Department of Electronic Engineering & Computer Engineering

BENG: Electronic Engineering

Course: Process Instrumentation 3A (PINA301)

Lecturer: Dr. N. Pillay (Pr. Tech. Eng)

Email: trevorpi@dut.ac.za

Version: 2021 Semester 1

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What can you expect from this course?

1. Extend knowledge of general instrumentation

and control devices.

2. Learn about typical plant processes and how

they function.

3. By the end of the course you should have a

good understanding of instrumentation and
control. 2
What is expected of you?

1. Read! Be able to find information on your own.

2. Proficient report writing skills.

3. Adept at using MATLAB.

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 Topic 1: Analysers
• Refer to sections 8.1 and 8.2.

• What is the purpose of analytical instrumentation?

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 Topic 1: Analysers

• Least understood instrumentation device.

• Cost implications.

• Problems due to the following – lack of understanding of

measurement principles, nature of process variable involved,
chemical makeup of target, sample systems, measurement
strategies and points.

• General classification of analyzer equipment:

- Water monitoring (pH, conductivity, turbidity,
chlorine, etc.)
- Air monitoring (CO2, NOx, O2, etc.)
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 Topic 1: Analysers

• Uses for analysers – raw material monitoring, process

control, process troubleshooting,
yield improvement, inventory
measurements, product quality, waste
disposal and monitoring.
• Pollutants
-Substances in the air/water that cause harm to humans
and the environment.
- Can be emitted directly from the process.

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 Topic 1: Analysers

• Common terms and definitions:

- Quantitative measurement: measures the amount of

material present in the sample. Chemical makeup of
sample is unknown. Eg. pH, conductivity.

- Qualitative measurement: Exact amount of

substance present in the solution is measured.
Measures the chemical makeup and its relative
quantity. Eg. gas chromatography.

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 Topic 1: Analysers

• Common terms and definitions:

- Analyte: Component of interest (COI), target

sample of the process, e.g. % Oxygen, pH,
conductivity,…

- Cross sensitivity: measurement is affected by more

than one variable. E.g. Temperature variations.

- Invasive measurement: In some way the

sensor/probe affects the normal process flow.

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 Topic 1: Analysers

Sampling methods:

• Accuracy of an analyzer measurement can be compromised

by poor sampling techniques/systems.

•Sampling can be achieved with continuous process stream

or discrete stream (grab and hold).

•Three general classifications of sampling methods:

• at-line,
• on-line,
• in-line.

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 Topic 1: Analysers
Sampling methods:

•At-line method: manual method of sample retrieval and

measurement.

•Accuracy of laboratory measurements? Human error.

•Contamination of sample.
•Temperature affects reading in laboratory environment.
•Large time lag.

Process pipeline

Sample point with tap.

To laboratory for assessment.
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drain
 Topic 1: Analysers
Sampling methods:

• On-line method : sample pipes are used to divert flow to the

analyzer device

•Sample pipes may change the nature of the process or

sample properties. Temp/state/velocity. Time lag?
•Filtering – coalescing and scrubbing.

Process pipeline

valve filter AT

drain 11
 Topic 1: Analysers
Sampling methods:

• Alternate scheme for changing the flow rate speed used in

the measurement.
10 m/s

Process pipeline

Takeoff return
point

15 m/s
valve filter AT

drain 12
 Topic 1: Analysers

Sampling methods:

• In-line method (in-situ) : probe is directly inserted into the

pipeline.

•Process changes are rapidly detected. Time lag?

•Filtering and cross contamination?
AT

Process pipeline

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 Topic 1: Analysers
Parts of an analyzer system:

•Sample extraction.
•Sample conditioning and cleaning.
•Sample transfer and preparation.
•COI separation and isolation.
•Measurement by specific signal transducer.
•System control and manipulation.
•Display and document relevant information.

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 Topic 1: Analysers
Parts of an analyzer system:

Process

Extract
Return sample

Condition

Measure/analyse

Display
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 Topic 1: Analysers
Continuous versus discrete sampling methods.

•Reach into process to obtain a representational sample,

small quantity.

•Switch from one stream to another (multi-stream switching).

• Transport packet of sample to a safe location without loss

or change in chemical makeup of analyte. Transfer to point of
return or rejection.

•Prepare sample for specific isolation of target chemical.

•Calibrate to a known standard.

•Display and report results. 16

 Topic 1: Analysers
Sample extraction and conditioning :

• Cleaning (removal of unwanted components)

-Filtration.
-Centrifuging.
-Washing (scrubbing).
-Bubble removal.
-Ultrasonic vibration.
-Condensing (air cooling, water cooling, refrigeration).
-Pressure reduction/flow control (orifice, regulator).
-Component isolation (column separation, membranes,
coalescing).

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 Topic 1: Analysers
Sample extraction and conditioning:

• Isokinetic sampling – maintain constant velocity of sample.

The velocity of the process flowing into the analyzer must be
the same as that of the process stream. Why?

• Higher mass components will only reach analyzer if velocity

of the sample is higher. Used for two phase samples. Eg.
liquid/gas.

•Non-isokinetic – Used to isolate one phase only. Eg. bubbles

in fluid.

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 Topic 1: Analysers
Sample extraction and conditioning:
• Phase preservation
- We must consider the liquid/gas properties.

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 Topic 1: Analysers
Sample extraction and conditioning:

• Average of multiple samples – used to find representational

measurement of varying concentration gradient in large
pipelines or smoke stacks.

•Use of multiple sample points?

•Sample at turbulent stream flow?

•Shape of process equipment may cause measurement

problems.

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 Topic 1: Analysers
Sample extraction and conditioning:

•Quenching reactions – sampling a system in which the

process gases/liquids are still undergoing a chemical
reactions. Usually desirable to stop reaction before it enters
the analyzer.

•Use of quench type probe – cooling water jacket.

• Expansion cooling – nozzle/orifice causes pressure to
drop and thus affects the temperature.
•Combination of the above methods usually more
effective.
•Dilution with specific gas/liquid- reaction quenched with
known dilution. (Must be checked before calibration
though to prevent measurement errors!)
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 Topic 1: Analysers
Sample extraction and conditioning:

• Scrubbing systems – devices used to remove some gases

or particulates from a gas exhaust stream for the purpose of
measurement.

• Wet scrubbing systems usually use water to run

through the exhaust gases to obtain a gas concentration
sample. Safe removal of the exposed water may be a
problem.

•Dry scrubbing systems use a gas adsorbent material to

remove the target gas from the exhaust stream. May need
replacement after surface has been saturated.
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 Topic 1: Analysers
Sample extraction and conditioning:

• Contaminant removal – rejection of unwanted solid particles

from the sample.

-Use probes fitted with filters (eg. Coalescing)

-Slipstream filters.
-Spargers and packed towers.
-Water washing probes.
-Internal separation probes.
-Homogenizers.

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 Topic 1: Analysers
Sample extraction and conditioning:

• Coalescing
filter – removal
of liquid.

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 Topic 1: Analysers
Sample extraction and conditioning:

• Slipstream plus coalescing filter

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 Topic 1: Analysers
Sample extraction and conditioning:

• Bypass filter with rotating mechanism (self cleaning)

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 Topic 1: Analysers
Sample transfer lines:

• Very important consideration as it affects both

transportation delay and velocity of sample.

•Consider the following for faster response time

-Supply pressure.
-Sample return point.
-Actual distance between takeoff point and the analyzer
electronics.
-Diameter of the sample pipeline.
-Delays caused by filters, rotameters, pipe bends etc.
-Sample transport properties (temperature, viscosity?)

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 Topic 1: Analysers
Sample extraction and conditioning:

• A typical liquid sample system.

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 Topic 1: Analysers
Sample extraction and conditioning:

•Discrete sampling versus continuous sampling.

-Less wastage of process/conditioning.

-Allows for automated system cleanup.
-Allows for high velocity sample transport.
-Can be designed for automatic calibration between
samples.
-Provides real time validation?

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 Topic 1: Analysers
Sample extraction and conditioning:

•Discrete sampling system. Extracted sample volume

Pipeline

To analyzer
Carrier gas

Reference
sample Vent

Retract

Extend
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 Topic 1: Analysers
Calibration and validation for analyzers:

•Methods for calibration.

External standards
- Use of known reference sample in place of the
process analyte.
- Standard reference must be known and from a
reliable source.
- Several measurements must be taken to ensure
stability and repeatability.
- Calibration tests must be carried out under similar
operating conditions if possible.

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 Topic 1: Analysers
Calibration and validation for analyzers:

•Methods for calibration.

Internal standards
- Introduce known amount of reference into unknown
process sample. (ratio of sample to reference is
critical).
- Concentration of target analyte is calculated from
the ratio of the responses of the reference and target
components.

Why use this method?

- real time measurement not substantially affected.
- system not disturbed by switching the reference
standard samples.
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 Topic 1: Analysers
Calibration and validation for analyzers:

•Methods for calibration.

Control sample
- Same method as the internal standard except we
inject reference at specified times.

- Used when the system cannot be stabilized easily.

- Must be used with careful consideration due to

cross contamination and degradation of precision of
both samples.

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 Topic 1: Analysers
Calibration and validation for analyzers:

•Methods for calibration.

Secondary standard
- We used laboratory analysis of the process sample
and compare it to the analyzer measurement.

- Used when there is no reference standard available.

- We calibrate analyzer to match the laboratory

results.

- May require several measurements to be taken.

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 Topic 1: Analysers
Calibration and validation for analyzers:

•Methods for calibration.

Auto calibration
- A standard sample is bottled and used periodically
by the analyzer to calibrate at every interval.

- Complex valve arrangement.

- May use a considerable amount of standard sample.

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 Topic 1: Analysers
Calibration and validation for analyzers:

•What is validation?

- Proof of performance in real time.

- Verify the stability of the analytical system for a

fixed period of time.

- Instrument drift is undesirable and affects accuracy.

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 Topic 1: Analysers
Calibration and validation for analyzers:

•What is validation?
A stable system response
Analyzer
measuring X
response X X X X X X X X
Actual analyte
X sample
X X
X Drifting
X error
X X X
X
A poor system response showing considerable drift

Time (days)
Instrument
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calibration
 Topic 1: Analysers
Analyzer measuring principles.

- Chromatography.
- Electromagnetic energy (UV Vis, IR and NIR).
- Electrochemical.
- Mass spectrometry.

- Why the need for so many techniques?

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 Topic 1: Analysers
Analyzer measuring principles.

Gas chromatography (Section 8.12)

- Most common apart from pH.

- Method used to separate the substance into its
individual components (COI).
- Qualitative measurement.

- How is this achieved?

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 Topic 1: Analysers
Analyzer measuring principles.

Gas chromatography Oven temp. varied( 50 – 225 degrees Celsius)

Sample in Sample out

Column
Detector
Carrier gas Vent
(Helium, Injection
Nitrogen, device
Hydrogen)

Mobile phase Stationary phase

Electronic signal
(measurement)
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 Topic 1: Analysers
Analyzer measuring principles.

Typical gas chromatogram readout

B
COI A
E

F
D

Elution time (minutes-hours)

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 Topic 1: Analysers
Analyzer measuring principles.

Gas chromatography
- Carrier gas transports the sample gas (mobile
phase) into the column (stationary phase).
- The degree of solubility of the sample components
in the column are temperature dependant (retention
time) .
- Oven temperature is linearly varied over time.
Usually a wide boiling range for each component.
- A detector that responds to the difference between
the carrier gas and the sample components is placed
at the end of the column.
- Chromatogram is observed.
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 Topic 1: Analysers
Analyzer measuring principles.

Gas chromatography
- Two types of detectors: Thermal conductivity
detector (TCS) and the Flame ionization detector (FID)

- TCD
R R
Signal DC
out

Gas from the column Reference gas

vent vent
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Tungsten elements (Resistive)
 Topic 1: Analysers
Analyzer measuring principles.

Gas chromatography
- FID
+
Signal output depends
on the ionized gas. Response
varies with identity of COI in the
column.
-

Carrier gas (H2)

Air

Gas from the column 44

 Topic 1: Analysers
Analyzer measuring principles.

-Useful properties of electromagnetic energy for

measurement devices. (Section 8.52, 8.61)
 Topic 1: Analysers
Analyzer measuring principles.
 Topic 1: Analysers
Analyzer measuring principles.

-Energy is absorbed (gas) or reflected (solids).

-Example of infrared (IR) absorbed by CO (carbon monoxide).
Absorbance
0
0.1
0.2
0.3 Strength of CO is a
0.4 measure of concentration.
0.5
0.6

4.0 4.5 5.0 5.5 6.0 6.5 Wavelenght

(micrometers)
 Topic 1: Analysers
Analyzer measuring principles.

Lambert-Beer Law:
 Topic 1: Analysers
Analyzer measuring principles.

-IR single beam configuration

Sample in Sample out

Measuring waveband filter

Light source Detector

Window cell
Reference waveband filter

Rotating chopper disc.

 Topic 1: Analysers
Analyzer measuring principles.

-IR single beam configuration

-Reference chosen not to absorb COI. Choice of filter is
not a trivial task.

-As the chopper spins from one filter to the other into the
optical path, the difference in ratio in the energies
received at the detector will be a function of the
concentration of the COI.

-Dirt on the window of the sample cell must not be

allowed.
 Topic 1: Analysers
Analyzer measuring principles.

-Refractometers
-Use of the refraction principles to determine sample.
Refraction index (RI) and Refraction angle (RA)
-Example of stick bending in water. Add sugar and it will
appear to bend even more. Temperature dependant.

RI = (Velocity of light in vacuum) / (velocity of light in

sample)

Velocity of light in vacuum = 0.3 billion m/s

RI = 1.0003 in air.
RI = 2-3 in most liquids, solids and gases.
 Topic 1: Analysers
Analyzer measuring principles.

-Single pass differential refractometer

Reference cell filled with solution
having RI of midrange scale. Photon detector

Light source
Beam Differential Electronic
splitter amplifier output

Photon detector

Sample in Sample out

 Topic 1: Analysers
Analyzer measuring principles.

- Electrochemical sensors: measures COI composition or

concentration by detecting the changes in voltage or current
that occur between two electrodes in a solution over time.

-Selected analyzers:
- Oxygen (O2) measurement.
- Conductivity.
- pH.
- Moisture.
 Topic 1: Analysers
Analyzer measuring principles.

Oxygen (O2) measurement. (Section 8.42)

• Zirconium Oxide Fuel Cells

 Topic 1: Analysers
Analyzer measuring principles.

Conductivity measurement. (Section 8.17)

 Topic 1: Analysers
Analyzer measuring principles.

Conductivity measurement. (Section 8.17)

 Topic 1: Analysers
Analyzer measuring principles.

Conductivity measurement. (Section 8.17)

 Topic 1: Analysers
Analyzer measuring principles.

pH measurement. (Section 8.48)

 Topic 1: Analysers
Analyzer measuring principles.

pH measurement. (Section 8.48)

 Topic 1: Analysers
Analyzer measuring principles.

pH measurement. (Section 8.48)

 Topic 1: Analysers
Analyzer measuring principles.

Moisture in air measurement. (Section 8.32)

 Topic 1: Analysers
Analyzer measuring principles.

-Mass spectrometry (Section 3.29):

-Technique used to identify amount and type of

chemicals present in a sample by measuring its “mass to
charge ratio”.

-Very fast analysis can be achieved. (12 COI in five

seconds.)
 Topic 1: Analysers
Analyzer measuring principles.
Current amplifier
-Mass spectrometry m/q=46
Magnetic m/q=45 Ratio
field output
m/q=44

Positively charged

Beam focus
Ion accelerator
Ionizing filament Electron trap

Sample gas inflow

 Topic 1: Analysers
Analyzer measuring principles.

-Mass spectrometry
-Consists of an ion source, mass amplifier and detector.
-Element gives of excess electrons (-ve charge).
-Electrons knock off one or more electrons from the outer
orbit of the sample atoms.
-Positively charged as atoms are directed and focused to
the magnetic field.
-Deflection of atoms depend on the mass to charge ratio.
Heavier ions are deflected more than lighter ions.
-Sorted streams of ions get detected and recorded to the
abundance of each type of ion.
-This information is used to determine the chemical
composition of the sample.
N2 – m/q=28, O2- m/q=32, Argon – m/q =40
 Topic 1: Analysers
Analyzer selection process.

• Problem definition – benefit of measurement, is the cost

justified? Use for closed loop control?

•Gathering of process info – reasons (environment, safety,

quality), gas or liquid, location of probes, sampling methods.

•Analyzer selection checks – COI?, pressure and

temperature, cross sensitivity, frequency of calibration, drift
and noise. What measuring type do we choose?
 Topic 1: Analysers
Analyzer selection process.

• Sampling – Continuous or discrete? Probe cleaners, probe

automation, filters?

•Analyzer location – Transportation lag, sample line diameter

and length important factor. Analyzer housing cost.
Heating/cooling jackets. EX zone?

• Data handling – local or remote display? Special inputs to

control system, alarms, etc.

•Maintenance – Spare parts, special test equipment,

calibration standard cost and shelf life, training
requirements?
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