Waste Management 54 (2016) 126130

Contents lists available at ScienceDirect

Waste Management
journal homepage: www.elsevier.com/locate/wasman

A solvent-free approach to extract the lipid fraction from sewer grease

for biodiesel production
Qingshi Tu a, Jingjing Wang a, Mingming Lu a,, Andrew Brougham b, Ting Lu c
a
Department of Biomedical, Chemical and Environmental Engineering, University of Cincinnati, Cincinnati, OH 45221, USA
b
Metropolitan Sewer District of Greater Cincinnati, 1600 Gest Street, Cincinnati, OH 45204, USA
c
Black & Veatch, 4555 Lake Forest Drive, Suite 310, Cincinnati, OH 45242, USA

a r t i c l e i n f o a b s t r a c t

Article history: Fats, oils and greases (FOG) are the number one cause of sewer pipe blockage and have been mostly dis-
Received 15 November 2015 posed of as a waste until recently. This study investigated a low cost and environmentally friendly
Revised 14 May 2016 approach to extract the lipid fraction (fatty acids and glycerides for biodiesel production) from sewer
Accepted 18 May 2016
grease (SG), i.e., FOGs obtained from wastewater treatment plants (WWTPs). The lipid fraction of the
Available online 30 May 2016
sewer grease was primarily in the form of free fatty acid (FFA), at 20.7 wt%. An innovative solvent-free
extraction approach was developed using waste cooking oil (WCO) to overcome the challenges of emul-
Keywords:
sion, impurities and high moisture content of the sewer grease. A 95% extraction yield of sewer grease
Biodiesel
Free fatty acid
was achieved under the optimum operating condition of 3.2:1 WCO-SG ratio (wt/wt), 70 C and
Sewer grease 240 min. In addition, the reusability of the WCO was also investigated. WCO can be used two to three
Solvent-free extraction times for sewer grease extraction with more than 90% extraction efficiency.
Waste cooking oil 2016 Elsevier Ltd. All rights reserved.

1. Introduction
Fats, oils and grease (FOGs) in the sewer system are primarily
responsible for pipeline blockage and the resulting damage is
expensive to repair (PPRIC, 2002; US EPA, 2003, 2007; Chan,
2010; Gutierrez, 2011; SFWPS, 2011; Bufe, 2013). Therefore, com-
mercial food services, such as restaurants and food processing
facilities, are required by law to install grease traps and to maintain
(pump) the traps properly to prevent FOG discharge into the sewer
system. The FOG and water mixture from these traps are called
trap grease, and usually contain 210% of grease (Chesebrough,
2008; Austic, 2010; Tu et al., 2012). Meanwhile, for domestic users
and non-commercial food services, FOGs generated (e.g. from dish-
ing washing) tends to be discharged into the sewer system. At
some waste water treatment plants (WWTPs), such as the
Metropolitan Sewer District of Greater Cincinnati (MSDGC), both
trap grease and sewer FOG are combined in the primary settling
tank, removed by the skimmer and further dewatered. The resul-
tant FOG is referred to as sewer grease (Fig. 1), or black grease since
the sewer water is also called black water (Jolis et al., 2010; Ward,
2012), or primary clarifier skimmings or primary sludge (Mondala
Corresponding author at: Department of Biomedical, Chemical and Environ-
mental Engineering, PO Box 210071, University of Cincinnati, Cincinnati, OH 45221,
USA.
E-mail address: LUMG@ucmail.uc.edu (M. Lu).
et al., 2009; Pokoo-Aikins et al., 2010; Siddiquee and Rohani, 2011).
Sewer grease and trap grease are mostly sent to landfills. In recent
years, more efforts have been focused on reuse of these greases in
order to reduce the burden on landfill, reduce the tipping fee and
recover energy.
Lately, interests have grown in utilizing sewer/trap grease for
biodiesel production (Ragauskas et al., 2013; Lpez et al., 2014)
to reduce feedstock cost. Biodiesel feedstock cost can take up to
80% of the total production cost (Haas and Foglia, 2005), which
motivated research and development for low cost alternatives,
especially from non-food sources. Trap grease-to-biodiesel prac-
tices have been reported by companies such as BlackGold Biofuels
(www.blackgoldbiofuels.com) and Pacific Biodiesel (www.biodie-
sel.com) with limited details on FOG pretreatment.
The technical challenge of sewer grease as a biodiesel feedstock
is due to the much lower oil quality: higher contamination (e.g.
soap, food debris), higher FFA content (due to hydrolysis and pro-
longed residence in water), and emulsion (Stacy et al., 2014). Given
the highly emulsified sewer grease from MSDGC, the reported lipid
separation method for trap grease, primarily heating, (Chakrabarti
et al., 2008; Wang et al., 2008; Ngo et al., 2011; Turner et al.,
2011; Jolis and Martis, 2013; Watson, 2011; Noshadi et al., 2014)
is insufficient to separate the lipid fraction (Chan, 2010; Chung
and Young, 2013; Ducoste, 2013). In addition, the presence of cal-
cium soap in the sewer grease that binds the lipids also adds to
the challenge in separating the lipid fraction by heating (Keener

http://dx.doi.org/10.1016/j.wasman.2016.05.017
0956-053X/ 2016 Elsevier Ltd. All rights reserved.
 Q. Tu et al. / Waste Management 54 (2016) 126130 127

Fig. 1. Definitions of trap grease and sewer grease.

et al., 2008; He et al., 2011). Solvent extraction and/or freeze-drying

practiced in laboratory (Yuttachana, 2006; Mondala et al., 2009;
Pokoo-Aikins et al., 2010) is likely cost-prohibitive to most biodiesel
manufacturers at commercial scales (Siddiquee and Rohani, 2011;
Voegele, 2012). Other extraction/separation methods, such as hot
centrifugation and acid wash (Pastore et al., 2014, 2015; Bi et al.,
2015; di Bitonto et al., 2016) may be effective, however, the poten-
tially high energy consumption and use of hazardous chemicals
(e.g. H2SO4) may be a concern. In-situ conversion may be an effec-
tive method to convert the lipids in the sewer grease directly into
biodiesel, however, the downside is the significantly extended reac-
tion time (up to 24 h) and substantial use of MeOH (Mondala et al.,
2009; Choi et al., 2014; Sangaletti-Gerhard et al., 2015; Wang et al.,
2016). In addition, the quantity of trap grease remains unknown for
most municipalities, which hinders its reuse in commercial scale. Fig. 2. A picture of the raw sewer grease from MSDGC.
The US average of 6.06 kg (13.37 lbs)/person/year of trap grease
may be outdated (Wiltsee, 1998), while much lower rates have
study was collected from the dining halls at the University of
been reported from limited studies at a few municipalities
Cincinnati.
(Chesebrough, 2008; Austic, 2010; Wang, 2012).
Therefore, the goal of this study is to develop an innovative and
low cost process that can be easily incorporated by biodiesel pro- 2.2. Experimental setup
ducers. The key requirement is not to add new solvents to the exist-
ing transesterification process. It will be even more cost effective if After initial screening (Wang, 2012), the parametric ranges
the water removal step can also be eliminated. Although oil is not a were narrowed down as follows: sewer grease ratio (WCO-SG
traditional solvent, FFA solubility in oil is very high (e.g. 93.7%, by ratio; wt/wt) of 3.2:1, 3.6:1 and 4.1:1, reaction temperatures of
Ngo et al., 2011), which makes it suitable for this application. 60 C, 70 C, and 85 C, and extraction times from 30 min to
Another advantage is that oil is almost immiscible with water, 360 min. For each experimental run, 30 g of sewer grease sample
which can extract the lipid fraction from sewer grease with a high were used with waste cooking oil of 105 mL, 120 mL and 135 mL,
yield. Therefore, a higher quality oil with low FFA content, e.g. respectively, based on the WCO-SG ratio. The reactor is equipped
waste cooking oil, was used to extract the lipid content from a lower with a thermocouple to monitor the temperature, a magnetic stir-
qualitied oil (the sewer grease). The resultant product is an oil with rer and a sampling port. The WCO was pre-heated to the desired
elevated FFA content, which can be easily converted to biodiesel temperature in the reactor before the sewer grease was added.
with the standard esterification and transesterification processes Limited stir was applied to the mixture was as suggested from
(Canakci and Van Gerpen, 2001; Chai et al., 2014). When using an earlier study, since continued stirring would result in finer par-
waste cooking oil to extract sewer grease lipid, the product is an ticles and hinder the subsequent filtration process (Wang, 2012).
oil with an elevated FFA content, which most biodiesel manufactur- For each time series study, 2 mL of liquid sample was taken for
ers can pretreat (Chai and Kellogg, 2014). This process will result in FFA titration at approximately every 30 min. After reaction, the
much lower costs and is more environmentally friendly. The feasi- mixture was pressed and filtered for solids removal.
bility and optimum conditions are presented in this study.
2.3. Analytical methods
2. Methodology
The moisture content of the raw sewer grease was determined
2.1. Materials by the weight difference before and after heating at 100 C for 24 h.
For compositional analysis, the dried sewer grease was immersed
Sewer grease samples (Fig. 2) were provided by the Metropoli- in dichloromethane (DCM) at a ratio of 1 g per 15 mL for 24 h at
tan Sewer District of Greater Cincinnati (MSDGC), which are wet, room temperature to extract the organic fractions. The resulting
odorous, non-oil like, and contained various solids (plastics, tree DCM solution was filtrated, and the glycerides (mono-, di- and
branches, pebbles, etc.). Chemicals such as n-hexane (HPLC grade), tri-glycerides) were analyzed by a GCMS following ASTM 6584
dichloromethane (HPLC grade), toluene (HPLC grade), isopropanol method (ASTM, 2000). The solids part was dried for weight
(HPLC grade), and KOH were all purchased from Fisher USA measurement. The FFA concentration was determined by titration
(www.fishersci.com). The waste cooking oil (WCO) used for the in accordance with AOCS Cd 3d 63 method (AOCS, 2007).
128 Q. Tu et al. / Waste Management 54 (2016) 126130
Considering its dominant presence in the FOG (shown in Sec-
tion 3.1), FFA was used as the indicator to reflect the progress/effi-
ciency of extraction in this study. The lipid extraction yield is
defined by Eq. (1):
FFAi
Extraction yield  100%
FFA0
where:
FFAi = the amount of FFA extracted into waste cooking oil at
sampling time i, (g).
FFA0 = the maximum available FFA in the raw sewer grease
sample, (g).
FFA0 was determined by the following procedure. 30 g dried
sewer grease sample was mixed with the waste cooking oil at a
WCO-SG ratio of 9:1. The extraction lasted 24 h, after which the
oil layer was separated from the solids. This method was compared
with the conventional solvent extraction method using hexane and
DCM, and the maximum available FFA (FFA0) obtained from this
method is very close to the result from the extraction using IPA/
hexane (1:1, vol/vol) solution (p-value = 1.0, Wang, 2012).
The amount of FFA from titration was calculated by Eq. (2)
(Wang, 2012).
C KOH  V KOH  V blank
Mass of FFA  V 2  MW WCO
Vs
where:
C KOH = concentration of KOH solution used as the titrant,
0.1 mol/L.
V blank = volume of KOH consumed for titrating the blank, L.
V KOH = volume of KOH consumed during titration, L.
V s = volume of the oil sample for titration, L.
V 2 = volume of WCO recovered, L.
MW WCO = molecular weight of WCO, 278 g mole/g (Chai et al.,
2014).
Each experimental condition was repeated at least three times
to ensure precision. Analysis of variance (ANOVA) was performed
for the experiment results by using the statistical package in
Microsoft Excel.
3. Results and discussion
3.1. Characterization of the sewer grease
The compositional analysis from six sewer grease samples
showed that the MSDGC sewer grease contained (58.9 1.5%) of
water, 0.2% of glycerides (mono-, di- and triacylglycerols), 20.7%
of FFA, 18.2% of solids and 2.0% unmeasured part on average. FOG
in the sewer grease was primarily in the form of FFA, which is con-
sistent with other studies (Chakrabarti et al., 2008; Ngo et al., 2011).
The moisture of a later batch of sewer grease averaged 56.3 1.3%.
The lipid fraction of the sewer grease is primarily in the form of
FFAs, which makes it feasible to use FFA level as an indication of
extraction efficiency. The high FFA concentration may be due to
hydrolysis of FOGs by microbial activities during the long sitting
time of in either grease traps or sewer pipes (US EPA, 1992).
3.2. Extraction of usable oil fraction for biodiesel production
3.2.1. Effect of temperature
The FFA of the WCO is 2.7 0.7%. According to Eq. (2), an FFA0 of
20.7 g/100 g raw sewer grease (20.7 wt%) is used. Three tempera-
ture levels, 60, 70 and 85 C, were studied under a fixed WCG-SG
ratio of 3.2:1 (Fig. 3). It showed that the extraction yield
100%
90%
80%
70%
FFAi/FFA0
60%
1 60C
50%
70C
40%
85C
30%
20%
10%
0%
0 60 120 180 240 300 360
Time (min)
Fig. 3. Effect of temperature on extraction yield (WCO-SG: 3.2:1).
approached 100% by the end of 360 min for all three temperatures.
Extraction yields at 70 C and 85 C are higher than that of 60 C
(p-value < 0.05), but no statistically significant difference (p-value
ranged from 0.5 to 1.0 for the null hypothesis at different times)
was shown between these two temperatures. This may be partially
attributed to the difference in viscosity of the FOG at different tem-
peratures. For soybean oil, the viscosity at 60 C is 16.1 cP, while it
is 12.3 cP at 70 C (Esteban et al., 2012) and 9.5 cP at 82.2 C
2
(Noureddini et al., 1992). On average, a 95% extraction yield can
be achieved within 240 min at 70 C and 85 C. Therefore, 70 C
was selected as the optimum temperature, and 240 min was
selected as the preferred extraction time.
3.2.2. Effect of WCO-SG ratio
The impact of WCO-SG ratio on the extraction yield was also
studied. Fig. 4 shows the progress of extraction under different
WCO-SG ratios at 70 C. It was evident that in order to achieve a
high extraction yield, the WCO-SG ratio had to be 3.2:1 or higher.
The result of the ANOVA single factor test showed no significant dif-
ference in the yields among the three WCO-SG ratios (3.2:1, 3.6:1
and 4.1:1; p-value range: 0.51.0). Therefore, a 3.2:1 WCO-SG ratios
was selected as the optimum dosage for WCO addition.
The average moisture content of the oil after SG extraction was
2.0 wt% (ranging from 1.3% to 2.8%). This is an indication of the
high effectiveness of the extraction process as the initial moisture
of the sewer grease is around 58.9%. The oil mixture after extrac-
tion has an average FFA level of 8.5 wt% and can be directly made
into biodiesel without moisture removal. Oil with a moisture level
less than 2% is also acceptable to the biodiesel producers for the
conventional alkaline-catalyzed transesterification (Chai, 2015).
When the moisture is slightly higher than 2%, mild heating may
be needed.
3.3. Waste cooking oil reuse during the extraction process
WCO reuse for sewer/trap grease extraction has a high economic
value at commercial-scale production. On the other hand, as FFAs
and glycerides dissolve into WCO, the FFA level of the mixture
increases, which may result in a lower grade oil and may decrease
the extraction yield. WCO was used twice (labeled as WCOx2) and
three times for sewer grease extraction (labeled as WCOx3) in
this study, with time series shown in Figs. 5 and 6. A new batch
(30 g) of sewer grease was added during each reuse without new
WCO addition. After extraction once, the FFA level increased from
2.7 wt% to 8.5 wt% (the starting point for WCOx2 in Fig. 5). During
the reuse (WCOx2), the FFA concentration in the WCO increased
in a more placid manner from 8.5 wt% to 14.1 wt% in 180 min,
beyond which no significant change (p-value: 0.6) in FFA
 Q. Tu et al. / Waste Management 54 (2016) 126130 129

100%
1.4:1
90% 2.3:1
2.7:1
80%
3.2:1
70% 3.6:1
4.1:1
60%
FFA/FFA0

50%

40%

30%

20%

10%

0%
0 60 120 180 240 300
Time (min)

Fig. 4. Effect of WCO-SG ratio (wt/wt) on extraction yield (at 70 C).

concentration in raw sewer grease was 20.7 wt%, the maximum

14.0%
available mass of FFA in each run should be 6.2 g. The FFA extracted
12.0% in the three runs was 6.2 g, 6.0 g and 5.2 g, respectively. After two
uses (WCOx2), the total extraction yield was 98.2% and it became
10.0%
FFA % in WCO

93.2% after three uses (WCOx3). However, extraction did not pro-
8.0% ceed further after 90 min of WCOx3. The product after two uses is
WCOX2 categorized as yellow grease (less than 15% FFA), while it is consid-
6.0%
ered brown grease (Canakci and van Gerpen, 2001) after three uses.
4.0% The sale price of yellow grease is higher, with one less WCO reuse.
The overall cost effectiveness of the reuse process should be evalu-
2.0%
ated at a commercial-scale production.
0.0%
0 30 60 90 120 150 180 210 240
3.4. Future work
Time (min)

Fig. 5. FFA concentration (%) in WCO (WCOx2). This study focused on the technical aspects of lipid extraction
from sewer grease. Cost analysis was not performed, as the sewer
grease and waste cooking oil were received for free for research
20.0% purposes. However, in order to evaluate the potential economic
18.0% benefits of this technology, it is essential to perform a cost analysis
16.0% in the future. Also, Calcium content measurement should also be
performed for the resultant biodiesel to ensure compliance with
14.0%
FFA % in WCO

ASTM 6571.
12.0%
10.0%
WCOx3 4. Conclusion
8.0%
6.0%
A sewer grease with 58.9 wt% moisture, 20.7 wt% FFA and
4.0%
0.2 wt% of glycerides was made into a biodiesel feedstock with
2.0% an innovative extraction method using waste cooking oil. This
0.0% method is especially effective for emulsified trap/sewer grease
0 30 60 90 120 150 180 210 240
where the lipid content cannot be separated by heating and filtra-
Time (min) tion. This method can be directly applied to trap/sewer grease with
Fig. 6. FFA concentration (%) in WCO (WCOx3).
up to 60% moisture without moisture removal. Comparing with
conventional solvent extraction, this method also eliminates sol-
vent recovery process. The parametric study showed that a combi-
concentration was observed. The total increase between the start- nation of 3.2:1 WCO-SG ratio (wt/wt), 70 C and 240 min of
ing and ending FFA concentrations during 2 WCO uses was 66.2% extraction time is the optimum configuration to achieve an extrac-
and the saturation time was determined as 180 min. Beginning tion yield of over 95% (almost all extracted). WCO could be used
with 14.1 wt% FFA, the WCO during the third use became saturated two or three times with more than 90% extraction efficiency. Using
in the first 90 min (p-value: 0.4) with an ending FFA concentration waste cooking oil for FOG extraction from raw sewer grease con-
of 18.9 wt%. The corresponding increase between starting and tributes to environmental friendliness by eliminating the use of
ending FFA concentrations during WCOx3 was 34.1%. As the FFA0 chemical solvents. This solvent free process also eliminates energy
130 Q. Tu et al. / Waste Management 54 (2016) 126130

consumption and the associated costs otherwise needed for mois- Lpez, R.J., Higgins, S.R., Pagaling, E., Yan, T., Cooney, M.J., 2014. High rate anaerobic
digestion of wastewater separated from grease trap waste. Renew. Energy 62,
ture removal and solvent recovery.
234242.
Mondala, A., Liang, K., Toghiani, H., Hernandez, R., French, T., 2009. Biodiesel
Acknowledgement production by in situ transesterification of municipal primary and secondary
sludges. Bioresource Technol. 100 (3), 12031210.
Ngo, H.L., Xie, Z.G., Kasprzyk, S., Haas, M., Lin, W.B., 2011. Catalytic synthesis of fatty
Funding to support the study from the People, Prosperity and the acid methyl esters from extremely low quality greases. J. Am. Oil Chem. Soc. 88
Planet (P3) Phase I (SU836038) and Phase II grant (SU835291) is (9), 14171424.
gratefully acknowledged. The authors would like to thank Dr. Ming Noshadi, I., Kanjilal, B., Du, S., Bollas, G.M., Suib, S.L., Provatas, A., Liu, F., Parnas, R.S.,
2014. Catalyzed production of biodiesel and bio-chemicals from brown grease
Chai (Green Leaf Biodiesel) for his help with ASTM 6584 analysis using ionic liquid functionalized ordered mesoporous polymer. Appl. Energy
and Mr. Mark Schutte for his contribution in trap grease inventory. 129, 112122.
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Greater Cincinnati (MSDGC) for their support. Pastore, C., Lopez, A., Mascolo, G., 2014. Efficient conversion of brown grease
produced by municipal wastewater treatment plant into biofuel using
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