Experimental Process

Technology
in Chemical and Biochemical Engineering

A practical handbook

Lars Kiørboe
DTU Chemical Engineering
Updated 2020 by Ivan Hundebøl and Steen Larsen
2
“I have been impressed with the urgency of doing.
Knowing is not enough; we must apply. Being
willing is not enough; we must do.”
Leonardo da Vinci (engineer, inventor, artist, mathematician)

3
Content.

Preface 5

1. Plant components 6
2. Utilities 33
3. Construction materials 38
4. Designing an experiment 46
5. Sampling techniques 47
6. Analysis 50
7. Measuring accuracy 61
8. Report writing 67
9. Process and plant design 76
10. Flow-sheets and P&I diagrams 78
11. Process control 83
12. GMP, CIP cleaning 88
13. Hygienic design 93
14. Process understanding and process problems 99
15. Heat and mass balances 103
16 Mollier diagram - H,x diagram 106
17. Working safety 111

Literature 112

Appendices 114

4
Preface.

The idea to this compendium came when teaching chemical engineering students in chemical unit
operations laboratory at the Department of Chemical and Biochemical Engineering, the Technical
University of Denmark. The need to know about practicalities is obvious for young engineers for
whom it may take many years to gain sufficient experience to fully apply the theoretical
engineering background into real industrial life.

For that reason this collection of information is primarily made as an aid for undergraduate and
graduate students working with pilot scale process plants and their excersize reports. However, it is
the hope that the compendium can be of assistance also to the chemical engineer working with
industrial equipment and processes, when designing plants in the engineering department, starting
up new manufacturing units or working with quality control.

The purpose of this compendium is to collect and describe topics, which typically constitute
beginners problems and often are not well described in ordinary textbooks or can be easily
overviewed. Therefore the subjects of this compendium is a mixed bag of many different topics.
This is not a text book on chemical unit ioperations and such teoretical and practical details on
individual unit operations must be found in relevant textbooks, some of which are in the reference
list. However, sometimes theory sections are included when useful to give an overview.

Many illustrations and information in the book are not individually referenced. Some are made by
the author, but most are picked up from internet sources, from textbooks or company brochures.

The background of the author for writing this book is more than 40 years engineering activities in
many different companies and institutions, and with almost any kind of job function a chemical
engineer can think of: R&D, production, engineering, consulting and service, sales and
management. And perhaps most important are the observations during years of teaching, of the
problems and challenges the students may have when making large scale testwork and the
associated technical reports.

Lars Kiørboe, May 2018

Minor revisions; Ivan Hundebøl & Steen Larsen, 2020

5
1. Plant components.
1.1 Valves

Valves are mainly shut-off valves and control valves, but other functions are mentioned below.
Valves can be operated manually using a handle or automatically using an actuator. The actuators
are often pneumatic (using pressurized air), but electric or hydraulic (using pressurized liquid)
actuators are well known too.
Talking about valve types one important issue is the valve-curve (characteristic), denoting the
relationship between the valve opening (spindle movement, for instance in percentage of full open)
and the flow. The capacity (or the size) of the valve is defined by the so-called Kv-value, which
denotes the flow through the valve in m3/h at 1 bar differential pressure for a fully open valve.

In gate valves a disk is gradually pushed from one side across

the pipe (figure 1.1). When the valve is fully open there is
practically no restriction to the flow. The valve-curve is far from
linear as the valve must be closed pretty much before the flow is
reduced. Therefore the gate valve is a very bad control valve. It
is typically used in heavy industries. The gate valve has some
similarities with the ball valve in figure 1.2, i.e. a non-linear
valve-curve and an unhindered and straight flow when fully
open. Ball valves are the modern version of the old fashioned
cock – known for instance from laboratory glassware. Ball
Figure 1.1
valves can be manufactured in small sizes and are cheap and
Gate valve
very popular on-off valves. Due to the gasket – made from
various kinds of plastics - around the ball, the application of
the valve is limited to temperatures below ~ 200 oC and often
lower.

Another very popular valve is the globe valve in figure 1.3,

which can be designed to achieve a rather linear valve-curve
and therefore can be used as control valve. The seat and cone
design is the secret to fulfil the various requirements, and in
some automatic control valves they may be interchangeable, so
Figure 1.2
the same valve body can be rebuilt to various capacities and
Ball valve

6
functionalities. The ideal liquid flow direction through a globe
valve is such, that the pressure tries to open the valve; in this
way the stuffing box (gasket around the spindle) will not be
pressurized when the valve is closed. A special version of the
globe valve is the needle valve , where the cone is formed like a
needle. They are used for very demanding control purposes.

The valves described so far are not very easy to clean due to the
gaps, voids, gaskets etc., which are part of the construction.
These kinds of valves are therefore mainly avoided in industries,
where sanitary/hygienic requirements are tough – food, bio- and
pharmaceutical industries. Valves which can be designed as Figure 1.3
hygienic are butterfly in figure 1.4 and especially membrane Globe valve
(diaphragm) valves in figure 1.5.

Figure 1.4 Figure 1.5

Butterfly valve Membrane valve

Like ball valves the butterfly valves have a very unlinear valve-curve and are therefore often used
as on-off valves in liquid systems. In gas systems – for instance in ventilation ducts – butterfly
valves are used to a large extent due to their simplicity and low costs in large dimensions.
Membrane valves are much better for control purposes, but due to their hygienic character they are
most often used as automatic on-off valves. One important hygienic issue of a membrane valve is

7
the drainability, when located on a horizontal pipe. For the valve and pipe to be completely
drainable it requires, that the valve body is turned a certain angle. The exact angle depends on the
size and the design, and information is given by the supplier.
Control valves are often globe or needle valves connected to a
controller and supplied with an actuator, the function of which
is to move the valve spindle to a certain position (figure 1.6 and
figure 1.7). The actuator is operated with a signal from the
controller - typically a pneumatic or electric signal. If the valve
opens due to an increase in controller signal, the function is said
to be normal or direct. In the opposite situation the control
function is reverse. Improvement of the control function takes
place with a so-called positioner, which report back to the
controller the actual position of the spindle (=degree of valve
opening).

Automatic control valves are said to be normally open (NO) or

normally closed (NC), which refers to the position when the
signal to the actuator is switched off (figure 1.7). In case of
accidents, where the power or air pressure is lost, it is important
that valves return to the right position. A natural gas valve
surplying a burner should be normally closed, while a cooling
water valve would often be normally open.
Figure 1.6

Control valve (NO)

Figure 1.7
Actuator. Left: NC. Right: NO

8
Reduction valves, see figure 1.8 and figure 1.9, are used to
reduce the high pressure in a pipe to a lower one and to keep the
low pressure at the prefixed set point even if the high pressure
varies.
On contrary to all other valves the reduction valves are
opened (i.e. increasing set point on the low pressure/down
stream side) when turning the handle clockwise.
This is important to remember. The reduction valves use a
spring to adjust the output pressure, and the turning of the valve Figure 1.8
spindle affects the compression – and ease of opening - of the Pressurized air reduction valve
spring.
The function of safety valves, figure 1.10, is very much the same as reduction valves apart from the
fact, that safety valves are designed to keep the up-stream pressure constant. Safety valves are used
to protect up-stream equipment against too high pressures. It is therefore very important that safety
valves are maintained in good condition and checked (by release of the handle) regularly.

Figure 1.9 Figure 1.10

Reduction valve Safety valve

9
In order to ensure flow in a pipe in one direction only check valves are applied. There are various
principles, for instance: A spring activated seat (figure 1.11) and a hinged locker (figure 1.12).

Figure 1.11 Figure 1.12 Figure 1.13

Spring activated check valve Hinged check valve Steam trap

Steam traps are another kind of special valve. As the name indicate they are mostly used in steam
systems. The function is to let the condensate (liquid) pass to the low pressure side but prevent
steam to pass. Steam traps can be designed from various principles, some of which also operate as
check valves and venting of air (non-condensing gases) from the steam pipe (figure 1.13). Steam
traps are very important for the proper function of steam heating systems and must never be
neglected (see section 2 concerning utilities).

1.2 Pumps.

The most generally used pump is the centrifugal pump, shown in

figure 1.14, 1.15, 1.16 and 1.17, due to its simplicity, sturdyness
and low cost. Pump inlet is in the centre and the outlet tangential
to the pump impeller. Centrifugal pumps are used to transport
liquids (including suspensions) and gasses (in which case they
are called fans or blowers).
Figure 1.14

Centrifugal pump principle

10
In these pumps mechanical/electrical energy is converted to
kinetic energy and finally to pressure. Due to the head
(pressure)-flow relationship (see the typical centrifugal pump curve in figure 1.18) they cannot be
used for dosing purposes. When connecting several impellers to the same shaft the pump pressure
level can be increased considerably (multi stage pump, figure 1.16 and 1.17).

Figure 1.15 Figure 1.16

Single stage centrifugal pump Multi stage centrifugal pump

A condition for proper function is the correct direction of rotation. For pumps running on 3-phase
voltage the direction is reversed by interchange of two phases in the socket. In addition it is
important to remove any air from the pump house, which is done by opening a vent screw during
running until all air is exhausted.

11
 Figure 1.17

Flow pattern inside a vertical multi stage centrifugal pump (Grundfos).

14

12

10
Pressure, bar

0
0 5 10 15 20
Flow, m3/h

Figure 1.18

Centrifugal pump characteristic curve

12
Centrifugal pumps are not very good at self-priming, i.e. to provide the necessary suction on the
inlet side. To improve the pumping function the dimensions of the pipe on the inlet side are usually
larger than on the outlet side (pressure side) – for instance by a factor of 1.5 on the diameter.

Centrifugal pumps are by nature not very sanitary in design, and centrifugal pumps constructed in
order to optimize the hygienic conditions are quite costly.

The pump “Net positive (or pressure) suction head”, NPSH, is a pump property related to the
pressure characteristics inside the pump head. Information about pump-NPSH is found in the pump
supplier technical data. In order to achieve good suction conditions with no cavitation it is required,
that the suction conditions provided by the system (called system-NPSHsy) shall always be higher
than the pump-NPSH. The available system NPSHsy is defined as:

NPSHsy = Ha – Hh – Hf – Hd

where Ha is the absolute pressure on the liquid surface in the vessel on the suction side, Hh is the
difference in height between this liquid surface and the centre of the pump inlet (Hh < 0 if the pump
inlet is lower than the liquid surface), Hf is the friction loss from liquid surface to pump inlet and Hd
is the vapour pressure of the liquid at the actual temperature.

A requirement for safe pumping at all conditions is: NPSHsy > pump-NPSH.

Ha
Hh>0

Figure 1.19

System NPSH conditions

13
A large group of pumps are positive displacement pumps, which means that they deliver a certain
liquid volume (on time or stroke basis) irrespectively of the system conditions (outlet pressure,
viscosity etc.). This is not 100 % correct for all positive pumps and of course limited to the pump
operational range. Important is however, that the pressure side of positive pumps must not be closed
off, because this can ruin the system or the pump itself due to the high pressure those kind of pumps
may deliver.

Piston pumps and membrane pumps are stroking high pressure pumps. Due to their nature they are
pulsating. Pulsations can be reduced by having for instance 3 feeding heads in the same pump but in
varying phase – or by using a pulsation damper. Inlet and outlet valves – for instance in the form of
moving balls – provides the correct flow direction by acting as check valves. Piston and membrane
pumps may be sensitive to particles in the pumping liquid, especially the piston pumps because
small abrasive particles may spoil the fine tolerances between the piston and the house. Positive
displacement pumps may also be rotating, as the gear pump in figure 1.21 and 1.22. Impeller
pumps are similar to the gear pump but often with flexible (rubber) impellers.

Figure 1.20 Figure 1.21

Membrane pump Gear pump

Figure 1.22

Gear pump

14
Mono pumps as in figure 1.23 usually have a rotor of steel and a stator of rubber. The mono pump
pressure can be increased by increasing the length of the rotor/stator. Mono pumps are able to pump
suspensions, provided the maximum size of the particles are considerably smaller than the space
between the stator and rotor. A mono pump must never run dry, in which case the rubber stator
immediately will be destroyed. Gear pumps, impeller pumps and mono pumps are practically not
pulsating.

Figure 1.23
Mono pump

A robust kind of positive pump is the peristaltic pump, which in principle is just a flexible hose
(figure 1.24). It is very sanitary and can withstand all the chemical and physical conditions
associated with the kind of rubber selected for the hose. Peristaltic pumps cannot provide very high
pressures, and the mechanical influence of the rollers on the rubber hose may cause abrasion with
reduced lifetime and rubber particles in the product as a consequence. Peristaltic pumps are
excellent for pumping suspensions, they can rotate either way, but due to their construction they are
pulsating.

Another sanitary pump is the so-called lobe pump, which is a special version of the impeller or gear
pump (see figure 1.25). Lobe pumps for sanitary applications are made from stainless steel and with
very small tolerances; consequently particulate matter in the liquid cannot be accepted.

Figure 1.24 Figure 1.25

Peristaltic pump Lobe pump

15
Positive pumps are generally applicable for dosing purposes, but the actual selection of pumping
principle depends on the demands of the application: Flow steadiness, pressure, capacity,
temperature, operational range, chemical nature of the liquid, suspension characteristics etc.

Vacuum pumps.

The most well known pump for medium vacuum is the socalled water ring pump, i.e. a cylinder of
rotating water creates a seal between the vacuum and the atmosphere. Figure 1.26 illustrates the
principle. The vacuum made from this kind of pump can never be lower than the pressure of
saturated water vapour at the actual temperature.

Figure 1.26

Ejectors are a special kind of pumping equipment which has no moving parts. It consists of a nozzle
in the centre of a pipe of a special geometry. The nozzle is for instance driven by compressed air or
steam and provides a suction in the up-stream side of the pipe around. Ejectors are used as vacuum
pump and as pressure pump within moderate pressure ranges. Ejectors are of special concern under
conditions, where moving parts are less applicable, for instance at high temperatures or under
ATEX-conditions when handling explosive fluids (ATEX: Atmosfaire explosive). Figure 1.27
shows an example.

16
 Nozzle

Steam or
Discharge
compr. air

Diffusor
Vapour inlet
Figure 1.27

Ejector

1.3 Fans and blowers.

The most simple fan for transportation of a gas is the axial flow turbine (figure 1.28). The pressure
capability is low, but they can be made for large flow capacities.

Figure 1.28

Axial flow turbine

Another simple fan is the centrifugal ventilator/fan, in principle similar to the centrifugal pump. An
example is shown in figure 1.29.

17
 Figure 1.29

Centrifugal fan

The air inlet is from the centre of the house and the pressurized air exit is tangentially to the rotating
impeller. The centrifugal fan is used for higher counterpressures than the axial turbine. The two
mentioned ventilators can also be designed as compressors, i.e. for higher pressure applications.
Roots blower (figure 1.30) is a positive displacement fan based on the sample operating principle as
the gear and loberotor pump. It is therefore capable for higher pressures than axial and centrifugal
ventilators.

Figure 1.30
Roots blower

Real gas compressing equipment are more complicated than the simple ventilators and shall not be
discussed in this context.

18
1.4 Measuring equipment

Temperature measurements are probably the most frequent measuring task in the chemical
technology. There are many principles, but in this context we shall encounter only three of them –
the thermocouple, the resistance thermometer and the infrared thermometer.

Thermocouples are based on the design principle that two different metallic wires (A and B) are
soldered/welded to each other in one end and to a different wire (C) in the other end (figure 1.31). If
the AC and BC soldering points are kept at the same temperature and different from the AB
soldering point, a voltage will develop in the system. The size of the voltage depends on the nature
of the two metallic wires (A and B) and the temperatures. If the soldering points AC and BC are
kept at an equal and constant temperature (the reference temperature, Tref), the temperature of the
soldering point AB (Tprocess) can be determined by measuring the voltage E (figure 1.24). On
modern instruments the reference temperature is kept constant using an automatic temperature
compensation. The thermocouple principle can be used up to temperatures of ~ 1600 oC. The
international standard controlling thermocouple design is called IEC 584.

Tref C
Tprocess A
E (mV)
B C
Tref

Figure 1.31

Thermocouple principle

The most generally used metal wire combinations are NiCrNi, PtPtRh, Fe-constantan (=CuNi) and
Cu-constantan. Figure 1.32 describes the various thermocouples in terms of their application
temperatures. The figure also includes the application temperature range for resistance termometers
(Pt100).

19
 Figure 1.32
Application temperature range for various thermocuples and resistance thermometers (Ametek homepage).

For thermocouples there are 3 tolerance classes according to IEC 584: Class 1, 2 and 3. The
tolerance is defined as the highest allowable deviation from the ture value for non-calibrated
conditions. Class 1 has the lowest tolerances and is therefore considered most accurate. Class 2 is
the standard quality, and class 3 has special specifications. The tolerences for instance for type K
(NiCrNi) according to class 2 in the temperature range -40 to 1200 oC is ± 2.5 oC or ± 0.0075 ·tactual
o
C (the highest value is valid). The tolerance of the sensor depends on the purity of the metal, but
the accuracy of the reading also depends on the setup of the total measuring system including the
quality of the instrument and of the length and quality of the wires connecting the sensor and the
instrument (compensating cables). Special connections between the wires are also necessary in
order to minimize additional voltages developed in the system. Figure 1.33 shows the standard
(norm) accuracy for various sensors. If these accuracies are not good enough it is necessary to

20
calibrate the sensor or the entire system. Calibrated thermocouples for industrial application are
seldom more accurate than ± 0.5-1 oC.

Figure 1.33
Standard tolerances for various sensors (Y-axis: Allowed deviations).

In resistance thermometers the electric resistance of a metallic wire depends on the temperature.
When applying a voltage across the wire, the measured current is therefore a function of
temperature. As for thermocouples the wire in the resistance thermometers is protected by a shield,
typically a tube of inert material and with ceramic insulation. The resistance wire is often made
from very pure platinum, and these kinds of thermometers is therefore denoted Pt100. The relation
between temperature and resistance is controlled by the standard IEC 751. Resistance thermometers
are supplied in 2 accuracy classes, A and B. These norm related tolerances are:

Class A: ± (0.15 + 0.002·tactual) oC

Class B: ± (0.3 + 0.005·tactual) oC

21
The total standard tolerance therefore consists of a temperature related contribution and a zero-point
contribution (see figure 1.33). In addition to the norm related tolerances also commercial and some
company specific tolerances are defined. As for thermocouples the real accuracy of the reading
from a certain sensor can be improved by calibration – whatever the official tolerances. For
industrial equipment real accuracies better than ± 0.1 oC is seldom achieved (or necessary).

The electric cables from the sensor to the instrument/transmitter are also important. Cables to
resistance thermometers may have their own electric resistance – especially important if the
distance between the measuring point and the instrument is long. Cable resistance errors are added
to the sensor tolerance, and consequently it is a very good idea to calibrate the entire measuring
system after installation.

There are many potential errors involved with temperature measurements using thermocouples and
resistence thermometers. Some have already been mentioned above. Others are:

• Heat conduction in the sensor or measuring pocket. To minimize this error use small
thickness of the sensor protection pipe/pocket material, long insertion of the sensor in the
process, earthed sensor, thermal insulation of the part of the sensor located outside the
process equipment.
• Radiation between the sensor and components around. Especially important at high
temperatures where the sensor “faces” cold spots from component walls etc. Errors can be
very high. Mount a radiation shield around the sensor, reduce sensor dimension, maximize
distance between sensor and cold spots.
• Dynamic factors. If the fluid around the sensor has a high heat transfer coefficient – i.e.
turbulent fluid flow – the better the sensor can react on fluid temperature changes. Small
sensor dimension also reduces the response times.
• Electric noise and missing earthing.

Infrared thermometers (pyrometers) are often used at – but not limited to - very high temperatures
where other measuring principles may be difficult to apply or may even fail. The operating principle
is a contact free measurement based on the infrared (IR) radiation coming from a body/surface and
detected by the optical sensor of the instrument.

The physical background for the measuring principle is Stefan-Boltzmanns law, which can be
written as:

22
 E = constant × ε × T4

where E is the emitted power per area, ε is the emissivity and T is the surface temperature in Kelvin.
As seen the emitted power from the hot surface – and therefore the reading of the instrument -
depends on the emissivity. The IR thermometer reading is therefore only correct if the emissivity set
on the instrument is identical to the emissivity of the surface in question. Emissivities are defined
in the range 0-1 and are temperature dependent. An ideal black body has an emissivity of 1 and has
the largest emitted power compared with other surfaces of the same temperature. Even if the
instrument emissivity can be adjusted, large measuring errors may occur because of the difficulty in
identifying the real emissivity of a certain surface.

Examples of emissivities of various surface materials are shown in table 1.1.

(Material (temperature) ε
Polished gold or silver 0.02
Aluminum (170 oC) 0.04
Frosen water (0 C)
o
0.97
Cast iron (100 oC) 0.80
Iron, polished (20 C)o
0.24
Glass (90 oC) 0.94
Plastik: PE, PP, PVC (20 C) o
0.94
Black paint, dull (80 oC) 0.97
Porcelain (20 oC) 0.92
Table 1.1

Emissivities of selected materials (ref. Testo Instrument user manual)

Pressure instruments used in the industry may be analog for visual reading and with electric
transmitters for data logging or process control. As well absolut pressure as differential pressure
instruments are frequently applied.

When talking about pressure we almost always mean the static pressure, which for a flowing media
is the force per area acting on the walls perpendicular to the flow direction. In the flow direction
there is an additional factor called the dynamic pressure, which is proportional to the density and

23
the square of the velocity ( ~ ½ ρv2). By means of a pitot-tube as in figure 1.34 the dynamic
pressure – and therefore the media velocity – as well as the static pressure can be determined.

For ordinary pressure measurements we only deal with Dynamic + static

pressure
static pressures: The static pressure is generally much Static
pressure
higher than the dynamic, and the measuring point
always perpendicular to the flow direction. Pipe flow
direction
Please remember that the recorded static pressure also
depends on the height of the fluid column above the
Figure 1.34
measuring point. For water a 10 meter high column
Pitot tube
corresponds to 1 bar.

Pressures can be absolute or differential. The term “bara” – bar absolute – is the pressure in bar
relative to the absolute zero. It is most important when working with vacuum systems in order to
avoid “negative” pressure-values.

Most pressure instruments have the zero value at atmospheric pressure and consequently determine
the “over-pressure”. To describe this (in comparison with the “bar absolut”) the term used is “barg”
(bar gauge) or “baro” (bar over-pressure). The principal difference between bara and barg is the
same as between degree Celcius and Kelvin – i.e. the point-of-zero, while the unit itself is
unchanged. Consequently, distinguishing between bara and barg has no meaning in case the
pressure difference between two points is the issue.

The most simple way of measuring a pressure (or a differential pressure) is to use a U-tube. This
can be a hose filled with a liquid – often water. The difference in height between the two liquid
surfaces is the (differential) pressure measured in for instance mm height of water = mmWG (water
gauge). 1 mmWG = 9.8 Pa ~ 10 Pa. This instrument can for practical reasons operate with low
pressure differences only. The reading accuracy can seldom be better than ~1 mmWG. If the
pressure differences are smaller a so-called inclined tube manometer can be used. The measuring
principle is the same as the simple U-tube.

A very typical mechanical analog instrument for absolute pressures is the Bourdon-manometer.
This is a circular hollow spring – the Bourdon tube - with the one end fixed to the measuring point

24
and the other end connected to a pointer (indicator). When a pressure is applied to the hollow spring
at the fixed end the tension will change the diameter of the spring and therefore the position of the
end with the pointer. On a circular instrument the pressure can be read as the position of the pointer.
In the membrane manometer the connection to the process is a membrane made from stainless steel.
The volume on the membrane back side (instrument side) is either filled with a high boiling oil and
for instance connected to a Bourdon tube or mechanically connected to the pointer. Membrane
manometers are easy to clean on the process side (sanitary design) – which is not the case for
ordinary Bourdon manometers – and therefore largely used in food, bio and pharma industries.
Figure 1.35 shows the principles of the manometer construction.

Figure 1.35

Bourdon tube (left) and membrane (right) manometer

construction

When pressure measurements are used in process control or for data logging, a transmitter is
necessary. Pressure transmitters are quite complex in construction and the output signal may be
electric or pneumatic. Also differential pressure transmitters are frequently used. Pressure
transmitters must be calibrated (zero and span) on a regular basis to be reliable. A high degree of
standardization has been attained for output signals with 4-20 mA and 0-1 V as typical sizes. These
standard signals are used in many other kinds of instrument.

In order to get the pressure signal from the process to the instrument/transmitter a pressure tap is
installed in the sidewall of the pipe or vessel. To maximize accuracy the media flow should not be
disturbed by the pressure tap. A drilled opening Ø 1-2 mm is considered to fulfil this requirement.
To ensure undisturbed flow in pipes due to other reasons the following rules must be obeyed (D is
the internal pipe diameter):

25
 • No pipe diameter changes 5 x D upstream of the pressure tap
• No valves or pipe bends 10 x D upstream of the pressure tap
• No components or pipe changes 2 x D downstream of the pressure tap
NB: These rules are not valid for pressure taps for flow measurements (see below).

Membrane manometers where cleaning is important are installed in a pipe-T with much larger
dimensions; the consequently lower accuracy is accepted for the benefit of better cleaning
conditions.

In the European standard for manometers EN 472 a range of accuracies are defined: 0.1% - 4%.

Level measurements are often performed as a differential pressure measurement, as seen in figure
1.36. In figure “a” to the left the differential pressure transmitter is connected with one side above
the liquid surface and the other side directly to the bottom, i.e. wet connection. If it is not possible
or desirable to have a wet connection to the transmitter, the arrangement as in figure “b” can be
applied. It is called a bubble tube level transmitter: A small flow of compressed air is added to the
tube leading to the bottom of the vessel in order to push any liquid out of the tube. The necessary air
pressure to counter balance the hydraulic pressure at the tube end is recognized by the one side of
the transmitter. For both conditions “a” and “b” the following relationship is valid: ∆P = h·ρ·g,
where ρ is the liquid density. The setup is valid irrespectively of the absolut pressure at the liquid
surface. If the vessel is open to the atmosphere the low pressure side of the transmitter can be left
unconnected; this is equal to a simple hydrostatic measurement.

Using a strain gauge (weighing cell) to record the total mass of the vessel including the content is
another way to record the level. This is also useful when recording levels of solid material in a silo.

26
 FI Compressed
air
∆P

h h

∆P
a b
Figure 1.36

Also various kinds of radiation can be used for level measurement. One such is an ultrasonic
instrument located in the top of a vessel. The time of the sound wave moving from the instrument
down to the liquid surface and back is recorded. The same procedure is used in X-ray and radar
instruments. Important for the radiation instruments is the angle of scattering, since the wave must
not be disturbed by contact to any other surfaces than the liquid surface. Agitators or other devices
generating splashes and waves on the surface will of course influence the accuracy of the level
signal.

In the instruments based on the capacitance/dielectric constant a rod is inserted from the top of the
vessel to the bottom, and the signal is proportional to the part of the rod, which is immersed into
the liquid.

In the float method a body is swimming on the liquid surface. The position can be recorded
visually; if the float contains a magnet the position can be recorded as an electronic signal and
therefore used for process control. A simple level indicator for manual reading is a vertical stand
pipe in glass located on the outside of the vessel and connected to the interior in top and bottom.

A float connected to a switch fixed to the inside of the vessel wall works as an on-off level switch
and can tell if the liquid surface is above or below a certain height.

Flow measurements encounter a large group of devices, and it is only possible to mention a few
principles. Most of principles are actually based on measurement of the volume flow and they are
not real mass flow instruments.

Venturies, nozzles and orifices use the differential pressure across a well-defined element to
calculate the media velocity. These elements are standardized to a large extend in order to ensure

27
 Figure 1.37

Venturi meter

standard deviations in the range ± 1-2%. As for other flowmeters they are sensitive to the flow
pattern of the media, and it is a general rule, that as a minimum there must be no disturbances 10 x
D upstream of the element and 5 x D downstream. Figure 1.37 shows a venturi meter and figure
1.38 an orifice. The general equation for calculation of the volumetric flow Q through venturis and
orifices is:

𝜀𝜀∙𝐶𝐶∙𝐴𝐴 2∙∆𝑃𝑃
Q= �
�1−𝛽𝛽 4 𝜌𝜌

where A is the area of the contraction, β is the ratio between the contraction and the pipe diameter,
ΔP is the measured pressure drop, ρ is the fluid density, ε is the expansion number which for gases ≠
1, and C is venture/orifice coefficient which for instance depends on the Re-number. Correlations
for C and ε can be found in the literature.

Figure 1.38

Flow and pressure profile through an orifice

28
A part of the pressure drop cannot be recovered; this is in particular the case for orifices, while
venturies are much better in this respect due to the shape of the divergent outlet. Un-recovered
pressure drop costs pump energy, and especially the application of orifices are nowadays reduced
for the benefit of newer and better principles.

Rotameters are another old and well proved ways of flow measuring. They belong to a family called
VA-instruments (VA = Variable Area), which are constructed as a conical tube with a float inside.

Figure 1.39
Rotameter for manual reading.

They have to be located vertically, and the position of the float indicates the flow rate and can be
read on the scale of the tube side. The float design may vary, and the reading point on the float may
not always be obvious. Figure 1.40 shows the reading point for a number of different floats.
The reading of a rotameter indicates that the float weight is balanced by the sum of the drag force
(friction) and the buoyancy. The general relationship between the volumetric flow rate Q and the
corresponding position, h (height about a “zero” level) of the float can be evaluated as:
𝜌𝜌𝑠𝑠 −𝜌𝜌𝑓𝑓
𝑄𝑄 = 𝐾𝐾 � ℎ
𝜌𝜌𝑓𝑓

where ρs and ρf is the density of the float and fluid respectively and K is a constant related to the
properties of the tube and the float.

29
Rotameters are usually calibrated for water or air at certain pressures and temperatures. When using
other fluids (or conditions) correction factors are needed. The volume flow of a liquid QL with a
density ρL different from that of water ρW (at standard conditions) is determined by:
(𝜌𝜌 −𝜌𝜌 )∙𝜌𝜌𝑊𝑊
𝑄𝑄𝐿𝐿 = �(𝜌𝜌𝑠𝑠 −𝜌𝜌𝐿𝐿 𝑄𝑄𝑊𝑊
𝑠𝑠 𝑊𝑊 )∙𝜌𝜌𝐿𝐿

where the water flow QW is determined at the same height of the float as the flow QL of the other
liquid. For gases the similar relationship for volume flow Qg and mass flow Wg of another gas with
density ρg is:
𝜌𝜌 𝜌𝜌𝑔𝑔
𝑄𝑄𝑔𝑔 = � 𝜌𝜌𝑎𝑎𝑎𝑎𝑎𝑎 𝑄𝑄𝑎𝑎𝑎𝑎𝑎𝑎 and 𝑊𝑊𝑔𝑔 = �𝜌𝜌 ∙ 𝑊𝑊𝑎𝑎𝑎𝑎𝑎𝑎
𝑔𝑔 𝑎𝑎𝑎𝑎𝑎𝑎

It is assumed that ρs – ρair ≈ ρs and ρs – ρg ≈ ρs.

Rotameters have for many years been quite popular for smaller flows of liquids as well as for gases.
The draw back is the manual reading, and for that reason modern design with magnetic scanning
and electronic output has been developed. Remember when metering gasses that the reading is very
dependant on the gas density (i.e. pressure and temperature).

Figure 1.40

Reading points on rotameter floats

A popular instrument in modern technology is the electro-magnetic flow sensor (figure 1.41).
Magnets are located on the outside of a pipe. According to Faradays law a voltage is induced in a
conductor crossing the field, and the voltage is proportional to the velocity. The flowing media acts
as conductor, and thus the velocity can be determined. The voltage is measured by electrodes
located in the pipe wall. The principle requires, that the media in the pipe has a certain conductivity;
flow of gasses, demineralised water or organic solvents cannot be detected using this method.

30
 Figure 1.41

Electro-magnetic flow sensor

Electro-magnetic flow sensors exhibit no obstruction to the flow, there is no moving parts and the
pipe is smooth. These flow elements are therefore applicable in industries, where sanitary design is
important, or for suspensions, as the particles can settle nowhere in the device.

Ultrasonic flow sensors base their vorking principle on the time it takes for an ultrasonic wave to
pass a certain distance in a pipe – from the transmitter to the receiver. The time is dependant on the
liquid flow, but also particles and air may disturb the signal.

Mechanical displacement flowmeters encounter a number of constructions. One example for liquids
is the oval wheel meter in figure 1.42, which can have smooth or toothed wheels. It is a very
accurate device (~ ± 0.5 %), but the pressure drop can be considerably (0.1-0.2 bar). A similar
meter is the gear wheel meter in figure 1.43.

Turbine meters are designed for liquids as well as gases. A small turbine or propeller is inserted
inside the measuring pipe (figure 1.44). The rotation of the turbine is proportional to the flow. The
pressure drop of these meters is low, but they are not very precise.
A special version of the turbine meter is the well known anemometer, often hand-held instruments
used for detecting gas flows.

31
 Figure 1.42 Figure 1.43

Oval wheel flowmeter working principle Gear wheel meter

Figure 1.44

32
2. Utilities.

Utilities is a name for the general process supplies, which are typically produced at a centrally
located plant and distributed to the user places. It encounters for instance steam, compressed air,
vacuum, water, cooling liquids and CIP (Cleanining-in-place) liquids.

Utilities may be supplied at various qualities, for instance high pressure process steam, clean steam
for sterilizing, hot city water, cold distilled water etc.

2.1 Steam.

Steam is used for heating purposes – directly injected into the process or indirectly used in a heat
exchanger. It may also be an active part of a chemical reaction, as in reforming or synthesis gas
production. Steam is also used as sterilizing agent in autoclaves in the food and pharmaceutical
industry. Steam is usually supplied as process steam at various pressure levels, saturated or
superheated. Saturated steam is generally preferred in the industry: It is cheaper than superheated
steam, and due to the high heat of condensation and high heat transfer coefficient it is more efficient
in heat exchangers. Autoclaves also requires saturated steam, which is more efficient as far as
bacteria killing is concerned compared to superheated (dry) steam.

Process steam is produced at a dedicated boiler of a kind or taken at a certain pressure level from
the turbine circuit at a power plant. Clean (pure) steam is used in the pharmaceutical industry,
where the quality requirements are large; clean steam is produced at dedicated steam generators,
where the requirements to design, construction materials, operation and maintenance play an
important role.

Steam may also be used for clean water production by evaporation. The pharmaceutical industry
applies an ultra-pure water quality called water-for-injection (WFI), which in Europe according to
the Pharmacopea can only be produced by distillation of water. WFI production plants are typically
multi-effect evaporators.

From a user point-of-view it is important to recognize the steam pressure and temperature – i.e. is
the steam saturated or superheated. In addition the user must know a few things about the design of

33
steam systems – from the main valve to the condensate outlet – and about the application and
maintenance.

The steam supply to a plant consists of a main shut-off valve, a filter to remove solid impurities, a
safety valve, a reduction valve if various pressure levels are encountered, manometers, a
temperature sensor, a flow measurement and a control valve to adjust the flow. A vacuum breaker is
useful to allow introduction of air in a steam system, when it has been closed down and the pressure
therefore due to the condensing steam is reduced tremendously. The function of the vacuum breaker
is to ensure, that the entire system when not in use is left at atmospheric pressure and therefore
sensitive components are protected against underpressure.

Heat loss in steam pipes cannot be avoided, and especially in saturated steam pipes condensation
takes place. Condensate (water) in steam systems are to be avoided, because liquid water at the high
steam velocities may create physical damages by hydraulic shocks in components, pipe bends etc.
To ensure proper function the condensate must be removed from the steam pipe on a regular basis
(i.e. at every 50 m) using automatic steam traps (also see section 1.1). In addition a steam trap must
always be located at a point, where the steam pipe is changing direction from horizontal to vertical
upwards.

After the heat exchanger (or other steam consuming component) the condensate shall be taken out
through a steam trap. Steam cannot pass the steam trap, and if the condensation in the exchanger
stops due to missing heat transfer, the steam flow is virtually stopped. The trap therefore acts as an
automatic valve. Many steam traps are of a design, which prohibit reverse flow from the condensate
line – i.e. the trap has a check valve function. It is also advantageous if air (or other non-
condensable gases) in the steam system can be vented out through the trap.

Regular maintenance concerns checking of the filter and the proper function of the steam traps.

2.2 Compressed air.

Compressed air is typically supplied at a pressure of 6-7 barg. Since most compressors are oil
lubricated, the compressed air has a mist of oil drops – even if there is a central oil demistor. At the
user points it is therefore normal to have a water and oil trap in connection with a reduction valve.

34
These components are often assembled into one unit, which may also include a small strainer (filter
for coarse particles). The extended use has made these pressure reduction stations quite cheap.

Pipes for ordinary compressed air are in galvanized or mild (black) steel.

Clean compressed air for the pharmaceutical industry demands completely oil free air, and
demistors and oil traps are not sufficient to meet the quality. In these cases an oil free compressor
must be used; in addition the pipes, reduction valves etc are all made from stainless steel. Clean
compressed air systems also include a sterile filter and often also a de-humidifier and an activated
carbon filter for removal of any gaseous trace components.

2.3 Water.

Water is an important utility in most industries, and there are many qualities: Cold and hot city
water, demineralised water, distilled water, cooling water etc. City water is drinking water from the
tap. The quality varies according to the location, i.e. the hardness due to the soil composition or
application of surface water. Cold water should have a higher hardness than the warm/hot water,
because the heating precipitates some of the dissolved Ca++ and Mg++ as practically insoluble
sulphates and carbonates. The application of chlorine for microbial control of drinking water –
especially surface water from lakes – is seldom in use today in Denmark.

More refined water qualities are based on drinking water. Usually met in the laboratory is the
demineralised water. It is produced by using ion exchange or reverse osmosis (RO) technologies.
The quality is not well defined and depends upon local regulations; the conductivity may be very
low, probably below 10 µS/cm, but the content of organic matter may depend very much on the
actual water source and the purifying technologies.

The best water qualities are found in the pharmaceutical industries: Purified water (PW), highly
purified water and water-for-injection (WFI). These water qualities are socalled “compendial
waters” where the quality and production methods are defined by the Pharmacopeia (see table 2.1).
Compendial waters are produced according to the following procedure:

Drinking water → Pre-treatment → Final treatment

35
There is no requirement for quality or pre-treatment methods, but the pre-treatment shall prepare the
drinking water for the final quality. Pre-treatment methods could be particle filtration, removal of
chlorine by active carbon filtration, microbila control by UV or ozone treatment etc. In Europe WFI
must be produced by distillation as the final treatment, in USA also by reverse osmosis. The
compendial waters are used for producing clean steam, for process cleaning purposes or as
component (solvent) in the final drug product. Whether one may call these waters for utilities or call
them a refined component for the final formulation of the drug can be discussed.

Type Requirements Recommendations

Purified water Produced from drinking water < 100 cfu/ml
No additives
Conductivity < 4.3 μS/cm at 20 oC
TOC < 500 ppb
pH = 5-7
Highly purified water As for WFI, apart from: < 10 cfu /100 ml
Conductivity < 1.1 μS/cm at 20 C o

Water for injection Fulfil all requirements to PW <10 cfu/100 ml

Final treatment: RO or distillation
Conductivity: < 2.1 μS/cm at 20 oC
Bacterial endotoxins: < 0.25 int.units /ml

Table 2.1
Specifications for compendial pharmaceutical waters

2.4 Cooling water.

Cooling water can be of any quality. It may circulate in more or less closed systems and may have a
high microbial load. Cooling water is often cooled in cooling towers located outdoor and can be
polluted from the atmosphere. Cooling in towers is limited to the ambient temperature level, but to
some extent depending on the air humidity (Re: The adiabatic cooling temperature).

Cooling at temperatures below the water freezing point requires additives in the water, as for
instance glycol in the cooling system of automobiles or brine-solutions of dissolved inorganic salts.
Cooling to lower temperatures also requires assistance from a compressor as in the ordinary fridges
and freezers.

36
2.5 CIP liquids.

CIP means clean-in-place and CIP liquids are typical food, biotech and pharmaceutical utilities.
Cleaning in place of process equipment can take place from a central CIP-liquid supply station with
distribution pipes leading to the various process units in the factory. It can also takes place from a
mobile CIP-unit, moving around from one production unit to the next. Whatever CIP-system is
used, the CIP-liquids are typically alkaline and acidic aqueous solutions. A range of commercial
CIP-liquids are available from many suppliers. They are sold as concentrates, which must be diluted
by water before application; the final user concentration is in the range of ~ 1% active substance.
Since much dirt in the pharmaceutical industries comes from proteins, alkaline and acidic agents are
quite dominating. Very often the alkaline formulations are based on sodiumhydroxide and the acidic
on phosphoric acid or nitric acid. The alkaline solution is used for breaking down and dissolving
proteins and fats, and the acid to take what is left, to neutralize the alkaline and to remove any
inorganic deposits (for instance limestone). Disinfecting and oxydising agents are often based on
hydrogenperoxide. Table 2.2 shows some examples on commercial formulations. Some companies,
however, use only simple and cheap hydroxides and mineral acids for their CIP processes.

Formulation Application pH
15-30 % HAc, <5% per-acetic acid, <5% phosphonic acid Disinfection 2.9-3.5
<30% H2O2, <5% non-ionic tenside, <5% phosphonic acid Oxidising agent 3.0-3.6
15-30% NaOH, <5% NTA (nitrilo-triacetate), >5% phosponate Alkaline cleaning agent 12.2-12.8
1-5% NaOH, 5-15 % alkyl amino-ethoxylate, 1-5% tri-ethanoleamine, Weak alkaline cleaning agent, 9.1-9.7
5-15% phosphonate manual agent
<30% organic acid, 5-15% formic acid Acidic cleaning agent 2.3-2.7

Table 2.2

Examples on commercial CIP liquids.

37
3. Construction materials

Materials for construction of process plants comprise a very broad range of qualities depending
upon the actual requirements and the economy. This overview is in no way comprehensive, but
intents to give the reader a picture of the structure of materials of relevance for the chemical
industry.

The main properties to consider when selecting a construction material are:

• The operational temperature

• The chemical/corrosion resistance
• Physical influence such as abrasion and pressure
• The cost of material
• Ease of installation, maintenance and the cleaning ability.
In some plants the appearence may play a role.

In this section we will discuss the following groups of materials:

• 3.1: Metallic materials

• 3.2: Plastic and rubber
• 3.3: Refractory materials

3.1 Metallic materials.

The wellknown ordinary mild steel (black steel, carbon steel, non-alloyed steel etc.) is still very
much in use in the chemical industry due to the price. Mild steel corrodes easily in humid
environments and must be protected by painting, galvanizing etc. The kind of corrosion is surface
corrosion, which can be calculated during the design phase and taken care of when determination of
material thickness relative to expected life time. Mild steel and galvanized steel is often used for
piping of utilities such as city water, cooling water, compressed air, exhaust and ventilation, steam
and condensate. Mild steel is used in the low temperature range, i.e. up to 400-500 oC. Mild steel
can be welded, but welding galvanized steel will destroy the protective zink layer at the welding
point.

38
Brass may be found in water systems because of a much better corrosion resistance than mild steel.
It is especially used in valves, strainers and similar components made by casting.

If the quality of the product is affected by using mild steel it is necessary to use corrosion resistant
steels, i.e. stainless steels. These are usually alloys with Cr and Ni and often also Mo, Ti and other
elements. Basicly we have three types of stainless steels: Ferritic, austenitic and martensitic. For
chemical plant application the austenitic steels are totally dominating. These steels are simply
identified among the other stainless steels by not being magnetic. Ordinary austenitic AISI 304 is
alloyed with Cr and Ni (for instance the well known 18-8 steel). AISI 304 is actually mainly
resistant only to humid and oxygen containing conditions, but for instance not to acids. The food
and pharma industries are always using better qualities such as AISI 316 (with an additional few %
of Mo) for plant components in direct contact with the products. Stainless steels of the socalled L-
quality have extra low carbon-content, so the steels can be welded without forming detrimental
chromium-carbides, which will reduce the corrosion resistance. Stainless steels have a wider
temperature application range than mild steel (typically up to 800-1000 oC). Stainless steels do not
show surface corrosion but pit corrosion, which is difficult to observe before the entire unit is
perforated and severe leaking of process liquid takes place. An important agent responsible for pit
corrosion in ordinary stainless steels is Cl- ions, so chlorides must never be used with stainless
steels unless the steel is of a very special (and more expensive) quality – for instance the socalled
duplex steels.

A thin layer of Cr-oxides is the factor which actually protects the stainless steels against corrosion.
If a steel has been in contact with process liquids for a long period the chromium-oxide layer may
be damaged. In pharmaceutical plants it is ordinary practise to recover the oxide layer by a
passivation procedure, which is actually an oxidation with > 20 % HNO3 for 5-10 hours.

Composition and dimensions for pipes, fittings, bars, plates etc. made of mild and stainless steels
are controlled by a number of national and international standards, which also define tolerances,
welding procedures, surface quality, testing methods etc. Well known standars are ASTM –
American Society for Testing and Materials, AISI – American Iron and Steel Institute, ISO –
International Standard Organisation, EN – European norms, SS (SIS) – Swedish Standard, DIN –
Deutsches Institut für Normung, W-nr – Werkstoff-Nummer, BS – British Standard and DS –
Danish Standard. Dimensions of pipes, for instance, are varying a lot from standard to standard and
is actually a jungle. Stainless steel products are identified by certificates, declaring results from

39
testing of a certain welding batch-number (lot number, heat number). The inspection certificate type
3.1.B is the most used declaration. On the steel product itself is often printed an identification.

When building pharmaceutical plants the identification of components is of utmost inportance, and
verification of the component steel quality based on the certificate and the physical ID marked on
the metal surface is one inportant subject of the socalled qualification procedure.

In table 3.1 is a list of materials with some specifications.

Material Standard Composition Properties

Non-alloyed steel Carbon steel, black steel, <1.7% C Corrodes in contact with
mild steel O2 and H2O.
Stainless steel AISI 304, SS 2333, W- < 20% Cr, 8-12 % Ni, 0.04% C, <2% 18-8 steel. Resistant to
(austenitic, non- nr. 1.4301 Mn, < 1% Si moist atmosphere
magnetic) AISI 304L, SS 2352, W- < 20% Cr, 8-12 % Ni, ≤ 0.03% C, Can be welded
nr. 1.4306 <2% Mn, < 1% Si
AISI 316, SS 2343, W- <19% Cr, 10-14% Ni, <0.04% C, 2.5- Acid resistant
nr. 1.4436 3% Mo, <1% Si, <2% Mn
AISI 316L, SS 2353, W- <19% Cr, 10-14% Ni, ≤0.03% C, 2- Acid resistant, can be
nr. 1.4435 3% Mo, <1% Si, <2% Mn welded
904 L, SS 2562 W-nr. 20% Cr, 25% Ni, 4.5% Mo, Cu Very resistant towards Cl-
4539 pit corrosion
353 MA 25% Cr, 35% Ni, Si, N, Ce High temperature
application. Scaling temp.
> 1150 oC
Duplex W-nr. 1.4462, SS 2377, 22-25 % Cr, 4-7% Ni, 0-4% Mo Application below 300oC.
(austenitic- SAF 2205 Good Cl- resistance.
ferritic)
Titanium Very corrosion resi-stant,
also towards Cl-
Brass Cu/Zn, max 38% Zn, + minor Subject to stress corrosion
quantities of other metals

Table 3.1

Aluminum metal is seldom in use in chemical plants: It is too soft, too expensive and may not have
sufficient anti corrosive properties. Thin aluminum sheets are however used as cover for insulation

40
of pipes and plant units; the cover keeps the insulation protected and gives a nice and cleanable
surface.

3.2 Plastics and rubber.

Plastics from a chemical engineering point-of-view can be grouped into thermoplastics and
thermosettings.While the first group after heating to a softening point can be formed/shaped, the
thermosetting polymers are irreversibly crosslinked during the manufacturing process, often by
condensation of two different components into a resin. Rubbers – elastomers – has a soft 3-D
network which can be reversibly stretched and retracted.

Plastics and rubbers are widely used for many purposes. There are many qualities, they are
generally cheap and they have excellent corrosion resistance towards acids, bases and salts. One
draw back is the limited temperature resistance.

A good example is glass fiber reinforced polyester, which is used for scrubber construction on
waste incineration plants due to its capability to withstand HCl solutions.

Rubbers are indispensable as gaskets and packings. In the food and pharma industries the special
requirements reduce the applicable qualities to EPDM, fluor elastomers as viton, silicons and a few
others.

Also for plastics the fluor-based polymers (PTFE, PVDF) show interesting qualities, mainly due to
the chemical inertness towards practical all inorganic and organic liquids and the temperature
resistance; PTFE are typically applicable up to 250 oC. More ordinary and cheap thermoplastic
products as PE, PP and PVC are very much used for vessels, valves, pipes at lower temperatures
and pressures in corrosive environments or for simplicity.

3.3 Refractory materials.

These materials are used for high temperature applications, i.e. combustors, calcination plants,
cement burning furnaces, foundaries, steel works, waste incinerators, boilers, ovens etc. We will
briefly discuss 5 groups of refractory materials:

41
 3.3.1 Castables, including precast bricks

3.3.2 Bricks

3.3.3 Ceramic fiber products

3.3.4 Glass

3.3.5 Other non-metallic high temperature products

Most refractory materials are based on oxides of mainly Al, Si, Mg, Ca, Cr and Zr, but also certain
nitrides and carbides are important. SiC-compounds are special due to their high thermal
conductivity and resistance to thermal chock. These compounds are not included in the tables
below.

Refractory constructions are usually designed with a high strength, high chemical and temperature
resistant lining next to the process. Behind this primary lining may be layers of materials with better
insulating capability but less temperature resistant and less resistance to abrasion and wear.

For refractory materials we consider 3 different bonding systems: Hydraulic, ceramic and chemical
bonding. In the hydraulic bonded products (for instance castables) a refractory cement (typically
high alumina cement) is mixed with grains of various minerals and water. In the ceramic bonding
the particles are sintering together at high temperatures, for instance using fine grained clay as
bonding agent. Chemical bonding may take place using for instance phosphoric acid, which at
elevated temperatures will polymerize and create long chains of poly-phosphates around all the
refractory grains. Other chemically bonding agents are water glass (silicates), boric acid and some
organic polymers.

3.3.1 Castables

These materials are similar to concrete: A dry mixture of formulated minerals are mixed with water
and casted, ususally using some kind of form, to make a monolithic construction. An exemption is
the gunning castables which are actually “sprayed” on the surface which has to be refractory lined.
For constructions made of castables it is normal to use anchors (of metal or ceramics) fixed to the
surface in order to integrate the lining with the structure behind. If the castable is hydraulically
bonded the lining will achieve a certain strength pretty soon after casting, but it has to undergo a

42
drying and curing process following a pre-determined time/temperature program in order to get the
final properties. Castables can also be supplied with a ceramic or chemical binder.

Castables can be grouped into low-cement castables (LCC), traditional castables, gunning and
insulating castables. LCC are a group of products with very high strength, low porosity, applicable
to high temperatures and harsh chemical environment. LCC are also used for making socalled
precast shapes, which are dried and burned before installed in the equipment. These elements can be
made in rather thin constructions and are very abrasion resistant. They are for instance used in
cement plants and for high temperature cyclons in fluidized bed boilers, but also in more simple
constructions for instance in slaughter houses in furnaces used to singe the pig skin or in industrial
pizza furnaces. Table 3.2 shows examples on castable qualities.

Type of castable Max. operating temp., Density, kg/m3 Thermal conductivity,

oC W/mK
Insulating 1100-1400 450-1700 0.14-0.65
Gunning 1300-1600 2000-2500 0.6-1.5
Traditional 1200-1800 2000-2900 0.6-1.9
Low cement 1400-1700 2200-2600 1.1-1.7

Table 3.2

3.3.2 Bricks

Refractory bricks (sometimes called pressed bricks) can be compared with bricks for building
houses. They are made from a mixture of solid particles, which are pressed in a form and burned at
rather high temperatures. Many bricks are ceramic bonded, and the strength of these bricks is due to
solid phase reactions, where various constituents react with each other and form solid solutions or
other binding concepts. The bricks can be classified as dense bricks, normal bricks and insulating
bricks in order of reducing strength and application temperature, but with increasing heat
conductivity. In the group of bricks one could include products made as sheets and plates, often less
dense and strong compared to ordinary bricks and also made from less refractory materials.
Examples are bricks and plates made from vermiculite and moler (vulcano sediments). The plates
can be cut with a saw and the material is often used in woodburning stoves and as back insulation.
Table 3.3 gives examples on various brick qualities.

43
 Brick quality Max. operating temp., oC Density, kg/m3 Thermal conductivity, W/mK
Moler 900-1100 300-950 0.1-0.3
Insulating 1200-1600 600-1000 0.15-0.5
Chamotte 1400-1500 2000-2200 1.0-1.3
(fire clay)
High alumina 1500-1600 2300-2700 1.3-1.6

Table 3.3

3.3.3 Ceramic fiber products

These qualities are compared with the wellknown mineral wool. The fiber products are made from
a refractory melt and spun during cooling to various products: From ligth blankets (similar to
Rockwool batts) over boards of various densities and shapes to refractory paper. Fiber products
have the highest insulating capabilities of all refractory materials, but they have very limited
compressive and abrasive strength. They are used as flexible high temperature gaskets and as
insulation behind a dense lining in order to optimize the heat conductivity – and thereby heatloss –
from a construction.

As for other refractory qualities the fiber products are manufactured with many different
specifications. Maximum application temperature may go up to 1600 oC for zirconia based
products. The thermal conductivity is typically in the range of 0.1 W/mK.

3.3.4 Glass

This material is wellknown from laboratories, pilot plants and small scale production plants. On
contrary to many other high temperature products glass is amorphous. It is chemically very
resistant. The various qualities also include products made of glass fibers, for instance blankets for
insulation and rope for packing and gasketing.

Glass and enamels are still much in use, for instance where corrosion of steels makes it necessary to
find different construction materials (sulphuric acid and hydrochloric acid manufacturing plants). In
such cases the inner surface of for instance a steel reactor is lined by enamel, which gives a smooth
and inert surface. Also stirrers and other components can be enameled.

44
3.3.5 Other high-temperature products

This mixed group includes refractory glue, mortars and cements, ropes, ramming mixes, etc. Glues
can be used to bond fiberproducts, rope, inorganic insulating plates etc. and are often water glass
based. Mortars and cements are used to fix bricks to each other. Ropes are delivered from Ø 3 mm
to more than Ø 60 mm withstanding temperatures above 1100 oC. Ramming mixes are chemically
bonded plastic products used for instance to construct burner cones.

45
4. Designing an experiment

This topic is not advanced science, but rather a list of matters of course which however can be
easily forgotten and for that reason create a lot of trouble, waste of time and in the end money. An
experiment may be a simple lab test, a pilot plant testwork or even a full scale experiment
performed in an industrial plant. Generally the following steps may be of assistance to avoid larger
errors:

1. Understand the ultimate goal of the experiment

2. Clarify the individual steps from start to the very end, i.e. describe shortly each consecutive
step for instance in form of a flow diagram
3. Describe the process components needed for each of the above mentioned steps
4. Test the individual equipment in order to catch functional errors
5. Describe the conditions and procedures for each step
6. Determine the need for sampling, i.e. where, when, how much, with what equipment etc.
7. Identify the equipment to be used for measuring and analysis for each step, i.e. equipment
for determining time, temperatures, pressure, volumes, flow, weight, titration,
spectrophotometric analysis etc.
8. Identify the chemicals to be used, in quantities and qualities
9. Clarify the need for manpower for running the experiment
10. Identify the need for supplementary support (from outside etc.)
11. Determine the need for allowances (official, company, QA, etc.) and ordering of supplies
12. Make a written script of the entire performance, step-by-step with a connecting list of
responsibilities, supplies etc. Include a list for measurements and sampling.
13. Make a risk assessment considering process and plant risks as well as environmental and
personal risks.
14. Prepare yourself by testing new and unknown individual components or process steps, so
you know they can actually be performed within the expected conditions.
15. In your mind go through all your considerations and preparations and convince yourself that
they are sufficient in order to achieve the goal of the experiment.
16. Have somebody else qualified person to control your preparations.

46
5. Sampling techniques

The general principle for sampling is that the composition of the sample in any respect shall be
identical to the bulk quantity (representative sampling).

Taking samples from solutions (one phase systems) is the most simple issue. Make sure the bulk
solution is homogenous by providing proper stirring or re-circulation by pumping. The sample is
most easily taken from a flowing fluid – for instance from a sample valve. When taking the sample
make sure that the still-standing liquid in the sample valve and in the pipe section between the main
pipe and the valve is drained before collecting the sample. If the sample cannot be taken from a
running fluid take it from a stirred vessel using a beaker or similar. Never take the sample from the
surface. Carefully consider if a varying sampling place (vertical/horizontal) is worthwhile.

Sampling of mixtures of solid particles and liquids can only be provided from suspensions under
constant mixing. Taking a representative sample is only possible if all particle sizes are equally
distributed in the liquid. If the biggest particles have a practical tendency for sedimentation – which
is the case when the particles are larger than colloids - taking samples from a running fluid is even
more important. In case this is not possible, sampling from various places in a vessel is a must in
order to achieve an average sample, but the quality may not be very good. So the old rule
“representative samples cannot be taken from a two-phase system” is in reality still valid.

Sampling of solids is a very difficult task, and good equipment, planned procedures and
experienced personel is of utmost importance. Un-correct sampling may result in errors 10-1000
times any total analytical error. A “theory of sampling” (TOS) has been developed, describing the
complex procedures for correct sampling (un-biased sampling). With the background from
sampling of coal from ship cargos an international standard has been made (ISO 1988), and
dedicated sampling equipment developed. The standard rules according to ISO 1988 may be quite
complicated due to the often very large quantities of material. In most cases, however, the chemical
engineer shall deal with much smaller lots of material, and for that reason the sampling procedures
can be simplified, although based on the same principles, and if possible adapted to the particular
application.

The international coal sampling standard first of all recommend samples taken from a continuous
flow of product (1-dimensional sampling), either from a band conveyer or from a falling stream.
The sample shall comprise all material between two complete cross sections. Samples taken from a

47
band conveyer or similar continuous transport device may require stopping of the flow during
sampling and careful removal of all material between two cross sections. Samples from a falling
stream is the easiest because it can be performed using a bucket with a minimum size equal to the
width of the falling stream.

For products which are not available as a continuous flow, but as a pile of bulk product (for instance
collected in a bucket or vessel from a cyclone or bag filter), sampling must take place in a different
way. This will be the typical situation in many chemical engineering productions. In these cases the
sampling and the sample division can often not be distinguished. The socalled “grab”sampling –
using a grab, shovel or spoon to take one sample from a pile – is the worst way of sampling and
should never be done. Random sampling from a pile must be performed by taking a number of
single samples in equal quantities from various locations in the pile; the number of single samples is
not well defined and depends for instance on the homogeneity of
the material, but probably at least 10-20 samples may be needed.
The sample size depends on the size of the largest particles in the
pile. The coal standard ISO 1988 requires a sample (kg) = 0.06D,
where D is the size in mm of the largest particles. A better way of
sampling from a bulk quantity is to devide the total lot by using the
coning/split procedure: Put up the bulk quantity into a cone on a
plane surface, press the top down in order to get a square of
meterial of equal height, divide the heap into 4 equal parts using 2
vertical right-angled cuts; then take the two opposite parts as a
reduced lot and discard the other two. Repeat this procedure as
Figure 5.1
many times as necessary until the quantity of material is small
Rifle splitter
enough to be handled using a rifle-splitter (figure 5.1), which will
devide the quantity into two parts.

The rifling can be repeated with one of the parts as many times as required, and this is supposed to
be an un-biased sampling procedure. A similar sampling procedure is to use a rotating sample
divider, splitting the amount of material into for instance 8 or 12 equally sized samples (figure 5.2).
This procedure is using laboratory equipment and is therefore limited to minor quantities.

For comparison qualitative sampling errors of different sampling and sample division methods can
be resumed:

48
 Sampling method Sampling error, %

Rotary tube sample divider ½

Sample splitter (rifling) 3

Dividing a cone 6

Random sampling 10

Table 5.1

Figure 5.2

Rotating sample divider (Retsch homepage)

To achieve the final sample for analysis it may in some cases be necessary to crush the particles.
This is a typical procedure when sampling minerals, coal etc. This is of course not possible if the
analysis concerns the particle size distribution.
Proper sampling and sample division of solids must consider the size and number of samples,
always related to the total quantity of material. When taking samples always describe the procedure
in the report.

49
6. Analysis

Much analytical work connected to the practical courses concerns ordinary wet chemical analysis:
Titrations, conductivity measurements, viscosity determination, liquid density, pH measuring etc.
They should not constitute any theoretical or practical problems.

However, analysis of solids may some times be a challenge to the chemical engineer. The problem
of providing a representative sample has been discussed above. Samples of solids are a mixture of
various particle sizes, and dry sieving (screening) analysis is the most simple way to determine the
particle size distribution for particles larger than about 30-40 µm.

A sieve consists of a cloth – usually made of steel fibres/wires –

with a well defined distance between the wires (figure 6.1).
Anglo-American literature talks about mesh, which denounces
the number of spaces (between the wires) per inch. In European
practise the distance in mm or µm is a measure of the sieve size.
A stack of sieves with varying mesh – with the most coarse at
the top and the finest openings at the bottom – is used for a
sieving analysis. The product is placed on the top sieve and the Figure 6.1
stack is vibrated. The time and amplitude for the vibration
Various sieve sizes
depends on the particle mixture and must be determined by trial.

It is important that the sieving process does not change the particle size distribution. The sieving
efficiency shall be high enough to separate all particles of different size from each other. However,
prolonged sieving times may for some products cause a disintegration of mechanically weak
particles into smaller ones with an analytical error as a consequence.

Hygroscopic and humid products are very difficult to sieve, because single particles tend to stick to
each other.

The particle size distribution can be described in various ways. The distribution curve reports the
results from the sieving, for instance in form of a bar diagram (histogram) on mass basis. Table 6.1
is an example on a sieve analysis, where the size of the population is described based on mass as
well as based on number (ref. 13). The particles could also be characterized based on surface. For
particles of the same density the mass fraction versus size is identical with the volume fraction. For

50
most size distribution calculations it is also assumed that the shape of the particles is constant with
the size. On the definition of the particle size for non-spherical particles see below.

Table 6.1 is to be understood as follows: During screening all particles will pass the sieve of size
1651 μm (under size), but 0.5 mass-% - corresponding to 300 particles ~ 0.01 % of the total number
of particles - will be retained on the next sieve 1168 μm (over size). The average arithmetic
diameter for this interval is 1410 μm and the diameter range between these two sieves is 483 μm
(1651-1168 μm). It is said that the fraction +1168 μm and ÷1651 μm is 0.5 mass-%.

The number of particles in each fraction is calculated from the fraction mass, assuming all particles
are spherical and all have the same average diameter. The total mass is 100 g and the density 1 g/ml.

Sieve Diameter Average Mass % Fraction Fraction Fraction Number of Particle

size, range, diameter under- mass, % mass, %/ particle particles, number,
μm μm μm size μm number % %/μm
1651 100.0
483 1410 0.5 0.001 300 0.01 0.00002
1168 99.5
335 1000 3.5 0.01 6700 0.32 0.00096
833 96.0
244 711 16.6 0.068 88200 4.24 0.01738
589 79.4
172 503 56.6 0.329 849400 40.84 0.23744
417 22.8
122 356 20.6 0.169 872600 41.96 0.34393
295 2.2
87 252 2.2 0.025 262600 12.63 0.14517
208 0.0
0 0 0
Σ=207980
Σ = 100 Σ = 100
0
Table 6.1

Example on particle size distribution taken from reference 13.

When drawing a bar diagram the area of each column should correspond to the relative quantity of
this fraction. If the width of all the columns are not the same, the unit on the Y-axis should therefore

51
rather be in terms of % per unit length (for instance %/μm) than in plain % (mass-% or number-%).
Figure 6.2 shows the size distribution for the population in table 6.1 based on mass as well as based
on number.

%/μm

Particle size distribution based on mass

0.4

0.3

0.2

0.1

μm
200 400 600 800 1000 1200 1400 1600 1800

%/μm

Particle size distribution based on number

0.4

0.3

0.2

0.1

μm
200 400 600 800 1000 1200 1400 1600 1800

Figure 6.2

Bar diagrams for the particle size distribution of table 6.1.

52
In case the size difference of the various sieves becomes smaller and smaller we end up with a
continuous curve, the differential frequency distribution as in the upper part of figure 6.3 (ref. 8).
Mathematically it is expressed as dF/dx. The frequency distribution can also be reported as a
cumulative curve with the range from 0-1. The cumulative curve is actually the integral F(x) of the
frequency distribution function from zero size to the maximum particle size.

For the two distributions in table 6.1 the cumulative curves are seen i figure 6.4.

In order to describe a particle population using one single size number several options are available.
The median is often used since this value is easily read from the cumulative distribution as the 50%
size. The medians for the particles in table 2 can be determined to 420 μm for the mass based
distribution and 344 μm for the number based distribution (see figure 6.4). The mode is the value of
the maximum size on the distribution curve,
i.e. the most frequently occurring size in the
sample. Other average values are the arithme-
tic, geometric, harmonic, quadratic and cubic.

As can be understood arithmetic mean particle

diameters can be based on several distributions:
Number distribution, surface, mass/volume.
For instance the mean arithmetic particle
diameter dN based on the number distribution
is calculated as (ref. 8, 14):

Sum of diameters of all particles (6.1)

Total number of particles

If the number of particles in the first interval is

called f1 and the average diameter for this inter-
val is d1 – and so on, then dN is calculated as: Figure 6.3

Particle size distribution and cumulative curve

dN = (f1*d1 + f2*d2 + ........)/(f1 + f2 + ........) or
dN = Σfidi/Σfi = Σfidi/N (6.2)

where N is the total number of particles.

53
Based on the values from table 6.1 the arithmetic number mean diameter dN is calculated to 420 μm
using this formula.

Similarly the mean arithmetic diameter based on mass distribution – the mass mean diameter dM –
is given by (ref. 14):

dM = Σmidi/M (6.3)

where mi is the mass of particles in the ith interval with average size di and M is the the total mass.

Accumulated particle size distribution

1
0.9 Number
distribution
0.8
0.7
Ac. distribution

0.6
Mass distribution
0.5
0.4
0.3
0.2
0.1
0
0 100 200 300 400 500 600 700 800 900 1000 1100
Particle size, μm

Figure 6.4

Accumulated frequency curves for mass and number based on data from tabel 6.1.

Since the quantity of material in each size fraction from sieving is usually weighed, the mass
distribution is often the most straightforward way of describing the particle size of a population.

Based on the values from table 6.1 dM is calculated to 524 μm.

54
mi in equation (6.3) can be written as: mi = kfidi3, where k is a constant for all particles, and in case
they are spherical k = πρp/6 with ρp as the particle density, equation (6.3) can be rewritten as (ref.
14):

dM = Σfidi4/Σfidi3 (6.4)

Using the data from table 6.1 dM is again calculated to 524 μm using equation (6.4).
In the same way the surface mean diameter (also known in literature as the volume-surface mean or
Sauter mean diameter) is given by:

dS = Σfidi3/Σfidi2 = Σsidi/S (6.5)

where si is the surface area of particles in the ith interval and S is the total surface area.
The Sauter mean diameter for the particles in table 6.1 is calculated to 484 μm.

Average values can also be described in a different way. For example is the average mass ma for all
particles of an average diameter dm equal to (ref. 14):

ma = Σmi/N = kdm3 (6.6)

Therefore dm for particles with shapes independant of size can be determined as:

dm = [ Σfidi3/N ]1/3 (6.7)

dm is the diameter of the sphere of average mass, not to be confused with the mass mean diameter
dM. For the population in tabel 6.2 dm can be calculated to 451 μm.

The reporting of a sieve analysis is most often based on the assumption, that the particles are
spherical, which seldom is the case in reality. In chemical engineering we often use the equivalent
sphere volume as a measure of the size, i.e. the particle is characterized by the diameter of the
sphere having the same volume as the particle. Other diameters are used – depending on the way the
size is determined. Using microscopy the equivalent circle diameter is used, defined by the circle
having the same area as the particle when inspected. Stokes diameter is used with sedimentation
experiments as the size of the sphere having the same settling rate as the particle in question.

55
A way to describe the shape of a particle is the sphericity ψ, which is defined as the surface area of
the equivalent sphere relative to the surface area of the particle. A sperical particle has a sphericity
of one, while the spericity of all other particles is less than unity; a cube for instance has a sphericity
of 0.806.

Another important particle parameter is the bulk density. It is determined by filling a well known –
typically cylindric - volume with the sample and weighing. The bulk density is very dependent on
the size distribution: Smaller particles can pack in the space between the larger particles and
increase the bulk density. The bulk density also depends on the degree of aeration, i.e. how much
air is mixed into the powder, for instance due to previous process steps. When determining the bulk
density one can distinguish between two different numbers: Loose bulk density and tapped. The
first is the density of the loose filling, while in the other one the cylindric container is tapped for
instance 10 times against the table in order to improve the packing of the particles and also to
remove air from the interparticulate space. Tapped bulk density can be considerably higher than the
loose one.

The difference between the various bulk densities is a way to consider a very unique powder/bulk
solid property: The ability to be compressed, i.e. the position/distance between individual particles
may be changed by exposing the bulk of material to an external stress (also often called
consolidation). The consolidation may change the bulk density, but also other properties such as
flowability. One simple way to characterize the flowability is through the Hausner-ratio, defined as
the tapped bulk density divided by the loose (aerated) bulk density. The lower the value the more
free flowing are the bulk particles expected to be.

The real particle density – i.e. the density of a single particle – is often very difficult to determine;
in addition the term it is not unambiguous. A single particle may represent a homogenous solid
structure at any cross section of the particle –like a stone. It may also be a solid shell with an empty
volume inside, or it can be a porous structure with open or closed pores, where even the size of the
pores may be important. The actual particle density depends on the way, the particles have been
formed.

What can generally be said is, that the particle density is higher than the tapped bulk density, but
equal to or lower than any solid material density found on the particular chemical product in the
literature. A microscopic investigation may clear up the structure of the single particle, and it may

56
also tell about the size distribution and the quality of the packing. It is equally important to realize
what the actual density number shall be used for. If for instance it is used for calculations of
terminal velocity using Stokes law, it is the matter of the total particle volume and the total mass. If
the density is used in calculations of ion exchange resin beds, where inter particle and pore moisture
takes part of the situation, the picture may become quite complex.

There are more scientific ways to determine particle densities – for instance mercury densitometry –
but these will not be discussed in this context.

If the particle is insoluble in a certain solvent a pycnometer-like procedure can be applied. A

pycnometer – or measuring flask – is partly filled with the particles, and the flask is filled to the
mark with the solvent. Since the density of the solvent is known, the particle density can be
calculated. Problems with this procedure are to ensure that gas is removed from the pores and to
realize to what extend the pores are filled with solvent. It may however be the only simple way to
get a value of the density.

A final issue to discuss is determination of dry matter. Dealing with products of organic origin one
must consider, that the normal drying conditions (+100 oC to constant weight) may be too severe
and degradation may take place. The drying can either be done at lower temperature at atmospheric
pressure or (better) under vacuum. Another solution is to use a heat radiation moisture analyzer, a
device where a balance is connected to a radiation source with temperature control, and where the
heating stops when the sample is dry. This is a quite fast and gentle way of analysing single
samples.

If the particles dry up with crystal water the actual drying temperature is of utmost importance,
since various hydrous crystals may be stable below – but not above - a certain temperature.

Gas analysis.

In many processes it may be of importance to know the concentrations of emitted or produced

gasses. That encounters for instance combustion, gasification and fermentation processes. A range
of electronic equipment is on the market for measuring the concentration of various gas
components, which include CO2, CO, O2, SO2, NO, NOx, CH4 etc. The instruments apply different
measuring principles; some instruments can be use in-line (i.e. directly in the process), but in most

57
cases it is necessary to extract a small part of the gas from the process pipe as a sample for analysis.
Since the electronic gas analyzers usually demand a very clean and dry gas in order not to pollute
and destroy the measuring cell, an extensive conditioning of the sample gas is necessary.

Figure 6.5 shows the overall way of analyzing dirty gas samples based on the principles used at the
Department of Chemical Engineering.

Final
Gassampling Sample Distributor sample
pretreatment station treatment Gas analyzers

Exhaust

Figure 6.5

Each step will be discussed in some necessary details.

The sampling point is usually just a small tube in the side of the process pipe. If the temperature in
the process is high a sampling tube made of steel may be necessary; otherwise inert teflon tubes are
often used. The important point is to make sure that the sample represents the overall gas
composition in the main process pipe. If the purpose of the sampling is to obtain information of the
content of dispersed solids in the gas (as for instance in stacks from solid fuel fired plants), it is
mandatory to use isokinetic sampling techniques, i.e. the flow rate into the sampling device is the
same as the gas flow rate in the main duct.

When the gas sample flows from the sampling point to the pretreatment station, it is important to
observe that condensation of water and plugging by dust do not prevent the free flow of gas.

In the sample pretreatment unit, which is schematically shown in figure 6.6, the gas is cooled in
order to remove moisture; the cooling temperature is just above 0 oC. The condensate is transferred
to a drain. A temperature controller after the cooler ensures correct cooling. In case unwanted gas
components are present they may be removed before entering the cooling device. That could be the
case for dust or for flue gasses containing NH3 (from injection before de-NOx SCR plants) together
with SO2 from sulphur in the fuel. When cooled the SO2 will react with NH3 and form salts which
may precipitate as solid crystals downstream of the cooling point and block filters and pipes. In this
case ammonia is removed by passing the gas through a bed of solid oxalic acid, where the alkaline
ammonia reacts with the acid.

58
After the cooler a particle filter is inserted; a moisture sensor in the bottom of the filter can be used
to control the cooler efficiency and take the gas directly to the exit through a 3-way valve in case
the moisture is too high. Finally a gas pump supplies the necessary head to make the gas flow
through the system. The size of the flow is determined by the demand of the gas analyzers. If the
flow is higher than needed the residual gas is vented.

At the department all gas analysis is centralized in order to minimize the number of expensive
devices and to improve the professionalism in application, maintenance and service. For that reason
samples from all user points meet in a distributor station, where the inlet pipe from the user point is
connected to the specific analytic equipment which is needed and available.

To analyzers

TIC FI
Cooler Filter

Pump Exhaust

Chemical HC
filter Pump
Humidity
controller
Sample gas

Figure 6.6

Before coming to the analyzers the gas has to pass a station (called gas panel) where final cleaning
takes place; this is also a site for adding calibration gasses, because the analyzers have to be
calibrated at specific intervals. A diagram of a gas panel station is shown in figure 6.7. The
incoming gas is again filtrated with moisture control as in the pretreatment unit. A 3-way valve
allows introducing calibration gas before the gas with the right flow and pressure is pumped to the
analyzers with excess sent to the vent. The gas flow needed must be 1 normalliter/min.

59
 Exhaust Exhaust

PI
Filter
To analyzers
Sample gas
FI
Humidity HC
controller Calibration
gas

Figure 6.7

In the end of the line we find the electronic gas analyzers. Numerous qualities and brands exist.
Here only a few relevant devices are shortly described.

When using in-situ gas analysis the resulting recorded gas composition would ideally be identical
with the real one. However, when the gas sample has passed a treatment station the final recorded
composition differs from the original. This concerns for instance the water vapor content; the
recorded composition is therefore on dry basis while the real one is on wet basis.

NGA 2000 for CO/CO2/O2. Manufacturer: Emerson Process Management. The instrument has 5
different channels for different gasses and measuring ranges. CO and CO2 are recorded due to their
infrared light absorption properties, while measurement of O2 is based on the paramagnetic
properties. Calibration must take place at least once a week or before the experiment.

CLD 700 EL for NO/NO2. Manufacturer: Eco Physics. The instrument has 4 measuring ranges
and is based upon the chemiluminiscence principle.

60
7. Measuring accuracy

Introduction.

A measurement can be either simple or complex. A simple measurement is typically a direct

reading of an instrument. A complex measurement – or indirect – can be based on several simple
measurements, usually including a mathematical equation to get the result.

Errors on measurements are systematic or random. Systematic errors are real – for instance if an
instrument is not calibrated. These errors can and must be avoided by careful planning of the
measurement. Random errors are not real ones, but deviations, as when many observations of the
same physical unit vary to a certain extent. Deviations can be reduced for instance by improving the
accuracy of the instrument, but not eliminated. The deviation therefore depends on the physical
object itself as well as the method of observation.

This section does not deal with systematic errors, but only with random deviations.

Uncertainty of simple measurements.

When doing measurements there may be some confusion in the applied glossary. Precision is
defined as the degree of concordance between the results of repeated measurements under same
conditions (repeatability). The accuracy is connected to the concept of error and is defined as the
degree of concordance between the measurement and the true value. The accuracy does not say
anything about the spreading of the individual results. Precise measurements are connected to low
spreading between the individual results, but do not have to be close to the true value. Refering to
figure 7.1 condition A the results may be described as not very accurate, but with high precision.
The contrary can be said for the results in condition B: They have very low precision, but the
average is accurate. In condition C the results are accurate and precise. Please remember that the
true value in many cases may not be known.
Reproduceability is related to repeatability, but is defined as the degree of concordance when the
measuring conditions are varying, for instance when the measurements are performed by different
persons or at various locations. The concept of tolerence is used by equipment manufacturers to
describe the documented accuracy at the time of purchase.

61
 Figure 7.1

A: High precision, low accuracy. B: Low precision, high accuracy of the average value. C: High precision and accuracy.

When many observations on the same physical phenomena under constant conditions are plotted as
frequency against size, they may often follow a Gaussian probability curve – a normal distribution
(figure 7.2). The definition of the standard deviation σ (or uncertainty) on a normal distribution
implies, that 2/3 of all observations are within the range of ± σ from the average value (μ in figure
7.2), 95 % of the observations within the range of ± 2σ and 99.7 % within ± 3σ.

Figure 7.2

62
Standard deviations may be in absolute terms – in oC, bar, m3 etc. – or as relative to the average
value - for instance in %.
If we for a certain parameter have n simple observations a1, a2, ....an with the average value am =
(a1+ a2 + ......an)/n and the deviations si of the individual observations from the average value are
equal to si = ai – am, the standard deviation σ on the simple observation according to the “theory of
error” is equal to:

∑ 2
𝑠𝑠
𝜎𝜎 = �𝑛𝑛−1𝑖𝑖 (7.1)

The standard deviation σm on the average value am is described as:

∑ 𝑠𝑠2
𝜎𝜎𝑚𝑚 = �𝑛𝑛(𝑛𝑛−1)
𝑖𝑖
(7.2)

The standard deviation of simple measurements is in the technical world seldom based on a large
number of observations. A few readings in addition to a skilled estimation on the accuracy of the
method are the typical situation. Important is the accuracy class of the instrument and the reading
accuracy. For digital instruments there is no reading error, but this is not the case for analog
instruments.

For instance dealing with temperature measurements it is important to know, that thermocouples are
seldom better than ± 0.5-1 oC and Pt100 sensors (depending on the accuracy class) are accurate to
about ± 0.1-0.5 oC. Manometers, pressure transducers, electronic flowmeters etc. are often in the
range of ± 1-3 %, and rotameters with manual scale reading may be even more inaccurate. See
section 1.3 for more details on accuracy of instruments.

Determination of the uncertainty of simple measurements is often a difficult task for the chemical
engineer, partly because of the number of observations and partly because of the nature of the
parameter. However, it is much better to identify a value with high uncertainty instead of having no
value at all.

Uncertainty of combined measurements.

A combined (complex, indirect) measurement depends on a number of simple measurements,

usually using a mathematical equation to define the relationship between the simple and the
combined measurements: Y = f(X1, X2,….Xk), where Y is the combined and X1…Xk are the simple

63
measurements. The standard deviation of combined measurements involving several simple
observations can be calculated from formulas (see below) based upon the standard deviations of the
simple measurements.

There are two accepted ways of calculating the combined uncertainty – either using equation (7.1)
or equation (7.2).

𝜕𝜕𝜕𝜕 𝜕𝜕𝜕𝜕 𝜕𝜕𝜕𝜕

𝜎𝜎(𝑌𝑌) = 𝜎𝜎
𝜕𝜕𝑋𝑋1 1
+ 𝜕𝜕𝑋𝑋2
𝜎𝜎2 + ⋯ + 𝜕𝜕𝑋𝑋 𝜎𝜎𝑘𝑘 (7.3)
𝑘𝑘

𝜕𝜕𝜕𝜕 2 𝜕𝜕𝜕𝜕 2 𝜕𝜕𝜕𝜕 2

𝜎𝜎(𝑌𝑌) = ��𝜎𝜎1 𝜕𝜕𝑋𝑋 � + �𝜎𝜎2 𝜕𝜕𝑋𝑋 � + ⋯ + �𝜎𝜎𝑘𝑘 𝜕𝜕𝑋𝑋 � (7.4)
1 2 𝑘𝑘

In these equations σ is a symbol for uncertainty on the variables. It is a prerequisite that the
variables are independent. The partial differentials in equation (7.3) may be either positive or
negative; the same could be the case for the uncertainties of the simple measurements, if the
uncertainty is calculated as the deviation between an actual value and an average value. σ(Y)
calculated from (7.3) may therefore not be very well defined. If we use the numerical values for all
differentials and all uncertainties the value of σ(Y) will achieve a “maximum” uncertainty.

σ(Y) calculated according to equation (7.4) is not influenced by positive or negative values of the
differentials or uncertainties. This σ(Y) is also called the standard deviation as defined by the
Gaussian graph in figure 7.2.

For the special case where Y = a + bX1 + cX2 + dX3 with standard deviations σ1, σ2 and σ3 the
combined uncertainty is:

𝜎𝜎(𝑌𝑌) = �(𝑏𝑏𝑏𝑏1 )2 + (𝑐𝑐𝜎𝜎2 )2 + (𝑑𝑑𝜎𝜎3 )2 (7.5)

For another special case where Y = kX1a·X2b·X3c the total combined relative standard deviation is:

𝜎𝜎(𝑌𝑌) 𝑎𝑎𝑎𝑎 2
𝑏𝑏𝜎𝜎 𝑐𝑐𝜎𝜎 2 2
= �� 𝑋𝑋 1 � + � 𝑋𝑋 2 � + � 𝑋𝑋 3 � (7.6)
𝑌𝑌 1 2 3

The relative uncertainty σ(Y)/Y can in many cases easily be determined by logarithmic
differentiation. As a example for the relation

𝑋𝑋13 ∙𝑋𝑋2 ∙�𝑋𝑋3

𝑌𝑌 = (7.7)
𝑋𝑋42

64
Taking logarithm on both sides we get: logY = 3 logX1 +logX2 +½ log X3 – 2 logX4.

By differentiation we get:

𝑑𝑑𝑑𝑑 𝑑𝑑𝑑𝑑1 𝑑𝑑𝑑𝑑2 𝑑𝑑𝑑𝑑3 𝑑𝑑𝑑𝑑4

𝑌𝑌
=3 + + ½ −2 (7.8)
𝑋𝑋1 𝑋𝑋2 𝑋𝑋3 𝑋𝑋4

If we consider dX1 = σ1 etc and take the numerical values we get according to equation (7.3) the
maximal combined uncertainty:

𝑑𝑑𝑑𝑑 𝑑𝑑𝑑𝑑1 𝑑𝑑𝑑𝑑 𝑑𝑑𝑑𝑑3 𝑑𝑑𝑑𝑑4

� 𝑌𝑌 � = �3 � + � 𝑋𝑋 2 � + �½ � + �2 � (7.9)
𝑚𝑚𝑚𝑚𝑚𝑚 𝑋𝑋1 2 𝑋𝑋3 𝑋𝑋4

If we in stead use equation (7.4) we get the combined standard deviation:

𝜎𝜎(𝑌𝑌) 3𝜎𝜎 𝜎𝜎 2
𝜎𝜎 2𝜎𝜎 2 2 2
= �� 𝑋𝑋 1 � + �𝑋𝑋2 � + �2𝑋𝑋3 � + � 𝑋𝑋 4 � (7.10)
𝑌𝑌 1 2 3 4

which is to be compared with equation (7.6).

It can be understood that uncertainties of simple measurements are often not very accurate and that
combined uncertainties consequently in a meaningful way is described using only few significant
digits. In addition the equations (7.3) and (7.4) are only valid with some approximations.
Uncertainties may therefore be presented with only one or two significant digits, as shown in the
example below.

Example.

As an example consider the calculation of the density ρ of a gas at 0 oC and 100000 Pa based upon
measurements of the mass m of a volume V of the gas at the actual pressure p (Pa) and temperature
T (oC):

𝑚𝑚 100000 𝑇𝑇
𝜌𝜌 = 𝑉𝑉
∙ 𝑝𝑝
�1 + 273�

(7.11)

m, V, p and T are simple measurements with the uncertainties 𝜎𝜎m, 𝜎𝜎V, 𝜎𝜎p and 𝜎𝜎T.

By differentiation we get:

𝜕𝜕𝜕𝜕 1 100000 𝑇𝑇
𝜕𝜕𝜕𝜕
= 𝑉𝑉
∙ 𝑝𝑝
�1 + 273�

65
 𝜕𝜕𝜕𝜕 𝑚𝑚 100000 𝑇𝑇
𝜕𝜕𝜕𝜕
=− 𝑉𝑉 2
∙ 𝑝𝑝
�1 + 273�

𝜕𝜕𝜕𝜕 𝑚𝑚 100000 𝑇𝑇
𝜕𝜕𝜕𝜕
=− 𝑉𝑉
∙ 𝑝𝑝2
�1 + 273�

𝜕𝜕𝜕𝜕 𝑚𝑚 100000 1
𝜕𝜕𝜕𝜕
= 𝑉𝑉
∙ 𝑝𝑝 273

By measuring the following values are found: m = 2.4875 g, V = 980 ml, p = 97.56 kPa and T =
21.4 oC. The resulting value of ρ = 2.6·10-3 g/ml = 2.6 kg/m3. The uncertainties are estimated to: σm
𝜕𝜕𝜕𝜕
= 2.3 mg, σV = 1.3 ml, σp = 120 Pa and σT = 0.3 oC. The partial differential values are found: 𝜕𝜕𝜕𝜕 =
𝜕𝜕𝜕𝜕 𝜕𝜕𝜕𝜕 𝜕𝜕𝜕𝜕
0.0011, 𝜕𝜕𝜕𝜕
= −2.9 ∙ 10−6 , 𝜕𝜕𝜕𝜕 = −2.9 · 10−8 and 𝜕𝜕𝜕𝜕 = 9.4 ∙ 10−6 .

Inserting the partial differentials and the uncertainties in equation (7.3) we get:

σ(ρ) = 0.0011·2.3·10-3 – 2.9·10-6·1.3 - 2.9·10-8 ·120 + 9.5·10-6·0.3 = (2.53 - 3.77 - 3.48 + 2.85)·10-6
= - 1.9·10-6 g/ml

If we use the numerical values we get:

σ(ρ) = (2.53 + 3.77 + 3.48 + 2.85)·10-6 = 13 ·10-6 g/ml

If we instead insert the differentials and the uncertainties in equation (7.4) we get:

σ(ρ) = �(0.0011 ∙ 2.3 ∙ 10−3 )2 + (2.9 ∙ 1.3 ∙ 10−6 )2 + (2.9 ∙ 120 ∙ 10−8 )2 + (9.5 ∙ 0.3 ∙ 10−6 )2 =

= �(6.4 + 14.2 + 12.1 + 8.1)10−12 = 6.4 ·10-6 g/ml

The relative uncertainty is therefore σ(ρ)/ρ = 6.4 ·10-6/2.6·10-3 = 2.5 ‰

It may be recognized that the designation “maximum uncertainty” for the results using equation
(7.3) with numerical values can somewhat be justified. It can also be seen, that the 4 parameters
contribute more or less equal to the total uncertainty.

66
8. Report writing

This guide is directed specifically for reports associated with the unit operations exercises performed
in the DTU dep. of Chemical & Biochemical Engineering Pilot Plant.
Reports made for other courses, projects and advanced research work may follow different procedures
or have other attributes and priorities, and therefore their layout can be different from the layout
proposed in the present guide.

Table of content:

8.1 General
8.2 General structure of the report
8.3 Before you hand in the report
8.4 Evaluation of the report

8.1 General.
The report must be based on the questions from the reporting section in the specific exercise manual and
must present, discuss and conclude on the individual and overall results and observations, including an
evaluation on the specific purpose of the exercise.

The report must show your results and observations. Research in the real world does not always give an
exact or the expected outcome or results, either way you must use and comment on the results you get from
the exercise.

Make the report easy to read and understand. The report must follow the general report structure described
below and must have a flow, which guides the reader in a natural way through the questions, results and
conclusions. The language shall be fluent and easy to read, with correct spelling and grammar. Avoid the use
of personal pronouns like “we”, “I” etc.

References must be made where data, formulas and graphs are introduced for the first time in the report. Do
not forget the references within the report to calculation examples, raw data, appendices, tables and figures.

Comment on all tables and figures, and make the interpretation from the data presentation relevant to the
subject being presented.

67
Students are encouraged to ask relevant questions to the teachers during the experiment and during report
writing, but discuss with your teammates and do some investigations in manual/textbooks and internet before
asking.

Be sure to read section 3: “Before you hand in the report”

8.2. General structure of the report

The following sections (except for the uncertainty analysis section) must be present in the report. The
sequence below is recommended.

• Front page
• Abstract
• Table of contents
• List of symbols
• Introduction
• Methods, results and analysis
• Discussions and conclusions
• Uncertainty analysis (if required or applicable)
• Calculation examples (If not in Appendix)
• References
• Appendices

In some cases, sections may be renamed according to the student’s home university preference.

Front page.
On the front page the following information is required:

- Identification/name of the experiment

- Name and student number (if DTU student)/e-mail address(es) of the performer(s)

- Responsible author (If such a person exists)

- Team/group name or number

- Home University (if not DTU)

- Date of issuing the report

68
Abstract
Typically about half a page.

A summary, which gives the reader the main information and conclusions of the report. In principle meant
for a reader who wants a fast and concise overview of the work. Only facts and results, preferably
quantitative (numbers).

No general descriptions, tables or figures.

Table of contents
Hint: Use header typography design to automatically generate a table of contents in Word.

List of symbols
Include the units for the symbol list. A table is often preferable.

Introduction
Approximately one page plus diagrams/pictures.

A descriptive summary of the exercise: Typical industrial applications, purpose of the exercise, used
equipment (Add a P&I diagram and/or a picture if relevant), and used methods, without repeating procedure
from manual.

This section shall not contain an introduction to the theory behind the experimental work or a detailed step-
by-step description of what has been done.

Methods, Results and Analysis

This is the main section of the report where answers to questions from the reporting section of the exercise
manual are presented and discussed.

To ease report reading, we want you to report your answers following the questions sequence in the exercise
manual.

Give calculation examples in this section only if it is relevant to facilitate the understanding. Calculation
examples are normally presented in the “Calculation examples section” or in appendices.

The purpose of this section is:

• explain how the experiments were performed,

• what results were achieved,
• comparison of results to other relevant results or theory. Are the results as expected?

69
 • relevant elaboration of the results validity, including the quality of the data/equations used (if possible
add some estimate of uncertainties).

Make sub-sections according to the question sequence of exercise manual. Each subsection may present used
equations (formulas) (remember references to sources). Remember to include references to where calculation
examples can be found. Also include references, if relevant, to where raw data can be found (appendix or for
large data amounts, EXCEL sheet).

The results are generally best presented in tables and figures. Each table and figure must be numbered and be
accompanied by a caption to facilitate references in the text. Remember units on axis. If you print the report
on a monochrome printer, make sure the datasets are distinguishable.

When commenting on the tables and figures, one may explain what obviously can be seen, but the main
expectation is to receive an interpretation and comparison between theory and practice and to extract any
surprising and interesting aspects from the data. Even your results do not match the theory this is what you
got from the exercise. Many exercises are based on empirical theory, which may not match perfectly the
actual exercise conditions.

Discuss the observations, results and conclusions, which can be drawn from the experimental work. Discuss
the reliability and accuracy of the results and explain any deviations between reality and theory/literature.

Even if the report does not include a formal uncertainty analysis section, it is good practice to give a
qualified engineers’ estimate on the accuracy. In case, explain the number of significant figures on the result
that reflect the accuracy of measurements.

Discussion and Conclusions

When the reader has read the Result section above, which contains result analysis and preliminary
conclusions, it is important to do an overall interpretation including all the results and observations, and to
draw the final conclusions.

For this, you may ask yourself questions like:

• What are the main conclusions and key messages you will extract from your excersice work?
• Is theory in agreement with practice? How much can I, as an engineer, rely on typical design and
upscaling calculations for this equipment.
• What are pro’s and con’s for using the equipment in industrial applications?

An important part for the discussion, and where the talented engineer stands out, is to go beyond the results
and use one’s critical mind and engineering skills to elaborate on the results and experiences. Try to

70
introduce new theoretical aspects by elaborating on the exercise manual or from other textbooks (references
if relevant!). This is where the report can show off as a top-notch engineering report.

Calculation examples
Calculation examples may be presented where it makes most sense to facilitate the readers understanding of
the results. It could be in the Results section, in a separate Calculation examples section, or in an Appendix,
or a mixture.

Drawings or sketches may be included if it facilitates the understanding of the calculations, i.e. to describe
mass and energy transfer processes and balances.

A copy of for instance a Matlab-code is normally not accepted as it may be difficult for the reader to follow.

Handwritten calculation examples, placed as appendix, are accepted.

Uncertainty analysis (If required or appropriate)

Data from technical measurements are generally not very precise. Most of our measuring devices and meters
are seldomly calibrated, so the accuracy can also be questionable.

Investigate what is the precision of the instruments being used. These data can be obtained from the
manufacturer’s datasheets online. I.e. pressure, flow and similar measurements from an electronic device are
rarely more precise than ± 2%. In addition to normal random instrument error, analogue instruments often
add reading errors. Also consider systematic errors for instance in case of non-calibrated devices.

Present the final results with the number of significant figures corresponding to the accuracy/precision of the
work. If you cannot complete an uncertainty analysis, use the rule of thumb: “The number of significant
figures in the result is the same as the least number of significant figures in data used in the calculation.”

Theory of uncertainty analysis may be found in the yellow handout “Experimental Process Technology by
DTU Chemical Engineering” or in the specific statistical literature.

References
A List external references used during the construction of the report.

Appendices
All relevant data necessary for the reporting and calculations and which has not been introduced in the main
report.

Typical examples are:

- Calculation examples

71
 - Raw data.
- Notes, figures, diagrams and drawings relevant for the report but not included in the main report.
- Any rough calculations not reported anywhere else (for instance Excel sheets).

Appendices including information of electronic origin (for instance Excel sheets), must be presented in a
way to make it easy to understand.

Embedded files are not allowed.

Do not include long printouts from log files, but if some data is needed clarity, isolate and present the
important data.

Remember: Appendices that are not referred to in the report, will not be read.

72
8.3. Before you hand in the report!
1. Proof read it! – Or better have a colleague who is not familiar with the exercise to proof read it.

2. Does the report answer the questions presented in the exercise manual’s reporting section

3. Check all references and units. Where new formulas, data and numbers are introduced, there must be
a reference. Remember to include references to your calculation examples, tables and figures!

4. Is there a calculation example for all introduced results?

5. Comment on the graphs and tables beside what the reader can obviously see.

6. Facilitate the structure and the flow of the report so that the reader naturally can read the report page
by page and do not need to scroll around in the report (Except for the calculation examples). Internal
references are crucial in this respect. Remember who reads it (the teacher) sees the report for the first
time, and even familiar with the theory, should understand your presentation and process of thought.

73
8.4. Evaluation of the report
The grading of the report will be done based on the evaluation of some key factors, and the weight and grade
of each factor will give the resulting grade of the report.

The key factors to be graded, as used in the experimental courses at DTU, will follow the weight distribution
as seen in Table 1 below:

Table 1: Grading scores

Factor % of total

Report structure, lay-out and formalities according to this document

(5), including logical sectioning, references and appendices; front 15
page (1), abstract (7), table of content (1) and list of symbols (1)

Scientific language, correct terminology, technical phrases 5

Introduction: 5%

Methods, results and analysis: 45%

Discussions and conclusions 10% 80

Uncertainty analysis (this can give bonus points) Max 5%

Calculation examples 20%

The grading will be done for DTU students according to the Danish grading scale, and for students from
international universities according to the American/ECTS grading scale. The comparison of the two grading
scales is shown in Table 2 below.

Table 2: Appoxiamate conversion from % score to grade

Danish scale 12 10 7 4 2 00 -3
American/ECTS A B C D E Fx F
scale
% completion >92 >84 >68 >60 >50 <50 <30

74
Reports and presentations generate separate marks. For these, both Danish and American graders may further
expand the scale by using “+” or “÷”, in addition to grades. The final course grade cannot be expanded with
“+” or “÷”. Grades below 2/E are considered non-pass.

A top graded report should not only describe the results and answer the questions adequately and correctly.
Engineers are expected to be able to analyse the experiences and data, to draw the conclusions and
consequences, to identify problems and compare various information, to comment on contradictory results
and in any way to apply critical process engineering skills on the observations.

75
9 Process and plant design

Building a chemical production facility involves a number of steps which can be grouped in several
ways. In order to know what to build one has to define the product, whether it is a simple chemical
compound or a complex formulation of many individual reagents. At this rather early stage it may
be advantageous to make a user requirement specification (URS), which is a number of demands
and requirements exposed to the process, equipment, facilities, procedures, manpower,
infrastructure etc. It can be anything from GMP demands (coming from the medicinal authorities
for use in pharmaceutical manufacturing companies) to in-house practicalities of using special
wellknown equipment, where spareparts may already be on stock. From here the design procedure
starts with designing the process – i.e. describing the manufacturing steps and their main conditions
from rawmaterials to the final product, including decisions to use batch or continuous processing
and the kind of reactor (backmix, plug flow). When these details are fixed it is time to focus on the
plant design, where individual components are defined, selected and dimensioned. In some later
step the detailed operating conditions and procedures for operation must be described – in some
industries called SOP´s (standard operation procedures). Procedures are not only for the
manufacturing process itself, but also includes procedures for quality control, laboratory analysis,
process cleaning, maintenance and so on.

Design phases can also be split into conceptual design, basic design and detailed design with an
increase in the details considered. The content could be:

• Conceptual design: A few pages comprising a simplified flowdiagram, capacities with a

gross list of consumables (feedstock, utilities etc.) and products, overall demands to
organisation, facilities and building area.
• Basic design: P&I diagram, components list, drawings of main components, process flow in
buildings, risk assessments, outline of QA documents, outline of data acquisition systems
etc.
• Detailed design: Everything ready for purchasing, contracting and erection of plant
including 3D drawings of the process plant, maintenance plans, building layouts

After the design phase and dimensioning/selecting plant parts and components it is time for the
physical erection, which include elements of purchasing, construction, building, testing,
commissioning and start up. In parallel to these ordinary engineering activities some industries deal

76
with formal quality activities – called qualification – in order to make sure that the plant is
established according to the approved design. This is especially important for the pharmaceutical
industries, where extended control of all activities having any possible influence on the final
product quality are required by the medicinal authorities. This is to some extend also valid for
biotech and food industries.

Going back to the process design phase one may ask about what is necessary to know in order to
perform the design:

• Knowledge of all process steps and their main operating conditions

• Defining for instance process cleaning procedures since it involves application of chemicals
and special access ports to the production plant
• Knowledge of raw materials and their packaging, destiny of waste products, batch size and
package size of finished products
• Knowledge of access to utilities, sewer, stack
• The selected control strategies play a key role for determining instruments, control
equipment, computers and datalogging etc.
• For pharmaceutical companies the quality assurance department must be involved in the
complete design, construction, erecting, commissioning and production phases.

The process design is most often performed in terms of an extended P&I diagram which is a two-
dimensional principal sketch of all components, all piping, some dimensions and quality of
materials, functionality and interlocking of control instruments, main operational parameters. See
section 10 for a detailed description of flow diagrams and P&I diagrams.

77
10 Flow-sheets and P&I diagrams

The flow-sheet is a simple way of showing the equipment which is involved in carrying out a
process. It is a diagrammatic model of the process and shows the arrangement of the main
components, how they are interconnected by the flow of components, and in the more advanced
versions also the flow-rates, compositions and operating conditions are mentioned on the diagram.
Figure 10.1 shows a flow-sheet for a simple process.

The flow-sheet is used to describe the process in order to understand, what is going on, but also as a
basis for mass- and heat balances and for the more detailed design and dimensioning of the plant.
The flow-sheet can be made as a simple block-diagram or as a more pictorial presentation, where
the nature of the components can be recognized immediately. Figure 10.1 is an example of the later.

Flow diagrams are expected to show the essential components and flow lines. It is a good idea not
to put too many details of minor importance into the diagram; details can easily cover the over-all
principles in the process and make it difficult to understand or get an overview. However, the
number of details must of course always reflect the purpose of the actual diagram. It is important

1530 kg/
batch

Component A

3000 liter/
batch
CIP
Component B
Respiratory filter

Reactor
CIP
< 2 g solids/
Process steam liter

5 m3
Product
Pump Cooling water
10 m3 vessel
Condensate

2.5 m3/h
70 oC Heat
exchanger

Draining Hydro cyclone

20 oC

Waste
1.5 tons/h
precipitate

Figure 10.1

78
that the sequence of components on the diagram reflects the reality and that the ordinary flow
direction is indicated.

As for PID’s (see below) a number of national standards exist for making flow-sheets and for the
use of symbols. However most companies and organisations are using their own standards. As far
as process data are concerned they can be added as shown in Figure 10.1. For more complicated
diagrams it may be preferred to combine the diagram with a table where all the data are listed. This
can be combined with a numbering of the stream lines, so there is no doubt about the identification.

Large plants may need a number of flow-sheets to describe the entire process; it may also be
advantageous to make a special diagram for supplies of utilities, for instance water, steam,
compressed air, cooling media etc.

The next step in process design after the flow-sheet is the piping and instrumentation diagram (P&I
diagram or PID), sometimes also called process instrumentation diagrams. An example is shown in
Figure 10.2. PID’s are identifying all components with tag-numbers, which are all valves, pumps,
filters, reactors, vessels, heat exchangers, other process components, instruments etc. Some
companies even address a tag-number to pipe sections, but that is not usual. In stead it is usual to
add pipe information on the diagram: AISI 316/Ø40x2.0 means a steel quality according to AISI
316 (acid resistant austenitic stainless steel) with an outside pipe diameter 40 mm and a pipe wall
thickness 2.0 mm.

The main components on the PID are shown as pictorial presentations, while smaller components
are identified according to the legend example following this chapter. As with the main components
every organisation has its own legend for the instruments, valves etc., and the legend below has
become a standard for the DTU Chemical Engineering Department used for the pilot plants. Some
important instrument first letter abbreviations are general: “P” means pressure, “T” means
temperature, “L” means level, “C” means conductivity, “A” means any other analytical instrument
(pH-sensor, gas analysis etc.), “V” means valve, etc. For instruments several second or third letters
are often used: “I” means indicator (others use “E”, for element), “T” for transmitter, “R” for
recording, “C” for controller, “A” for alarm, “H”/”L” in the third letter for high/low in connection
with alarms, all used to identify the nature of the instrument and the context of automation in which
it is located. For instance “TI” means temperature indicator or element, “PT” means pressure
transmitter, “CIC” means a conductivity indicator connected to a controller function. While “PR”

79
previously was very often used to identify a pressure recording unit (typically a paperbased printer
in the switch board panel), the present days wide application of datalogging to computers with
unlimited possibilities for printing graphs etc makes the “R” information a little bit outdated.

V1 U1 TI PI FI
3 3 3
Component A
AISI 316L/Ø40mmx1.8 mm
CIP
Component B V10
V2 F1 V11
TAL TAH
1 1 U3
V31 TIC
1

V4 V12 V5 Product
Process steam
V30 V32 V33 Cooling water vessel
PI PI
TI

AISI 316L/DN50
1 2
T1 4

P1 AI
1 V20
T2
V3
U2 TSH
HE1 2

V8 V7 V6
Condensate TIC
2
TAH
2

Hydro cyclone
T3

T4

Figure 10.2

As can be seen from figure 10.3 and 10.4 the location of the instrument can be specified in the
symbol. Figure 10.3 represents a pressure indicator (manometer) located at the actual measuring
point on the plant, while figure 10.4 indicate, that the pressure signal can be seen on the central
control panel. For small plants it makes no sense to distinguish between those two positions.

PI1 PI1

Figure 10.3 Figure 10.4

Figure 10.5 shows a temperature controller function indicating, that the device to be activated from
the controller is the valve located upstream of the temperature indicator. It is also indicated that the
controller is equipped with a “high alarm”(TAH = temperature alarm high) and a “low alarm”
(TAL), meaning that the controller shows an alarm (visual, auditive) if the temperature is increased
above the “high alarm” level or below the “low alarm” level. It is also possible to indicate a switch

80
function using the letter “S” as the third letter. The controller will in this case switch off some other
device (pump, close valve etc) in case the switch point is passed. Controllers may therefore have a
high alarm point, high switch point, low alarm point and low switch point.

TAL

TAH

TIC

NO

Figure 10.5

Figure 10.5 also inform about the characteristic nature of the control valve, that it is normally open
(NO), i.e. in un-powered condition the valve is fully open. The opposite is normally closed (NC).
The wording in the American nomenclature is “Fail open” and “Fail closed”.

Neither flow-sheets nor PID’s are able to tell about the 3-dimensional physical location of the
various components relative to the other. For this kind of layout an isometric drawing – or better a
real 3D drawing – is necessary. Computer programs are available for these applications. The 3-
dimensional arrangement of the pipes and components relative to each other is necessary for the
actual construction of the plant; it may also be useful for determining the lengths of pipes, the slope
of pipes for draining purposes (as in GMP complying plants), exact position of components etc.
Figure 10.6 shows an example of an isometric drawing.

3.0 m

PI
1.3 m

m
3.6
2.8 m

1.7 m

Figure 10.6

81
 P&I diagram legend

Control valve AI Analytic instrument

Globe valve TI Temperature indicator

Ball valve PI Pressure indicator

Gate valve PT Pressure transmitter

Membrane valve FI Flow indicator

Three way valve FT Flow transmitter

Reduction valve LI Level indicator

Safety valve LS Level switch

Check valve WE Weighing element

Powered valve WT Weighing transmitter

Butterfly valve CI Conductivity indicator

F Filter
Heat exchanger
P Pump/fan
Pump/fan
T Tank, vessel

Steam trap V Valve

U Various kind of component

In line filter
SP Sample point
Filter
M Motor

SY Frequency converter PC Pressure controller

HE Heat exchanger

82
11 Process control

The purpose of automatic process control is to keep a certain process variable within pre-defined
limits - often called the set point – irrespective of any process disturbances and the inherent process
dynamics. The selection of control principles and equipment to perform the actual control task
depends on the expected difficulty of the control, the consequences of lack of control, price of
equipment etc. A theoretical pre-analysis of the operation may be advantageous, especially if the
process and therefore also the control task is complicated with many interfering variables.
The purpose of this section is the give a short overview of the basic control principles in order for
the reader to be able to select the right procedure in simple practical situations. For more theoretical
considerations and selection of control equipment see the relevant literature (textbooks, supplier
information etc.).

Basic glossary and terms.

Control theory talks about a step function, in which case the variable to be controlled is suddenly
changed by a step, for instance due to an outside process change. In many cases the controlled
variable is changing in a more slow way, for instance a drifting following a ramp function. This is
typically the case for temperature changes, as an instantaneous large change can often not takes
place due to large heat capacities in the process or system; however a sudden change in pressure or
flow is very likely.
Control principles are often described by using a simplified block diagram as in figure 11.1:

Control
Setpoint Deviation signal Controlling
Controller
+ component Controlled
÷ variable
Transmitter

Figure 11.1

The deviation (error) = setpoint ÷ transmitted controlled variable. The ideal objective of every
control system is to keep the deviation = 0 or in a well defined narrow range. The comparison
between setpoint and controlled variable usually takes place inside the controller resulting in an

83
output called the controlled signal (controller output). The controlled signal may be a voltage or air
pressure, the effect of which is to influence the output of the controlling component. This can be a
valve, pump, heating element etc. In order for the controller to read the actual controlled variable a
transmitter is often necessary.

Example: The controller has to keep a liquid flow constant. The controlling component could be a
valve, the position of which will adjust the flow rate. The transmitter could be a flow sensor
identifying the actual flow value, which is returned to the controller for comparison with the
setpoint.

On-off control.

The simplest control method is the on-off procedure: The controlling component can only be
positioned in two conditions. A valve can be open or closed, a pump can run with a fixed speed or
be stopped etc. The controlled signal (controller output) may consequently look like in figure
11.2(a):
a

Figure 11.2

The resulting respons of the controlled variable depends on the nature of the variable and the
controlling component, but could for instance look like the curve in figure 11.2(b). The setpoint
should be half way between the upper and the lower value of the variable. The difference between
upper and lower value – and therefore the accuracy of the control - can be adjusted by varying the
values of the controlled signal where the controller changes from on to off or vice versa. The
frequency (wave length) depends on the process respons dynamics.

Proportional control.

The control methods to be discussed now are continuous on contrary to the discontinuous on-off
procedure.

84
The simplest continuous control method is the proportional control, called P. The definition is that
the change in controlled signal (y) is proportional to the deviation (error) e:

y = Kp·e (11.1)

The constant Kp is called the gain. Let us consider a situation where the deviation e = 0, in which
case according to equation (11.1) the change in controlled signal (y) from the expected value is
zero. A certain change in the process conditions may only be dealt with by a certain change in
controlled signal (y ≠ 0) resulting in a change in controlled variable. The deviation e is
consequently ≠ 0 at a new equilibrium. This phenomenon is called offset, which according to
equation (11.1) is unavoidable at all situations apart from the process condition where the change in
y is zero. In most cases the resulting controlled variable therefore differs from the setpoint. This is
the main disadvantage of the P-control function.

This is shown in figure 11.3. The upper curve (b) represents a change in process conditions, and the
resulting change in controlled variable is seen in curve (a), which also indicate the resulting offset.

Figure 11.3

The value of Kp defines the sensitivity of the control function: A high Kp-value results in a sensitive
controller, which could even give an un-stable respons, but also a small offset.

Another term used is the so-called proportional band, PB, which is defined as the percentage
deviation required to bring the controlling component from one extreme to the other relative to the
entire span. The proportional band is inversely proportional to the gain. A high Kp means a low PB.

85
The higher the PB the higher offset, but also a slower respons and a faster damping of the varying
respons. When PB approaches zero the control functionality approaches on-off control.

The gain/proportional band can be adjusted on most controllers, but the optimal value is a
compromise between low offset and fast and stable control function. Figure 11.4 shows the respons
to a step change in process conditions - curve (a) - with 3 different gains. The 3 lines denoted “B”
represents the average value of the controlled variable after some time with initial oscillation. Curve
(b), (c) and (d) is the result of increasing PB (decreasing gain) which results in increasing offset.

Figure 11.4

Integral control.

The integral control function, I, is defined by:

𝑑𝑑𝑑𝑑
𝑑𝑑𝑑𝑑
= Ki·e (11.2)

The rate of change in control signal is proportional to the deviation. The consequence of integral
control is a zero offset, but also a slow and continuously oscillating respons, which are due to time
delays. If Ki = 0 there is no integral control. The term integral time, ti, which can be adjusted on the
controller, is inversely proportional to the Ki value. A large integral time means a low integral effect
of the controller. Anglo-American literature use a term called reset rate – proportional to the Ki.

Integral control is seldom performed alone, but combined with proportional control – PI control.

86
Derivative control.

This control form is defined by equation (11.3):

𝑑𝑑𝑑𝑑
y = Kd∙ 𝑑𝑑𝑑𝑑 (11.3)

The derivative action – also called rate action – is effective towards large sudden changes of the
controlled variable, but cannot influence the offset. Derivative control is used in processes with fast
changes in conditions. The derivative constant Kd – proportional to the derivative time (td) often
used in controllers– is small for low derivative action. The derivative control is never done alone.

PID control.

The best control is achieved by combining all three continuous control methods, individually
adjusted according to the need of the actual process. However, as it can be seen from equation
(11.4) the three methods are not totally independent, since Kp – due to the definition of ti and td –
also influence the integral and derivative control:

𝐾𝐾𝑝𝑝 𝑑𝑑𝑑𝑑
y = Kp·e + ∫ 𝑒𝑒 ∙ 𝑑𝑑𝑑𝑑 + Kp·td· 𝑑𝑑𝑑𝑑 (11.4)
𝑡𝑡𝑖𝑖

Feed forward/feed back.

The control procedure as shown in figure 11.1, where the controlled variable as output from the
controller is measured and used as controller input in order to influence the output and the process,
is called feed back control through a closed loop action. This is the dominating control function.
Feed forward control is based upon a known relationship between disturbancies of the input
variables to a process, for instance the relationship between two raw material feed flows to a
reactor. A change in flow of one component can be immediately corrected by a change in flow of
the other component, so there is no need for the resulting controlled variable – the product – to be
reported back to the controller input. Feed forward control fails in case unknown factors not taken
into account appears, in the example above for instance if the concentration of one of the feed
streams suddenly changes. If feed forward control can be applied the control action may be faster,
because we do not have to wait for the resulting influence on the output of the control.

87
12 GMP and CIP cleaning

GMP means Good Manufacturing Practice and is a mindset established over the last 30-40 years –
especially in the pharmaceutical industry, but also more and more in biotech and food industry – on
how to behave in almost all aspects of production.

The philosophy behind GMP is the need of imposing the pharmaceutical industry with regulations
which could ensure the quality of the products for the benefit of the patients. GMP like regulations
are also valid for manufacturing of veterinary products and medical devices.

Good Manufacturing Practice is not only related to the production processes, but covers all
activities within a pharmaceutical company which may have any influence on the product quality.
This includes the purchasing of raw materials, construction of the buildings, production facilities
and ware houses, education of staff involved with production, control and distribution, engineering
and design of new facilities and maintenance of existing equipment, procedures for production,
analysis and storage, audit, documentation etc. etc. GMP is an issue governed by the top
management, who has the final responsibility, but all employees may be involved with ensuring
fulfilment of the quality requirements.

Although GMP is a system with the purpose of ensuring product quality it may not be confused
with ordinary standard quality systems, as for instance the ISO standards. GMP is based on a range
of frame requirements imposed on the pharmaceutical and related industries by the authorities, and
it is generally up to the companies to define how they want to understand and live up to the GMP
rules. However, GMP can not be interpreted freely, since all details in processes, procedures etc.
may be argued for with the authorities, which in the end shall approve all decisions and steps taken
if they may have any influence on the quality of the products used for treating the patients. A
company is not allowed to produce a certain drug until a manufacturing license has been issued, and
it can not sell the product before reception of a marketing authority.

Control of the pharmaceutical industry through GMP rules takes place through the Medical
Agencies in the various countries. Well known is the American FDA – the Food and Drug
Administration, and in Denmark the control takes place through the Danish Health and Medicines
Authority (Sundhedsstyrelsen). GMP rules are issued by for instance FDA and the European
Community (Eudralex, valid for EU countries and handled by EMA – European Medicines
Agency).

88
For food safety a special range of demands are valid, in some cases even more precise than the
GMP rules. In Europe an organisation called EHEDG – European Hygienic Engineering & Design
Group – is dealing with specific recommendations for design of components for the food industries.

GMP is generally identified with a lot of administrative issues and a lot of paperwork (GMP is
sometimes interpreted “Great Mountains of Paper”), and it is correct that severe documentation is
involved with performing GMP. That includes any phase of providing finished pharmaceutical
products, from design, construction and commissioning of new plants over phase 1, 2 and 3 patient
testing results to daily batch journals and regular validation of procedures and performances during
production. However, the documentation is not supplied just because the authorities want it, but to
make sure that no error within reasonable certainty can take place.

From a chemical engineers and an experimental point-of-view a number of subjects and activities
are connected with dealing with GMP and food safety:

• Hygienic design of process plants

• Operating and maintaining GMP and food manufacturing plants including all steps from
purchasing of raw materials to shipment of finished goods
• Design and operation of clean utilities
• CIP processes (clean-in-place, industrial cleaning)
• Risk management
• Quality control
• Documentation and test work during qualification and validation of plants and procedures

Some of the aspects mentioned in the list above are discussed in other sections of this book.
Hygienic design is described in section 13. Clean utilities (clean steam, compressed air,
pharmaceutical waters) and CIP liquids are covered briefly in the section 2. Reference 15 is a more
detailed introduction to the many different aspects of GMP.

The GMP concept is sometimes extended with the abbreviation GXP, where X can identify other
related important aspects. GLP – Good laboratory practice – is described somewhere else in this
book (section 16). GDP – Good documentation practice – is an important subject used during
experimental work in many industries. It covers the necessity of being able to document
unambiguously the findings during experiments. In practice this includes use of a laboratory journal

89
with printed page numbers – of course no pages must be removed from the journal. All data etc. are
written using a pen with non-erasable ink; in case of writing errors the wrong data are crossed out
and the correct written next to. Date and initials may be written next to in order to identify the
writer. Also every page is dated and signed. In addition GDP encounters a readable hand writing
and a structured and orderly reporting of data and results.

CIP cleaning.

CIP means “Clean-In-Place” which is meant to be on contrary to “Clean-Out-of-Place” (COP).

When CIP-cleaning a plant nothing is dismantled into smaller components or moved away; the
equipment is washed as it is, typically using spray nozzles inserted at selected places in the plant
and supplied with CIP-liquids from a stationary CIP supply station or from a mobile unit.
Some equipment can be cleaned more practically by separation into pieces or minor components,
which are cleaned individually for instance in a washing cabinet – cleaning-out-of-place. COP is
also used for instance in case a device has to be cleaned both inside and outside.
Cleaning processes not only encounter removal of dirt but also sterilizing. The term SIP –
Sterilizing-In-Place is used when the plant is sterilized on site as it is; sterilizing-out-of-place is the
well known process typically taking place in an autoclave.
CIP (as an over-all term defining a cleaning process) is considered as an important utility in the
pharmaceutical industry. As CIP-liquids are in contact with the equipment in which the final
pharmaceutical products are produced, the hygienic design requirements for CIP equipment is the
same as for the ordinary production equipment. The same is valid for SIP equipment.

CIP/SIP systems can be either stationary or mobile. Stationary plants are integrated parts of the
ordinary production equipment. It comprises a central CIP station, where the CIP liquids are
prepared in vessels to the right composition, concentration and temperature. The CIP station is
connected to the storage for raw chemicals used for making the CIP-liquids. In case the system is
also used for sterilizing with steam, the CIP station may also be connected to the clean steam
generator. In addition to the CIP station the system includes pipes connected to the various kind of
equipment to be cleaned. The piping may be a ring system, where the CIP liquid circulates
continuously.

90
In stead of having a comprehensive stationary CIP system it may in some cases be more practical to
use a mobile unit. The mobile unit is transported to the production equipment to be cleaned, where
it is physically connected to the equipment – often using hoses – and to power, water, compressed
air, process steam and perhaps clean steam. On the mobile unit are cans with raw chemicals, a CIP
vessel, pumps, instruments, computer etc. – all what is necessary to run a specific automatic CIP
process.

CIP liquids can be considered as utilities and are therefore discussed in section 2.

When operating stationary or mobile CIP systems an automatic procedure is almost always the case.
The plant operation is controlled by a computer or PLC (Programmable Logic Computer), and the
software is designed to perform a well defined set of operations, often described in a SOP (Standard
Operation Procedure) or recipe.
A typical automatic CIP procedure is designed according to the following steps:
1. Flushing the equipment with water to remove coarse and loose impurities. What can be
removed by simple means does not need harsher conditions.
2. Washing with a (warm) detergent solution – alkaline or acidic.
3. Flushing with water to remove detergents from step 2 above.
4. Wash with another detergent solution – often in the opposite pH-range to the first detergent.
If the first detergent is alkaline, the second will be acidic.
5. Final flush(es) with water to remove traces of detergent chemicals and dirt residues.
6. Sterilizing. Sometimes the CIP is followed by a SIP. This is used in case the process
equipment subsequently is used for an aseptic or sterile process.
7. Drying. If the plant is to be left for some time without product all residues of water should
be removed (to avoid biofilm growth). Drying can take place using heated air – from a
blower or compressed air.

For all steps the conditions (temperature, duration, flow rate, quantity) may be selected according to
a skilled judgement. Every step may be repeated several times if necessary. The process engineer
must also determine what kind of water quality is to be used.

Cleaning nozzles.
To dispense the CIP-liquid into the process equipment and in order to cover all surfaces in contact
with product efficient spraying devices are necessary. Liquid spray equipment may be divided into

91
spray balls and spray nozzles. Spray balls are simple devices where the liquid ejection takes place
through a simple drilled hole or slot. In spray nozzles the ejecting point is designed in a more
sophisticated way in order to fulfil special demanding
requirements, especially to giving rise to physical
impact of the water beam on the equipment surface.
In this case cleaning is not only taking place by
dissolving dirt when wetted but also to be mechanically
removed. Balls and nozzles may be stationary or rota-
ting. The rotating ones are usually driven by the flow/
pressure of the liquid; only large nozzles may have a
separate motor. Figure 12.1

Spray balls for surface wetting

Figure 12.2
Figure 12.3
Rotating liquid driven spray nozzles
Large tank cleaning 3-dimensional
rotating nozzle (jet head).

92
13. Hygienic design

The construction of chemical plants reflects various philosophies. Especially food and pharma
industries are very demanding as far as plant design is concerned. This is connected with the severe
requirements on hygiene and sanitation/cleaning. Pharmaceutical plants with products for
international export have to follow Good Manufacturing Practise (GMP) as discussed in section 12.

Some of the practical GMP hygienic design topics are:

• Weld the pipes together in order to avoid joints, in which impurities may stick and be
difficult to clean.
• In case joints are necessary, use clamps. Joints with threads are forbidden.
• The process system should be completely drainable.
• Pipes are dimensioned to a minimum liquid velocity of 1.5 m/s.
• Equipment in contact with the process liquid shall be made from a steel quality equal to
AISI 316 or better. For plastics and rubber a list of approved qualities are available, which
include fluor polymers and EPDM rubber.
• Dead legs and areas, where product can adhere for a long period and may be difficult to
clean shall be avoided. The length of T-connections for instance to instruments or sample
valves should be minimized and placed horizontally.
• Approved valves are membrane (diaphragm) valves and sometimes butterfly valves.
• Pumps must be of sanitary design.

What especially concerns the authorities and the users of pharmaceutical process equipment is the
risk of microbial infection. It has to do with the phenomena of biofilm formation: Where water –
even ultrapure water – is left to stand still, bacteria may grow and form biofilm, a slime which can
be very difficult to get rid of and provide basis for serious pollution of the plant and therefore the
products. In addition, to avoid biofilm formation by means of the above mentioned design
measures, pharmaceutical plants are cleaned and sanitized on a regular basis.

Below are a few examples on practical important design details.

93
Horizontal pipes should be sloped towards the drain point with at least 5 mm per meter (some
companies require even more) in order to ensure that no liquid can be left standing still in the pipe,
as illustrated in figure 13.1.

Min 0.5 cm

1 meter

Drain

Figure 13.1

If pipe reductions are necessary they should be made according to figure 13.2 (bottom). Again the
important point is that the pipe should be completely drainable.

Wrong

Correct

Figure 13.2

Dead legs are parts of a plant where dirt or liquid can be left untouched for some time, or parts
which are difficult to clean during the CIP (cleaning-in-place) process. As illustrated in figure 13.3
a dead-leg may be a pipe section leading to a valve which is not opened regularly. If dead legs are
unavoidable their size should be minimized. Generally the following maximum lengths are
accepted: Length (L) from main pipe centre line to the shaft of the valve (or instrument, or
equipment) must not be longer than 3 times the dead leg pipe diameter (d) as in case B in figure
13.3. In some cases this may not be possible for practical reasons (dimensions versus accessability
for welding etc.); in these situations the conditions in case A are usually accepted.

94
 A B

d d

L L

L/d < 3 L/d < 3

Figure 13.3

The connection between the process system and the drains should be made in such a way, that
liquid waste from the drain under no circumstances can be sucked back into the process. Usually
this demand is solved by applying a certain minimum distance – for instance 50 mm - between the
end of the process drain pipe and the drain itself, as can be seen from figure 13.4.

H > 50 mm

Drain

Figure 13.4

The most hygienic way of connecting pipes and other components is by welding. There is very
much focus on the quality of the welds, and strict requirements apply in terms of welding
procedure, applied material, welders documented performance, non-destructive testing of the welds
and detailed documentation of the welding work. For practical reasons pipe sections and process
components need to be disassembled, and some kind of a hygienic coupling must be applied. Due to
the poor sanitary properties, couplings and connections involving threads are generally strictly
forbidden in the food and pharmaceutical industries for equipment with product contact. Generally
accepted sanitary couplings are first of all the so-called clamps (T-clamps), a drawing of which is
shown in figure 13.5.

95
 Clamp ring

Gasket

Pipe
Ferrule

Figure 13.5

The clamp consists of 2 ferrules connected with a gasket and fixed by a clamp ring. Figure 13.6
shows the one ferrule and figure 13.7 the entire assembled clamp coupling.

Figure 13.6 Figure 13.7

The application of valves in GMP plants is restricted to very few valve types. Membrane valves
(diaphragm) are generally considered as the most sanitary kind of valve (figure 13.8 and figure 1.5).

Figure 13.8 Figure 13.9

96
When membrane valves are located in horizontal pipes it is necessary to turn the valve to a certain
angle in order to ensure drainability through the valve (figure 13.9). Information about the
magnitude of this angle should be provided by the valve supplier.
While membrane valves normally are the only accepted type of valve in the pharmaceutical product
plants, butterfly valves (figure 1.4) and the so-called mixed proof valves are accepted also in various
food industries. For butterfly valves the seal around the shaft through the pipe wall constitutes a
potential pollution problem.

Centrifugal pumps are by far the most used kind of pump in the process industries due to their
excellent characteristics for liquid transportation purposes, but they are not very hygienic. They
have very often a complex construction with a lot of cavities, corners and crevices where stagnant
water may remain and dirt may settle. However, a process plant cannot work without pumps, so
compromises are necessary. Due to an increasing industrial demand so-called hygienic centrifugal
pumps have however been developed in the recent years, and these pumps are first of all more
drainable than standard pumps. The shaft between the motor and the pump head also constitutes a
potential pollution problem. Pumps with magnetic power transmission do exist, but are limited to
smaller pump sizes and flow rates.

The most hygienic pump is the peristaltic pump, where the only part in liquid contact is the hose.
The quality of the rubber, from which the hose is made, must of course fulfil requirements
according to the purpose of the application. Generally fluor-based polymers are widely accepted
from a chemical point of view, because these polymers are typically inert to many substances.
However, the designer must also be aware of the mechanical strength and the abrasion properties of
the rubber. The constant compression/decompression of the hose due to the rotating wheels of the
pump may create wear, which can result in undesirable release of small rubber particles into the
process liquid.

Dosing of chemicals – for instance in CIP systems – is usually performed by membrane pumps,
which also have corners, crevices, internal balls and other less hygienic design features. However,
as long as the pump construction materials are inert to the chemicals that are used, the application of
membrane pumps will normally not constitute a problem since microorganisms cannot survive in
the harsh chemical environment, which is usually present .

97
As far as process instruments are concerned they must not introduce any risk of product pollution
and must be easy to calibrate and maintain. For that reason pH instruments are avoided, since the
electrolyte behind the glass membrane cannot be said to be isolated from the process liquid.
Manometers with Bourdon-tube, orifices, pitot-tubes and most mechanical flow meters are also
black-listed. Ideal for flow measuring are the so-called magnetic flow sensors, made from a tubular
pipe with 2 electrodes inserted into the wall.

Temperature sensors are usually located in pockets, which are welded into the process pipe, often in
bends, as shown in figure 13.10. The flow direction is important: From left to right it is more easy
to keep the upper corner clean compared to the situation, where the flow is coming from below.

Figure 13.10 Figure 13.11

Pressure sensors must be supplied with a membrane towards the product side (figure 13.11), and the
dead leg between the membrane and the main pipe should be minimized. The membrane is easy to
clean and is for practical purposes located in a clamp connection.

As with the manometer above conductivity and other sensors are often inserted into the process via
a pipe-T and a clamp connection.

Construction materials for application in hygienic plant design are described in section 3.

98
14.Process understanding and process problems
This topic defines the somewhat indefinable concept of understanding a process, not only in terms
of the chemistry or mechanical engineering, but especially the combinations of chemical and
physical behaviour in various kinds of process equipment and the function and necessity of every
component in conjunction with the others.

Due to the indefinable character this topic is almost never taught during systematic educational
programs, but is only subject to personal experience during many years practical work with process
plants.

The purpose of this section is – at least partly - to try to bypass these many years of necessary hard
work and help the un-experienced process engineer to improve the understanding of the many
details working together to ensure a qualified design and successful operation of a plant.

The method selected to achieve the goal is for instance to raise questions and in this way open the
eyes for the sub-surface details of considerable importance. The questions may be the base for
discussions in various fora.

Pumps.

Pump operation is a subject of great importance to any process engineer. For positive displacement
pumps it is a general rule never/ever to start the pump against a closed valve. Since the liquid
cannot excape, high pressures are built up very fast and may either destroy the pump or brake the
equipment downstream between the pump and the valve, sometimes with fatal consequences.
Centrifugal pumps are not positive pumps and may be able to run against a closed valve – at least
for some time. Without any flow through the pump the temperature of the liquid in the pump may
rise due to dissipation of the pumping energy, and eventually the liquid will boil or make other
temperature related damages.

Problem: The centrifugal pump starts, but there is no flow or pressure.

Answer: Make sure any valves on either side of the pump are not closed. Also convince yourself
that the pump is able to lift the liquid to the prescribed height, i.e. that the pump pressure head is
sufficient; it may be necessary to consult the characteristic pump curve.

99
Not all pumps are able to self priming, so make sure the pump house is full of liquid. Generally the
conditions on the suction side are much more important than on the pressure side (larger pipe
dimensions, liquid level in the feed vessel is preferred higher than the pump level); in addition some
pumps prefer to be started against a certain counter pressure, especially if it is not completely filled
with liquid. In case of air in the pump: Start and stop the pump a number of times; or open the air
relief screw carefully while the pump is running and be ready to close it again when liquid is
blowing out.
If the pump is used for pumping liquids, where suspended particles may be an option, mal-function
could be a simple physical blocking.

Problem: The vacuum pump is running, but no or very little vacuum is achieved in the process.

Answer: Is there a physical blockage between the process and the pump (for instance a closed
valve). If there is a leakage in the process or pipe system on the suction side it may be possible to
isolate a part of the system and hence identify the leak. If the pump is of the water ring type a
certain flow of water is necessary. Is the process running under conditions where vapors are emitted
to an extent higher than the capacity of the vacuum pump? What kind of vapors (condensable or
not) are to be removed to reduce the pressure in the process? If the process is a boiling liquid the
vapors may be water, which can be condensed in a heat exchanger upstream of the vacuum pump
and thereby improve the working function of the pump. If the vacuum pump has an air valve on the
suction side (gas ballast valve) with the purpose of adjusting the pressure in the process or diluting
the vapors, this air valve can be adjusted to give a better control of the vacuum.

Problem: When designing a pump system what is important to consider?

Answer: Apart from pump selection the most important is to optimize the pump suction conditions.
The suction side pressure drop (upstream pressure drop) must be minimized, since a pump can
accept max. 1 bar suction pressure drop (from atmospheric pressure to full vacuum), while the
downstream pressure drop – equivalent to the pumping height – normally is much higher. Valves,
filters and other components with potential pressure drops must therefore be located on the pump
pressure side. In addition the upstream pipe dimension must be larger than at the downstream side,
and the pump physically located close to a feeding vessel and preferable at a lower altitude
compared to the vessel.

100
Valves.

Problem: No liquid is coming out by opening a sample valve.

Answer: Either there is no liquid on the inner side of the valve, there is a blockage in the flow path
or the pressure on the inner side is lower than on the outside. Also make sure that you really are
opening the valve: Turning clockwise you close the valve – unless it is a reduction valve, which
functions the opposite way. For on-off valves (for instance ball valves) the handle must be in
parallel to the pipe when the valve is open; make sure the handle is fastened to the valve body in the
right way.

Problem: Why is it theoretically a bad idea to use a reduction valve to control the gas flow?

Answer: A reduction valve is designed to maintain the pressure constant on the downstream side
independent on upstream pressure variations. It is not designed to maintain the flow. However, in
many situations where upstream and downstream process changes are actually minimized, the
practical application of a reduction valve for flow control is doing well as long as it is not a part of
an automatic control loop.

Measuring equipment.

Problem: The manual pressure indicator (manometer) is not responding.

Answer: If you believe there is a pressure the manometer is either broken or the bourdon tube inlet
is blocked by some solid material. Remove the pressure of the system, open carefully to the
atmosphere, dismantle the manometer and check (by blowing, using compressed air etc) if the
instrument respond to pressure changes. Visually inspect the process side entrance to the
manometer.

Problem: The signal from the pressure transmitter does not respond to process changes.

Answer: The instrument or the pressure transmitter does not work (for some reason damaged) or the
connection from the process to the transmitter is out of order. Stop the process, relieve any pressure,
dismantle the physical connections (pipe etc.) on the transmitter from the process. Are the
connections free or blocked on the process side (plugged by dirt, deposits etc.)? Does the instrument

101
react if a slight air pressure is added to one of the sides of the transmitter? Measure the signal from
the transmitter to the instrument (often 4-20 mAmp or 0-1 Volt, see info on the instrument).

Problem: The float in a variable area flowmeter (rotameter) is not moving despite actual change in
flow.

Answer: The float is probably hanging due to physical reasons: A piece of dirt in the liquid has
caused the float to become wedged. This is typical for solid-liquid systems and for instance for
steam or compressed air systems with insufficient strainer function or with pipe corrosion due to
longer periods of no operation.

Other subjects.

Problem: What is the necessary pressure for a gas to pass a liquid air lock?

Answer: Air locks are use to prevent gas from escaping a system at the wrong place without
blocking for liquid to run out. The height of the liquid column defines the necessary pressure for a
gas to pass the lock. If the liquid is water and the height of the liquid column is for instance 50 cm,
the water constitutes a barrier of 500 mmWG = 5000 Pa = 50 mbar. The gas pressure must therefore
exceed the downstream pressure by 5000 Pa in order for the gas to pass the lock.

A similar situation takes places in a tray column for absorption/distillation. The liquid height on
each tray is necessary to ensure good mass transfer, the higher the better equilibrium. However, the
consequence is a higher pressure drop – proportional to the liquid height – so a balanced optimum
has to be found.

102
15.Heat and mass balances

Mass balances.

The primary purpose of mass balances is for the process engineer to keep track on all components
and all flows – in principle at any time. In practice mass balances are made according to specific
needs and depend upon the character of the process. The process may consist of chemical reactions
as well as steps of unit operations. For a continuous process in steady state the mass balance is
usually made as a momentary picture of all flows and components since nothing changes over time.
For processes in non steady state it is often a challenge to find a period of pseudo steady state for
which a momentary balance can be made; if the task is to follow change in composition over time it
is of course a different (but still difficult) matter. Balances for batch processes – where the dynamic
progress of the process is of no concern – are usually made as start versus end conditions, i.e. what
was the initial masses of the individual components and what was the composition when everything
was over.

Mass balances may include flows/components in the direct process as well as in indirect ones,
which for instance could be interfering utilities such as cooling water, steam, compressed air etc.

Mass balances are the main basis for making heat balances.

A mass balance for a continuous process in steady state can be made considering the process as a
black box and use the following equation:

Input + produced = output + accumulated

The input is understood as flows of matter which are entering the process (the black box). It can be
split into single components and/or a total mass. If no chemical reaction takes place the incoming
components may be individual molecular matter, such as water, nitrogen, filter aid, citric acid etc. If
reactions take place the components may be based on atoms such as sodium, carbon, hydrogen and
so on. When possible the use of mass flow (kg/h etc.) is preferred, and when concentrations are
encountered use weight per weight (kg/kg, mass %) instead of volume based concentrations,
because the sometimes laborious work of determining densities are avoided.

The produced quantity is the result of chemical reactions. Outputs are the exit streams from the
process and the accumulated mass are for instance material sticking to the surfaces inside the plant.

103
Heat balances.

What is actually considered in the heat balances is the enthalpy. As for mass balances it is often a
help to consider the process as a black box, identifying all flows in and out. The physical flows are
taken from the mass balances; in addition you must remember other heat flows such as heat loss to
surroundings, heat supplied through heaters or heat exchangers and so on. Also power for pumping
may in principle be part of a heat balance.

It is often forgotten to define a basis for the enthalpy. We can set the zero for the enthalpy as we
wish, but by doing it in an intelligent way can save a lot of work. You should consider the kind of
process taken place when defining the zero level, but also consider the enthalpy basis applied in
your information sources/references. For many processes zero enthalpy is defined at 0oC and – if
water is a part of the process – liquid water. For cryo processes however a completely different
basis may be practical. Let us take a few examples (based on 1 kg of material):

For liquid water at 0oC the specific enthalpy Hw = 0 kJ/kg (per definition). For gaseous water (water
vapor, steam) at 0oC the enthalpy Hg = Hw + the heat of evaporation ΔHvap (at 0oC). ΔHvap = 2494
kJ/kg, so Hg = 2494 kJ/kg at 0oC.

The enthalpy of water vapor at 100oC can be calculated in two ways, both giving the same result:

1) Use Hw at 0oC, heat the liquid water to 100oC using the average cp for water and then evaporate
the liquid at 100oC. The average cp (water) = 4.2kJ/kg K, and ΔHvap at 100oC = 2259 kJ/kg. The
specific enthalpy Hg (at 100oC) = 0 + 4.2 (100-0) + 2259 = 2679 kJ/kg.

2) Evaporate the liquid water at 0oC and heat the water vapor to 100oC using the average cp for
vapor. The average cp of water vapor = 1.85 kJ/kg K, so based on this way of calculation the
specific enthalpy Hg = 0 + 2494 + 1.85 (100-0) = 2679 kJ/kg.

As can be seen the latent heats (in this case heat of evaporation) are functions of temperature. The
same is the case for cp values and for that reason average values – as above – are used for the
relevant temperature range.

Calculating enthalpies of air always remember that air has a certain quantity of moisture, usually
described as kg moisture/kg dry air (denoted X). Since dry air at 0oC as per definition above has an
enthalpy of zero, the enthalpy of moist air at 0oC equals 0 + 2494 X kJ/kg.

104
With the basis of enthalpy now defined the heat balance for a process using the black box concept
can be made in the following way:

• Identify a period in which the process seems to be in steady state

• Define all stream/component flows in and out of the process, for each one identify the mass
flow, temperature and physical condition (solid, liquid, gas). Based on this any average cp
and any latent heats can be found, the specific enthalpy calculated and finally the total
enthalpy of the stream/component.
• Identify heat inputs/outputs not related to enthalpy of flows.
• Forget about heat effects (evaporation, condensation, heat of reaction etc.) taking place
inside the process (black box), since these heat effects will be reflected in the temperatures
of the outgoing streams.
• Use the relation “In = Out” to make the balance. If you did not calculate or measure the heat
loss this will be reflected in the difference between “In” and “Out”.

For streams containing more than one component (for instance solutions, moist air) it is often
convenient to split the stream into separate components, for instance to divide a solution into solute
and solvent and treat each component separately. In principle this may introduce an error
(especially for condensed phases), because dissolution is often followed be heat effects (heat of
solution, heat of dilution, heat of mixing, heat of crystallization etc). In many chemical process
systems these heat effects are small compared to temperature related specific enthalpies, so the error
is often drowning in ordinary uncertainty of the measuring data. However in systems with high
concentrations – for instance evaporation and crystallization processes – these heat effects may be
high enough to be taking into account.

cp values for solids are often much lower than for liquids and gases.

For many normal processes the enthalpy is practically independent of the pressure.

105
16.Mollier diagram - H,x diagram

A Mollier diagram shows information about humid air (mixtures of atmospheric air and water vapor) and is a
very useful tool when designing and calculating on drying processes and air conditioning plants.

Normal processes for drying and conditioning is run at atmospheric pressure, so most Mollier diagrams are
made for processes at atmospheric pressure (1 atm = 1.013 bar).

All information in the Mollier diagram is related to mass of dry air (mDA), which makes it independent of
temperature and moist content.

Conversion from air velocity to mass flow of dry air

If we measure air velocity in an air duct, we can convert this to volumetric flow if we knows the dimension
of the duct (area).

To convert from volumetric flow to mass flow of dry air we need to have information about the air at the
point of measurement. We need information about temperature and moist content (humidity). Moist content
is typically read as relative humidity ϕ or percentage relative humidity.

Now we can mark a point in the Molliers diagram using measured temperature and relative humidity. – See
figure X which shows an example with t=83°C and ϕ=0.15.

From this point, we can find information in the Molliers diagram (see figure 1) about:

• Energy content in the moist air (Hair) using the enthalpy lines. Unit is either: kJ pr. kg dry air or in
older versions of Molliers diagrams: Kcal pr. kg dry air. Ex.: 50.0 Kcal/kg dry air
• Absolute moist content (x) going vertically down in the diagram. Unit is typically gwater pr. kg dry
air. Ex.: 48,0 grams of water/kg dry air.
• Partial pressure of water vapor going first vertical and then horizontal. Unit is typically Pa, mmHg or
mmWater. Ex.: 55 mmHg

Figure 1 – How to read values from Mollier diagram

106
To make an equation for calculating mass flow of dry air based on volumetric flow, pressure and temperature
we need to consider the mixture as an ideal gas, where we can use this equation:

𝑝𝑝 ∙ 𝑉𝑉 = 𝑛𝑛 ∙ 𝑅𝑅 ∙ 𝑇𝑇 1

Where p is the total pressure in Pa, V is total volume in m3, n is total number of moles, R is the gas constant
(=8.31447 m3Pa/K/mol) and T is the absolute temperature in Kelvin [K].

We consider atmospheric air as air with the composition: 20.9% oxygen, 78.1% nitrogen and 0.9% Argon,
which gives an average molar mass of 28.92 g/mol.

Moist, which is water has a molar mass of 18.02 g/mol.

Now we will express n (total moles) by x and mDA:

𝑥𝑥 ∙ 𝑚𝑚𝐷𝐷𝐷𝐷 𝑚𝑚𝐷𝐷𝐷𝐷 2
𝑛𝑛 = +
18.02 28.92

Combining equation (1) and (2) we can find mDA:

𝑝𝑝 ∙ 𝑉𝑉 3
𝑚𝑚𝐷𝐷𝐷𝐷 =
0.4614 ∙ (623.1 + 𝑥𝑥) ∙ (273.2 + 𝑡𝑡)
Where mDA is mass of dry air in kg, p is the total pressure in Pa, V is total volume in m3, x is absolute moist
content in grams of water pr. kg dry air and t is temperature in celcius (°C).

Equation 3 can now easily be transformed into relationship between mass flow of dry air (𝑚𝑚̇𝐷𝐷𝐷𝐷 ) in kg dry air
pr. time and volumetric flow (𝑉𝑉̇ ) in m3/time.

An example based on the data from above.

Volumetric airflow through a spray dryer is measured to 360 m3/h. Measurements on the outgoing airstream
reads temperature 83°C, ϕ=0.15, which gives x=48.0 gwater/kgDA.

Using modified eq (3):

𝑝𝑝 ∙ 𝑉𝑉̇ 3a
𝑚𝑚̇𝐷𝐷𝐷𝐷 =
0.4614 ∙ (623.1 + 𝑥𝑥) ∙ (273.2 + 𝑡𝑡)

1.013 ∙ 105 ∙ 360

𝑚𝑚̇𝐷𝐷𝐷𝐷 [𝑘𝑘𝑘𝑘𝐷𝐷𝐷𝐷 ⁄ℎ] = = 331 𝑘𝑘𝑘𝑘𝐷𝐷𝐷𝐷 ⁄ℎ
0.4614 ∙ (623.1 + 48.0) ∙ (273.2 + 83)

Typical operations in Mollier diagram for drying processes

Heating and cooling processes:

If humid air is heated or cooled in a heat exchanger, enthalpy is changed without changing the water content
pr. Kg dry air. For heating processes this is shown by going vertically upwards in the Mollier diagram from
inlet point based on temperature and humidity to the temperature after the heat exchanger.

107
The difference in enthalpy for the 2 points is the energy transferred to the air pr. Kg dry air. If mass flow of
dry air (𝑚𝑚̇𝐷𝐷𝐷𝐷 ) is known, necessary energy supply (kW) to the heat exchanger can be estimated.

The same operations are also valid for cooling processes, both for situations where the air is cooled in a heat
exchanger or “cooled” by simple heat loss in the duct.

Drying processes:

It is easy to follow drying processes in a Mollier diagram with knowledge of airflow, temperature and
humidity for the inlet stream and temperature and humidity for the outlet stream.

Mark the inlet point and the outlet point. Now enthalpy values pr. kg dry air as well as moist content pr. kg
dry air can be found for both points.

If there is no change in enthalpy (Hin = Hout ) we have an adiabatic drying process, which is seldom.
Normally the enthalpy for the outlet will be lower than the inlet due to heat loss from the system.

By subtracting water content (Xout – Xin) and multiplying with 𝑚𝑚̇𝐷𝐷𝐷𝐷 we can find water removed from the
goods pr. Time unit.

If airflows, inlet conditions, outlet temperature and weight loss (evaporated water) from the goods over a
certain time are known, we can calculate the opposite way to show the drying process in the Mollier
diagram, from evaporated water to increase in the drying air humidity (Δx).

For a batch drying process this will be shown as a number of lines related to accumulated drying time from
start.

108
109
110
17.Working safety

Good laboratory practise (GLP) is a set of generally accepted rules also dealing with safety aspects.
Work with pilot plants and units in semi technical scale however rise further attention, because we
handle larger volumes of material, fast running motors, application of utility steam, assembly of
equipment which can be harmful if done incorrectly etc.
The following points are valid for work at the DTU Dep. of Chemical & Bioquemical laboratories
and pilot halls:

• Never work alone

• Make yourself acquainted with the location of fire extinguishers, emergency showers, plant
emergency stops, shut off valves of steam and other utilities
• Anybody to work in a laboratory or the Pilot Plant must receive a safety introduction by an authorized person
before work can start.
• Before starting any practical work, the safety data sheets for the chemicals to be used must be studied
carefully. Before the work can start in the Pilot Plant, the students must be approved by the teacher
regarding the hazards and the emergency response for the chemicals in use.
• When working in the laboratory or Pilot Plant; lab coat, safety glasses, long trousers and closed shoes are
mandatory. (Preferable bring your own lab coat and safety glasses)
• When handling chemicals or hazardous substances gloves are mandatory.
• Make sure to know the location of emergency equipment like; fire extinguishers, eyewash stations, emergency
shower, defibrillator, and first aid equipment.
• No eating and drinking in the laboratories or Pilot Plant.
• Never leave a running plant alone, even for a short while.
• Small amounts of chemicals or diluted chemicals may be disposed of to sink or drain. Larger amounts of
chemicals for disposal must be marked with name, date, content and waste code. Ask the lab technician for
further action.
• Keep the work area and workstation tidy and clean up when the experiment is finished.
• Use the study room, cloakroom or similar place for civilian clothes and properties.
• Clearly mark your samples to be stored with name, date, content and required safety information.
• Use a Laboratory Notebook for writing all raw data, comments, drawings etc.
• Use of headphones in the labs or pilot halls are not allowed.

111
Literature.
1. Heilmann, T.: Praktisk regulering og instrumentering. Eget forlag, seneste udgave.
2. Seborg, D.E.: Process Dynamics and Control. Wiley 2003.
3. Hansen, L.A.: Måling og regulering i den kemiske industri. Akademisk Forlag, 1972.
4. Møller Andersen, E.: Industrielle Rør- og beholderanlæg. 1970
5. Oddershede Larsen, M.: Statiske grundbegreber. Udgivet på ”Den Private
Ingeniørfond ved DTU”.
6. Esbensen, K.H. (red): Introduktion til repræsentativ prøvetagning for stationære og
dynamiske systemer. Særtryk fra Dansk Kemi & Plus Process. ATV Jord og
Grundvand 2006.
7. Petersen, L. et al.: Representative sampling for reliable data analysis: Theory of
sampling, in Chemometrics and Intelligent Laboratory Systems 77 (2005) 261-277.
Elsevier. www.sciencedirect.com
8. Rhodes, M., Introduction to Particle Technology. Wiley 1998.
9. Clement, K.H. et al.: Kemiske Enhedsoperationer. Polyteknisk Forlag 2004.
10. McCabe, W.L. et al.: Unit Operations of Chemical Engineering. McGraw-Hill, any
edition.
11. Perry, R.H. & Chilton, C.H.: Chemical Engineers Handbook. McGraw-Hill, any
edition.
12. Coulson & Richardsons Chemical Engineering, vol 6. Pergamon Press.
13. Søltoft, P.: Faste stoffer i kemisk industri. Polyteknisk Forlag 1970.
14. Seville, J. et al.: Processing of Particulate Solids. Powder Technology Series.
Blackie Academic & Professional 1997.
15. Kiørboe, L.: GMP and quality in pharmaceutical, biotech and food industry; lecture
notes to DTU course 28855. Latest version.
16. Woods, D.R.: Rules of Thumb in Engineering Practice.Wiley 2007.
17. Thomas, C.E.: Introduction to Process Technology. 3. ed. Delmar, Cengage Learning
2010.
18. Thomas. C.E.: Process Technology Equipment & Systems. 3.ed. Delmar, Cengage
Learning 2011.
19. Thomas, C.E. : Process Technology Troubleshooting. Delmar, Cengage Learning
2009.

112
20. Smith, R.: Chemical Process Design and Integration. Wiley 2010
21. Himmelblau, D.M. & Riggs, J.B.: Basic Principles and Calculations in Chemical
Engineering. Pearson Education 2013.
22. Plumbing Engineering Design Handbook vol. 1-4. American Society of Plumbing
Engineers. Available from DTU Library e-book database Knovel.
23. Harris, C.M. (ed.): Practical Plumbing Engineering, 1998. American Society of
Plumbing Engineers. Available from DTU Library e-book database Knovel.
24. EHEDG Guidelines (European Hygienic Engineering & Design Group, 2007.
25. Towler, G. & Sinnott, R. : Chemical Engineering Design. Principles, Practice and
Economics of Plant and Process Design. Elsevier/BH, 2.ed. 2013
26. Callister, W.D. & Rethwisch, D.G.: Materials Science and Engineering. Wiley, 8.
Ed. 2011.
27. Branan, C.R.: Rules of Thumb for Chemical Engineers. Elsevier 2013.
28. Krüger, E.: Usikkerhedsberegning ved fysiske målinger. Jul. Gjellerups Forlag.
København 1965.
29. Ellison, S.L.R. & Williams, A. (ed): Quantifying Uncertainty in Analytic
Measurement. Eurachem/CITAC Guide, 3. Edition, 2012. Download from
www.eurachem.org.

113
Appendix

Steam tables - metric units

Saturated steam

Specific enthalpy
Specific
Water Evaporation Steam volume
steam
Pressure Temp (hf) (hfg) (hg)
bar kPa °C kJ/kg kJ/kg kJ/kg m3/kg
absolute
0.30 30.0 69.10 289.23 2336.1 2625.3 5.229
0.50 50.0 81.33 340.49 2305.4 2645.9 3.240
0.75 75.0 91.78 384.39 2278.6 2663 2.217
0.95 95.0 98.20 411.43 2261.8 2673.2 1.777
1.00 100.0 99.63 417.51 2257.9 2675.4 1.694
1.013 101.3 100.00 419.06 2257.0 2676.0 1.673
gauge
0 0 100.00 419.06 2257.0 2676.0 1.673
0.10 10.0 102.66 430.2 2250.2 2680.2 1.533
0.20 20.0 105.10 440.8 2243.4 2684.2 1.414
0.30 30.0 107.39 450.4 2237.2 2687.6 1.312
0.40 40.0 109.55 459.7 2231.3 2691.0 1.225
0.50 50.0 111.61 468.3 2225.6 2693.9 1.149
0.60 60.0 113.56 476.4 2220.4 2696.8 1.088
0.70 70.0 115.40 484.1 2215.4 2699.5 1.024
0.80 80.0 117.14 491.6 2210.5 2702.1 0.971
0.90 90.0 118.80 498.9 2205.6 2704.5 0.923
1.00 100.0 120.42 505.6 2201.1 2706.7 0.881
1.10 110.0 121.96 512.2 2197.0 2709.2 0.841
1.20 120.0 123.46 518.7 2192.8 2711.5 0.806
1.30 130.0 124.90 524.6 2188.7 2713.3 0.773
1.40 140.0 126.28 530.5 2184.8 2715.3 0.743
1.50 150.0 127.62 536.1 2181.0 2717.1 0.714
1.60 160.0 128.89 541.6 2177.3 2718.9 0.689

114
 1.70 170.0 130.13 547.1 2173.7 2720.8 0.665
1.80 180.0 131.37 552.3 2170.1 2722.4 0.643
1.90 190.0 132.54 557.3 2166.7 2724.0 0.622
2.00 200.0 133.69 562.2 2163.3 2725.5 0.603
2.20 220.0 135.88 571.7 2156.9 2728.6 0.568
2.40 240.0 138.01 580.7 2150.7 2731.4 0.536
2.60 260.0 140.00 589.2 2144.7 2733.9 0.509
2.80 280.0 141.92 597.4 2139.0 2736.4 0.483
3.00 300.0 143.75 605.3 2133.4 2738.7 0.461
3.20 320.0 145.46 612.9 2128.1 2741.0 0.440
3.40 340.0 147.20 620.0 2122.9 2742.9 0.422
3.60 360.0 148.84 627.1 2117.8 2744.9 0.405
3.80 380.0 150.44 634.0 2112.9 2746.9 0.389
4.00 400.0 151.96 640.7 2108.1 2748.8 0.374
4.50 450.0 155.55 656.3 2096.7 2753.0 0.342
5.00 500.0 158.92 670.9 2086.0 2756.9 0.315
5.50 550.0 162.08 684.6 2075.7 2760.3 0.292
6.00 600.0 165.04 697.5 2066.0 2763.5 0.272
6.50 650.0 167.83 709.7 2056.8 2766.5 0.255
7.00 700.0 170.50 721.4 2047.7 2769.1 0.240
7.50 750.0 173.02 732.5 2039.2 2771.7 0.227
8.00 800.0 175.43 743.1 2030.9 2774.0 0.215
8.50 850.0 177.75 753.3 2022.9 2776.2 0.204
9.00 900.0 179.97 763.0 2015.1 2778.1 0.194
9.50 950.0 182.10 772.5 2007.5 2780.0 0.185
10.00 1000.0 184.13 781.6 2000.1 2781.7 0.177

Ref: www.simetric.co.uk

115
Ref: http:/hyperphysics.phy-astr.gsu.edu

116