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Abstract
A laboratory procedure is described for measuring methane potentials of organic solid waste. Triplicate reactors with 10 grams of
volatile solids were incubated at 55 C with 400 ml of inoculum from a thermophilic biogas plant and the methane production was
followed over a 50-day period by regular measurements of methane on a gas chromatograph. The procedure involves blanks as well
as cellulose controls. Methane potentials have been measured for source-separated organic household waste and for individual
waste materials. The procedure has been evaluated regarding practicality, workload, detection limit, repeatability and reproducibility as well as quality control procedures. For the source-separated organic household waste a methane potential of 495 ml CH4/g
VS was found. For fat and oil a lag-phase of several days was seen. The protein sample was clearly inhibited and the maximal
methane potential was therefore not achieved. For paper bags, starch and glucose 63, 84 and 94% of the theoretical methane
potential was achieved respectively. A detection limit of 72.5 ml CH4/g VS was calculated from the results. This is acceptable, since
the methane potential of the tested waste materials was in the range of 200500 ml CH4/g VS. The determination of methane
potentials is a biological method subject to relatively large variation due to the use of non-standardized inoculum and waste
heterogeneity. Therefore, procedures for addressing repeatability and reproducibility are suggested.
# 2003 Elsevier Ltd. All rights reserved.
Keywords: Methane; Biogas; Organic waste; Characterization; Laboratory measurement
1. Introduction
Several batch methods exist for measuring methane
potentials of waste. The basic approach is to incubate a
small amount of the waste with an anaerobic inoculum
and measure the methane generation, usually by simultaneous measurements of gas volume and gas composition. However, the technical approaches in terms of
pretreatment of the sample, inoculum, gas measurement
technique and incubation vary signicantly among the
published methods (Adani et al., 2001; Eleazer et al.,
1997; Harries et al., 2001; Heerenklage and Stegmann,
2001; Owen et al., 1979; Owens et al., 1993). Some of
these dierences originate from the purpose of measuring
* Corresponding author. Tel.: +45-4525-1603; fax: +45-45932850.
E-mail address: thc@er.dtu.dk (T.H. Christensen).
0956-053X/$ - see front matter # 2003 Elsevier Ltd. All rights reserved.
doi:10.1016/j.wasman.2003.09.009
394
395
2.5. Monitoring
396
TStandard Pm
Tm PStandard
397
3.3. Inoculum
The inoculum contains many particles and is not a
homogeneous suspension. Thus, a careful set-up procedure is essential to prevent variations between the samples that originate from variations in the inoculum. The
inoculum is thus continuously stirred and distributed
to all the bottles in the beginning of the set-up and
three bottles are randomly chosen for each sample
(triplicates).
It was necessary to discard all data from one experimental series because the cellulose controls or the
blanks showed too large variation among triplicates,
indicating that the distribution of inoculum to the
reactors was not suciently homogenous.
3.4. Substrate concentration
The substrate concentration of 2 g VS/100 ml in the
reactors is a compromise of, on one hand, the need to
use a large sample to have good representativity and
to get a high easy-to-measure gas production, and, on
the other hand, to avoid too large and impractical
volumes of reactors and gas production and keep the
solution dilute to avoid inhibition from accumulation of
VFA and ammonia. If signs of inhibition are observed,
Fig. 4. Examples of triplicate methane production curves for food oil (rape seed oil), pork fat, protein (gelatine), paper bags for collection of organic
household waste and chemically produced starch and glucose.
398
where tv, is the 95% quantile in the Student t-distribution with v degrees of freedom; s2 , is the estimated
variance of the blanks; n1 , is the number of replicates
used to measure the sample; n2 , is the number of replicates used to measure the blanks.
In the present case the degrees of freedom are 12 and
the numbers n1 and n2 are 3 derived from the use of
triplicates for any measurements. Using s=0.408 ml
CH4/ml solution from above the following is obtained:
DL 2:1788 0:408 2
p
1=3 1=3 ml
4. Conclusions
A laboratory procedure is described for measuring
methane potentials of organic solid waste showing high
methane potentials, for example in the context of treating the waste by anaerobic digestion. The lower detection limit of the presented method based on experiences
from about 100 sample is of the order of 70 ml CH4/g
399
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