe
sample box
Typical Sample Box

P.G
:Note
As an analyzer man (woman) you are
responsible to check and maintain not only
sensor and transmitter but also sample
!probe, sample line and sample box
Conductivity Measurement
Cell Constant (K) Values
k=L/a a=A*B
Units of Conductivity
Resistance(ohm)
Conductance(µs)
0.056 18,000,000
0.084 12,000,000
0.167 6,000,000
1 1,000,000
2.5 400,000
20 50,000
200 5,000
2000 500
20000 50
:Conductivity transmitters
:Calibration
sensor
:Caution
In some applications there is no chamber or
isolation valve to separate sensor from
process line and it is located directly in the
process line. In such situations if you
remove sensor, sample will come out with
high pressure and flow that can be very
dangerous. Please inform process people
.before any action
Temperature compensation
PH Measurement
PH means power of hydrogen ions

PH = -log10[H+]
sensor
Temperature
Calibration
:Temperature effects on PH sensor life time
?When is the time to replace a sensor

Transmitter sends this error: sensor defected /sensor damaged -1

Unstable reading -2

Late sensor action-3

Applications

11- DESALINIZATION OF SEA WATER

PH control of boiler water -2
Plants with acid production -3
Dissolved oxygen •
Fiber optic oxygen sensors consist •
of an optical fiber with a sensor tip •
-that contains a thin layer of oxygen •
sensitive fluorescent dye dissolved •
in pure silicon. The optical •
fiber carries blue light from a lightemitting •
.diode (LED) to the sensor •
This stimulates the dye to emit fluorescent •
light that travels back up •
.the optical fiber to a photodetector •
Oxygen diffusing into the sensor •
,tip binds to the fluorescent dye •
which reduces (“quenches”) the •
intensity of light emission. The •
extent of quenching is directly •
.related to oxygen concentration •
Fiber optic sensors are very sensitive •
.at low DO concentrations •
Gas Measurement
 Units

PPM : part per million

PPB : part per billion
PPMw :part per million by weight
PPMV :part per million by volume
PPBv :part per billion by volume
PPBw :part per billion by weight
PPMm:part per million by mole
PPBm: part per billion by mole
:Oxygen measurement

?Why should we measure oxygen

To prevent explosion-1
To prevent polymerization-2
To prevent oxidation-3
Oxygen as impurity-4
Oxygen as final product-5
Measurement methods
Paramagnetic method (Is used for -1
percentage values)
Electrochemical method (Is used for-2
percentage, ppm, ppb values-percentage
is better not to be used)
Zirconium method (for places with high -3
temperature like furnaces or ovens)
Paramagnetic Oxygen Sensors

This method is used for percentage values

.It is not applicable for ppm or ppb values
:Advantages
. Fast and linear sensor response
Paramagnetic sensor Structure
Electrochemical oxygen sensors

Trace oxygen is an intrinsic part of many

.manufacturing or packaging processes
The solid state coulometric oxygen sensor isused to •
measure oxygen by counting the numberof electrons
flowing through its circuit. The circuitis connected
between the sensor’s cathodeelectrode and its anode
electrode. A Polarizing DC voltage is used to facilitate
the flow ofelectrons. Oxygen from the sample gas gets
tothe cathode electrode by diffusing through a verysmall
hole in a barrier covering the cathode.Oxygen molecules
in contact with the cathodeare reduced according to the
:followingelectrochemical reaction

. O2 + 4e- = 2O •
- 2
The oxygen ions, O2-, are attracted •
though asolid electrolyte that is heated to
400°C and areconverted back to molecular
oxygen at the anodeelectrode. The
electrochemical oxidationreaction that
:takes place at the anode is
-
2O = O2+ 4 •
2- e
 Life Time
Lifetime of the electrochemical sensor-1
can be increased by leaving it open circuit
when the instrument is switched off, but
this has the disadvantage that the sensor
takes about 20 minutes to settle down
.after reconnection
The commonest solution is to short the-2
.terminals of the sensor when not in use
Another possible solution is to disconnect-3
the sensor when the instrument will not be
used for a longer period of time, but this is
a somewhat unsatisfactory answer, and
raises questions about warranty
.conditions
Zirconium Oxide Oxygen Sensors
Hydrocarbon Measurement

Infrared sensors
Fundamentals
Of
Chromatography
Moisture (Dew point)
Measurement
Rosemount (GCX)
Siemens (Maxum)
Yokogawa (GC1000)
GCX - Modular GC Configuration
Mounting Plate with Lifting Hooks

Increased Safety Box; Power and

I/O Wiring Termination

Electronics Section: Display

Interface, Power Supply and Modular
Electronics

Chromatographic Section: Oven,

Valves, Columns, Detector and
Pressure/Flow Control Section

SHS Interface Plate

GCX - Modular GC Components

Electronics Oven
GCX- Networking and Communications

RS 232 Local Serial Interface

RS 422 Modbus Interface
RS485 Network Interface

GCX- 36
One Analogue
Output(Chromatogram)

4-20 mA DC
Isolated Outputs (6)
Alarm Relays
GCX- 3 GCX- 2 GCX-1 (TTL) (6)
5-24 VDC
Digital Inputs

Network
PC DCS
Controller
First Exposure To Chromatography
Was In Elementary School

Dipped a piece of absorbent paper into

Black Ink
The ink wicked up the paper forming
various color bands
The color bands were from the various
pigments in the ink absorbing onto the
paper at different rates
This showed that a mixture of
compounds could be separated by
differences in how fast they moved
Bottle of Black Ink
through the media
 Basic Chromatograph System
Process Sample Chromatograph GC
Line System Oven Controller

Probe Bypass Sample Separation Detector

Filter Valve Column

Sample
Return

Slip Heater
Stream

Carrier Ref. Det. Analysis

Gas Vent Vent Results
?What happens in analytical oven

Sample injection into the separation columns .1

(sample valve)

Separation of the injected sample into individual .2

components. (columns)

.Detection of concentration of individual components .3

 Rotary Valve
Sample Loop Sample Loop

Sample In Sample Out Sample In Sample Out

Carrier In To Columns Carrier In To Columns

Valve Off Valve On

 Mobile & Stationary Phase

Carrier Gas Column Tubing

Pushing Chemical
Of Interest
 Mobile phase

:In gas chromatography there are two phases

Stationary phase

Mobile phase is an inert carrier gas and stationary

phase is the internal coating of the column which is used

. for component separation

 Introduction to Gas Chromatography

Flow of Mobile Phase

Injector Detector
T=0

T=10

T=20

seperation in column
 GC Basics
Column Separation
TO
CARRIER GAS
COLUM DETECTOR

A C BA C A C BA C AAAA N AAAA CCC BBB

B A CB A B ACB CCC BBB
INJE
CT FULL
INJECT PARTIAL
SEPARATION SEPARATION
 Column Switching — Backflush
To Vent
Carrier

Column # 1 Column # 2 Detector

SIV

Carrier
 Column Switching — Heart cut
Ethylene Tail

100% Product Ethylene

(1,000,000 ppm) 1 ppm Acetylene
1 ppm Acetylene

INJECT DETECTOR

Column # 1 Column # 2

Bulk of Ethylene peak

Typical GC Column Arrangement
 Types Of Detectors Available

Flame Photometric Detector (FPD)

Flame Ionization Detector (FID)

Thermal Conductivity Detector (TCD)

1 PPM 10 PPM 100 PPM 1000 PPM 1 Mole % 100 Mole %

Thermal Conductivity Detector
Amplifier/s

Reference Measure

Vent Vent

Universal Detection
Sensitive Down To 100 ppm
Flame Ionization Detector
Vent

Igniter

Collector
Amplifier

Flame

Polarizing
voltage

Hydrogen
Carrier
Air
 Flame Photometric Detector
Vent

Igniter

Flame Amplifier

Optical Filter
Photo-Multiplier Tube
Hydrogen
Carrier
Air

Sulfur & Phosphorus Detection Only

 Dual Detector System
Sample In

Sample Valve 1 Column Train 1 Detector 1

Carrier 1 Detector Vent

Sample Valve 2 Column Train 2 Detector 2

Carrier 2 Detector Vent

Sample Out
Peak Integration
Residence Time

Retention Time identifies •

which component is which
Area under the peak •
determines concentration

Integration Integration
On Off
Baseline

Time
Typical chromatogram
Different resolutions
) Typical Chromatogram
Functions Of The Chromatograph Controller

Control system operation

% Convert peak area to mole

Perform system diagnostics

Provide user interface

Transmit results and operational status

 Lab Results Vs. Process

Seldom agree
Differences in sample handling
Differences in calibration standards
 What Makes A GC Complex

More than three measured compounds

More than three process streams

Multiple measurement ranges

Multiple detectors