Bioresource Technology 45 (1993) 53-58
THE R E U S E OF SPENT B L E A C H I N G EARTH: A FEASIBILITY
STUDY IN WASTE MINIMISATION FOR THE EDIBLE OIL
INDUSTRY
Simon J.T. Pollard *, Christopher J. Sollars & Roger Perry
hnperial (bllege Centrefor Toxic Waste Management, Imperial College of Science, Technology and Medicine, South Kensington,
London, UK, SW7 2BU.
(Received 4 November 1992; revised version received 6 January 1993; accepted 13 January 1993)
Abstract
Spent bleaching earth, a solid waste from the edible oil
industry can be converted to a clay-carbon adsorbent
for potential reuse in the adsorptive cleansing of
vegetable oils. Commercial and laboratory-prepared
adsorbents were screened for their ability to remove
coloured pigments, impurities and trace contaminants
from rapeseed and crude coconut oils. Activated spent
bleaching earth demonstrated efficient removal of
benzol[a]pyrene from crude coconut oil reducing the
concentration .from 1.2.8 lag kg ~ in the crude oil to 1.3
pg kg i (89"8% w/w removal) in the treated product at a
2"0% w/w adsorbent dose. Soybean and rapeseed
process wastes activated under identical conditions
exhibited similar removal efficiencies of 89 and 86%
w/w, respectively. This compared with a reduction in
benzo[a]pyrene concentration to 10.8 lag kg- i for virgin
bleaching earth (15.6% w/w) and to less than 0"1 pg
kg - I for commercial powdered activated carbon
(> 99"2% w/w). Activated spent bleaching earth ex-
hibited limited removal of chlorophyll derivatives (27%
w/w) and negligible uptake of the fl-carotenoids and
phosphorus from degummed rapeseed oil compared
with the virgin bleaching earth which showed effective
bleaching o/ chlorophyll derivatives (98% w/w), the fl-
carotenoids and removal of phosphorus (71% w/w).
Adsorptive differences between these materials are inter-
preted with reference to interactions at the surfaces of
acidulated montmorillonite and activated carbon. Pro-
cessing incentives for the recovery and reuse of spent clay
are discussed.
Key words: Edible oils, decolourisation, spent bleach-
ing earth polynuclear aromatic hydrocarbons, active
carbon.
*Current address: Department of Chemistry, University of
Edinburgh, King's Buildings, West Mains Road, Edinburgh,
UK, EH9 3JJ
Bioresource Technology 0960-8524/92/S06.00 © 1993
Elsevier Science Publishers Ltd, England. Printed in Great
Britain
53
INTRODUCTION
The adsorptive cleansing of edible oil is performed on
an industrial scale using acidulated calcium montmoril-
lonite clay (bleaching earth) to remove a variety of
undesirable impurities which would otherwise impart
colour, odour and taste to the refined product. These
include chlorophyll, fl-carotene (and their derivatives),
residual soaps, fatty acids, phosphatides and trace
metals (Patterson, 1976; Norris, 1982). Activated
carbon is also periodically used in an admixture with
virgin bleaching earth for the removal of trace quanti-
ties of polynuclear aromatic hydrocarbons (PAH) from
edible oils (Biernoth & Rost, 1967; Norris, 1982;
Larsson et al., 1987). These contaminants, some of
which are suspected human carcinogens, are occasion-
ally present in crude oils in quantities sufficient to be of
concern to edible oil processors.
Spent bleaching earth (SBE), the principal solid
waste product from the edible oil industry, routinely
contains in excess of 20% w/w residual oil which can
rapidly oxidise to the point of spontaneous ignition as a
consequence of clay-catalysed auto-oxidation reactions
(Svensson, 1976; Sonntag, 1979). For many years, the
conventional route for the disposal of this waste has
been direct landfill, but recent changes in environ-
mental legislation and a growing concern for the safe
disposal of catalysts (Agoos, 1986; Habermehl, 1988)
have led to restrictions being placed on the dumping of
spent clay (McDermott et al., 1989). A re-evaluation of
waste management options for this material is there-
fore required.
'Waste minimisation' is an umbrella term used to
denote any process which results in a reduction of the
waste stream prior to treatment or disposal (Patterson,
1989). Source reduction, waste reco,~ery, reuse, and
recycling are examples of waste minimisation strate-
gies. The reuse of SBE and the concomitant recovery
of residual oil has been a recurrent focus of research
within the edible oil industry for nearly 50 years. Clay
regeneration has been attempted by steam (Penninger,
1979), alkali (Smith et al., 1977) and solvent extraction
54 Simon J. T. Pollard, Christopher J. Sollars, Roger Perry
(Orth, 1980; Ong & Sinkeldam, 1983; Kheoh, 1986),
wet oxidation of adsorbed oil (Kalam & Joshi, 1988a,
b) and by thermal treatment methods (Bahl & Dayal,
1977). Most recently, extraction of oil from the clay
surface using supercritical carbon dioxide has been
investigated (Anon., 1992). Alternative disposal
options for SBE have included biological treatment by
landfarming, its proposed use as a fuel supplement
(McDermott, 1982; Daido, 1987) and as a potential
chicken feed (Blair et al., 1986).
As part of our own investigations into the reuse of
SBE, we have previously reported the conversion of a
laboratory-synthesised soybean filter cake to a low-
cost adsorbent (Pollard et al., 1991a, b). In this process,
residual soybean oil present in the spent earth is first
carbonised and then activated on the clay surface to
yield a clay-supported active carbon (Pollard et al.,
1990; 1992) (Fig. 1). The present feasibility study
investigates the reuse of activated SBE for the removal
of pigments and trace contaminants from crude
vegetable oils. In an assessment of bleaching perform-
ance, activated SBEs were screened together with
selected commercial adsorbents for the removal of
coiour from degummed rapeseed oil (an oil high in
chlorophyll derivatives) and benzo[a]pyrene B[a]P)
from crude coconut oil (with which trace PAH in some
edible oils are occasionally associated).
METHODS
Materials
Degummed rapeseed oil and crude coconut oil were
obtained from a commercial UK supplier. Virgin
bleaching earth was supplied by Laporte Industries,
Widnes, UK. Norit SA4 powdered activated carbon
was supplied by Norit (UK), Glasgow and Brimac CC
bone char obtained from British Charcoals and
Macdonalds, Greenock, UK. Additional powdered
carbons were obtained from BDH Chemicals, UK
(decolourising charcoal) and Chemviron Carbon, UK
(Grade C). An admixture of 4 parts virgin bleaching
earth to 1 part Norit SA4 was prepared by powder
blending and represented an adsorbent blend used
commercially for the occasional removal of PAH from
edible oils.
An optimised procedure for the preparation of zinc
chloride activated SBE (clay-carbon adsorbent) from a
C RBO SA ON ACtAeON
r - - ] ib ~ " [ : l
[~ AcidulatedM0ntmorilloniteSupport
[ ] Residual0il • CarbonaceousChar [ ] ActivatedChar
Fig. 1. Schematic structural model for the preparation of
zinc chloride activated spent bleaching earth.
laboratory-synthesised filter cake containing 30% w/w
soybean oil has been previously described (Pollard et
al., 1991a). Two additional control materials were
included in this study: ( 1 ) carbonised SBE, in which the
residual oil was pyrolysed on the montmorillonite
support without chemical activation, and (2) deacti-
vated SBE, in which the chemically activated char was
subsequently oxidized in air at 850°C to the point of
complete carbon burn-off. These materials allowed
comparison of the activated materials with the carbon-
ised char and the mineral support, respectively.
Actual ex-factory spent soybean and rapeseed filter
cake process wastes were activated using the optimum
amount of zinc chloride established using the labora-
tory-synthesised material. Adsorbent properties are
summarised in Table 1.
Benzo[a]pyrene (99%) was supplied by the Commis-
sion of the European Community, Community Bureau
of Reference, Brussels, Belgium.
Methods
Colour, chlorophyll and phosphorus removal from
rapeseed oil
Adsorbent samples were pre-dried (105°C, 16 h) and
sieved to a particle size of less than 150 ~m. Sub-
samples (1'25 g) were then used to bleach degummed
rapeseed oil (100 g) in open 250 ml pyrex beakers at
95°C for 35 min atmospheric pressure with constant
stirring. Bleaching was performed under the fume hood
in batches of six samples at a time using a thermo-
coupled stirrer-hotplate (RS Instruments). Bleached
oils were then simultaneously vacuum-filtered whilst
hot (Whatman No. 3 paper) using a Buchner apparatus
and vacuum manifold.
Colour removal from degummed rapeseed oil was
determined at 60°C using a colorimetric method (EEL
Absorptiometer Model 4, Evans Electroselenium Ltd,
UK). Absorption was monitored over wavelength
bands 601 ( 2max 430 nm) and 602 ( 2,rlax 470 nm) in
3"2 cm (1~ inch) glass cells using a distilled water blank.
Evans activity (EA; bleaching performance) is
expressed as the sum of the two values and is represen-
tative of general colour removal rather than the uptake
of specific chromogenic compounds. An increase in
Evans activity denotes increased bleaching perform-
ance.
Lovibond red and yellow values were obtained at
60°C in 6"6 cm (5J inch) glass cells using a Lovibond
colorimeter (Colourscan, Tintometer Ltd, UK). A
reduction in these parameters is indicative of the
bleaching of carotenoids in oils. Residual chlorophyll-
derivative concentrations in the degummed rapeseed
oil were analysed using a 2maX of 600 rim. Residual
phosphorus contents in bleached rapeseed oils are
indicative of phosphatide impurities and were deter-
mined for crude and bleached rapeseed oils by X-ray
fluorescence using a Phillips PW 1400 XRF system.
This technique has previously been found to be com-
parable to graphite-furnace atomic absorption spec-
 Reuse of wastes for bleaching edible oils 55

Table 1. Adsorbent properties

Adsorbent Base material Apparent N 2 BET Carbon content pH

surface area (m2 g- 1) (% w/w)

Commercial
virgin bleaching earth acidulated calcium montmorillonite 397 0-23 3-0-3"2
Norit SA4 peat-based active carbon 629 86'4 9"8
Brimac CC hydroxyapatite bone char 100 9"8 9"3
BDH decolourising charcoal wood charcoal 515 79"1 3'7
Chemviron c Coal-based active carbon 866 73"3 NA
clay: carbon 4 : 1 virgin clay: Norit SA4 blend NA 69"2 NA
Synthesised SBE
activated SBE spent bleaching earth 239 20"1 4"1
carbonised SBE (control) spent bleaching earth 270 8"7 NA
deactived SBE (control) spent bleaching earth 15 <0-3
Ex-factorv SBE wastes
activated rapeseed SBE spent bleaching earth 143 16"7 NA
activated soybean SBE spent bleaching earth 193 16"6 NA

NA, not available; SBE, spent bleaching earth.

trometry for residual phosphorus determinations RESULTS AND DISCUSSION

(Morgan et al., 1985).
Benzo[a]pyrene removal from crude coconut oil
Crude coconut oil was liquefied in a microwave oven
for 1 min prior to bleaching. Selected adsorbents (2-00
g) were then used to open-bleach the crude oil (100g)
at 95°C for 35 min. Bleached oils were filtered as
above and stored in a freezer prior to analysis. Bleach-
ing curves of adsorbent dose in the range 0-3"5% w/w
against residual B[a]P concentration were constructed
for the activated filter cakes and Norit SA4 to observe
the lower adsorption threshold in each case.
B[a]P concentrations in open-bleached coconut
samples were determined by reversed-phase HPLC.
Bleached coconut oil samples (2"00 g) were dissolved
in HPLC grade petroleum ether (40-60°C fraction,
Vickers. UK) and diluted to 10 ml in volumetric flasks.
Clean up was performed on a deactivated alumina
iSupergrade IV; ICN Biomedicals GmbH, Germany)
gravity column with petroleum ether elution. The last
60 ml of a 100 ml eluate was collected and reduced
first using a rotary evaporator and then under a stream
of dry nitrogen for 20 min in a crimp-top vial (Hewlett-
Packard, UK). The residue was re-diluted to 200 #1 in
HPLC grade tetrahydrofuran (Vickers, UK), shaken
vigorously to disperse the residue in the solvent and
stored in the freezer.
Chromatographic analysis (Hewlett Packard
HP1090 Series M chromatograph) was performed on a
20 cm RF Chromsep 20 PAH column (ChromSpher).
Gradient elution (60-100% ACN over 20 rain; flow
rate 1-7 ml min-~) was employed using acetonitrile in
HPLC grade water. Programmed fluorescence detec-
tion was performed for B[a]P with excitation and emis-
sion wavelengths of 384 and 406 nm, respectively at
slit widths of 10 rim. A sample injection volume of
20-0/A was used throughout.
Colour removal from degummed rapeseed oil
Table 2 shows the bleaching performance of commer-
cial and laboratory-prepared adsorbents. A range of
base materials and porosities are represented among
the commercial adsorbents including predominantly
mesoporous materials (pore widths 2-50 nm; Brimac
CC bone char, virgin bleaching earth) and microporous
carbons (pore widths < 2 nm; Chemviron C, BDH
decolourising charcoal).
Virgin bleaching earth exhibited its characteristic
superiority for the removal of chlorophyll derivatives,
the fl-carotenoids and phosphorus from degummed
rapeseed oil and demonstrated a high Evans activity
confirming efficient overall colour removal (Table 2).
In comparison, the colour removing performance of
activated SBE was negligible. Noteworthy is the
behaviour of the carbonised SBE which exhibited
intermediate adsorptive characteristics in terms of
Evans activity and fl-carotenoid removal.
The removal of coloured pigments fiom edible oils
by mineral-based and carbonaceous adsorbents can be
interpreted with reference to the accepted mechanisms
of adsorption in each case.
Properties of bleaching earth credited with a role in
the removal of colour and trace impurities from edible
oils include pore size distribution, particle size, extent
of acidulation, total surface area and moisture content
(Siddiqui, 1968; Brimberg, 1982; Zyla & Olszar, 1984;
Morgan et al., 1985). Adsorption of coloured pigments
at the protonated surface of montmorillonite is
generally accepted as involving a combination of
acid-base (Bronsted) interactions and physical adsorp-
tion (Siddiqui, 1968; Fahn, 1976; Morgan et al., 1985:
Taylor et al., 1989).
In contrast, activated carbons adsorb largely on the
basis of their extended surface area and highly
56 Simon J. T. Pollard, Christopher J. Sollars, Roger Perry

Table 2. Bleaching performances of commerical and laboratory-prepared adsorbents

Bleaching parameter Colour removal Chlorophyll Lovibond colour Phosphorus

(/,g kg- ~) (absorbance) (pg g ~)
601 602 EA
Red Yellow
Rapeseed blank 0 0 0 6650 4.5 69 17
Commercial
virgin bleaching earth 44 56 100 140 1-0 7 5
Norit SA4 0 0 0 1080 4-1 68 12
Brimac CC 0 0 0 2450 4.4 68 14
BDH decolourising charcoal 0 0 0 970 4.1 69 3
Chemviron C () 0 0 620 3.4 68 12
clay:carbon 4:1 41 37 78 160 0.9 7 10
Synthesised SBE
activated SBE 0 0 0 4840 4.8 69 18
carbonised SBE 29 35 64 610 1-0 11 10
deactivated SBE 0 0 0 5750 4.2 68 15

developed microporosity. Many activated carbons also Residual Benzola[pyrene Concentration Oag k g q )

exhibit some surface acidity but this is believed to be 14

more a consequence of carboxylate functionality at the 12
edges of their extended polynuclear structure (Bansal
I0
et al., 1988) rather than direct protonation. Hence, this
lack of protonation may account for the reduced Evans 8

activity observed for these adsorbents. Chlorophyll 6

derivatives removed by the carbons in this study are
more likely to have been adsorbed on a physical basis,
the molecular dimensions of the isolated chlorophyll a
molecule (1.2 nm x 1"5 nm; Taylor et al., 1989)being
suitable for physisorption across the micro- and meso-
pore size range in these materials.
Whilst approximately 27% w/w of the available
chlorophyll derivatives were removed by the activated
SBE, no Evans activity was observed. Comparison
with the carbonised SBE control suggests that the
ZnC12 activation process employed causes a deteriora-
tion in bleaching capacity at the protonated silicate sur-
face.
The commercial materials exhibited a range of phos-
phorus-removal capacities, the most significant uptake
being demonstrated by virgin bleaching earth and the
B D H decolourising charcoal. Lovibond red and yellow
values remained essentially unaltered by the commer-
cial carbonaceous adsorbents whilst the virgin bleach-
ing earth again indicated significant removal of both
the lighter (yellow) and deeper (red) chromogenic
carotenoids present in the degummed rape sample.
Whilst fl-carotene is reported to be removed by both
bleaching earth and activated carbons (Sonntag, 1979),
these results indicate the varying specificity exhibited
by a range of commercial adsorbents for carotenoids,
chlorophylls and phospholipids and highlight the com-
petitive nature of adsorption for these substances from
rapeseed oil.
Benzo[a]pyrene removal from crude coconut oil
Residual B[a]P concentrations remaining in open-
bleached coconut oils treated using a number of
selected adsorbents are presented in Fig. 2 with 10%
4
2
0
TREATMENT
Fig. 2. B[a]P removal, by industrial and laboratory-pre-
pared adsorbents, from crude coconut oil.
error bars indicating the analytical error associated
with triplicate determination of B[a]P in the crude
sample.
Norit SA4, a standard carbon for PAH removal
from edible oils, reduced the B[a]P concentration from
a mean value of 12"8 pg kg I in the crude oil to trace
levels (< 0"1 pg kg -t) at a 2"0% w/w adsorbent dose.
The admixture of Norit SA4 with virgin bleaching
earth removed all but 0-8 pg kg- l B[a]E Virgin bleach-
ing earth alone, however, displayed a limited capacity
for B[a]E Carbonised SBE and deactivated SBE like-
wise adsorbed limited amounts of B[a]E In com-
parison, the ZnC12 activated SBE demonstrated an
appreciable capacity for B[a]P, reducing the residual
concentration in the bleached coconut oil to 1'3 pg
kg-J.
A comparison of PAH removal for these materials
with the colour removal data confirms the differential
mechanisms for the adsorptive behaviour of bleaching
 Reuse of wastes for bleaching edible oils
Residual BIaIP Concentration (~g kg 1 )
Q Synthesised S B E
14"
A Ex-Rape
12" [] Ex-Soya
+ Norit SA4
10
8 may be overcome by using admixtures of activated
6-
Mininmm Adsorption
Attained with Activated
4
Spent Bleaching Earths
2 fi _ ~
0 ,, , I ~ I
I 1.75 2 3
Adsorbent Dose (%w/w)
Fig. 3. BalP bleaching curves from crude coconut oil for
activated filter cakes and Norit SA4 carbon.
earth and activated carbon. These results suggest that
the adsorption of coloured pigments and PAH from
edible oil are distinct and at the extreme, associated
with the surface properties of acid-activated mont-
morillonite and active carbon, respectively. This is to
be expected on account of the non-polar nature of
PAH adsorbates which are more effectively adsorbed
by van der Waals attraction at the microporous carbon
surface than at the protonated surface of acidulated
montmorillonite. Uptake of B[a]P by the activated SBE
is therefore attributed directly to the active carbon
present on the interlamellar surface of this material
(['ollard eta[., 1991a,b, 1992).
Real process wastes activated under optimised con-
ditions were examined for BIaJP removal from a
second coconut oil sample and compared with the
laboratory-synthesised actiw~ted SBE (Fig. 2). Bleach-
ing curwrs were constructed for these three adsorbents
in order to assess the required dose during reuse and
l or comparison with the corresponding curve for Norit
SA4 (Fig. 3). At a 2"0% w/w dose, activated spent rape
and soybean filter cakes exhibited similar behaviour to
the laboratory-synthesised activated SBE, with residual
B[a]P levels of 1"8, 1.4 and 1.3 /~g kg i, confirming
lhem as suitable adsorbents for PAH removal. These
values correspond to B[a}P removal efficiencies of 86,
89 and t)0%. Norit SA4, in comparison, reduced BIa]P
to trace levels { < 0.1 ~ g k g 1) a t a 1 % w / w d o s e . In
these curves, our activated SBE adsorbents demon-
strated a limiting capacity for B[a]P with residual B[a]P
concentrations of approximately 1"5 /~g kg-~ remain-
ing at approximately 1"75% w/w dose.
l¥ocessing considerations
Handleability, bulk density and particle compatibility
are of principal concern when processing admixtures
of finely powdered adsorbents for edible oil bleaching.
An excess of fine particles in some powdered activated
57
carbons occasionally causes 'burst-through' problems
during filtration of the bleaching admixture, and
extremes in bulk density can result in settling during
powder blending and/or bleaching. These problems
often lead to ineffectual cleansing of the oil or even
spoiled batches of the refined product at considerable
expense to the processor. Such processing problems
SBE (which has adsorptive properties similar to acti-
vated carbon) and virgin bleaching earth for the con-
current removal of PAH and pigments from edible oils.
Activated SBE has an apparent bulk density of appro-
1.5 ppb ximately 0-6-()-7 g cm -3 compared with approxi-
mately 0-5 g cm 3 for the virgin bleaching earth
(Pollard, 1990), values which are similar enough to
4 alleviate concerns over particle incompatibility.
ACKNOWLEDGEMENTS
Materials and analytical support from Laporte Adsor-
bents and Laporte Research and Development is grate-
fully acknowledged. Technical support from Laporte
was provided by Dr D.B. Mobbs and Dr R.S. Taylor
throughout the course of this work and the authors also
wish to thank Dr M. Davies and Dr J. Williams for their
valuable comments prior to submission. One of us
(S.J.P.) wishes to acknowledge the SERC for the pro-
vision of a research studentship.
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