29/12/23, 8:55 Transferability of Results from Laboratory Scale to Biogas Plants at Real Scale

REVIEW
Transferability of Results from Laboratory
Scale to Biogas Plants at Real Scale

Transferibilidad de resultados a escala de laboratorio

a plantas de biogás a escala real

Hans Oechsner
University of Hohenheim, Germany

Benedikt Huelsemann
University of Hohenheim, Germany

Carlos M. Martínez Hernández *

Universidad Central “Marta Abreu” de las Villas, Cuba

Transferability of Results from Laboratory Scale to Biogas Plants at Real Scale

Revista Ciencias Técnicas Agropecuarias, vol. 29, no. 2, 2020
Universidad Agraria de La Habana

Received: 02 November 2019

Accepted: 13 March 2020

ABSTRACT:
The costs of biogas plants are determined by the costs of the substrates they use, representing 40 to
60% of the annual operating costs of these in Germany, with energy crops being widely used as
substrates in anaerobic digesters. The determination of methane performance in different substrates
via Batch tests is carried out using the German VDI-4630 standard in approximately 40 different
laboratories installed in Germany. The results obtained in the methane yield of the substrates valued
at the laboratory level show great correspondence with those achieved at real scale in the active
plants. The Biogas Guide compiled by KTBL German Agency based on the results obtained by several
well-known laboratories and institutes in that country, has shown that the accuracy of these results
can be taken into account for the economic planning studies of new biogas plants. Fermentation tests
are the most accurate method for determining the methane yield of the parts of the plants under
analysis. In recent times, the use of biogas laboratories has increased in the validation of methane
yield at the laboratory scale of different substrates, motivating the cooperation and use of standard
research protocols among them, thus ensuring a high quality of the results obtained and its
replicability.

Keywords:
Batch tests, anaerobic digester, German standard, VDI-4630.

RESUMEN:
Los costos de las plantas de biogás están determinados por los costos de los sustratos que estas
utilizan, representando un 40 a 60 % de los costos de operación anual de estas en Alemania, siendo
muy utilizados cultivos energéticos como sustratos en los digestores anaeróbicos. La determinación
del rendimiento de metano en diferentes sustratos vía pruebas Batch se realiza mediante la norma
alemana VDI-4630 en aproximadamente 40 diferentes laboratorios instalados en Alemania. Los
resultados obtenidos en el rendimiento de metano de los sustratos valorados a nivel de laboratorio
muestran gran correspondencia con los alcanzados a escala real en las plantas en activo. La guía de
Biogás compilada por la agencia alemana KTBL basada en los resultados obtenidos por varios
laboratorios e institutos bien conocidos de ese país ha mostrado que la exactitud de dichos resultados
puede ser tenidos en cuenta para los estudios de planificación económicas de nuevas plantas de
biogás. Las pruebas de fermentación es el método más exacto para la determinación del rendimiento

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de metano de las partes de las plantas objeto de análisis. En los últimos tiempos, se ha incrementado
el uso de laboratorios de biogás en la validación del rendimiento de metano a escala de laboratorio de
diferentes sustratos, motivando la cooperación y utilización de protocolos investigativos estándar
entre estos, de esta forma se asegura una alta calidad de los resultados obtenidos y su replicabilidad.

Palabras clave:
Pruebas Batch, digestor anaeróbico, norma alemana, VDI-4630.

INTRODUCTION

W hat are F ermentation T ests R equired for ?

The economic efficiency of biogas plants is largely determined by the substrate costs.
Approx. 40% to 60% of the annual costs of a biogas plant, fed with energy crops, are
attributable to substrate procurement. It is, therefore, essential to calculate standard figures
when planning a biogas plant. When using liquid manure and by-products, it is also essential
to know the specific methane yield of the substrates used in order to enable optimum
planning of a biogas plant. In addition to the data on the specific methane yield, further
information on the fermentation substrate used is also required. In particular, the yield per
unit area of fresh matter, the dry matter yield and the quality of the fodder have a
considerable influence on the amount of methane that can be achieved.

In principle, the content of carbohydrates, fats and proteins correlates directly with the
energy content of the substrate used and should actually be sufficient as a basis for
calculating the methane yield. There are also a number of methods for this estimation.
Starting with the calculation by Buswell (1939), who estimated the biogas yield, and the
methane and carbon dioxide content in the biogas on the basis of the elementary
composition of the substrate. Other calculations were made to determine the nutrient
composition by Baserga (1998) and later by Keymer & Schilcher (1999). These values can only
be used as a rough guide for simple planning of full scale biogas plants. As Czepuck et al.
(2006), proved in comparison studies, the results deviate by 10 % to 20 % from the measured
value in the biogas yield test. Since the plant substrate mass is composed of very different
nutrient combinations, further estimation formulas have been proposed by Amon et al. (2007)
and Kaiser (2007), as well as the laboratory determination of the fermentable volatile solid
(FVS) value. VDI 4630 (2016) refers that some of these indicators allow a limited extension of
the reliability of the results.

FIGURE 1
Methane yields and formation kinetics of different nutrient fractions (according to Czepuck
et al., 2006)

Above all, the different compositions of the carbohydrate fraction and its extremely
different digestibility have a clear effect on the degradability, the degradation kinetics and
finally the achievable gas yield. While starch can be completely converted into biogas in about
5 days depending on its storage in the plant, the conversion of plant supporting tissues such
as hemicellulose and cellulose is significantly slower. Especially if a high proportion of
lignocellulose complexes is present, this has a negative effect on the methane yield and the
substrate degradability. Therefore, a fermentation test is the most exact and recommended
method for the exact determination of methane yield of plant mass (Czepuck et al., 2006).

DEVELOPMENT

R eference on the M ethane Y ield of C ommon S ubstrates

For the use of common substrates, German KTBL (Advisory Board for Technology and
Construction in Agriculture) has considered a great amount of research, which has been
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compiled with the help of a large number of individual results from several well-known
laboratories and research institutions (KTBL, 2011). As a rule, these reference values are
extremely valuable and very useful for the design and planning of biogas plants.

However, it must be noted that depending on the location, variety, vegetation course during
the year, harvest time, storage and silage, significant deviations from the standard values are
possible. For this reason, laboratory analysis in the biogas laboratory is useful in many cases
for determining methane yield.

G uidelines for F ermentation T rials

Many guidelines are available to get a higher reproducibility of Biomass Methane Potential
(BMP). Beside European standards (Holliger et al., 2016), VDI 4630 is the most common
guideline used in Germany. Guideline 4630 (VDI 4630, 2016) describes both, the procedure for
carrying out batch and continue tests. KTBL "Interlaboratory Tests" working group developed,
together with the VDLUFA, the VDLUFA Method for "Determination of biogas and methane
yields in fermentation tests" VDI 4630 (2016), which somewhat simplifies the most important
criteria for carrying out fermentation tests. The aim of this method is to improve the quality
assurance of laboratory tests on biogas yield.

The regulations stipulate that a minimum number of test conditions must be satisfied:

Use of suitable, gas-tight and tempered "small fermenters"

Use of a suitable inoculum (either specially bred or fermentable material from active biogas
fermenters; inoculum);

Mixing ratio of inoculum and fermentation substrate (volatile solid (VS)-related) in a ratio of at least 2:1
to find sufficient buffer capacity in the fermentation Batch;

Inoculum ferment in parallel as a zero sample;

At least one standard substrate is also fermented (e.g. microcrystalline cellulose) in internal laboratory
conditions;

Fermentation temperature should be 37°C ± 1°C;

Measure biogas formation as often as possible and determine the methane content with each gas
extraction;

At least 25 days of fermentation time. Termination criterion for the test batch: if less than 0.5 % of the
gas quantity formed to date is produced on at least 3 consecutive days;

Reference of the methane yield to the VS input in the test substrate;

If silages or substrates with volatile components (fermentation acids, alcohols) are used, the value of
the VS content must be corrected (Mukengele & Oechsner, 2007);

Standardization of gas production (0°C, 1013 hPa); consideration of water vapor.

In the evaluation, the inoculum own production of biogas/methane is deducted from the
total production in order to determine only the biogas/methane yield of the sample tested.
The amount of biogas/methane produced over the experimental time is shown as a sum
curve.

C omparisons among L aboratories to E nsure T est Q uality

Now in Germany, at least 40 laboratories offer tests to determine the methane yield of
substrate samples. These laboratories are very experienced and they are involved in reducing
the risk of errors due to the complex and multi-stage test procedures. In previous
publications, the methane yields differ sometimes significantly from each other.

For this reason, KTBL working group has established a system of comparisons among
laboratories of biogas in cooperation with VDLUFA-NIRS GmbH and with the financial support
of BMELV. So far, eleven tests have taken place. The number of participating laboratories has
been in the range of 20 to 33 laboratories. By evaluating the test results and a comprehensive
description of the method as well as a detailed error analysis, the participants were able to
identify and eliminate errors in their own procedures. All participating laboratories were
required to comply with the VDI Guideline 4630 and the VDLUFA method regulation.
Microcrystalline cellulose was used as the standard fermentation substrate for each pass.
Besides that, other fermentation substrates were chose. These substrates should cover the
usual range of substrate variations from practice. Identical sample material was sent to all
laboratories in all rounds. The samples were crushed. The substrates valued were wheat
grain, dried maize, dried grass, maize silage and grass silage and rape press cake. When fresh
silages were shipped, the effects of sample storage and sample homogenization on the final
result were also possible to investigate.
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It was noticeable, in the first run in 2006, the results for cellulose showed a relatively wide
dispersion, although it was a very homogeneous and standardized substrate. The comparison
of methane yield among the different laboratories show a variation coefficient between 19.5%
and 8.4% in the eleven tests analyzed. When comparing the test setup and the results, it
became clear that the differences were not due to the type and size of the respective test
facilities, but to the accuracy of methane measuring instruments, their regular calibration, the
mathematical evaluation under consideration of the reference variables for standard
conditions and the consideration of water vapor correction in the event of deviations, which
played a more relevant role.

I nfluence of the M ode of O peration - T ransfer from B atch to C ontinuous O peration

With the exception of a few systems, biogas plants are not operated as batch type in
practice. Instead of this, they operate as continuous systems with addition of fresh
fermentation substrate several times a day. As a result, the process steps for anaerobic
decomposition of organic matter run parallel and simultaneously. While the batch approach
shows a clear change in biogas composition during the test sequence, the continuous
approach hardly allows a difference in gas quality to be measured over the course of the day,
if the same substrate is fed continuously. In addition, with fully mixed fermenters, but also
with the so-called "plug flow fermenters", in close correlation with the hydraulic retention
time of the substrate in the fermenter as well as with the fermenter geometry and the feeding
frequency, certain parts of fresh or only partially degraded substrate, always leave the
fermenter before the hydraulic retention time has elapsed. This occurs even before their
entire methane yield potential has been obtained in the substrates.

In batch systems, on the other hand, it is waited until the fermentation process has almost
completely decayed. For this reason, deviations are to be expected when batch results are
transferred to continuous operation. Today, biogas plants in Germany are equipped with very
long hydraulic retention times, partly due to legal requirements and also due to many of them
operate in cascade arrangement to achieve the methane yield potential be fully exploited.
Methane potentials and methane yields per substrate could then be determined at the same
time in the experiments. By determining the residual gas potential as in the overflow of
biogas fermenters, it is relatively easy to check to what extent the fermentation substrate
used is utilized or whether there are still reserves in its potential energy. Investigations in
various biogas plants in production as well as in plants in cascades have shown a narrow
correlation between the gas potential of substrates and the hydraulic retention time (Mönch,
2014). As a rule, only a very low residual gas potential (< 5 % when determining the residual
gas potential at mesophilic temperature) was measured in the retention time of the
fermenter (including the secondary fermenter) over 100 days. The results of two federal
measurement programs (FNR, 2005; 2009), confirm these statements. Research carried out at
25 biogas plants with different substrates and different cascade digesters showed, that the
transferability from laboratory results to real plants is possible (Ruile et al., 2015). In case of
comparison of batch to full-scale biogas plant, it seems like the influence of low data quality
on the full-scale biogas plant results in a bigger mistake than the measurement error based
on batch tests.

In an extensive trial at the University of Hohenheim, various fermentation substrates were

investigated in a combination of batch tests and continuous trials in the biogas laboratory.
For continuous trails the residual gas potential of the fermenter in overflow was measured in
batch tests. In these tests, maize silage, ground wheat seed and mixtures of both substrates
were fermented. The substrates were dried at 60 °C and ground to inhibit possible effects of
these pretreatments, then they were fermented in the digesters. The substrates were
supplemented with liquid manure (17 % VS content) to enable stable operating conditions.
Liquid manure was also fermented alone as a control variant. In continuous operation, 15
horizontal fermenters each with a useful fermenter volume (FV) of 17 l, were used with two
organic loading rates (2.5 and 4.0 kg VS m-³ FV d-1). The hydraulic retention time in the
continuous fermenters was 35 days at a fermentation temperature of 37 ± 2°C. For each
variation two repetitions were applied and the experiments lasted over 123 days, (= more
than 3 retention times). In addition to the amount of biogas and methane, the volatile fatty
acid content and the FOS/TAC value were regularly monitored.

The fermenter operation was very stable in all variants investigated. Only the maize silage
variant with an organic loading rate of 4 kg VS/m³FVd showed an increase in the fatty acids
(HAC) to a maximum of 6,500 mg/l and a slight drop in the pH value to 7.2 from the 67th day
of the experiment onwards. All other variants were stable (pH values 7.4 to 7.6) (Mukengele,
2017).

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The discharge (fermentation residue) of the continuous running fermenters was collected
towards the end of the experiment (105th, 108th and 115th days) in order to determine the
residual methane potential in the Hohenheim biogas yield test (HBT) at a fermentation
temperature of 37 °C for 35 days. In addition, the methane yield of fodders used as
fermentation substrates was determined as standard in the HBT at 37 °C and a retention time
of 35 days. This resulted in relatively high methane yields between 0.377 and 0.399 Nm³
methane per kg VS. Values between 4.7 and 5.3 kWh/kg VS were measured with the bomb
calorimetric bomb.

In Figure 2 a balance of the various experimental approaches is shown. It can be seen, that
with a high volume load (OLR 4) in continuous running digesters, especially with maize silage,
less methane yield (81.0 % of the HBT potential) can be achieved than with a low loading rate
(89.5 % with OLR 2.5). This also tends to be the case for cereals, but due to the very good
degradability of ground cereal grain this is of little significance (89.7 % and 91.2 %).

FIGURE 2
Methane yields from a continuous test at different OLR with subsequent determination of
the residual methane potential in comparison to the methane yields from batch tests using
the HBT method - comparative presentation.

The potential of residual gas and methane yields of the continuous tests resulted near to
the values obtained in batch tests (values between 98.7 and 101.1 %). This proves that the
results from batch tests can be transferred with high precision to continuous tests. However,
it is essential to ensure that part of the methane potential that is flushed out of the fermenter
via the fermentation residue, particularly in short retention times, (35 days), is quantified and
utilized. It is not like that in cases of substrate hydraulic retention times of more than 100
days and several fermenters are connected in cascade.

T ransferability of the R esults in B atch T est to P lants in P roduction

Possible causes for deviations in the gas yields between laboratory and practice are the
different fermentation conditions, e.g. the rate of organic loading or the "unpredictable"
influences of biological processes in real practice. An overview of the differences between
batch tests and real biogas plants is shown in Table 1 below.

In the design of biogas plants, the ratio of fermenter size and volume of organic load
planned of the CHP plays an important role. In biogas plant management, the daily supply of
substrates through the substrates used and their gas yields is decisive. Some uncertainties
still exist related to fermentation tests, their evaluation and transferability to practical plants,
mainly referred to biogas production (KTBL, 2011).

Possible deviations from the guideline values can result from the substrates, as they are
required in large quantities for the biogas plant and their substrate properties can vary
depending on the variety, harvest time and year of cultivation. For example, the substrate
also changes its composition (DM/VS content, content of fermentation acids, pH value) in the
bunker silos over the storage period. The determination of the substrate input quantity is
difficult despite existing weighing equipment, because the scales often do not have the
required accuracy, between the mixing vessel and the input screws and because the
individual substrates are often not recorded separately and exactly, specially, if mixed silage is
used as substrate. Neither the amount of liquid manure nor other liquids (rainwater, silo
leachate) are measured.
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TABLE 1
Selected process differences between batch test setups and biogas plants

In the fermenter, process-related factors such as the mixture of substrates, their content of
nutrients (especially trace nutrients), the biological environment in the fermenter, the
retention time and the load volume also have an effect on the methane yield.

As with the implementation of measurement programs, like Federal Measurement

Programs I and II. (FNR, 2005; 2009), there are in practice considerable problems in
determining the biogas yield and especially the biogas quality. The electricity yield is often
measured and estimated via the electrical efficiency of the CHP due to a lack of gas meters.
The actual proportion of ignition oil and possibly own electricity consumers running through
the meters must also be taken into account. In most cases, no conversion of standard
conditions is carried out when providing practical measurement data. This can cause an
overestimation of the gas volume over 20 % (Ruile et al., 2015).

P ractical D ata and B atch T ests

The University of Hohenheim has a research biogas plant on a practical scale with an output
of 350 kW-h/day. This plant is equipped with two separate fermenter lines (800 m³ usable
volume each), so that comparative investigations are possible. The plant is also high
equipped. The measurement devices are also frequently calibrated. It guarantees a high
quality of data. In a study carried out by Mönch (2014), a comparison was made between the
data at this plant and those on a practical scale, similar to what had previously been made
with data obtained at laboratory scale. This biogas plant is intensively monitored, the quantity
and quality of all input materials and the results obtained are precisely recorded and, as far
as technically possible, kept constant during all the process. In the experiment, a relatively
high proportion of liquid manure (50.0 %) was used (fresh mass). In addition, horse manure
with other solid manure (23.6 %), maize silage (10.1 %), grass silage (8.8 %), cereal whole plant
silage (4.6 %) and ground cereal grain (2.9 %) were used. The VS share of horse manure was
27.5 %. The substrate quality of all input materials was determined and as well as biogas and
methane yields obtained in fermentation tests. The fermenters are equipped with a
mechanical processing technology (Cross flow grinder, MEBA, Nördlingen, Germany). The
daily input quantity of fresh mass was 12.1 t/d with a standard deviation of 2.9 %. The organic
loading rate was 2.49 kg VS per m³ of FV/day and the HRT was 62.4 days.

With the aid of the weighed input quantities, their content of volatile solids and the
laboratory values for the methane yield, the expected methane quantity of the fermenter was
calculated and compared with the values measured by the gas meter of the fermenter. The
results are shown in Figure 3.

FIGURE 3
Comparison of the methane production determined by input quantity and HBT batch
measurement with the actually measured methane production of the fermenter (Mönch,
2014).

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During the 20-days observation phase there were certain fluctuations in the measured
values, which were more variable in the input quantities. This dispersion can be explained by
the fact that the daily fluctuations of the VS input have a direct effect on the calculated value
for methane formation and are thus clearly visible in the graph, while these fluctuations in the
measured values are compensated by the substrate degradation in the fermenters while
several days passed. The mean specific methane yield of the values calculated via HBT was on
average 305 l CH4/kgVS respect to the values measured in the fermenters, 311 l CH4/kgVS,
only 2 % higher. This very small deviation between the methane yields determined from
laboratory values and the measured values at the practical fermenter confirms that the
laboratory values can be used very well for an estimate of the methane yield to be expected
and thus for an economic efficiency estimate. This applies if a representative sample was
analyzed for the methane yield; the VS content of the substrate input and its exact weight
were recorded regularly and at short intervals. As a rule, as this last example has shown,
inaccuracies are more likely to occur when determining the mass in practice than when
determining the methane yield in the laboratory.

RESULTS AND DISCUSION

The work shows the feasibility of extrapolating results obtained to laboratory scale to real
scale in the aspects related to the design and exploitation of biogas plants. These techniques
of simulation of processes to small scale are much utilized at international level. In the Cuban
case, this constitutes an obligatory reference and their applicability saves time, resources and
money. In the last decade, works based on the simulation of fermentation processes to small
scale in this thematic have been developed by investigators at Central University "Marta
Abreu" of Las Villas and by others at University "José Martí Pérez" of Sancti Spíritus, where
investigation projects, master and Doctorate thesis have being developed in theme analyzed
in this work.

CONCLUSIONS

The determination of methane yield by batch tests is now widely used in Germany and is carried out
by at least 40 laboratories. Their quality is regularly assured by inter laboratory comparisons.

Examples in the laboratory and in practice have shown that there is a relatively good correlation
between laboratory and practical values for the methane yield. This also proved that the gas yield
guidelines compiled by the KTBL on the basis of laboratory values from several well-known biogas
laboratories are important and indispensable for the economic preliminary planning of biogas plants.

In some cases, there are certain deviations from the assumed values at the biogas plant operated
later. However, a large number of influencing factors affect the fermentation substrate used and its
quality, but are also linked to the process and operating mode of the biogas plant.

The production of biogas is a microbial degradation process involving a large number of

microorganisms. Here, certain deviations in the range of 5 to 10 % are always possible. In order to
ensure the accuracy of the laboratory tests when determining the methane yield, regular participation
in inter laboratory comparisons and constant internal laboratory testing using standard substrates
should be a way of validating the results obtained.

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VDI 4630: Fermentation of organic substances - characterization of substrate, sampling,

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Notes

5 The mention of trademarks of specific equipment, instruments or materials is for

identification purposes, there being no promotional commitment in relation to them,
neither by the authors nor by the publisher.

Author notes

Hans Oechsner, Professor and Researcher, University of Hohenheim. State Institute of

Agricultural Engineering and Bioenergy (740). Garbenstrasse 9. Stuttgart. Germany. e-mail:
[email protected].
Benedikt Huelsemann, Professor and Researcher, University of Hohenheim. State Institute
of Agricultural Engineering and Bioenergy (740). Garbenstrasse 9. Stuttgart. Germany. e-
mail: [email protected].
Carlos M. Martínez Hernández, Profesor Titular, Universidad Central “Marta Abreu”de las
Villas. Carretera a Camajuaní km.5.5. CP: 54830. Santa Clara. Villa Clara. Cuba. e-mail:
[email protected]

*Author for correspondence: Carlos M. Martínez Hernández, e-mail: [email protected]

Conflict of interest declaration

The authors of this work declare no conflict of interests.

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