Manual PAQUES IC_1era parte (1)

BIOPAQ®IC
MINIMUM PACKAGE
IC-4.0, IC-5.0, IC-5.7, IC-6.5,

IC-7.3, IC-8.0, IC-9.5 and IC-11
Operating & maintenance manual

Disclaimer
Copyright by Paques bv, The Netherlands. All rights reserved.
No part of this document may be reproduced, stored in a retrieval system or transmitted, in any form
or by any means, electronic, mechanical, photocopying, recording or otherwise, for any purpose,
without the prior written permission of Paques bv.
Page II
Project- and document information
Project number: Number appears automaticaly if document is made project specific
Project name: Name appears automaticaly if document is made project specific
Technology: BIOPAQ®IC
Customer:
Report ID: SMAN000028_ENF
Title: Operating & maintenance manual IC Minimum Package
Subtitle:
Authors: WOB
Approved by: WOB
Last issued by: WOB
Issue date: 16-05-2013
Issued by: Paques bv

P.O. Box 52
8560 AB BALK
The Netherlands
t: +31 (0) 514 60 85 00
f: +31 (0) 514 60 33 42
e: info@paques.nl
i: www.paques.nl
Contact person: Paques services

t: +31 (0) 514 60 86 73
f: +31 (0) 514 60 33 42
e: services@paques.nl
Page III
Table of contents
1 Introduction 1
1.1 Support 1
2 Safety instructions 2
2.1 Safety at work 2
2.2 Dosing 2
2.3 Sludge and process liquids 3
2.4 Hazardous gases and vapours 3
2.4.1 Biogas 3
2.4.2 Hydrogen 4
2.4.3 Ventilation and chemicals vapours 4
2.4.4 Hazardous area classification 4
2.5 Working at a height 6
2.6 Working in confined spaces 6
2.7 Malfunctions 7
2.8 Disasters 7
2.8.1 Shutting down the installation 7
3 Process description 8
®
3.1 BIOPAQ IC reactor 8
®
3.1.1 The process in the BIOPAQ IC reactor 9
3.2 Biogas treatment 11
3.2.1 Biogas flow metering 11
3.2.2 Condensate separation 11
3.2.3 Overpressure protection 12
3.2.4 Buffering 13
3.2.5 Gas flare 13
3.3 Ventilation 13
3.4 Influent 14
3.4.1 Nitrite & nitrate 14
3.4.2 Sulphite & sulphate 14
3.4.3 Fats, oils & greases (FOG) 14
3.5 Control parameters 15
3.5.1 Biomass (granular sludge) 15
3.5.2 Chemical Oxygen Demand (COD) 16
Page IV
3.5.3 COD load and volatile fatty acid concentration 16
3.5.4 Pre-acidification degree 17
3.5.5 Specific biogas production 17
3.5.6 pH 17
3.5.7 Alkalinity (pH buffering) 18
3.5.8 Temperature 18
3.5.9 Nutrients 18
3.5.10 Calcium (precipitation) 19
3.5.11 Hydrogen sulphide 20
3.5.12 Summary of control parameters 20
4 Start up procedure 21
4.1 Technical inspection 21
4.1.1 Leakage test 21
4.1.2 Hydraulic test (water run) 21
4.1.3 Checking of functional specification 21
4.2 Technological start up 22
4.2.1 Start up conditions 22
4.2.2 Inerting biogas system 22
4.2.3 Sludge inoculation 23
4.3 Start up 24
4.4 Normal operation 25
4.5 Restart 25
4.5.1 With external recirculation or shorter than 5 days 25
4.5.2 Without external recirculation or longer than 5 days 25
5 Operating instructions 27
5.1 General process control 27
5.2 Routine work 27
5.2.1 Daily 27
5.2.2 Weekly 28
5.2.3 Monthly 28
5.3 Cleaning instructions 28
5.4 Temporary shut down 28
5.5 Major maintenance 29
5.6 Emptying the installation 29
5.7 Dismantling and disposal of the installation 29
Page V
5.8 Protection against frost 29
5.9 Spare parts 29
6 Process malfunction and Troubleshooting 30

6.1 Process malfunction 30
6.1.1 Acidification of the reactor 30
6.1.2 Blockage of downer 31
6.1.3 Inhibitors 32
6.1.4 Wash out of granular sludge 33
6.2 Troubleshooting 33
6.2.1 Process Troubleshooting 33
6.2.2 Mechanical troubleshooting 33
7 List of (technical) terms 34
Appendices 37
Page VI
1 Introduction
The BIOPAQ® Internal Circulation (IC) reactor is designed to convert dissolved and degradable organic
impurities from wastewater into biogas.
This operating manual describes the safety aspects, functioning and operation of the
BIOPAQ® IC reactor.
In section 2 the safety aspects regarding the BIOPAQ® IC reactor are described. Then, in section 3 the
process description of the installation is given. The start up procedure of the BIOPAQ® IC process is
described in section 4. Section 5 gives a summary with regard to recommended maintenance and
monitoring procedures. For process malfunction and troubleshooting please refer to section 6.
Specifications, operating instructions and troubleshooting manuals are given in appendices A to C.
Note: All figures given are illustrative examples. These can differ with respect to actual delivery.
1.1 Support
For components not made by Paques, please refer to the relevant supplier’s manual.
For operating or technical support please contact:
Paques Services
services@paques.nl
Tel: +31 514 608 759 (direct)
Fax +31 514 603 342
Reference: -SMAN000028_ENF 16-05-2013 Page 1 of 37

2 Safety instructions
For safe operation Paques recommends that the following regulations be taken into account
as a minimum.
2.1 Safety at work

 Everyone, working or otherwise present on the site of the BIOPAQ® IC reactor, must work in
accordance with the local applicable safety provisions. The following general regulations must
be taken into account as a minimum:
 Smoking and open fire are prohibited.
 Warning signs and other instructions must be taken into account.
 Eliminate any hazardous situation and report it.
 Maintain order and tidiness in the workplace.
 Keep all paths, platforms etc. free of obstacles.
 Use personal protection equipment if necessary.
 Be responsible for personal hygiene.
 Do not eat, drink and smoke in the vicinity of the installation.
 Be aware of all applicable Material Safety Data Sheets (MSDS or safety sheet).
 Always wear a portable H2S detector.
 While working on the installation wear a mobile gas detector for H2S, LEL (Lower Explosion
Limit) and OX (low oxygen alarm).
 Immediately leave the area, with the use of an escape gasmask with a proper filter, when the
H2S concentration exceeds 10 ppm.
 Evaluate possible hazardous situations before (a section of) the installation is shut down.
 Inform all persons involved in advance of work on the installation and the possible hazardous or
unacceptable situations during this work.
 Be careful with moving parts. Keep hands and loose clothing and long hair away from rotating
parts.
 Only qualified personnel may carry out work on the electrical installation. Other personnel may
not open the control cabinet and other electrical components.
Use your common sense regarding safety measures!
2.2 Dosing
Advice and instructions on safe handling of chemicals can be found in the MSDS of the relevant
supplier(s). An MSDS can be obtained from the supplier and must be affixed by the dosing installation.
An MSDS provides among other things information on:

 Preventive measures and personal protection equipment that must always be used when
working with the chemicals in question.

 Treatment procedures in case of exposure to or ingestion via the skin, eyes, mouth or
respiratory tract.
 Procedures for removing spilled chemicals.
2.3 Sludge and process liquids

Hydrogen sulphide (H2S) gas may be given off by sludge (biomass) and process water, particularly if it
is stored in a (sealed) container. Dried sludge is flammable. The following minimum precautions are
recommended:
 Always wear a H2S detector.
 Spilled sludge must be removed immediately in accordance with the specified procedures of the
MSDS.
 The personal protection equipment specified in the MSDS must always be present and used.
 Avoid direct contact with sludge and process water. If the eyes or skin of a person have been in
contact with sludge or process water, they must be cleaned immediately with clean water.
All process liquids in the reactors and tanks may contain chemicals and micro-organisms. For this
reason it is recommended that these process liquids be treated with extreme caution. Take the right
personal protection measures such as the use of waterproof shoes, gloves and safety goggles.
2.4 Hazardous gases and vapours

Biogas, hydrogen gas, ventilation air and chemical vapours may be released by the installation during
sampling, maintenance work and/or disasters. All these gases involve potential risks because they may
be explosive, flammable, suffocating and/or toxic.
2.4.1 Biogas
Biogas has approximately the following composition:
 Methane (CH4) 50 - 90 vol. %
 Carbon dioxide (CO2) 10 - 45 vol. %
 Hydrogen sulphide (H2S) 0.2 – 3.5 vol. %
 Water (H2O) 0 - 5 vol. %
The exact biogas composition depends on the wastewater characteristics and the pre-treatment. Biogas is
potentially flammable, suffocating, toxic and/or explosive because it contains methane and hydrogen
sulphide.
Methane (CH4)
 Lower explosion limit (LEL) 4.4 vol. % in air.
 Upper explosion limit (UEL) 16.0 vol. % in air.
Hydrogen sulphide (H2S)

 Minimum odour limit 0.1 ppm
 Maximum odour limit 70 ppm
 MAC value 10 ppm

Hydrogen sulphide is a toxic gas and in low concentrations can be identified by its penetrating odour of
rotting eggs, in high concentrations it can no longer be smelled. Hydrogen sulphide irritates the eyes
and the respiratory tract. In high concentrations hydrogen sulphide is lethal.
Anyone in an area where hydrogen sulphide can be released must carry a portable H 2S detector and be
equipped with a fully certified (and regularly checked) gas mask with a suitable filter.
2.4.2 Hydrogen
Hydrogen may be produced during the acidification of wastewater. If the relevant tanks are
continuously ventilated the hydrogen concentration remains sufficiently low. However, if the ventilation
fails or is manually shut down, within a few hours the hydrogen concentration may rise to a critical
level.

2.4.3 Ventilation and chemicals vapours

Certain rooms and/or tanks are ventilated. This ventilation air may contain different gases and vapours,
such as hydrogen sulphide (toxic), hydrogen gas, methane (explosive) and carbon dioxide (may
displace oxygen).
The vapours of chemicals used may have the same harmful effect as the liquid or solid form. For this
consult the MSDS of the supplier.
2.4.4 Hazardous area classification

Around the BIOPAQ®IC reactor a hazard zone applies that relates to the possible exposure to biogas.
Biogas is flammable, suffocating, toxic and/or explosive because it contains (among other things)
methane and hydrogen sulphide.
This hazard zone is schematically drawn in Figure 2.1. Please check the applicable ‘Hazardous area
classification’ for reactor specific details.

Figure 2.1: Explosion and fire hazard zone BIOPAQ®IC reactor
Everyone, present in the hazard zone of the reactor, must work in accordance with the local applicable
safety provisions. The following general regulations must be taken into account as a minimum:
 The entrance to the top of the reactor must be restricted.
 Only instructed and authorize personal may enter the top of the reactor.
 Workers must carry a mobile gas detector for H2S, LEL (Lower Explosion Limit) and OX (low
oxygen alarm) and an escape gasmask with a proper filter. Workers must know how to use
these personal safety guards.
 Workers must withdraw immediately, with the use of an escape gasmask with a proper filter,
when the H2S alarm sounds.
 The BIOPAQ®IC reactor is equipped with a high biogas pressure- and a low water level- alarm
[see figure 3.4 and 3.5]. Both alarms warn for the possibility of biogas escaping at the top of
the reactor. An alarm situation should be indicated by an optical and/or acoustic alarm and
workers should withdraw before the explosion conditions are reached.
During maintenance activities, the critical explosion conditions must be carefully

watched using a LEL and H2S detection. In the BIOPAQ® IC process methane (CH4)
and hydrogen sulphide (H2S) gas are produced simultaneously in reasonable fixed
ratio. Therefore Paques uses H2S as an additional indication for critical explosion
conditions, due to this specific biogas composition. The H2S alarm will sound long
before the critical explosion conditions are reached.
Maintenance with a LOW chance of unwanted biogas release

Sometimes it is inevitable to perform maintenance within the hazard zone, with a LOW chance of
unwanted biogas release, due to normal operation (for instance the visual inspection of the internal
circulation via the inspection glasses of the gas/liquid separator). This maintenance is only permitted if
the worker at least follows the regulations as mentioned above.

Maintenance with a HIGH chance of unwanted biogas release
It is also inevitable to perform maintenance within the hazard zone, with a HIGH chance of unwanted
biogas release, due to normal operation. This maintenance is only permitted if the worker at least
follows the regulations as mentioned above and is wearing a full-face gasmask with a proper filter.
Maintenance with a HIGH chance of unwanted biogas release involves the following activities:
 Taking a biogas sample.
 Measuring the gas pressure of the gas/liquid separator.
 Opening the covers on top of the reactor in order to inspect and/or adjust (the overflow of) the
top separation module.
 Unblocking the downer.
 Adjusting the level measurement of the gas/liquid separator.
For all other maintenance the reactor has to be taken out of operation, inertisized and emptied
according to operating procedures Shutting down the reactor, Shutting down and inerting the biogas
system and Emptying the reactor (Appendix B).
Special risks, concerning the BIOPAQ®IC reactor, are:

 When draining the spray water line from the gas/liquid separator (both at the top and at the
bottom) biogas may be released. To minimise this risk, the drain valve has to be executed as a
manual fail-safe spring activated self-closing valve.
 Biogas may unexpectedly be released from the granular sludge (even some time after shutting
off the feed). For this reason during work/inspections in the top of the reactor all the sludge
must also be removed from the reactor.
 Never open the manholes in the headspace during operation as well as during a process stop.
 (Sudden) under pressure in the reactors’ headspace can cause material damages and/or
explosive biogas/air mixtures. Always use the (BIOPAQ®) flare for biogas/air removal, when
this gas mixture has been generated.
2.5 Working at a height

Make sure prior to working at a height that the right fall protection equipment is present. Check the
fixing of cage ladders, platforms and fencing (if present) each month.
2.6 Working in confined spaces

Work in confined spaces must be carried out following the local applicable standard. The following
minimum safety regulations are advised:
 Close all inflow gas, water and chemical pipes with blind or plug flanges.
 Remove all process liquids and sludge from the tank and rinse/flush with clean water.
 Put an extra ventilator at a tank opening for extra fresh air.
 Ventilate the tank well. Maintain ventilation during work.
Before and during the inspection or work it must be established whether the empty tank is safe for the
operating personnel to do the work or inspection. To do this, the following measurements need to be
carried out:
1 LEL measurement: the concentration of explosive gases must be lower than 1 % LEL
(H2 < 0.04 vol. % and/or in combination CH4 < 0.04 vol. %).
2 OX measurement: the oxygen concentration must be between 20 and 21 vol. %.

3 H2S measurement: the hydrogen sulphide concentration must be less than 10 ppm.
These measurements can be carried out with a portable gas detector. If, despite all the precautionary
measures, the gas alarm does go off, everyone in the area should stop work immediately and leave.
Work in confined spaces should always be carried out by at least two people. One person keeps watch
outside the confined space and keeps in contact with the person in the confined space. This ‘tank
watcher’ raises the alarm if there is an accident. The tank watcher must, under all circumstances,
remain outside the confined space and should never enter it to help other employees.
2.7 Malfunctions
A malfunction results in an unusual situation. Take extra care during a malfunction, because this can
create hazardous situations. For example:
 Accumulation of hazardous gasses, causing higher pressures.
 Extreme pH value of a process liquid.
 Release of biogas into unusual and unexpected places.
2.8 Disasters
During disasters always follow the locally applicable safety provisions. Shut the installation down and,
during an evacuation, leave the site calmly; do not run! Always walk at right angles to the wind
direction from the source.
2.8.1 Shutting down the installation

During accidents the influent and all other dosing must be stopped. Take into account that the biogas
production may fall slowly (may take several days) and will not stop immediately after the influent has
been stopped. Effluent may leave the reactor hours (days) after the influent has been stopped, because
the biogas production continues. This may result in too low a liquid level in the reactor and ultimately in
biogas leakage via the upper separation module of the reactor.
The shut down of the installation is further described in the operating procedures Shutting down the
reactor and Shutting down and inerting the biogas system (Appendix B).

3 Process description
In the BIOPAQ® Internal Circulation (IC) reactor anaerobic biomass (granular sludge) converts organic
components (expressed in Chemical Oxygen Demand, COD; explained in chapter 7: List of Technical
Terms and section 3.5.2: Chemical Oxygen Demand, (COD)) from wastewater into biogas. Biogas
consists mainly of methane (CH4), carbon dioxide (CO2) and a small fraction of hydrogen sulphide
(H2S).
The reactor contains two reactor compartments on top of each other. The lower compartment contains
the expanded sludge bed and is under high load; most of the biodegradable COD is converted here. The
upper compartment serves as polishing step for optimal COD removal.
3.1 BIOPAQ® IC reactor

The influent is pumped into the bottom of the reactor, where it is immediately mixed in the mixing
section (1) with recirculated sludge and effluent from the downer (6). The influent then flows to an
expanded bed of granular sludge (the biomass) in the lower reactor compartment (2). Here most of the
biodegradable COD is converted into biogas. This biogas is collected in the lower separation module (3).
This causes a gas lift, during which water and sludge in the riser (4) are also carried to the gas/liquid
separator on top of the reactor (5). The biogas leaves the reactor via this separator, and the
water/sludge mixture flows via the downer (6) back into mixing section (1) at the bottom of the
reactor, where it is again mixed with fresh influent: internal circulation. The effluent from the lower
compartment flows through the separation module (3) to the upper compartment (7), which is low loaded
for final treatment. Here the remainder of the biodegradable COD is converted into biogas. This biogas is
separated in the upper effluent separation module (8) after which it is discharged via the gas/liquid
separator(5) together with the biogas from the lower compartment (2). The polished effluent leaves the
reactor through the top. The lower and upper three phase (water, granular sludge and biogas)
separators (3 & 8) are made of plastic to prevent corrosion. Figure 3.2 shows a BIOPAQ ® IC separation
module.
Figure 3.1: BIOPAQ® IC reactor Figure 3.2: BIOPAQ® IC separation module

3.1.1 The process in the BIOPAQ® IC reactor
The following four process sections that are connected by the internal circulation system, characterise
the BIOPAQ® IC reactor: the mixing section (1), the expanded sludge bed (lower compartment, 2), the
polishing section (upper compartment, 7) and the gas/liquid separator (5).
The internal circulation is based on the gas lift principle that is caused by the difference in gas hold-up
between the riser (4) and the downer (6). A high loading requires more mixing. The internal
recirculation flow rate depends on the quantity of biogas produced and hence depends on the
biodegradable COD load. This principle makes the system self-regulating.
Higher COD load.


Higher biogas production.

More recirculation.

More influent dilution.
The liquid recirculation flow rate is on typically 0.7 – 1.1 times the biogas flow rate.
Mixing section (1)

The incoming wastewater (influent) is effectively mixed at the bottom of the reactor with the internal
circulation coming from the top of the reactor. This results in immediate dilution and conditioning of the
wastewater. This makes the BIOPAQ® IC reactor suitable for the treatment of wastewater with a high
biodegradable COD concentration.
The distribution system in the mixing section ensures that the reactor has a proportionate influent
distribution to the expanded sludge bed by using special nozzles and the sludge roof.
Expanded sludge bed (2)

The lower reactor compartment contains a highly concentrated, fluidised (granular) sludge bed. The
upward liquid flow and the biogas production cause the sludge expansion. The effective contact
between wastewater and biomass allows a higher biodegradable COD load.
The biogas produced is collected under the gas hoods of the separation modules. It flows upwards
through the riser and drags along granular sludge and process water, due to the gaslift principle as
explained previously.
Polishing (7)
In the upper compartment effective polishing of the wastewater occurs due to the low sludge loading
rate, the relatively long hydraulic retention time and the gentle flow character. In this compartment the
turbulence and the upflow velocity are low due to small biogas production and the absence of the
internal circulation. These conditions also create extra space for sludge from the expanded sludge bed,
which prevents sludge loss during short peak loads.

Biogas, produced in the upper compartment, is collected in the gas hoods of the upper separation
module and flows via the gas line (figure 3.3: 4b) to the gas/liquid separator (5). A water seal (50 cm
water column) prevents the release of biogas through gas hoods of the upper separation module to the
headspace of the reactor. A pressure regulator (for example a pressure-resistant gas buffer, see
paragraph 3.2) must maintain a gas pressure in the range of 25 to 35 cm water column. Biogas will
escape through the gas hoods when the pressure exceeds 50 cm water column.
Gas/liquid separator (5)

Biogas is separated from the granular sludge and process water in the gas/liquid separator (figure 3.3).
The granular sludge/process water mixture flows back to the mixing section (1) via the downer (6).
Biogas leaves the gas/liquid separator via an outlet on the top. The measured biogas flow rate may
differ by up to 50% from the average biogas flow rate due to the irregular/pulsating gas flow.
Figure 3.3: Gas/liquid separator (5) [4a = riser lower separation module (granular sludge, water and
biogas), 4b = gas line upper separation module (biogas), 6 = downer (valve), A = spray
water line, B = inspection glass, C = nitrogen dosing point A, D = water separator and E =
biogas pipeline]
The gas/liquid separator is equipped as standard with a spray water connection (A), two inspection
glasses (B), a liquid level sensor (figure 3.4), a water separator (D) and two connections for nitrogen
gas dosing (figure 3.3: C and figure 3.5: B). These components are necessary to ensure internal
circulation during operation, to prevent fouling of the biogas pipeline (E) and to suppress foaming.
These aspects will be further explained in the following sections.

Figure 3.4: Liquid level sensor on top of the gas/liquid separator
Figure 3.5: Downer valve (A) and connection for nitrogen gas dosing on the downer (B)
3.2 Biogas treatment

For safe operational management, Paques strongly recommends that the biogas system has at least
been equipped with flow metering, condensate separation, overpressure protection, buffer and flare.
The overpressure protection can be present either mechanically (valve) or as a water seal.
3.2.1 Biogas flow metering

Paques recommends the use of continuous biogas flow metering for optimum process control of the
BIOPAQ® IC reactor. The link between biodegradable COD load and biogas production allows optimal
adjustment of the loading to the reactor capacity while preventing COD overloading.
3.2.2 Condensate separation

Biogas is saturated with water. The temperature of the biogas in piping outside of the bioreactor will fall
resulting in condensation. The condensate must be removed from the biogas via a condensate drainage
point with water seal [figure 3.6 and 3.7, water seal A]. This water seal must continuously be checked
and adjusted automatically.

3.2.3 Overpressure protection
The biogas system must be equipped with uncontrolled biogas release detection and overpressure
protection. Uncontrolled biogas release is monitored with an effluent level alarm (L) on the BIOPAQ ® IC
reactor and an overpressure alarm (P) on the biogas pipeline. Once unwanted biogas release is
detected (L- and/or P-alarm), a beacon/sounder combination unit on top of the reactor as well as at the
bottom of the reactor alarms the reactors’ surroundings. The influent pump is now only operated to
control the effluent level of the reactor.
The overpressure protection can be effected both mechanically [figure 3.6, B] and by means of a water
seal [figure 3.7, B]. The mechanical overpressure protection device must be located at the highest
point in the gas line, as close as possible to the BIOPAQ ® IC reactor. This principle is shown
schematically in figure 3.6. Contact the owner of the installation when neither of these safety measures
is in place, because safe operation of the installation is impaired.
Figure 3.6: BIOPAQ® IC reactor with mechanical overpressure protection device [B, 45 cm water
column (mbar)], reactor effluent level alarm (L) and overpressure alarm (P), scrubber
(optional), gas buffer, gas flare and condensate separation via water seal [A, 60 cm
water column (mbar)].
An example of overpressure protection using a water seal is shown schematically in figure 3.7. The
blow off of the overpressure protection device must be located near the highest point in the gas line, as
close as possible to the BIOPAQ® IC reactor.

Figure 3.7: BIOPAQ® IC reactor with overpressure protection via water seal [B, 40 cm water column
(mbar)], reactor effluent level alarm (L) and overpressure alarm (P), scrubber (optional),
gas buffer, gas flare and condensate separation via water seal [A, 60 cm water column
(mbar)].
3.2.4 Buffering
The biogas produced leaves the BIOPAQ® IC reactor with an irregular, pulsating flow. Paques
recommends that these fluctuations are being buffered using a pressure-resistant buffer (operating
pressure of 31 cm water column) with variable volume.
3.2.5 Gas flare

Depending on the situation the biogas produced can be used as a fuel, e.g. for a boiler. Irrespective of
the situation Paques has recommended that the BIOPAQ® IC reactor be equipped with a downstream
gas flare (operating pressure 28 cm water column). In this way the biogas can always leave the reactor
under controlled and safe conditions.
3.3 Ventilation
According to Paques’ standards, the top of the reactor should always be actively ventilated with the
help of the ventilation system. This prevents odour emission and possible accumulation of biogas. The
ventilation flow is set during start up.

3.4 Influent
The influent properties determine the success of the anaerobic degradation. The influent normally comes
from a pre-acidification tank or buffer tank. In this tank fluctuations in chemical composition and flow
rate are balanced and the wastewater is partly pre-acidified. In addition, this (these) tank(s) can be
used for nutrient dosing and pH correction.
During shut down the reactor contents (process water and granular sludge) may NOT flow out of the
reactor via the influent pump and influent line. This would result in biomass loss. If the liquid level in
the reactor falls too low, biogas may escape from the reactor via the separation modules. Backflow of
the reactor contents must be prevented at all times by a well-functioning non-return (check) valve and an
actively controlled valve that closes when the pressure or level drops.
A good understanding of the influent is the basis for optimum process control, because it enables
identification of a process malfunctions at an early stage. To prevent a process malfunction the influent
may not contain any toxic or disrupting substances, such as poly-aluminium chloride and quaternary
ammonium compounds.
3.4.1 Nitrite & nitrate

The influent of the BIOPAQ® IC reactor may not contain more than 1 mg/l nitrite (NO2--N) and 10 mg/l
nitrate (NO3--N). As a result of higher nitrite and/or nitrate concentrations nitrogen gas (N2) producing
bacteria may develop in the methane producing granular sludge. The biological anaerobic conversion of
nitrite/nitrate into nitrogen gas is called denitrification. The intermediates of denitrification (nitrite and
other nitrogen oxides) have an inhibiting effect on methane producing bacteria.
3.4.2 Sulphite & sulphate

A sulphite (SO32-) concentration of 150 - 250 mg/l is toxic, which results in a decrease in biogas
production of 50% due to the toxicity of sulphite. The toxic effect on the biomass can be reduced by
slowly accustoming the biomass to sulphite. Normally a continuous sulphite load does not therefore
jeopardise the reactor operation. Big variations are however harmful.
Sulphate (SO42-) is a relatively inert compound. Biomass requires small quantities as a nutrient (as a
source of sulphur). Sulphate reducing biomass can convert sulphate into hydrogen sulphide (H2S) under
the consumption of biodegradable COD. Sulphate has no COD but the COD contents of H2S is 2 g
COD/g H2S.
3.4.3 Fats, oils & greases (FOG)

Fats, oils and greases are sometimes present in the influent of the BIOPAQ® IC reactor. As long as
these are not toxic, fats, oils and greases are acceptable up to a total concentration of 50 mg/l. Higher
concentrations may have an inhibiting effect on the biodegradable COD removal and cause blockages of
the reactor and/or wash out of granular sludge.

3.5 Control parameters
3.5.1 Biomass (granular sludge)
The sludge bed of the BIOPAQ® IC reactor consists
of biomass in the form of granules: the granular
sludge. Figure 3.8 shows a number of these
anaerobic sludge granules, both intact and sliced
by a laboratory analyst. The granular sludge
contains various bacteria groups, including
acidifying bacteria that convert complex organic
compounds into readily degradable volatile fatty
acids (VFA) and biogas producing bacteria.
Figure 3.8: (Sliced) BIOPAQ® IC granular sludge
The sludge bed is present in the lower compartment of the BIOPAQ® IC reactor. Due to biomass growth
the quantity of granular sludge in the reactor increases in time. In addition to biomass growth, wash
out and natural death of bacteria also takes place, which results in the loss of a certain fraction of the
biomass. The net biomass increase depends on the ratio between growth and biomass loss.
The actual quantity of granular sludge and the ratio between biomass (VSS) and inorganic solids (ash
residue of TSS) is determined in the light of a sludge profile (Determination of sludge profile – Appendix
B). In general it can be stated that the BIOPAQ® IC reactor contains too much or too heavy granular
sludge if the 4th sampling point contains more than 50 ml/l sludge and/or the 1st sampling point more
than 250 g/l TSS and/or 50 – 60% ash residue of TSS.
Heavy sludge needs to be (partial) removed from the reactor on a regular basis, because excess
amounts can:
 Oust the biomass (inert material replaces the biomass).
 Damage the reactor internals.
 Disturb or stop the internal circulation.
The (Heavy) sludge removal procedure is described in appendix B.
The BIOPAQ®ICC reactor may be damaged internally if it is operated with excess or

too heavy anaerobic granular sludge.
A surplus of granular sludge can easily be tapped off and stored (Storage of anaerobic granular sludge -
Appendix B). Even after a storage period of more than two years this sludge can be reactivated almost
as fast as fresh biomass. Consequently, the reactor can be quickly started up again after a process
malfunction by inoculation with the stored granular sludge. In addition stored granular sludge can also
be used to start up new reactors. You can contact Paques Services to organise this.

3.5.2 Chemical Oxygen Demand (COD)
The Chemical Oxygen Demand (COD) of a wastewater is that quantity of oxygen necessary to
chemically oxidise the oxidisable substances present in the water. Paques makes a distinction between
the following COD fractions as shown in Figure 3.6.
Wastewater usually contains a dissolved and solid COD fraction. This fraction distribution can be
obtained by means of filtration. The colloidal material is also found in the dissolved fraction. Both the
dissolved and the solid COD fraction contain an inert and a degradable part.
Note: The final fraction distribution depends on the analysis method used (for example centrifugation,
filtration, pore size of the filter, etc.).
Figure 3.9: COD fraction distribution in wastewater
3.5.3 COD load and volatile fatty acid concentration

Complex organic compounds from the wastewater (measured as COD) are converted in a number of
stages to biogas. To summarise:
1 Acidifying bacteria convert biodegradable COD into volatile fatty acids (VFA), including acetate
and hydrogen (H2) in a number of stages. VFA belong to the dissolved, degradable COD
fraction.
2 Biogas producing bacteria then convert the acetate produced into biogas.
For stable operation of the BIOPAQ® IC reactor it is important that the load is proportionate to the
activity of the granular sludge. The granular sludge and biodegradable COD load are well adjusted to
each other when the VFA concentration measured in the effluent is less than 5 meq/l. In addition to
remaining VFA, the residual COD concentration in the effluent depends on the inert COD fraction [see
Figure 3.9] and the quantity of sulphide produced. This varies per type of wastewater.
The VFA concentration of the water phase is determined by means of titration; this method is described
in operating procedure Determination of alkalinity and volatile fatty acid (VFA) concentration (Appendix
B).

3.5.4 Pre-acidification degree
VFA is formed both in the upstream (buffer tanks, pre-acidification or other pre-treatment) and inside
the BIOPAQ® IC reactor. The ratio between the VFA fraction (expressed in COD) and the dissolved COD
fraction in the influent determines the degree of pre-acidification of BIOPAQ® IC influent. An optimum
pre-acidification degree is necessary for a good ratio between acidifying and biogas producing biomass
in the sludge granule. Paques recommends a pre-acidification degree of approximately 35% of the
dissolved COD. A pre-acidification degree that is too high (> 50%) or too low (< 30%) results in
unbalanced growth, deteriorating granular structure, reduction of the COD removal efficiency and
potential biomass loss.
The pre-acidification degree is determined using the calculation method in the operating procedure
Calculations (Appendix B).
3.5.5 Specific biogas production

The specific biogas production is that quantity of biogas that is produced per 1 kg of biodegradable COD
removed.
The specific biogas production is determined using the calculation method in the operating procedure
Calculations (Appendix B).
3.5.6 pH
Optimum
The optimum pH in the sludge bed is between 6.5 and 7.5. For stable operation of the BIOPAQ ® IC
reactor the pH must be kept within this range.
Checking
The pH in the sludge bed of the BIOPAQ® IC reactor can be measured with an on-line pH meter. If the
reactor is not designed with an on-line measurement, Paques recommends that the pH be regularly
checked manually. Use the second sampling valve for this (Technical Data Sheets - Appendix A).
Note:
In the case of manual pH checking the pH measured is usually higher than the actual
pH in the sludge bed. This is caused by the escape of CO 2. The reliability of the
manual pH measurement can be increased as far as possible by preventing contact
with outside air and the pH in the liquid measured during sampling.
Acidification
VFA and sulphides (H2S) occur both dissociated (charged, like HS-) and undissociated (uncharged, like
H2S). The ratio between the dissociated and undissociated fraction depends on the pH. If the pH of the
process water is reduced the undissociated fraction increases. This undissociated fraction is the
problematic form, because it can penetrate through the cell membrane, which poisons the cell. A
decrease in the reactor pH below 6.5 must therefore be prevented at all times.

Influent pH
Because the pH in the reactor generally rises, the influent pH can be set a little lower than the optimum
pH. If the reactor is operated with a low influent pH, then it is important that:
 The reactor liquid has sufficient buffer capacity.
 The reactor contents are well mixed (sufficient biogas production  good recirculation flow rate).
3.5.7 Alkalinity (pH buffering)

Alkalinity is the capacity of a solution to buffer pH fluctuations. For the BIOPAQ ® IC reactor the most
important buffer system is the carbonic acid (H2CO3) / bicarbonate (HCO3-) system (pH between 6.5
and 7.5). The alkalinity of the water phase is determined by titration, this method is described in
operating procedure Determination of alkalinity and volatile fatty acid (VFA) concentration (Appendix
B). To prevent acidification of the BIOPAQ® IC reactor the effluent alkalinity must be at least 15 meq/l.
Alkalinity increasing processes are:
1. Stripping CO2 from the BIOPAQ® IC reactor.
2. Conversion of fatty acids into biogas.
3. Sulphate reduction.
3.5.8 Temperature
Optimum
The temperature has a strong effect on the growth rate and the activity of the bacteria in the granular
sludge, in particular on the biogas producing bacteria. These bacteria have a temperature optimum
between 30 and 38C. Above 40°C their activity decreases considerably. It is therefore necessary to
keep the reactor temperature below 38C.
Continuously lower temperature

If the reactor is continuously operated at a lower temperature (< 25°C), the initial start up and any
recovery after a restart will take longer. But, ultimately good biological activity rates and hence COD
removal efficiencies can also be obtained at a lower process temperature.
Sudden temperature drop

VFA producing bacteria are less sensitive to sudden temperature drops than biogas producing bacteria.
In case of a sudden temperature drop the biogas production falls more quickly, which means that the
chance of acidification of the sludge bed increases. To protect the sludge bed against acidification the
reactor must have a reduced load during a temperature drop. In addition Paques recommends that the
pH of the sludge bed be temporarily checked more often. Use the second sampling valve for this
(Technical Data Sheets - Appendix A).
Considerable temperature fluctuations within a short time must be avoided because they almost always
cause a reduction in the biodegradable COD removal efficiency.
3.5.9 Nutrients
Biomass needs macro- and micro-nutrients for growth. Normally the wastewater contains sufficient
nutrients and extra dosing is not necessary. In some industries, such as for example in the pulp &
paper industry, the wastewater contains insufficient nutrients. In these industries extra nutrient dosing
is necessary because a long-term nutrient deficit has a negative effect on the sludge quality and
ultimately the removal efficiency.

Extra dosing is always carried out upstream (for example pre-acidification tank or buffer tank) and is
matched to the composition of the specific wastewater. After start up the dosing of the macro-nutrients
N and/or P is further adjusted based on the measured effluent concentrations of the nutrients.
As for all mirco-nutrients, Paques B.V. supplies the BIOPAQ® Micromix. This is a balanced solution of
trace metals, specifically developed for the BIOPAQ® IC process.
Nitrogen (N), phosphate (P) and sulphur (S)

Bacteria need nitrogen (N), phosphate (P) and sulphur (S) for growth. Nitrogen is usually dosed as urea
solution (chemical formula written as CO(NH2)2 or CON2H4) and phosphate as phosphoric acid (H3PO4).
Compared to N and P, the sulphur (S) requirement is much lower. Normally, S is present in a sufficient
quantity in wastewater. If this is not the case, extra sulphur is normally dosed as sulphuric acid
(H2SO4). Paques recommends that the initial dosing be calculated in the light of the following
guidelines:
1. Fully acidified influent: CODbiodegradable : N : P = 900 : 5 : 1 (kg/m3)

2. Fully unacidified influent: CODbiodegradable : N : P = 350 : 5 : 1 (kg/m3)
After start up, control can best be carried out on the ammonium and phosphate concentration in the
effluent of the BIOPAQ® IC reactor, taking into account any variations in the biodegradable COD load. The
following guidelines apply for this: NH4+-N > 5 mg N/l and PO43--P > 1 mg P/l.
Calcium (Ca), magnesium (Mg) and potassium

Bacteria need calcium (Ca), magnesium (Mg) and potassium (K) to function well. Whether dosing is
necessary depends on the type of wastewater.
Calcium improves the granule forming properties of the sludge. In wastewater with high calcium
concentrations there is a high risk of calcium carbonate precipitation formation, because calcium
carbonate is poorly soluble. To keep the dissolved calcium concentration high, the pH must be kept low.
In wastewater with low calcium concentrations Paques recommends dosing a soluble calcium salt until the
dissolved calcium concentration in the wastewater is 70 mg Ca2+/l.
There is usually sufficient magnesium present. In wastewater with a high sodium concentration (> 5000
mg Na+/l) Paques recommends that the dissolved magnesium concentration be increased to 10 – 20 mg
Mg2+/l, by dosing a soluble magnesium salt.
Extra potassium dosing also depends on the sodium concentration (> 5000 mg Na+/l). Sodium and
potassium are optimal balanced when the Na : K ratio is around 20 : 1.
3.5.10 Calcium (precipitation)

Under normal circumstances calcium (Ca2+) has a limited solubility in water. But the dissolved calcium
can be much higher (well over 1 g/l) when fatty acids are (temporarily) produced in the clients’
production process. Calcium and the fatty acid produced are as it were coupled to one another,
enabling the calcium to be dissolved. In the BIOPAQ ® IC reactor the fatty acid is converted into biogas
and disappears from the water phase. Dissolved calcium is left behind.
Biogas consists mainly of methane (CH4) and carbon dioxide (CO2). Depending on the pH, part of the
carbon dioxide produced as bicarbonate (HCO3-) and/or carbonate (CO32-) is left in the water phase,

where it functions as a new anion for calcium. With a pH of 6.5 – 7.0 the majority will be present in the
water phase as bicarbonate, as a result of which calcium remains in solution. If the ratio between
bicarbonate and carbonate changes and the carbonate fraction in the water phase increases, calcium
will then precipitate with carbonate as calcium carbonate (CaCO 3). Calcium carbonate precipitation can
cause blockage of the pipe work and must therefore be prevented.
In these cases Paques recommends that the following guidelines be taken into account:
1. Keep the Ca2+ influent concentration below 600 mg/l.
2. Keep the pre-acidification degree sufficiently low.
3. Prevent the stripping of carbon dioxide (CO2) from the water phase (for example by keeping the
effluent line completely filled with water).
4. The COD/Ca2+ ratio should not exceed 10 : 1 (kg : kg).
3.5.11 Hydrogen sulphide

In addition to methane producing bacteria anaerobic granular sludge also contains sulphate reducing
bacteria. Sulphate reducing bacteria function in a comparable environment as methane producing
bacteria. They convert sulphate and/or sulphite into (hydrogen) sulphide under the consumption of
biodegradable COD from the influent. Hydrogen sulphide formation is undesirable for the following
reasons:
 H2S gas may be released from the effluent, as a result of which odour problems and toxic H 2S
concentrations may occur in the ventilation air.
 Sulphate has no COD, but sulphide has a COD of 2 mg/mg S2-. Because sulphide in the effluent
is measured as COD, this gives a reduction in the COD efficiency.
 Corrosion problems in the water/air separators.
 Part of the sulphide leaves the reactor as H2S in the biogas. The biogas becomes toxic and
corrosion problems may arise for example in combustion plants, when biogas is used as a fuel
without pre-treatment or the permitted SO2 discharge limit may be exceeded.
 Hydrogen sulphide is toxic. At concentrations of 150 mg/l H2S in the water phase the biogas
production falls by 50%. Increasing the liquid pH by one to two tenths can reduce the toxic effect
on the biomass.
 Methane producing biomass competes for biodegradable COD with the sulphate reducing
biomass.
In addition to the pH the COD/Sulphate (SO42-) ratio in the influent is also an indication that there is a
chance of toxic effects due to sulphide. With a COD/SO42- ratio of 10:1 the effects are negligibly small.
Once the granular sludge is accustomed to sulphide the reactor can be operated without problems at a
ratio rising to 5:1.
3.5.12 Summary of control parameters

The general control parameters are summarised in the table (Project-specific) control parameters in
appendix A. Any project-specific changes can be entered by the process specialist on the spot in the
same table.

4 Start up procedure
Paques recommends that Paques personnel be present at the initial start up, because the experience of
the Paques start-up engineers will result in a start-up that is as smooth and fast as possible. However,
the installation should be fully completed and tested. It is recommended that a month’s stock of all the
required nutrients, neutralising chemicals and nitrogen gas (N2) be present on the site. Also all the
required analysis materials and chemicals must be present in the laboratory.
All the equipment must be started up in accordance with the suppliers’ specifications.
4.1 Technical inspection

Prior to the technological start up the installation is technically inspected to ensure safety and efficient
start-up. The technical inspection consists of the following components:
 Leakage test
 Hydraulic test
 Functional specification check
4.1.1 Leakage test

The leakage test is carried out at the start of the hydraulic test. During the leakage test it is determined
whether the reactor with relevant pipe work is gas and watertight.
The leakage test is preferably carried out with clean (industrial or river) water (for the reactor) and
compressed air (for the gas system). If this is not present, the leakage test may if necessary be carried
out with process water. Pay attention here to the quality of the process water used. Think particularly
about the biodegradable COD concentration, TSS concentration, pH and temperature.
4.1.2 Hydraulic test (water run)

During the hydraulic test the reactor hydraulics are tested. For example, whether the pumps and lines
can cope with the flow rate and whether there are blockages in the pipe work or nozzles. In addition
the different set points are set and determined.
Always carry out the hydraulic test with water with a low COD concentration!
Set the height of the level measurement in the gas/liquid separator in accordance with operating
procedure Setting level measurement of gas/liquid separator (Appendix B).
4.1.3 Checking of functional specification

During this check it is determined whether the installation operates as described in the functional
specification. Carry out this check during the hydraulic test (where possible) and note here:
 Whether the signals of the on-line metering & control equipment in the field come in on the
right scale and place on the SCADA system (report deviations to the programmer).

 Whether all controls (for example pump) and regulations (for example pH) function well from
the SCADA system in the field.
 Test alarm and stand-by situations.
4.2 Technological start up

4.2.1 Start up conditions
Before the anaerobic granular sludge can be added to the reactor, the conditions indicated in this
paragraph must be checked and if necessary adjusted.
Process conditions
The water already present in the BIOPAQ® IC reactor must meet the conditions given in table 4.1.
Table 4.1: Process conditions during start up
Process condition Minimum Optimum Maximum
VFA (meq/l) 0 <5 10
Pre-acidification degree (%) 30 35 50
pHsludge bed (-) 6.5 7.0 – 7.5 8.0
Alkalinity (meq/l) 15 - -
Temperature (°C) 25 30 – 38 40
Nutrients: Nitrogen (N) (CODbiodegradable : N) Depending on pre-acidification degree
Nutrients: Phosphate (P) (CODbiodegradable : P) Depending on pre-acidification degree
Influent
The influent of the BIOPAQ® IC reactor must comply with the output data described in the contract.
Set the influent distribution system as described in Setting of influent distribution system (appendix B).
4.2.2 Inerting biogas system

During the hydraulic test the system is filled with water and air. Biogas production can be expected
directly after the inoculation of anaerobic granular sludge. To prevent critical oxygen-biogas mixtures
(LEL, see section 2) the biogas system must, before the sludge inoculation, be inerted with nitrogen
gas.
Inert the biogas system with nitrogen gas in accordance with operating procedure Inerting biogas
system in appendix B.

4.2.3 Sludge inoculation
The gas system of the BIOPAQ®IC reactor must be tested and guaranteed gas-tight
before the reactor may be inoculated with anaerobic granular sludge.
In the ideal case the reactor is inoculated with anaerobic granular sludge, with a volume of 50 - 65% of
the reactor contents, up to a maximum of 1 metre below the underside of the lower separation module.
The ideal sludge volume for start up depends on the reactor type and the anticipated biodegradable
COD load. It takes more time to bring the reactor to the design COD conversion capacity if the reactor
is started up with less sludge than recommended.
It is recommended to analyse the anaerobic granular sludge (or have it analysed) beforehand for the dry
matter content (TSS), the organic matter content (VSS) and the biological activity. With these data the
total biodegradable COD conversion capacity of the sludge inoculation can be calculated. This conversion
capacity determines the biodegradable COD load during start up. An example calculation is given in table
4.2.
Table 4.2: Example calculation of total conversion capacity of sludge inoculation. For the total
conversion capacity the conversion capacities of one or more sludge types are added
together. In this example a sludge mixture is assumed that comes from supplier A and
supplier B.
Example calculation of total conversion capacity of sludge inoculation
Volume of sludge
Sludge inoculation A 300 m3
inoculation
VSS concentration 63 kg * m-3
kg COD * kg VSS-1 * day-
Sludge activity 0.6 1
Volume of sludge
Sludge inoculation B 100 m3
inoculation
VSS concentration 59 kg * m-3
kg COD * kg VSS-1 * day-
Sludge activity 0.6 1
Conversion capacity sludge inoculation A: 300 * 63 * 0.6 = 11340 kg COD * day-1

Conversion capacity sludge inoculation B: 100 * 59 * 0.6 = 3540 kg COD * day-1
Total conversion capacity sludge inoculation 14880 kg COD * day-1
During the initial start up the optimum reactor temperature is usually not yet reached and the biomass
still has to get accustomed to the new process conditions. This temporarily results in a lower sludge
activity. To prevent overload the reactor is loaded during the initial start up with a convertible COD load

that is based on 50% of the total conversion capacity. During the initial start up the reactor from the
example can be loaded with a COD load of:
Convertible COD load = 0.5 * 14880 = 7440 kg CODbiodegradable*day-1.
Based on an anticipated efficiency of for example 75% the reactor can be loaded during the initial start
up with a total COD load of:
Total COD load = (100/75) * 7440 = 9920 kg CODtotal*day-1.
During the first two weeks of the biological start up 10% sludge loss is normal. This is the result of
natural selection and adaptation of the biomass to the new situation. Small granules of biomass can
usually be found in the effluent from the reactor. The effluent is then usually coloured black.
Fill the reactor with anaerobic granular sludge in accordance with operating procedure Filling the
reactor with granular sludge in appendix B.
4.3 Start up
The BIOPAQ® IC reactor is started up, charged with influent, as soon as the biogas system has been
inerted with nitrogen gas, the reactor filled with anaerobic granular sludge and the start up conditions
have been met.
Procedure
1. Determine the total conversion capacity of the sludge inoculation (see example calculation table
4.2).
2. Start up the BIOPAQ® IC reactor with a biodegradable COD load that is equal to 50% of the
total conversion capacity of the sludge inoculation.
3. Monitor the reactor as described in the Analysis schedule (appendix B).
4. Check the internal circulation (via the inspection glasses of the gas/water separator).
5. Increase the load in stages, depending on the analysis results.
Increase the COD load by 10% if:

 the effluent VFA concentration is lower than 5 meq/l and
 the effluent pH is 6.5 or higher and
 there is no exceptionally high sludge wash out (less than 1 to 2 ml/l)
Reduce the COD load by 10% if:

 effluent VFA concentration is higher than 5 meq/l or if
 effluent pH is lower than 6.5 or if
 a lot of sludge is washed out (> 10 ml/l).

Note:
If the effluent VFA concentration is between 5 and 10 meq/l, after a few hours a fatty acid analysis
must be repeated.
 If the VFA concentration is falling  Maintain the present COD load

 If the VFA concentration is increasing  Reduce the COD load.
An effluent VFA concentration < 5 meq/l indicates that the reactor is performing well.
The COD efficiency during the start up is normally 10 to 20% lower than the design efficiency. This is
caused by:
1. A reduced sludge activity, which gives a higher effluent VFA concentration.
2. Wash out of sludge (both sludge and VFA are measured as COD).
3. Too little (adapted) sludge in the reactor.
4.4 Normal operation

The BIOPAQ® IC reactor functions under normal operation, when all the measured values lie within the
specified range.
4.5 Restart
This paragraph describes how the BIOPAQ® IC reactor is restarted after this has been temporarily shut
down. The method depends on the configuration (with or without external recirculation) and the
duration of the shut down (longer or shorter than 5 days).
4.5.1 With external recirculation or shorter than 5 days

1 Start up the BIOPAQ® IC reactor at 100% of the COD design load.
2 Monitor the reactor as described in the start up procedure (paragraph 4.3).
4.5.2 Without external recirculation or longer than 5 days

1 Refluidise the sludge bed if necessary with nitrogen gas in accordance with operating procedure
Refluidisation of sludge bed (appendix B).
2 Start up the BIOPAQ® IC reactor at 60% of the COD design load and set the influent
distribution system as described in the operating procedure Setting influent distribution system
(appendix B).
3 Monitor the reactor as described in the start up procedure (paragraph 4.3). Pay special
attention to reactor acidification (A) and the internal circulation (B). Check the internal
circulation via the inspection glasses of the gas/water separator.
4 Increase the load in stages, depending on the analysis results.

Reactor monitoring on restart
A. Acidification of the reactor
Reduce the biodegradable COD load as described in the start up procedure (paragraph 4.3) and
increase the pH to 7.0 – 7.5.
B. Poor internal recirculation

After long-term shut down of the BIOPAQ®IC reactor the mixing section and the downer may get
blocked by sludge deposits. There may also be settlement in the expanded sludge bed in the lower
reactor compartment. These blockages can be eliminated with the help of the following instructions.
 Unblock the mixing section by dosing the influent via a quarter of all influent nozzles and alternating
the open and closed nozzles every 5 minutes.
 Unblock the downer in accordance with operating procedure Unblocking downer (Appendix B).
 Refluidise the sludge bed in the lower reactor compartment in accordance with operating
procedure Refluidisation of sludge bed (Appendix B).

5 Operating instructions
5.1 General process control
For continuous, safe operation Paques recommends that one person or a small group of people must be
given the responsibility for the operation of the installation. It is advisable to keep an up-to-date
logbook or datasheet in which measurement data and chemical consumption are noted. If required,
Paques can advise on process control in the light of this datasheet. This can be done for various service
levels. For this you can contact Paques Services (see paragraph 1.1). In addition it is advisable to
regularly update a checklist. This guarantees that there are always sufficient chemicals and spare parts
present and that all equipment is in the optimum state of maintenance.
A stably operating BIOPAQ® IC reactor is characterised by:

 Constant average biogas production;
 Low volatile fatty acid concentration in the effluent;
 Constant effluent pH;
 pH in the sludge bed is higher than influent pH;
 No loss of granular sludge;
 TSS wash out is roughly the same as the TSS washed in;
 High effluent alkalinity;
 A constant COD efficiency (for constant influent COD).
5.2 Routine work

In this paragraph a summary is given of the routine work (inspection and maintenance) on the
BIOPAQ® IC reactor as recommended by Paques. To support this, the following appendices have been
enclosed with this operating manual.
 Appendix B - Operating procedures.
 Appendix C - Troubleshooting.
5.2.1 Daily
Process
 Check whether any alarm situations exist and if so, rectify them.
 Check the trending of the on-line measurements of the last 24 hours and check the
Troubleshooting procedures (Appendix C) in case of abnormal process values.
 Carry out the analysis programme (Analysis schedule - Appendix B) and check that the values
found fall within the specified values ((Project-specific) control parameters - Appendix A).
 Assess the quality of the influent and effluent; report and note deviations.
 Check that the setting of the influent distribution system is in proportion to the current flow
rate and if necessary rotate between the number of opened and closed valves (see Setting
influent distribution system – Appendix B).
Mechanical
 Check the operation of all pumps. Note leakage, flow rate and noise. Rectify the malfunction in
accordance with the supplier’s instructions.
 Check the installation for leaks and blockages.
 Check the levels of the chemical storage tanks and fill up if necessary.

Metering & control equipment
 Check the control parameters and check that these parameters are within the specified value
((Project-specific) control parameters - Appendix A).
 Compare the pH readings of the field equipment with the daily calibrated laboratory pH meter.
If these two measurements differ from one another by more than 0.2 pH units, the field
electrode must be calibrated. It must be cleaned (refer to supplier’s manual) or replaced when
calibration fails.
5.2.2 Weekly
 Clean and check metering equipment in accordance with the supplier’s instructions.
 Check the usability of safety materials.
5.2.3 Monthly
 Carry out the analysis programme (Analysis schedule - Appendix B) and check that the values
found fall within the specified values ((Project-specific) control parameters - Appendix A).
 Check if the covers show signs of wear (top coating fades away, fibres become visible/tangible
and dirt is absorbed). Coat the covers with a polyurethane (PUR) coating if these signs are
present.
 Check if the rubber cover seals are damaged. Replace worn seals.
 Maintenance of equipment in accordance with the supplier manuals.
 Keep the covers closed while recoating them.
 There is a HIGH chance of unwanted biogas release, if the seals of the covers
are being replaced. Consult § 2.4.4 Hazardous area classification before
starting this replacement.
5.3 Cleaning instructions

The installation can generally be cleaned with soap and water. Ensure that soap does not get into the
reactor liquid.
5.4 Temporary shut down

It may be necessary for the BIOPAQ® IC reactor to be shut down for a particular period. This may vary
from a few hours to a few weeks. The BIOPAQ® IC reactor is shut down via a number of stages.
1 Shut down the supply of COD by stopping the influent flow.
2 (If possible: Maintain the recirculation flow rate.)
3 Reduction of the biological activity, the biogas production falls.
4 Shut down biogas production.
The procedure is described in operating procedure Shutting down BIOPAQ® IC reactor in appendix B.
The restart procedure is described in paragraph 4.5.
Biogas production
After the influent has been stopped, the biogas production from readily degradable COD gradually falls
and will finally stop completely. Due to the reduction in the biogas production the mixing of the sludge

bed in the reactor is also reduced. Depending on the type of wastewater the sludge bed may contain a
certain concentration of slowly degradable COD (for example solid matter). When the mixing has been
reduced, but biogas production from this slowly degradable COD is still taking place, the gas lift in the
riser may suddenly start again after many hours (days!) of shut down. This sudden thrust is also called
the ‘belching’ of the reactor. Take this into account when working on the gas/liquid separator. The
same safety measures as during operation should be followed after shut down.
5.5 Major maintenance

Paques recommends a major overhaul on the BIOPAQ® IC reactor every 5 years. Paques personnel or
personnel trained by Paques could do this for you. Take into account that the reactor must always be
empty and clean before any major maintenance can take place.
5.6 Emptying the installation

For any inspections and maintenance it may happen that the BIOPAQ ® IC reactor (or components of it)
must be temporarily empty.
In the BIOPAQ® IC reactor are three manholes that each give access to a section of the reactor. The
first manhole is located in the lower section, the second manhole is below the lower separation module
and the third manhole is approximately two metres below the top of the reactor.
The emptying of the BIOPAQ® IC reactor is described in the operating procedure Emptying of the
reactor in appendix B.
5.7 Dismantling and disposal of the installation

Dismantling and disposal of the installation must be carried out in accordance with the local
environmental regulations. Electrodes, gas Venturi tubes and cuvettes for chemical analyses are
chemical waste and must be disposed of as such.
5.8 Protection against frost

If there is a risk of frost Paques recommends insulating the installation and in addition wrapping the
lines that cannot be emptied with thermal tape (this might have been supplied as an option).
Particularly during shutdown there is a great danger of frost damage.
5.9 Spare parts

Paques recommends that at least one spare pH electrode be kept in stock. If the life of the pH electrode
is considerably shorter than the life specified by the supplier, it is recommended that the electrode be
replaced by a double junction (two chamber) system or the reference electrode be placed outside the
system (diaphragm tube & KCl solution). Paques Services can help you further.

6 Process malfunction and Troubleshooting
6.1 Process malfunction
6.1.1 Acidification of the reactor
‘Acidification of the reactor’ means: The accumulation of VFA in the reactor liquid with a pH of less than
6.5. Possible causes of reactor acidification may be:
 Too low influent pH.
 A sudden temperature decrease.
 Presence of toxic components.
 Insufficient mixing of the sludge bed.
 Too high or too low reactor temperature.
 Too high COD load.
 Nutrients deficit.
 Too low pre-acidification degree.
 Too high solids concentration in the influent.
 Accumulation of solids in the reactor.
Under normal process conditions biogas is formed by the biogas producing bacteria in the granular
sludge from VFA. The optimum pH for this is between 6.5 and 7.5. If the normal process is disrupted,
for example by one of the above causes, the pH in the sludge bed falls below 6.5 and the biogas
production is inhibited and/or the biogas producing bacteria may die.
The acidifying bacteria are less sensitive to low pH values. They remain active down to a pH of 4. So for
pH values of 4.0 and 6.5 the creation of VFA continues, while the breakdown ceases. As a result of this
the VFA will accumulate easily in the reactor liquid.
During acidification there is a chance that the BIOPAQ® IC reactor gets into a vicious cycle (figure 6.1).
Methane producing Poor buffer capacity

capacity exceeded of process water
Poisoning of methane
producing bacteria
VFA concentration increases
increases
Fraction of undissociated
VFA increases
pH falls
Figure 6.1: The vicious cycle of reactor acidification

Immediately after a malfunction or overload, the VFA concentration in the effluent increases. As a
result the biogas production falls and depending on the alkalinity in the reactor, the pH falls and the
carbon dioxide content in the biogas increases. These effects reinforce one another as a result of which
ultimately, if no measures are taken to eliminate the cause, the whole reactor activity comes to a
standstill.
To break the vicious cycle the following measures must be taken:

 Reduce the COD load.
 Increase the influent pH.
As long as the pH of the sludge bed is above 7.0 (preferably around 7.5), a VFA concentration of 10 to
15 meq/l has a slightly negative effect on the biogas producing bacteria.
6.1.2 Blockage of downer

The downer of the BIOPAQ® IC reactor may get blocked with sludge. A blocked downer can be
recognised by the high liquid level in the gas/water separator on top of the BIOPAQ ® IC reactor (see
figure 6.2).
In case of a blocked downer the liquid level in the gas/water separator increases up to the riser. The
water pushed upwards leaves the separator via this riser instead of via the downer. If this situation
occurs for a few minutes the level measurement in the gas/water separator gives a high level alarm,
after which the influent pump stops. Visual inspection of the internal recirculation via the inspection
glasses of gas/water separator remains necessary.
Biogas outlet Setting level measurement
Gland nut
Nitrogen
dosing point A
Inspection glass High water level
Normal water level
Spray water
Downer valve
Nitrogen Biogas line

dosing point B top
separation module
Riser
Downer lower
separation module
Figure 6.2: Normal and high water level indication gas/water separator

A blocked downer results in a malfunction of the internal circulation that has the following
consequences for the sludge:
1. Toxicity may occur because the mixing over the reactor ceases and the sludge is overloaded
with COD.
2. The process water now leaves the gas/water separator via the riser outlet instead of via the
downer. This causes extra turbulence in the upper compartment (further treatment) that may
result in extra sludge wash out.
The downer is unblocked by filling it a couple of times with nitrogen gas and blowing it off with great
force. This method is described in the operating procedure Unblocking downer in appendix B.
Causes of downer blockage

Under normal operating conditions it is unlikely that the downer will get blocked with sludge. Causes of
a blocked downer may be:
Formation of precipitation
Due to salt precipitation (for example calcium carbonate, CaCO3) sludge granules may become
heavy. In the case of precipitation formation, it is recommended that the sludge is regularly
discharged from the lower section of the reactor (using the ‘Sludge output connection’, see
operating procedure Emptying the reactor – Appendix B) to guarantee good mixing in the
reactor. Formation of precipitation on/in the sludge granules is determined by means of
operating procedure Determination of sludge profile (Appendix B).
Too much sludge

Due to biomass growth the sludge volume in the reactor increases in time. Too much sludge
in the bioreactor has a negative effect on the recirculation in the reactor. The quantity of
sludge is determined with the help of the operating procedure Determination of sludge profile
(Appendix B). A surplus of sludge must be removed from the reactor. Part of the sludge is
removed from the reactor according to the operating procedure Emptying the BIOPAQ® IC
reactor (Appendix B).
Low influent flow rate

If the BIOPAQ® IC reactor is operated for long periods with a low influent flow rate (< 50%
design flow rate), the downer may become blocked with sludge. The low influent flow rate
results in a low liquid velocity at the influent nozzles in the mixing section under the sludge
roof. As a result there is insufficient turbulence below the sludge roof and unwanted
accumulation of sludge under the sludge roof. This may ultimately result in accumulation of
sludge in the downer or even a blockage of the downer. A correct setting of the influent
distribution system can prevent blockage of the downer due to a low influent flow rate. This
procedure is described in operating procedure Setting influent distribution system (Appendix
B).
6.1.3 Inhibitors
If, at a constant load, a slow but sure increase of effluent VFAs is observed, there may be an inhibitor
in the influent. This inhibitor affects the activity of the sludge with the result of a slowly deteriorating
situation. An inhibitor may also be present for a very short period, for example due to an unforeseen
discharge.

6.1.4 Wash out of granular sludge
The more granular sludge is washed out, the higher the sludge loading rate for the remaining granular
sludge will be. Possible causes for sludge wash out are:
 Too much grease or oil. These substances may form a thin layer round the sludge granule, as a
result of which the substrate cannot enter the granule and the biogas cannot get out of it.
 The hydraulic load is too high (too high up flow velocity).
 The COD load is too high. The sludge granules cannot let go of the biogas produced quickly
enough and as a result they float.
 Fibres or other solid particles in the influent. These solid particles can attach themselves to the
granule, which results in a reduced settlement velocity.
 The pre-acidification degree in the influent is too high, as a result of which the content of
acidifying bacteria in the sludge granule may be too low. As a result the granules are not so
strong and they disintegrate as time passes.
 Nutrient deficit.
 An increasing VFA concentration in the effluent.
6.2 Troubleshooting
6.2.1 Process Troubleshooting
The troubleshooting instructions have been prepared in accordance with current knowledge. New
insights can result in changes to these procedures.
Process malfunctions that may affect the process parameters, mentioned in section 3, can result in a
reduction in activity of the biomass. In extreme situations the biomass can even be killed.
The reason for the reduction in the biological activity must be identified and resolved. The information
that is given in section 3, 4 and 5 is important for this.
The troubleshooting procedures in appendix C describe different events and measures that can be
taken. It is obvious that these procedures cannot be complete. Only the most probably events are
shown. You can contact Paques Services for advice when you encounter an event not mentioned.
6.2.2 Mechanical troubleshooting

For the mechanical troubleshooting of the various process components please refer to the relevant
operating instructions of the supplier.

7 List of (technical) terms
AEROBIC
There is dissolved oxygen present in the water phase.
ANAEROBIC
There is no dissolved oxygen present in the water phase.
BIOGAS PRODUCTION - [m3/day]

Quantity of biogas that is produced per day.
BOD (Biological Oxygen Demand) - [mg O2/l]

The quantity of oxygen that bacteria need for the biological oxidisation of the oxidisable
substances present in the water. Several standardised procedures exist.
BOD/COD ratio
This ratio is a measure of the biological degradability of a wastewater; readily degradable
wastewater has a BOD/COD ratio of between 0.5 and 0.9.
COD (Chemical Oxygen Demand) - [mg O2/l]

The quantity of oxygen that is necessary for the chemical oxidisation of the oxidisable
substances present in the water.
COD Balance
The anaerobic system must be in balance, i.e. as much COD must enter the reactor (influent) as
leaves it (effluent, biogas and sludge).
CODinfluent = CODeffluent + CODbiogas + CODsludge
COD removal efficiency - [%]

The percentage COD in the influent COD that is removed.
COD load - [kg COD * day -1]

The COD load of an anaerobic reactor is the quantity of COD that enters the reactor per day.
FLOW RATE - [m3/hour or m3/day]

The quantity of wastewater that flows to a particular process component.
EFFLUENT - [m3/hour or m3/day]

The outgoing, treated wastewater.
HYDRAULIC RESIDENCE TIME (HRT) - [hour]

The residence time of the wastewater in the reactor.
IMHOFF SETTLEMENT VOLUME - [ml/l]

The quantity of settlable solids in the wastewater after half an hour of settlement time.

INFLUENT - [m3/hour]
The incoming wastewater.
KJELDAHL NITROGEN (Kj-N) - [mg Kj-N/l]

The total quantity of ammonium and organically bound nitrogen.
MSDS
Material Safety Data Sheet
REACTOR VOLUME - [m3]

The maximum quantity of water that the reactor can hold.
RECIRCULATION - [m3/hour]
The quantity of effluent that is recirculated to the reactor.
SEPARATION MODULE (THREE PHASE SEPARATOR)

In the separation module the wastewater, biogas and granular sludge are separated from one
another.
SLUDGE ACTIVITY - [kg COD * (kg VSS)-1 * day-1]

The quantity of COD that can be converted per day by a quantity of biomass (VSS). The quantity
of biogas produced and the production time are a measure of the sludge activity.
SLUDGE BED VOLUME - [m3]

The volume of sludge that is present in the reactor.
SLUDGE LOADING RATE (SLR, Sludge Loading Rate) - [kg COD * (kg VSS)-1 * day-1]
The quantity of COD per quantity of biomass (VSS) that enters the reactor per day.
SPECIFIC BIOGAS PRODUCTION (SGP) - [m3/kg CODremoved]

The quantity of biogas produced per kg of COD removed.
TSS (Total Suspended Solids) - [mg/l or %]

The quantity of suspended solids in water (so EXCLUDING dissolved substances).
VLR (Volumetric Loading Rate) - [kg COD * m-3reactor * day-1]

The COD load per reactor volume per day.
VFA (Volatile Fatty Acids) - [meq/l]

Acetic acid : CH3 COOH
Propionic acid : C2H5 COOH
Butyric acid : C3H7 COOH
Lactic acid : C2H5OCOOH
An indication that the anaerobic polishing is not functioning well is when butyric acid
contributes significantly to the total VFA (i.e. >5%). Butyric acid can be noticed by its
characteristic odour (sweaty feet).

VSS (Volatile Suspended Solids) – [mg/l or % of TSS (VSS = TSS – ash residue)]
The organic fraction of the TSS. This fraction can be determined by reducing to ashes the
sample from which TSS is determined. The higher the organic content, the higher the activity of
the sludge (more organic material means more bacteria).

Appendices
Appendix A: Specifications
Appendix B: Operating procedures
Appendix C: Troubleshooting

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BIOPAQ®IC

IC-4.0, IC-5.0, IC-5.7, IC-6.5,

Operating & maintenance manual

Project name: Name appears automaticaly if document is made project specific

Report ID: SMAN000028_ENF

Title: Operating & maintenance manual IC Minimum Package

Approved by: WOB

Last issued by: WOB

Issue date: 16-05-2013

Issued by: Paques bv

Contact person: Paques services

6 Process malfunction and Troubleshooting 30

7 List of (technical) terms 34

Specifications, operating instructions and troubleshooting manuals are given in appendices A to C.

For operating or technical support please contact:

Reference: -SMAN000028_ENF 16-05-2013 Page 1 of 37

2.1 Safety at work

Use your common sense regarding safety measures!

An MSDS provides among other things information on:

Reference: -SMAN000028_ENF 16-05-2013 Page 2 of 37

2.3 Sludge and process liquids

2.4 Hazardous gases and vapours

Hydrogen sulphide (H2S)

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 Lower explosion limit (LEL) 4.0 vol. % in air.

2.4.3 Ventilation and chemicals vapours

2.4.4 Hazardous area classification

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During maintenance activities, the critical explosion conditions must be carefully

Maintenance with a LOW chance of unwanted biogas release

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Special risks, concerning the BIOPAQ®IC reactor, are:

2.5 Working at a height

2.6 Working in confined spaces

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2.8.1 Shutting down the installation

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3.1 BIOPAQ® IC reactor

Figure 3.1: BIOPAQ® IC reactor Figure 3.2: BIOPAQ® IC separation module

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Higher COD load.

Mixing section (1)

Expanded sludge bed (2)

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Gas/liquid separator (5)

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3.2 Biogas treatment

3.2.1 Biogas flow metering

3.2.2 Condensate separation

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3.2.5 Gas flare

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3.4.1 Nitrite & nitrate

3.4.2 Sulphite & sulphate

3.4.3 Fats, oils & greases (FOG)

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Figure 3.8: (Sliced) BIOPAQ® IC granular sludge

The BIOPAQ®ICC reactor may be damaged internally if it is operated with excess or

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Figure 3.9: COD fraction distribution in wastewater

3.5.3 COD load and volatile fatty acid concentration

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3.5.5 Specific biogas production