Composition Analyzers

Lecture no. 11

Contents
Introduction
Testing methods
Composition analyzing techniques:
1.

Density Measurement

Magnetic Method

Hydrometer

2.

Optical concentration transducers

Turbidimeters

Refractrometers

Spectrophotometry

3.

Electrochemical composition measurement

Thermal conductivity measurement

pH measurement

4.

Analytical techniques

Chromatography

Industrial Instrumentation- Ms. Qandeel Almas

Introduction

Introduction
Knowledge of the composition of the process
stream is often of major importance. This
information may help us to determine the quality
of the product or to control the changing
composition of any process stream .
In the measurement of composition, 1st we have
to analyze which property of the material is to be
used for determining the composition. This
property may be physical or chemical & this
quantity should differ between the components of
the material.
The analysis of the stream may be online or
offline. If online, then the response time of the
measuring instrument should be smaller than that
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of the plant being
controlled.

Cont. .
The various properties which may be employed to
determine the composition include
Preferential
adsorption
of
the
components
(chromatography)
Absorption of electromagnetic rays (UV rays)
Refractive index
Conductivity
Electric potential
pH
Density
The measurement of composition may be direct, or
inferential. Inferential means use the measure of some
property as a function of composition.,(e.g. the use of
B.P in distillation column as a measure of liquid
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composition).
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Cont. .
A wide array of methods is available to measure composition
and these methods are based on following types of analysis:
Various physical property measurements (density and
specific gravity)
Photometric analysis
Mass spectrometry
Electrometric analysis
Chromatography
The first step is to decide between measuring physical or
chemical properties to determine the composition. If physical
property is to be measured, make sure that it is unique to the
desired component of the mixture and will accurately allow
determining the composition.
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Testing Methods

Online Testing
Off-line Testing

Online Testing

On-line analysis is the continuous monitoring of the

composition of a sample.
On-line testing can either be performed in-line or by slip
stream testing.
In in-line testing, the sensor is attached directly to the
line and provides feedback via a transmitter.
In slip stream testing, a side stream of the process
runs alongside the main line. Such an apparatus
closely resembles the set up of a bypass. The slip
stream process conditions can be continuously
manipulated to make the measurements easier to
obtain. Similar to in-line testing, the sensor is directly
attached to the slip stream and provides feedback
through a transmitter.
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Online Testing-Characteristics
Advantages
On-line analysis include an immediate and
continuous feedback responding to changes in
process conditions and so on-line testing prevents
the continued production of undesired product, with
an immediate response and correction of the flawed
material.

Disadvantage
On-line testing is usually much more complicated
and more expensive.

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Off-Line Testing

Off-line analysis involves the extraction of a

sample from the process or reaction, and its
subsequent testing in a machine that may
be situated at a location far away from the
process line in a lab.
In this case, a sample is manually removed
which is later sent to the composition
analyzer. The results of the analysis are
examined and then they are sent to the
control system to make the appropriate
adjustments.
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Off-line Testing-Characteristics
Advantages
Off-line testing is more robust and has more
varied application
Disadvantages
Sample dead-time is introduced (the time
lost during transportation)
Variability of sample testing locations
Lag time for adjustments to be made to
the process
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1. Density Measurement

Magnetic Method

Hydrometer

Introduction
Density is the most fundamental of all the
physical properties. It applies to substance in
any of the three physical states. Density
measurements are made for the following
reasons:
To determine the mass and volume of products
To assess the quality of products.
To
determine
the
composition
and
concentration of a process stream.
To convert volumetric flow measurements into
mass flow information.
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Solid Density Meters

Density of solid may vary both with operating

pressure and temperature.
In many applications the effect of pressure
may be neglected in solids and incompressible
fluids.
In some cases, effect of temperature can also
be neglected if operational temperature is not
significantly higher from temperature at which
density measurements are made, or high
degree of accuracy is not required.

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Fluid Density Meter

Overall density of a fluid is ratio of total mass

to total volume.

Point density is ratio of molecular mass in a

volume element centred at a point to
elements volume (the volume being much
smaller than total volume).

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a) Magnetic method:
The magnetic densitometer consists of a small
ferromagnetic cylinder, encased in a glass jacket.
The jacket and ferromagnetic material combination
constitutes a buoy or float. Therefore float is
suspended electromagnetically, totally immerses in
the process fluid whose density is to be measured.

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Magnetic method (contd.):

When the density of the fluid decreases, the float

will start sinking. The change in position is
detected by search coils and it results in an
unbalanced signal to the amplifier and
demodulator, causing an increase in the current
to the solenoid. This increases the force of
attraction of the magnet on the float and restores
it to its original centered position.

The density sensor can be mounted on tank or

pipeline nozzles, directly immersed in the process
stream, or provided with a sample chamber for
mounting in a sample bypass line.

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Magnetic Density Meter

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Magnetic Densitometers-features
Advantages
Magnetic densitometer allows the determination of
affects of pressure and temperature down to
cryoscopic range.
It allows high measurement accuracy
Disadvantages
Sample flow rates exceeding a few GPH (gallon per
hour) or viscosities above a few centipoises can
result in vertical forces on the float, causing error in
the measurement.
Deposits on the float will also result in measurement
error, for this reason the detector is not
recommended for slurry service.
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b) Hydrometers
Hydrometer is used to
determine directly the
specific gravity of a
liquid.
Construction:
It usually consists of a
thin glass tube closed at
both ends, with one end
enlarged into a bulb that
contains fine lead shot or
mercury to cause the
instrument
to
float
upright in a liquid.

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Working:

The hydrometer is based on Archimedes'

principle.
In the glass tube is a scale so calibrated that
the reading on it in level with the surface of
the liquid (in which the hydrometer is floating)
indicates the number of times heavier or
lighter the liquid is than water, i.e., the
specific gravity of the liquid.
The level at which the hydrometer floats
depends only on the density of the liquid.
Hence this level can be used to measure both
the density and the specific gravity, which is
proportional to it.

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Types of Hydrometers

Lactometers

Alcoholmeters

(Alcohols)

Saccharometer

(Sugar Solutions)

Barkometers

(Tanning Liquors)

Acidometer

(Acids)

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(Milk)

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2.

Optical Concentration
Transducers

Introduction
These include such instruments as opacity
monitors,
turbidmeters,
colorimeters,
refrectrometres
&
spectrophotometers.
Selection of these instruments is more
general where we need online process
analysis

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Turbidimeters
Refractrometers
Spectrophotometer
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a) Turbidimeters

Turbidity:
Turbidity is the cloudiness or haziness of a fluid
caused by individual particles (suspended solids)
that are generally invisible to the naked eye, similar
to smoke in air.

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Cont. . .

Fluids can contain suspended solid matter

consisting of particles of many different sizes.
While some suspended material will be large
enough and heavy enough to settle rapidly to the
bottom of the container if a liquid sample is left to
stand (the settable solids), very small particles
will settle only very slowly or not at all if the
sample is regularly agitated or the particles are
colloidal. These small solid particles cause the
liquid to appear turbid.
Turbidity is most often used to describe the
measurement of low concentrations of particles
that should not be in the process stream, like
particles in drinking water or filtrate.
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Turbidimeters - Types
Turbid meters consist basically of three
components:
A

light source
One or more detectors
A sample cell

Types of turbidity instrumentation are:

Forward

scatter
90 scatter (Nephalometers)
Backscatter
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Turbidimeters - Principle:
As light passes through absolutely pure water,
the light beams travel along relatively
undisturbed paths. However, some distortion
occurs as light is scattered by molecules
present in the pure fluid.
When light passes through a fluid containing
suspended solids, the light beam interacts with
the particles, and the particles absorb the light
energy and re-radiate light in all directions.
Particle size, configuration, color, and refractive
index determine the spatial distribution of the
scattered light intensity around the particle.

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Cont. . .
Particles much smaller than the wavelength
of the incident light, which is typically
expressed in nanometers (nm), scatter light
of approximately equal intensity in all
directions.
However, particles larger than the
wavelength of the incident light, form a
spectral pattern that results in greater light
scattering in the forward direction (away
from the incident light) than in the other
directions.
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Turbidimeters - Applications
Turbidimeter applications number in the hundreds
because the measurement is relatively simple and
versatile.

Particles that should not be in the process stream, such

as water in a petroleum product or catalyst in filter
effluent.
Concentration, of which examples are tomato juice
concentration and the concentration of particles in a
filter feed line.
The detection of changes, such as the onset of
crystallization and immiscible interface zones.
Blending, such as adding the appropriate amount of
filteraid to a filter feed stream.
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b) Refractrometers

Principle:

This
involves the measurement of refractive index

of optically transparent material. When light is

passed between two different media having
different densities it will be refracted & Snells law
applies:

As the composition of a sample changes its refractive index

changes, this change in refractive index changes the critical
angle occurring at interface between glass prism & sample.

1, 2 are angles of incidence & 1, 2 are refractive indexes of the two

media.

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c) Spectrophotometers

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Spectrophotometry
Spectrophotometry is the quantifiable study
of electromagnetic spectra. It deals with
visible light, near-ultraviolet, and nearinfrared.

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Spectrophotometer

A spectrophotometer is a photometer (a device

for measuring light intensity) that can measure
intensity as a function of the light source
wavelength.

The concentration of a substance in solution is

measured by calculating the amount of
absorption of light at the appropriate wavelength
or a particular color.

The
most
common
application
of
spectrophotometers is the measurement of light
absorption.

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Working:

A spectrophotometer consists of two instruments,

namely a spectrometer for producing light of any
selected color (wavelength), and a photometer for
measuring the intensity of light.
The instruments are arranged so that liquid in a
cuvette can be placed between the spectrometer
beam and the photometer.
The amount of light passing through the tube is
measured by the photometer.
The photometer delivers a voltage signal to a
display device, normally a galvanometer.
The signal changes as the amount of light absorbed
by the liquid changes.

Applications:

To measure the concentration of solutions like:

Alanine Amino Transferase

Cholesterol
D-malic acid
Fruit juice
Glucose
Honey
Olive oil
Phosphate
Urea

Analysis of:

Drug
Food
Agri supplies

3.

Electrochemical Composition
Measurement

Thermal conductivity Measurement

pH Measurement

Introduction:

Electrochemical analysis in liquid solutions is

concerned with the measurement of electrical
quantities, such as potential, current and
charge, to gain information about the
composition of the solution and the reaction
kinetics of its components.

The main techniques are based on the

quantitative
determination
of
reagents
needed to complete a reaction or the reaction
products themselves.

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pH Measurement

Introduction:

pH is a measure of the acidity or basicity of a

solution. It is defined as negative the decimal
logarithm of the hydrogen ion activity in a
solution.

The pH is normally measured by chemical

indicators or by pH meters. The final color of
chemical indicators depends on the hydrogen
ion concentration, and their accuracy is only
from 0.1 to 0.2 pH units.

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pH Meters - Working

When one metal is brought in contact with

another, a voltage difference occurs due to their
differences in electron mobility. Similarly, an
electric potential develops when one liquid is
brought in contact with another one, but a
membrane is needed to keep such liquids apart

The pH probe measures pH as the activity of

hydrogen ions surrounding a thin-walled glass
bulb at its tip. The probe produces a small
voltage (about 0.06 volt per pH unit) that is
measured and displayed as pH units by the
meter.

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48

1 = Solution being tested;

2 = Glass electrode, coated
with special silica glass,
and containing potassium
hydroxide;
3 = Silver electrode;
4 = Hydrogen ions interact
with silica glass bulb;
5 = pH meter converts
voltage
(potential
difference) into pH reading;
6 = Reference electrode

Features:
Advantage
PH
meters
have
good
accuracy
and
reproducibility.
Disadvantages
In poorly buffered solutions, accuracy may be
lost by the presence of suspensions and gels.
Glass electrodes used for pH measurement are
hydrogen ion selective but they do not uniquely
respond to hydrogen ions only, so they will also
respond to sodium and other ions especially at
alkaline pH. This effect causes the pH value to
be underestimated.
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Thermal Conductivity
Measurement

Introduction:

Thermal conductivity, k, is the property of a

material that indicates its ability to conduct
heat.

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There are a number of possibilities to measure

thermal conductivity, each of them suitable for a
limited range of materials, depending on the
thermal
properties
and
the
medium
temperature.
Two classes of methods exist to measure the
thermal conductivity of a sample:
Steady-state methods
Transient methods
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Steady-State method:
Steady-state
techniques
perform
a
measurement when the temperature of the
material measured does not change with
time. This makes the signal analysis
straightforward
(steady
state
implies
constant signals).
The disadvantage is that a well-engineered
experimental setup is usually needed

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Transient Methods:
The transient techniques perform a measurement
during the process of heating up. The advantage
is that measurements can be made relatively
quickly. Transient methods are usually carried out
by needle probes.
Non-steady-state methods to measure the thermal
conductivity do not require the signal to obtain a
constant value. Instead, the signal is studied as a
function of time.
The advantage of these methods are that they
can in general be performed more quickly, since
there is no need to wait for a steady-state
situation.
The
disadvantage
is
that
the
mathematical analysis of the data is in general
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4.

Analytical Techniques
* Chromatography

Chromatography:

Chromatography is physiochemical method by which

the components of a mixture
can be separated.
It has become one of the
primary analytical methods
for the identification and
quantification of compounds
in the gaseous or liquid
state.
The basic principle is based
on
the
concentration
equilibrium
of
the
components
of
interest,
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between
two
immiscible

Chromatography Detectors
A chromatography detector is a device that
locates, in the dimensions of space and
time, the positions of the components of a
mixture that has been subjected to a
chromatographic process and, thus, permits
the senses to appreciate the nature of the
separation.

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On-line chromatographic analysis

One of the most widely employed instruments for

online analysis of the samples of multicomponent
gases or volatile liquids; is the gas liquid or gas solid
chromatograph (GLC) or (GSC). This is an instrument
which analyses discrete samples of material but the
disadvantage is that it takes too much time to extract
the sample & to produce the result from the signal.

It consists of
Sampling assembly
Chromatograph
Detector

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Thank You

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