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ANAEROBIC DIGESTION OF AGRO-INDUSTRIAL WASTES: INFORMATION NETWORKS Technical Summary on Gas Treatment

AD-NETT Project FAIR-CT96-2083 (DG12-SSMI)

FINAL VERSION

August 2000

Barbarossastraat 35 P.O. Box 151 6500 AD NIJMEGEN 00 31 24 328 42 84 00 31 24 323 93 46

ANAEROBIC DIGESTION OF AGRO-INDUSTRIAL WASTES: INFORMATION NETWORKS Technical Summary on Gas Treatment

AD-NETT Project FAIR-CT96-2083 (DG12-SSMI)

FINAL VERSION

Prepared by Approved by

: ir. A.H.H.M. Schomaker, ing. A.A.M. Boerboom, Dr. ir. A. Visser, ing. A.E. Pfeifer (Novem) : ir. A.H.H.M. Schomaker Initials:

Our reference: H0489.A0/R002/TS/GR

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AD-NETT Project FAIR-CT96-2083 (DG12-SSMI) Technical Summary on Gas Treatment

DISCLAIMER Contract number: 355299/4010 This project is cofunded by the Dutch energy from waste biomass program (EWAB). Control and co-ordination of the EWAB program are at: Novem Catharijnesingel 59 PO Box 8424 3503 RE Utrecht The Netherlands telephone : +31-30-239.36.31 telefax : +31-30-231.64.91 The project has been executed by: HASKONING Consulting Engineers and Architects PO Box 151 6500 AD Nijmegen Date of report: August 1999

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CONTENTS Page ABSTRACT 1. INTRODUCTION 1.1 AD-NETT 1.2 Anaerobic digestion 1.3 Gas treatment BIOGAS COMPOSITION 2.1 Biogas components 2.2 Biogas composition STANDARDS ON GAS QUALITY AND EMISSIONS 3.1 Standards applicable gas quality for biogas utilisation. 3.2 Standards applicable on flaring of biogas 3.3 Standard emission for biogas fuelled internal combustion engines TREATMENT OF RAW BIOGAS 4.1 Introduction 4.2 Removal of water 4.3 Removal of H2S 4.4 Special gas engine lubricants 4.5 Removal of dust 4.6 Removal of CO2 TREATMENT OF FLUE GAS 5.1 Lean burn engines 5.2 DeNOx systems UPGRADING OF BIOGAS 6.1 Pressure Swing Adsorption (PSA) 6.2 Membrane separation 6.3 Physical (water, methanol) or chemical CO2 -absorption techniques 6.4 Evaluation of CO2 removal techniques CONCLUSIONS 1 3 3 3 5 7 7 8 9 9 10 11 13 13 14 15 18 18 18 19 19 19 21 21 22 22 23 24 25 27

2.

3.

4.

5.

6.

7.

REFERENCES SUPPLIERS OF GAS TREATMENT EQUIPMENT

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ABSTRACT This technical summary on gas treatment in relation to anaerobic digestion (AD) deals with the treatment processes for biogas in all stages of AD. Three major topics are discussed: the treatment of raw biogas in order to produce a biogas quality which is according to the required standards for driving gas engines or gas fired boilers; the treatment of flue gasses produced by gas engines or gas fired boilers in order to meet the emissions standards in a certain country; the upgrading of biogas to natural gas quality or a required synthesis gas quality by the removing of macro components like CO2. The context for the discussion of these three topics is presented in the first three chapters of this technical summary. Chapter 1 presents a short introduction of the AD-NETT context; the basic technology of anaerobic digestion; the topic of gas treatment with the identification of the three main concepts i.e. treatment of raw biogas, treatment of flue gas and the upgrading of biogas; the principles of gas treatment i.e. removal or conversion, application of additives, catalysts, bacteria or based on a physical principle; identification of specific elements in AD and gas treatment i.e. scale (small, big) and budget (low, high), ease of operation, ease of monitoring, ease of maintenance, fail safety, production of hazardous or toxic pollutants. Chapter 2 gives a review on the composition of biogas. The description of the composition concerns: available components in the biogas; treatment objectives for specific components i.e. reduction of toxicity, acidification, harmfulness for equipment or compliance with emission standards; effect of the digester feed and the AD-process itself on the composition of the biogas; variation of the biogas composition under normal operating conditions. In chapter 3 the emission standards dealing with AD in the countries participating in the AD-NETT are discussed. First of all the policy and intentions of the European Community and the available standards are presented. Furthermore attention is paid to: emission of components which have high priority in reduction; standards in relation to biogas flaring; standards in relation to biogas utilisation in gas engines, gas boilers or in relation to the delivery of upgraded biogas to the natural gas grid. Chapter 4 focuses on the treatment of the raw biogas in the form as the digester produces it. Attention will be given to: the removal of water; the reduction of H2S by aerobic bacteria;
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wet gas treatment systems; gas treatment by utilising special gas engine lubricants; removal of dust particles.

In chapter 5 the possibilities for treatment of the flue gasses that are formed by the gas engine or gas boilerare reviewed. In this respect flue gasses are those specifically generated from: lean burn gas engines; catalytic and non-catalytic DeNOx systems. Chapter 6 deals with the possibilities to upgrade biogas to a quality required by the natural gas grid. Upgrading techniques discussed are: membrane separation; wet treatment; active carbon; pressure swing adsorption. In chapter 7 conclusions on the maturity of gas treatment for AD are presented based on the present state of the art. Chapter 8 presents a list of the main literature references with short descriptions of the scope of each reference and relevant ordering information. In this chapter an overview is given of the main suppliers of gas treatment equipment.

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1. 1.1

INTRODUCTION AD-NETT AD-NETT is a network of professionals working in anaerobic digestion (AD) of agro-industrial wastes in Europe and Canada. AD-NETT is sponsored by the EC FAIR programme in the EU and by national programmes in Switzerland and Canada. The network began in January 1997 and will continue to December 1999. The prime motive of AD-NETT is to enable exchange of information and experience and to disseminate this information to relevant organisations, such as potential users and developers. In this respect AD-NETT publishes amongst others on its Internet site http://www.ad-nett.org - news on developments in the network, information about technical developments on AD and reports from databases of plant and contacts. AD-NETT aims to examine and compare successes and failures of the world wide application of AD technology in order to gain from past experience and to pass this information on to potential users of the technology. The information presented in this report is restricted to the application of AD for treatment of agro-industrial wastes, although many of the gas treatment techniques described are also suited for anaerobic wastewater treatment, treatment of landfill gas, and digestion of VGF and other organic waste streams. The technical summary on gastreatment is the Dutch contribution to the ADNett, and was prepared by HASKONING, a Dutch engineering and consultancy firm, in close co-operation with Novem, the Dutch Agency for Energy and the Environment.

1.2

Anaerobic digestion AD is applied in particular in the agricultural sector all over the world in the form of small on-farm digesters producing biogas to heat farmhouses, dairies and other farm buildings. Larger scale centralised anaerobic digesters (Centralised AD) have also been developed, using feedstock imported from a number of sources, specifically residues from livestock farming (such as dairy, beef and pig slurry, or poultry litter) and the food processing industries (including vegetable preparation and dairy food processing). Figure 1 presents a basic layout of an AD-plant. Anaerobic digesters produce conditions that encourage the natural breakdown of organic matter by bacteria in the absence of air-oxygen. Figure 2 shows the degradation routes in the AD-process, during which organic material is converted by various types of micro-organisms into methane (CH4) and carbon dioxide (CO2), the main components of the biogas |ref 1|.

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Fe e ds tock

St orage and pre -tre atm ent (m ixing, s cre e ning)

D ige s te r

Biogas s torage

D ige s tate

Biogas claning e

Engine t urbine

Gas burne r boilr e

Upgrading (natural gas)

Fl gas claning ue e Fl gas ue Gas tre atm ent te ch niq ue s re v w e d ie

Fl gas claning ue e Fl gas ue Natural gas

Figure 1: PRO CESS

Basic Layout of an AD-plant M A TERI L A


PARTI CUL TE O RGA NI M A TERI L A C A
P TEI RO NS CARBO H Y D RATES LPD S II

BACTERI A

H ydrol ysis AMI NO A CI / SUGARS DS Fe rm e ntation (acidoge ne s is ) FA TTY ACI DS Fe rm e ntation (ace toge ne s is ) ACETA TE / H YDROGEN M e th anoge ne s is M ETH A NE / CARBO ND I XI E O D

L ytic, prote ol ipol ytic and ce l ytic bacte ria l ul

Fe rm e ntativ bate ria e

H ydroge n producing bacte ria

M e th anoge nic bacte ria

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Figure 2:

Anaerobic conversion of organic material into biogas.

In addition to CH4 and CO2 other volatile components like hydrogen sulphide (H2S) and ammonia (NH3) are also formed by the mineralisation of organic material during the AD-process and will finally end up in the biogas in small amounts. 1.3 Gas treatment At the site of the AD plant two gas streams are produced that need treatment: biogas and flue gas. Biogas is produced as an end product in anaerobic digesters and is normally stored and utilised on site. Storage can be done in different types of storage facilities like: a water sealed, floating gas holder; a gas bag; the digester head space with a foil membrane; a separate gas tank for high-pressure storage. Gas engines or gas boilers produce flue gas. In order to meet emission standards applicable in a certain country flue gas treatment is needed. In this report the following concepts of gas treatment are reviewed: The treatment of the raw biogas as it is produced in anaerobic digesters in order to protect storage facilities or to make the gas suitable for gas engines or gas fired boilers. The treatment of the biogas focussed on upgrading the biogas to a natural gas quality or a required synthesis gas quality. The treatment of the flue gasses that are produced by gas engines or gas fired boilers in order to meet emission standards in a certain country. The various treatment techniques that are considered in this report are based on one of the following principles: removal of certain constituents of the biogas; conversion of certain constituents of the biogas into other, non or less harmful components. Table 1 lists the techniques that can be used for the treatment of biogas in relation to the compound to be removed. If relevant, specific elements in AD and gas treatment like scale and budget (high, low) of the plant, ease of operation, ease of monitoring, ease of maintenance, fail safes and the production of hazardous or toxic pollutants are included. Table 2 lists the importance of such parameters in relation to the size of the AD-plant. From table 2 it is clear that for small scale AD-plants the treatment technique to be considered should be a low-budget reliable technique that is easy to operate, monitor and maintain. These demands have implications on the type of treatment that can be applied and the possible end-use of the biogas. Table 3 shows these possibilities for using biogas in AD-plants.
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Table 1:

Overview of techniques used for biogas treatment


TECHNIQUE Demister Cyclone separator Moisture trap Water tap Adsorption to silica Glycol drying unit Air oxygen dosing FeCl3 dosing to digester slurry Adsorption to Fe2O3 pellets Absorption with caustic solution Absorption with iron solution Absorption closed loop systems Membrane separation Biological filters Activated carbon Molecular sieves Pressure swing adsorption Membrane separation Absorption techniques PRINCIPLE physical physical physical physical physical physical biological chemical physical-chemical physical-chemical physical-chemical physical-chemical physical biological physical-chemical physical physical-chemical physical physical-chemical

COMPOUND REMOVED Water

H2S

CO2

Table 2:

Importance of gas treatment aspects in relation to the size of the AD-plant (+ = important, - = less important)

PARAMETER SMALL SCALE AD-PLANT1) LARGE SCALE AD-PLANT2) Low budget + +/Ease of operation + +/Unattended operation + Ease of monitoring + Ease of maintenance + +/Safety standards + + Health standards + + 1) AD-plant with capacity lower than 5.000 tons feedstock per year (arbitrarily set) 2) AD-plant with capacity higher than 5.000 tons feedstock per year (arbitrarily set)

Table 3:

Possible application of biogas in relation to the size of the ADplant (+ = yes, - = no)

END-USE SMALL SCALE PLANTS1) LARGE SCALE PLANTS2) Direct gas use (e.g. heating) + + Production electricity +/+ Combined heat power generation + Upgrading to natural gas + 1) AD-plant with capacity lower than 5.000 tons feedstock per year (arbitrarily set) 2) AD-plant with capacity higher than 5.000 tons feedstock per year (arbitrarily set)

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2. 2.1

BIOGAS COMPOSITION Biogas components Biogas produced in AD plants is primarily composed of methane (CH4) and carbon dioxide (CO2), with smaller amounts of hydrogen sulphide (H2S) and ammonia (NH3). Slight concentrations of hydrogen (H2), nitrogen (N2), carbon monoxide (CO) and oxygen (O2) are occasionally present in the biogas. Finally the biogas is usually saturated with water and might contain dust particles. The properties of the main gas components mentioned above are outlined below: CH4 gas is considered as a valuable fuel. The gas is non-toxic, non-smelling, and is lighter than air. When burned CH4 is converted into a molar equivalent amount of CO2 and water. CO2 is an inert colourless, odourless gas and is heavier than air. CO2 is mildly toxic, is an asphyxiant and has an occupational exposure standard (OES) of 5.000 ppm. A higher CO2 concentration in the biogas results in a lower calorific value of the biogas. H2S is a colourless gas. Since H2S is heavier than air, it might cause extra danger at low levels. At low concentrations this gas has the typical smell of rotten eggs. At higher, more dangerous concentrations is has no smell. Due to its toxic properties hydrogen sulphide has an OES of 10 ppm. In addition to its toxicity H2S is corrosive which can cause problems during combustion of the biogas. When burned the H2S in the gas is converted into SO2, also a toxic product, which can cause acidification. NH3 is a pungent and lachrymatory gas that is lighter than air. The OES is 10 ppm. When burned in a flare or a gas engine, NOx-products are formed. Normally, NH3 concentrations in the biogas are rather low. Water vapour, although a harmless product, becomes corrosive in combination with the NH3, CO2 and especially the H2S of the biogas. The maximum water content of the biogas is governed by the gas temperature. When water saturated biogas leaves the digester, cooling of the gas will result in condensation of water. In view of the properties of the main biogas components listed above, treatment of biogas will often be required. The treatment is commonly focussed on: Removal of water, which is needed because of potential accumulation of moisture in equipment in the gasline, the formation of a corrosive acidic solution when water is combined with H2S and in order to create optimal conditions for the end-use of the biogas. Removal of H2S, which is required because it is toxic, corrosive and since it can damage gas-equipment. The H2S concentration in the gas should be kept below the recommendations of the manufacturer of the equipment used. Furthermore, burning of biogas results in the oxidation of H2S to SO2. In order to comply with environmental regulations for SO2 emissions the H2S level in the biogas should be kept sufficiently low. Removal of CO2 will be required if the biogas needs to be upgraded to the quality of natural gas (in terms of Wobbe-index, corrosion, etc).

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2.2

Biogas composition The biogas production and composition in AD-plants is dependent on the type of feedstock and the operational parameters used in the digestion process. The feedstocks used for anaerobic digestion vary considerably in composition, homogeneity and biodegradability. Table 4 shows some characteristics and operational parameters for different agricultural feedstocks. Table 4: Characteristics and operational parameters for different agricultural feedstocks |ref. 2|.
TOTAL SOLIDS (TS), % 3-8 5-12 10-30 60-70 15-20 10 VOLATILE SOLIDS (VS), % of TS 70-80 75-85 70-80 90 75 80 BIOGAS YIELD, m3/Kg VS added 0.25-0.50 0.20-0.30 0.35-0.60 0.20-0.50 0.25-0.50 0.50-0.60 METHANE CONTENT, VOL. % 70-80 55-75 60-80 n.a. n.a. 70-80 RETENTION TIME, days 20-40 20-30 > 30 8-30 8-20 10-20

FEEDSTOCK

Pig slurry Cow slurry Chicken slurry Garden waste Fruit waste Food remains

Tables 5 show a comparison between biogas from an average AD plant and natural gas. Table 5: Composition of biogas from an AD-plant and natural gas in the Netherlands |ref. 3, 4|.
DIMENSION vol-% vol-% vol-% vol-% vol-% vol-% vol-% mg/m3 mg/m3 -MJ/m3 MJ/m3 NATURAL GAS 85 0,89 2,85 0,37 0,14 14,35 < 0,5 <5 --dew point at 10C 32-35 40-44 BIOGAS 55-70 30-45 ----------0-15.000 0-450 saturated 20-28 20-30

COMPONENT CH4 CO2 C2H6 C3H8 C4H10 N2 O2 H2S NH3 Humidity Caloric value, lower-upper Wobbe index, lower-upper

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3. 3.1

STANDARDS ON GAS QUALITY AND EMISSIONS Standards applicable gas quality for biogas utilisation. The biogas as produced in AD plants can be used for several purposes: direct-gas use; fuel for an engine connected to a generator to produce electricity; combined heat and power generation; upgrade of biogas to natural gas quality to run motor vehicle engines or to supply to the local gas net (pipeline or substitute natural gas quality). In the case of direct-gas use water and H2S removal will be the appropriate treatment steps. If the gas is to be used by gas engines, or if it is upgraded to a natural gas quality, the biogas composition should comply with the appropriate requirements. Table 6 list typical requirements for gas engines. Table 6: Typical requirements for gas engines |ref. 3|.
DIMENSION MJ/m3 MJ/m3 C mbar % mg/m3 mg/m3 RANGE 13-21 0-2 40-60 25-80 < 70-80 < 1000-2000 < 60-80

COMPONENT Energy content Variation in energy content Maximum temperature feed Minimum delivery pressure Humidity biogas H2S Chloride and Fluor (total)

For upgrading biogas to natural gas quality removal of CO2, H2S, NH3, water and dust is essential in order to achieve the required quality. Table 7 lists the required gas quality in order to be used as natural gas substitute in the Netherlands. At the moment no European standard has been defined, but it can be assumed that differences in the European countries will be small. Table 7: Typical requirements for biogas to be injected in natural gas line applicable the Netherlands |ref. 3|.
DIMENSION MJ/m3 MJ/m3 mg/m3 C VALUE 34,7-34,9 43,5-44,4 <5 - 35

PARAMETER Caloric value Wobbe-index H2S H2O (dew point at 1 bar)

For utilisation of biogas as vehicle fuels the same upgrade technique is used as for natural gas. In practice the upgrading of biogas up to vehicle fuel quality involves removal of CO2, H2S, NH3, particles and water. The methane contents should be at least 95 % |ref. 5|. Quality requirements for vehicle fuel of biogas are different in different countries.

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3.2

Standards applicable on flaring of biogas If biogas utilisation is not possible, biogas combustion with flares is required, since direct emission of the biogas into open air is prohibited for safety and health reasons. Guidelines in the Netherlands In the Dutch emission guidance (NER 3.5/90.1) the following restrictions for permanent flares are mentioned: the outlet temperature of the flue gas has to be at least 900 C; the residence time in the flare has to be at least 0.3 seconds; the flare has to be of the closed type(no visible flame). However, if flares are only being used during periods of maintenance (of utilisation equipment), the use of a simple open or half-open flare is allowed. The maximum limit of H2S and other organosulphur compounds in the biogas to be flared is 50 ppm. If this limit is exceeded, sulphur has to be removed from the biogas with a sulphur removal to this limit of 50 ppm or a removal efficiency of at least 98 %. To prevent the formation of dioxins, the halogenated hydrocarbons content has to be lower than approximately 150 mg/m3. Guidelines in other countries At present there is no European guideline regarding standards for the flaring of biogas. Based on the information available at this stage it seems that in many European countries specific rules for the flaring of biogas do not exist. For example: Denmark, Spain, Austria, the United-Kingdom and Italy do not have any regulating rules for flaring of biogas. In countries that do have emission standard, there can be considerable differences. Table 8 shows the standards on emission control on landfill gas flares in Germany and Switzerland. In addition the recommended values for the United Kingdom are shown. Table 8 Emission controls on landfill gas flares based on the German TAluft regulations, the Swiss regulations and the recommendations used in the United Kingdom |ref 6|.
GUIDELINES UK 50 150 10 ------------TA LUFT GERMANY 50 200 10 10 50 30 0.05 0.05 0.18 SWISS 60 80 20 20 50 20 0.1 0.1 --DIMENSIONS mg/m3 mg/m3 mg/m3 mg/m3 mg/m3 mg/m3 mg/m3 mg/m3 ng/m3

Carbon monoxide Nitrogen oxides Unburned hydrocarbons Dust SO2 HCl Cd Hg Dioxins and furans (TEQ)

Furthermore it is expected that in the near future the use of open flares will be limited and that flaring of biogas will be restricted to enclosed flares in the UK.

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3.3

Standard emission for biogas fuelled internal combustion engines Guidelines in the Netherlands In the Netherlands, the emission of NOx in exhaust gasses of biogas fuelled internal combustion engines is restricted |ref. 7|: new engines < 50 kW: 800 g NOx/GJ * 1/30 of the engine efficiency; new engines > 50 kW and < 50 MW: 140 g NOx/GJ * 1/30 of the engine efficiency. This means that if the engine efficiency increases, higher emissions are accepted. The engine efficiency is the percentage of power (energy) output that can be obtained from the energy input. Guidelines in other countries There can be considerable differences in the regulations between the different European countries. In addition to the restrictions for emission during biogascombustion used in the Netherlands, the standards as applied in Spain, Denmark, Italy and Austria are given as examples for the various regulations and standards which are applied within Europe. Austria Table 9 gives the data regarding emission restriction during the combustion of biogas as applied in Austria. The emission restriction are based on: - Lufteinhaltverordnug fr Kesselanlagen BGBI Nr. 19/1989 idgf(LVR-K); - Deutsche Technische Anleitung zur Reinhaltung der Luft (TA-Luft 1986) |ref 8 |; - Richtlinienvorschlages Entgasung von Deponiekrpern der WAV (WAV, 1997) |ref 9 |. Table 9: Maximal emission values as applied in Austria based on the LVRK, TA-Luft 1986, and WAV 1997.
LVR-K1) 50 100 30 0,7 5 1 0,1 0,1 20 0,1 0,002 11 TA-LUFT 19862) 5 200 500 100 20 5 5 1 0,2 0,2 5 3 WAV 1997 < 2.000 m3/h > 2.000 m3/h 5 5 200 100 100 100 100 20 20 5 5 5 5 1 1 0,1 0,1 0,1 0,1 20 20 0,1 0,1 0,002 0,002 5 5 3 3 DIMENSION mg/m3 mg/m3 mg/m3 mg/m3 mg/m3 mg/m3 mg/m3 mg/m3 mg/m3 mg/m3 mg/m3 ng/m3 mg/m3 %

PARAMETER Dust NOx SO2 CO HCl HF Pb, Zn, Cr As, Co, Ni Cd Hg Total organic carbon PCDD/PCDF CO:CO2 H2S O2 content
1)

small plants, 2) landfill gas

Denmark
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Danish regulations are focussed on natural gas and natural gas fuelled engines. For engines > 120 kW the following restrictions exist |ref 10 |: - NOx 550 mg/Nm3 - CO 500 mg/Nm3 - unburned carbonhydrogens 1500 mg/Nm3 with 30 % electric efficiency Biogas is not specifically mentioned in the regulations in Denmark. Spain In Spain there are no strict regulations regarding NOx emission standards during combustion with gas engines using natural gas or biogas. Other more general regulations regarding diverse industrial activities give some tentative guidelines regarding emission standards. These guidelines are |ref 11 |: - SO2 4300 mg/m3 - NOx 615 mg/m3 (measured as NO2) - CO 625 mg/m3 Italy In Italy a number of regulations exist regarding anaerobic digestions systems and biogas utilisation. Table lists 10 emission standards as defined in Italy. Table 10: Conditions for biogas-utilisation and maximal emission standards for the combustion of biogas as applied in Italy |ref 12|.
AVERAGE DAILY 10 200 50 10 1 10 AVERAGE 30 Minutes 10-30 100 10-60 2-4 AVERAGE 1 hour 0.05 0.5 UNIT mg/m3 mg/m3 mg/m3 mg/m3 mg/m3 mg/m3 mg/m3 mg/m3 mg/m3

PAREMETER Dust NOx SO2 CO HCl HF Cd, Ti Hg Total organic carbon

When evaluating the regulations in the different countries it is seen that there is a considerable variation. To our knowledge, at present there is not yet a standard European guideline or European regulation. When applying anaerobic digestion one should check local and national regulations and legislation.

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4. 4.1

TREATMENT OF RAW BIOGAS Introduction The raw biogas produced in a digester is normally treated in order to remove water, H2S, dust and/or CO2. The choice of the cleaning method employed and the compound to be removed depends on the type of end use of the gas. Table 10 shows the compound(s) of the biogas that needs to be removed in relation to the end-use of the gas. Table 11: Removal of specific compounds present in biogas, in relation to the gas utilisation (+ = yes, - = no).
BIOGAS UTILISATION Direct heating (gas boilers/burners) Electricity (gas engine) Upgrade for natural gas
1) 2)

WATER + + +

H2S +1) +1) +

DUST + + +

CO2 +/-2) +

removal required if input limits are exceeded dependent of CO2 content biogas and manufacturers specification.

The treatment methods for the removal of water, H2S and dust are reviewed below. The more sophisticated removal methods for CO2 are discussed in detail in chapter 6 that deals with biogas upgrading techniques to natural gas quality. Figure 3 show the different removal techniques which will be discussed in more detail in the chapter.

DI GESTER

Re m ov of w ate r, foam al and dust

Re m ov al of H 2S

Re m ov al of CO 2

Spe cific re m ov of dust al

Figure 3

Treatment techniques for biogas.

Removal of water and foam is always needed for the prevention of corrosion in the biogas line. At present very simple and cheap methods exist that will remove water in sufficient quantities. Water removal is normally accomplished with the removal of foam and dust. If the biogas is to be used removal of H2S is needed in most cases. CO2 removal and specific methods for the removal of dust is only need when a high quality gas is required. This can be the case when the biogas is to be used as a substitute for natural gas or when sensitive equipment is used.

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4.2

Removal of water In AD plant technology the removal methods for water are commonly based on separation of condensed water or gas drying. In addition to water also other impurities in the biogas such as foam and dust are removed. Condensation methods Methods employed using separation of condensed water are based on the principal that water droplets are caught or entrapped and subsequently removed. The removal can be either manually or automatic. Techniques using separation of condensed water include the application of: demisters, in which liquid particles are separated with a wired mesh (micro pores); cyclone separators, in which water drop(let)s are separated using centrifugal forces equal to several hundred gravities; moisture traps, in which condensation of water by expansion of the biogas takes place; water taps in the gaspipe, from which condensed water from the biogas can be removed from the gas. Of the methods mentioned above the simplest method is based on using water taps in the gas-pipe. Normally this will give a sufficient removal of water for the gas to be used in gasengines. Drying methods Methods based on gas drying include: Cooling of the gas and leading it through a demister with micro pores (cool dryer) When the gas is cooled the gas becomes over-saturated with water. Dew points of 20 tot 2 can be reached. As a result, condensation of the water C in the gas occurs. The condensed water is entrapped in a demister. In order to have a high efficiency the demister is equipped with micro pores. Adsorption of the gas to silica (adsorption dryer) Using adsorption dryers a high removal of water can be achieved. The gas is led through a column filled with silica in which dew points of -10 tot -20 C can be reached. Usually two columns are used simultaneously: one column for adsorption of water, while the other is regenerated in that stage. Regeneration can be done by evaporation of the water by heating. As alternatives for silica also activated carbon or molecular sieves can be used for this drying process.

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Project FAIR-CT96-2083 (DG12-SSMI)

Glycol drying unit (glycol dryer) Drying takes place using tri-ethylene-glycol (a water binding component). Dew points of -5 tot -15 can be reached. Used glycol is pumped into a reC generation unit, where regeneration takes place with a temperature of 200 C.

Removal of water is essential in preventing potential accumulation of moisture in equipment installed and the formation of a corrosive acidic solution. However, as indicated in paragraph 1.3 and tables 2 and 3 the appropriate technique is strongly dependent on the size of the AD-plant and the end-use of the gas. For small scale AD-plants water removal techniques are limited to the application of moisture traps or water taps in the gas line. These methods are commonly used and are sufficient for using of gas in gas-engines. The other techniques mentioned are not justified economically or do not fulfil the criteria mentioned in tables 2 and 3. Only if the objective of the biogas treatment is upgrading to a natural gas or vehicle fuel quality, water removal based on drying methods can be considered. 4.3 Removal of H2S A number of techniques have been developed over the years for the removal of H2S from the biogas. These techniques are outlined in this section. Air/oxygen dosing to the biogas system This technique is based on the biological aerobic oxidation of H2S to elemental sulphur by a group a specialised micro-organisms. In order to have the bacteria developed in the biogas system, liquid-manure-wetted surface is required. The following reaction occurs in the biogas: 2 H2S + O2 2 S + 2 H2O The small amount of oxygen (approximately 5 %) required in this method is introduced in the biogas system e.g. by using an air pump. As a result the sulphide in the biogas is oxidised into sulphur and the H2S concentration of the biogas is lowered. The results obtained with this method to date are very promising. A reduction of H2Slevels down to 20-100 ppm H2S which equals 30- 150 mg/m3 H2S, and removal efficiencies of H2S between 80-99 % have been achieved |ref. 13|. The H2S removal obtained with this method is sufficient for a direct use of biogas in gas-engines. On the other hand, the H2S concentration remains too high for the use of biogas as a substitute of natural gas. The major advantages of this removal method are: Investment and exploitation costs are very low compared with other H2S removal methods. Operation, monitoring, maintenance and unattended operation are very easy to realise. No special chemicals or equipment are required.

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Project FAIR-CT96-2083 (DG12-SSMI)

Addition of iron chloride to the digester slurry This technique is based on the formation of insoluble iron sulphide salts in the digester slurry. The precipitation reaction of the iron salt can be written as: 2 Fe3+ + 3 S2- 2 FeS + S Due to the precipitate formed stripping of H2S to the biogas is prevented. The method is very effective in reducing high H2S levels. A reduction of H2S concentrations in the biogas down to 100 ppm has been achieved. The major advantages of this method are: Operation and exploitation costs are low. Operation, monitoring, maintenance and unattended operation is easy to realise. H2S is prevented from being transferred to the biogas, so no part of the gas line, including the part prior to a biogas treatment, is brought in contact with the H2S. Adsorption using iron oxide pellets In this technique, in which the gas is led through a box of pellets, the iron oxide pellets reacts with the H2S in the biogas according to the following reaction: Fe2O3 + 3 H2S Fe2S3 + 3 H2O Regeneration of the iron pellets is done with oxygen: 2 Fe2S3 + 3 O2 2 Fe2O3 + 6 S Normally two boxes of pellets are installed in the gasline. One box is loaded whereas the other is regenerated. When the iron pellets are completely covered with sulphur the pellets are replaced. Adsorption using iron boxes is a simple, cheap and easy to operate and maintain method in which high removal efficiencies can be obtained. The disadvantages of the method are: the great amount of heat released during the regeneration, dust of the packing can be toxic and the method is sensitive for a high water content of the biogas. Absorption with liquids In this method we can distinguish physical and chemical absorption processes. In physical absorption H2S is removed by absorption of H2S in water or organic solvents. Due to high consumption of water or high cost associated with regeneration of the liquid this method is not suitable for use in AD plants. By adding chemicals to the water the absorption process can be greatly enhanced resulting in a chemical absorption process. We can distinguish the following options of chemical absorption of H2S: Chemical absorption with a diluted sodium hydroxide (NaOH) solution. The NaOH reacts with hydrogen sulphide to form sodium sulphide or sodium hydrogen sulphide. The sodium salts, which are formed, have to be disposed of and the method is not regenerative.
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AD-NETT Technical Summary on Gas Treatment

Project FAIR-CT96-2083 (DG12-SSMI)

Chemical absorption with iron salts solution. In this process an iron chloride solution is used. The process is based on the formation of insoluble precipitates that needs to be removed. Chemical absorption using closed systems. In closed systems the absorption phase is followed by regeneration. An example is the Gluud-process. In this process, H2S is removed using iron(III)hydroxide resulting in the formation of Fe2S3 . Regeneration is done with oxygen-air. Another example is the direct formation of elemental sulphur using an iron(III)chloride solution. By adding complexing chemicals the formation of FeS or Fe(OH)3 is prevented. Regeneration again is done with oxygen-air.

The physical and chemical absorption processes mentioned above in general have the disadvantage of a relative high consumption of water and/or chemicals, which makes the method less attractive for small-scale AD-plants. For large-scale AD-plants the method may become economically more feasible. Other methods Other methods that can be used include: Membrane separation. H2S can be separated from the gas using a semipermeable membrane. In this process the biogas is led through a membrane. H2S can pass the membrane whereas CH4 and CO2 cannot pass the membrane. Biological treatment. Biological treatment methods are based on using specific bacteria that are able to oxidise the H2S. In this method the biogas is led through a special biological filter. In this filter H2S is in a first step absorbed to a liquid phase and subsequently oxidised by the bacteria present in the filter. Activated carbon processes. Application of molecular sieves. Evaluation of H2S removal techniques Table 12 shows a comparison between the different techniques for H2S removal. Table 12 illustrates clearly that air dosing or FeCl3 dosing are the best solutions to remove H2S, especially for small-scale low budget AD plants. However, when a natural gas quality is needed, techniques like chemical absorption have to be applied, In this case H2S removal is normally combined with CO2 removal.

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Project FAIR-CT96-2083 (DG12-SSMI)

Table 12: Comparison of different available H2S removal techniques


REMOVAL TECHNIQUE Air dosing FeCl3 dosing Fe2O3 pellets Chemical absorption using caustic Chemical absorption using iron solution Chemical absorption based on closed loop system Membrane separation Biological treatment Activated carbon Molecular sieve 1. Application on small scale (+ = yes) 2. Application on large scale (+ = yes) 3. Simplicity (+ = simple) 4. operation and maintenance (+ = little) + + + +/+/+/1 + + + + + + +/+/+/2 + + + +/+/+/+/+/+-/ 3 + + +-/ +/+/+/+/+/+/4 5 + + + + + + + + + + + + +/+/+/+/+ + +/+/6 + +/+/+/+/+/+/+/7 ++

5. H2S treated gas < 250 ppm (+ = yes) 6. environmental impact (+ = low) 7. costs (+ = low)

4.4

Special gas engine lubricants Special gas engine lubricants are available that can deal with a relatively large amount of contaminants, and research is on going. Engine suppliers are well known with the different types of lubricants. The choice of the type of lubricant depends mainly on the biogas quality and combustion conditions, which are both specific for feedstock and location. If this information is known, a choice can be made. Other factors to be considered include the frequency of lubricant analyses and maintenance.

4.5

Removal of dust As mentioned in paragraph 4.1 removal of water is accomplished with dust removal. Normally the dust removed in this way is sufficient. Only if the gas is used in sensitive equipment additional specific dust removal is required. If specific dust removal is needed, dust filters have to be used. For this purpose air filter type filters are needed and are often placed before regulator valves or gas utilisation equipment. To prevent dust filters from clogging, the gas must be free of any oil or water droplets. Dust filters must therefore be placed behind the condensation traps and oil separators. The use of dust filters has consequences for the choice of extraction machines, due to pressure losses. As mentioned in paragraph 1.3 and tables 2 and 3 the appropriate technique is strongly dependent on the size of the AD-plant and the end-use of the gas. This means that dust removal will only be considered for large-scale AD plants.

4.6

Removal of CO2 As indicated in the introduction of this chapter ( 4.1) treatment techniques for the removal of CO2 are reviewed in chapter 6.

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5. 5.1

TREATMENT OF FLUE GAS Lean burn engines The emission of flue gas from internal combustion (IC) engines can be controlled using lean burn engines. Lean burn engines use a lambda sonde, which measures the oxygen contents of the exhaust gas. With this information the oxygen inlet, and in this way the oxygen-fuel mixture, is regulated. The lambda control regulation results in optimal combustion conditions and low NOx emission. The lambda sonde occasionally causes problems. Due to contaminants in the biogas, the lambda sonde gets contaminated after a while, and gives inaccurate results. Minimising the lambda (richer fuel mixture) causes a low NOx emission, but results in an undesired increase of CO and hydrocarbons emission, and results in lower engine efficiency. A high lambda (lean mixture) leads generally to a low NOx emission too. Frequent maintenance is therefore necessary to keep the lambda sonde and engine in optimal condition and to fulfil the required emission standards. Replacement of the oxygen measurement device is required at least every year.

5.2

DeNOx systems DeNOx can take place by the use of non-catalytic and catalytic systems. The systems described in this paragraph are usually applied at waste incineration plants |ref. 14| and might be used at large scale utilisation of biogas from ADplants. Non-catalytic systems Non-catalytic DeNOx-systems are referred to as SNCR-systems. SNCR stands for Selective Non Catalytic Reduction. SNCR-systems use ammonia or urea as a reactant to reduce NOx. The reactant is injected with steam into the fluegas just above the fire zone at temperatures of 800 to 1000 C. Catalytic systems Two types of catalytic DeNOx are being discussed |ref. 15|: non-selective catalyst, which reduces the emission of NOx, but also reduces the emission of CO and hydrocarbons; selective catalyst, which reduces NOx by using ammonia or urea, also referred to as the SCR, Selective Catalytic Reduction-system.

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Project FAIR-CT96-2083 (DG12-SSMI)

Non-selective catalyst With the non-selective catalyst system NOx is reduced using CO as reactant: NO + CO N2 + CO2

The amount of CO is essential for optimisation of the DeNOx. The lambda of the engine therefore has to be regulated. With this method also hydrocarbons (excluded CH4) are oxidised to water and carbon dioxide. Selective catalyst (SCR) NOx is changed into N2 by using ammonia or urea as a reactant. Large scale plants use ammonia (gaseous or in solution): 4 NO + 4 NH3 + O2 8 NO2 + 8 NH3 4 N2 + 6 H2O 7 N2 and 12 H2O

Small scale DeNOx plants use urea for safety reasons. The catalyst material in SCR-systems generally consists of a carrier of titanium oxide (TiO2) with added active substances like vanadium oxide (V2O5) and tungsten oxide (WO3). For the catalytic reaction, the lambda has to be higher than with the noncatalytic system, and an exhaust gas temperature of at least 300 is needed. C In the case of biogas fuelled engines, this type of catalysts is being used if a very high DeNOx removal efficiency (> 90%) is required. For example if the exhaust gas is used as CO2 source for greenhouses. The costs of a selective catalyst DeNOx system are relatively high compared to the non-selective DeNOx system.

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6.

UPGRADING OF BIOGAS Upgrading of biogas to substitute natural gas (SNG) involves a number of steps |ref. 16, 17,18, 19, 20, 21|. At first, water (vapour) and H2S have to be removed. Subsequently CH4/CO2 separation must be carried out, using one of the following techniques for the removal of CO2: Pressure swing adsorption (PSA); Membrane separation; Physical or chemical CO2-absorption. If the gas is meant for input in a natural gas piping system, the gas has to be cooled and has to be compressed. Dust and (halogenated) hydrocarbons have to be removed, and the gas needs to be odorised for safety reasons. The three techniques focussed on the removal of CO2 are reviewed below. The techniques for the removal of water, H2S, dust and hydrocarbons are discussed in chapter 4.

6.1

Pressure Swing Adsorption (PSA) The PSA unit is schematically shown in figure 4. The unit exists of at least three active carbon beds. The process in each bed (successively) is as follows: The bed is fed with biogas under pressure. In this step the bed will be loaded with carbon dioxide upon saturation, while methane is released. If the break through point is reached, the process will be switched to the next bed. After saturation the bed is depressurised to ambient pressure. In this step a CH4/CO2 mixture is released with a high content of CH4 and will be recycled into the feed. The next step is to regenerate the active carbon bed by putting it under vacuum, in which the carbon dioxide is released. The PSA technique gives high efficiency rates (to 98%), but it is a relatively expensive process due to capital costs (control system).
M olcul s ie v s e ar e 2 3 M ixing v s s e l e

H 2S

CFC 1

Subm itte d Biogas natural gas CO 2 M e th ane rich re cycl e

Figure 4: Pressure Swing Adsorption process

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6.2

Membrane separation Membrane separation is based on selective permeability of membranes for different components. Figure 5 shows the process scheme of this separation process. The membrane efficiency varies between 73 % and 83%. Advantages are the simple techniques and operation. Disadvantages are the efficiency and the energy input for high pressures that are needed (20-35 bar) and high temperature.
H 2S M e m brane s CF C Substitute Natural gas

Biogas

CO 2

Figure 5: Upgrading biogas using gas separation membranes A pilot study has been carried out |ref. 16| with a low-pressure (8 bar) membrane separation system. An active carbon filter is needed in the feed line to remove trace components. Relatively to high-pressure membrane separation techniques, a reduction of costs could be achieved of 10 % per m3 natural gas equivalents. The major lack of knowledge during the pilot study was the longterm behaviour of the membranes. Research on this has been initiated. 6.3 Physical (water, methanol) or chemical CO2 -absorption techniques These absorption techniques are based on the principle of separation of CO2 and CH4 by using an absorbent. Figure 6 shows the technique schematically. One of the methods is the use of water as absorbent liquid. Biogas is fed into a vessel. In this vessel the water is sprayed. During the flushing the concentration of carbon dioxide decreases with distance and the gas becomes more concentrated with methane. The washing liquid is generated in two depressurisation steps. At a pressure drop from 10 bar down to 4 bar, methane and part of the carbon dioxide is released and is recycled. After the next pressure drop CO2 is released. The efficiency is about 95 %.

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6.4

Evaluation of CO2 removal techniques In Table 13 the three reviewed CO2 removal processes are compared.
H 2S Absorbe r D rying CF C

Biogas

Substit ute Nat ural gas

W as h ing l uid iq re ge n e ration

CO 2

Figure 6: Upgrading biogas using physical absorption techniques Table 13: Comparison of different available CO2 removal techniques
UPGRADING BY PSA Application Stage in the development Experience (in years) Emission to the air Energy efficiency Gas pretreatment Application Stage in the development Experience (in years) Emission to the air Energy efficiency Gas pretreatment Application Stage in the development Experience (in years) Emission to the air Energy efficiency Gas pretreatment H0489.A0/R002/TS/GR Large scale plants (CDA) Proven technique 12 years Chlorinated and fluor hydrocarbons (can be flared) CO2 reduction and CH4 reduction Energy input : energy output rate: 1:15 Gas drying, H2S removal UPGRADING BY MEMBRANE SEPARATION Large scale plants (CDA) Proven technique (high pressure separation) Pilot stage (low pressure separation) Appr. 10 years (high pressure separation) Chlorinated and fluor hydrocarbons (can be flared) CO2 reduction and CH4 reduction Energy input : energy output rate: 1:10 (high pressure) Gas drying, H2S removal Large scale plants (CDA) Proven technique Appr. 10 years Chlorinated and fluor hydrocarbons (can be flared) CO2 reduction and CH4 reduction Information not available Gas drying, H2S removal - 23 25 January 2000

UPGRADING BY PYSICAL/CHEMICAL ABSORPTION

AD-NETT Technical Summary on Gas Treatment

Project FAIR-CT96-2083 (DG12-SSMI)

7.

CONCLUSIONS This technical summary has dealt with different aspects of gas in AD plants. The topics have been: production and composition of biogas, treatment of biogas, treatment of flue gas. On an average base the biogas formed in AD plants consist of: 55-80 vol.-% CH4 20-45 vol.-% CO2 0-1,5 vol.-% H2S 0-0,05 vol.-% NH3 saturated with water. Prior to utilisation the biogas needs to be treated in order to: prevent corrosion of equipment installed. fulfil demands on gas quality either for gas equipment or in case of gas upgrading to natural gas quality. Biogas treatment can involve the removal of water, H2S and/or CO2. For the removal of water several methods based on separation of condensed water or on gas drying are available. For small scale AD plants water removal is limited to moisture traps and water taps in the gas line. If upgrading of biogas is the treatment objective gas drying techniques become necessary. In order to remove H2S several methods have been developed. Based on the economics and simplicity in terms of (unattended) operation and maintenance, air-oxygen dosing in the biogas and iron chloride dosing to the digester slurry are the most suitable, especially for small-scale farms. For large-scale farms or when upgrading of biogas to natural gas is the objective, chemical absorption of H2S might become more feasible. When biogas is upgraded to natural gas quality, in addition to water and H2S removal, CO2 removal is one of the gas treatment objectives. CO2 removal techniques that can be applied are a pressure swing adsorption unit, a high or low-pressure membrane separation unit, and physical or chemical absorption techniques. Flue gases as produced at the site of AD plants by gas engines or boilers need to be treated. Emission control can be done using lean burn engines or catalytic or non-catalytic DeNOx systems.

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REFERENCES |1|Biogas technology in The Netherlands; Anaerobic waste and waste water treatment with energy production, Netherlands Agency for Energy and the Environment (NOVEM), Utrecht, The Netherlands, 1988. |2|Feedstocks for anaerobic digestion. AD-Nett report. |3| Guidebook on landfill gas extraction and utilisation. Netherlands Agency for Energy and the Environment (NOVEM), Utrecht, The Netherlands, 1997. Manure digestion in the Netherlands. 10 years of knowledge and experience. Netherlands Agency for Energy and the Environment (NOVEM), Utrecht, The Netherlands, 1990 (in Dutch).

|4|

|5|Upgrading of biogas to vehicle fuel standard. Sweco 1998. |6| Clampdown on emissions from landfill gas flares. UK Policy, ENDS Report 290. Besluit emissie-eisen stookinstallaties (BEES), recalculated to ISO standard air conditions, Ministry of Housing, Spatial Planning and Environment, The Netherlands, 1998 (in Dutch). Ta-LUFT Technische Anleitung zur Reinhaltung der Luft vom 27.2.1986. Erste Allgemeine Verwaltungsvorschrift zum BundesImmissionsschutzgesetz (BlmSchG) vom 15.3.1974. Deutsches BGBI IS 721,1986. WAV Entgasung von Deponiekrpern. Heft 110 sterreichischer Wasser- und Abfallwirtschaftsverband, Marc-Aurelstrae 5, 1010, Wien, 1997.

|7|

|8|

|9|

|10| H. Ortenblad, Hernig Kommunale Vaerker. Hernig, Denmark. personal communication. 1999. |11| N Carreras. CIEMAT, Instituto de Energias Renovalbes, Lubia, Spain personal communication. 1999. |12| S Piccinini. Centr Ricerche Produzioni Animali, Reggio Emilia, Italy. personal communication. 1999. |13| Desulphurization of biogas. Practical experience with the biocatalytic Desulphurization process. Biogas forum. |14| NOx-removal in waste incineration, full scale demonstration and research in the Netherlands, Novem report DV3.5.92 97.03, The Netherlands, July 1995.
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Project FAIR-CT96-2083 (DG12-SSMI)

|15| DeNOx-installation gas engines oil production site at Berkel, NAM/BUO, The Netherlands, July 1998 (in Dutch). |16| Feasibility study low pressure (8 bar) landfill gas separation system (Haalbaarheid toepassing nieuw membraan voor opwerking stortgas naar aardgaskwaliteit bij lage druk (8 bar)), Novem 355220/0440, The Netherlands, 1997. |17| Landfill Gas, from environment to energy, Commission of the European communities, 1992. |18| Listing of Dutch landfill gas projects (1983-1991) (Overzicht stortgasprojecten in Nederland (1983-1991)), Dutch Landfill Gas Advisory Centre (Adviescentrum Stortgas), The Netherlands, March 1993. |19| Evaluation of Landfill Gas Upgrading Project Carbiogas B.V. at Nuenen, Novem /Gastec, The Netherlands, December 1992. |20| Evaluation of Landfill Gas Upgrading Project COGAS N.V. at Vasse, Novem/Gastec, The Netherlands, July 1993. |21| Guidebook on landfill gas extraction and utilisation, NOVEM/Thermie, The Netherlands, 1997.

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SUPPLIERS OF GAS TREATMENT EQUIPMENT

Carbiogas B.V. PO Box 90 8500 AB Joure The Netherlands

Carbotech Anlagenbau GmbH PO Box 130140 D-45291 Essen Germany Cirmac B.V. PO Box 995 7301 BE Apeldoorn The Netherlands Dynaf Energietechniek B.V. PO Box 54 800 AB Alkmaar The Netherlands Eltacom PO Box 276 2700 AG Zoetermeer The Netherlands Petrogas Gas systems B.V. PO Box 20 2800 AA Gouda The Netherlands Spruyt Energiesystemen B.V. PO Box 8349 3503 Utrecht The Netherlands Zanthingh Energie systemen B.V. PO Box 255 1430 AG Aalsmeer The Netherlands

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