Methods for Quantifying Lime Incorporation into Dewatered

Sludge. I: Bench-Scale Evaluation

Jason M. North1; Jennifer G. Becker2; Eric A. Seagren, A.M.ASCE3; Mark Ramirez4; and
Christopher Peot, P.E.5

Abstract: The addition of alkaline material 共usually lime兲 to treated municipal sludge can be used to raise the pH to 艌12 and generate
Class A or B biosolids. When lime is added to dewatered sludge, it must first be made into a slurry before the pH can be measured to
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demonstrate regulatory compliance. In this study, pH 12 was achieved in slurries prepared from lime-amended dewatered sludge, even
when the lime was poorly incorporated and relatively high fecal coliform levels were detected. Thus, quantitative indicators of lime
incorporation are needed to complement slurry pH measurements and ensure that sufficient contact occurs between lime and sludge
particles to achieve adequate stabilization. In this study, the usefulness of several potential measures of lime incorporation—pH, CO2
consumption, distribution of calcium, fecal coliforms, NH3 and reduced sulfur compound production, and ATP—was systematically
evaluated using a bench-scale system. Sludge pH and CO2 consumption were not influenced by the extent of lime incorporation. The
distribution of calcium and fecal coliform levels appear to be useful measures of lime incorporation. NH3 and reduced sulfur compound
emissions and ATP levels can also be used to assess lime incorporation provided recommended experimental techniques are used.
DOI: 10.1061/共ASCE兲0733-9372共2008兲134:9共750兲
CE Database subject headings: Sludge; Lime; Mixing; Full-scale tests; Dewatering; pH; Laboratory tests.

Introduction Unfortunately, the addition of water to sludge–lime mixtures

Incorporation of alkaline material, especially lime, into mechani-
cally dewatered municipal wastewater sludge 共postlime stabiliza-
tion兲 can be used to produce materials that meet the U.S.
Environmental Protection Agency 共USEPA兲 minimum criteria for
Class B or A biosolids 共USEPA 1993兲. To meet the Class B Pro-
cesses to Significantly Reduce Pathogens 共PSRP兲 requirement for
lime-stabilized biosolids, levels of indicator organisms in these
materials must fall within maximum allowable limits, and the pH
of the biosolids must be maintained at 12 for 2 h and at 11.5 for
an additional 22 h. Achievement of the pH criterion is demon-
strated by making measurements on a slurry prepared by adding
water to the lime-amended sludge and subjecting it to additional
mixing.
1
Regional Manager, Natgun Corporation, 4500 Black Rock Rd.,
Hampstead, MD 21074. E-mail: jnorth@Natgun.com
2
Associate Professor, Dept. of Environmental Science and
Technology, Univ. of Maryland, College Park, MD 20742 共corresponding
author兲. E-mail: jgbecker@umd.edu
3 cycling of plant nutrients and organic in biosolids may not be
Associate Professor, Dept. of Civil and Environmental Engineering,
Univ. of Maryland, College Park, MD 20742. E-mail: eseagren@
eng.umd.edu
4
Biosolids Process Engineer, District of Columbia Water and Sewer
Authority 共DC WASA兲, 5000 Overlook Ave. SW, Washington, DC 20032.
E-mail: mark_ramirez@dcwasa.com
5
Biosolids Division Manager, District of Columbia Water and Sewer
Authority 共DC WASA兲, 5000 Overlook Ave. SW, Washington, DC 20032.
E-mail: chris_peot@dcwasa.com
Note. Discussion open until February 1, 2009. Separate discussions
must be submitted for individual papers. The manuscript for this paper
was submitted for review and possible publication on May 21, 2007;
approved on August 27, 2007. This paper is part of the Journal of
Environmental Engineering, Vol. 134, No. 9, September 1, 2008.
©ASCE, ISSN 0733-9372/2008/9-750–761/$25.00.
and the subsequent homogenization step make it difficult to infer
any information about the extent of lime incorporation in the
original undiluted sample. The pH levels that meet regulatory
requirements for classification as biosolids could conceivably be
measured in slurries derived from sludge samples that contain
poorly incorporated lime. In the micromorphology analyses
shown in Fig. 1, differences in the extent of lime incorporation
into biological sludges that were generated at the same wastewa-
ter treatment plant 关District of Columbia Water and Sewer Au-
thority’s 共DC WASA’s兲 Blue Plains advanced wastewater
treatment plant 共Blue Plains WWTP兲兴, but were treated in distinct
dewatering and post-lime-stabilization systems, are visually obvi-
ous. However, the pH levels measured in the two systems were
generally very similar. The apparent inability of slurry pH mea-
surements to distinguish significant differences in the extent of
lime incorporation is important because poor incorporation of
lime can result in production of malodors, which in turn can lead
to decreased public acceptance of biosolids processing and land
application programs. As a result, the potential for beneficial re-
fully realized.
It is generally recognized that adequate contact between lime
and sludge particles must occur in order to achieve adequate in-
corporation of the lime and a stable residuals product 共Metcalf &
Eddy 1991兲. As a result, most laboratory studies of postlime sta-
bilization used extended mixing times 共on the order of hours兲
共e.g., Riehl et al. 1952; Wong et al. 2001兲. Counts and Shuckrow
共1975兲 used short mixing times 共20– 30 s兲 to examine the effects
of two different bench-scale mixing types on the pH of lime-
amended sludge. However, their study involved liquid sludge,
rather than dewatered cake. The extended mixing times used in
most bench-scale studies may not be reflective of the mixing that
occurs in full-scale systems. Consequently, there is little infor-

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Fig. 1. 共Color兲 Thin sections of postlime stabilized biosolids produced by treating sludge generated at Blue Plains WWTP. Sludge dewatering and
lime stabilization was carried out either by 共A and B兲 Blue Plains WWTP or 共C and D兲 by K-F Environmental Technologies Inc. Lime-stabilized
sludge samples were obtained from the full-scale system, impregnated with clear plastic resin, dried, hardened, sliced into thin sections, attached
to slides, and polished. Sludge has a brown color; lime appears blue, and the white areas are voids.

mation available on the relationships between various stabi-
lization process parameters and lime incorporation. Further,
quantitative methods that can be used to measure the extent of
lime incorporation into mechanically dewatered sludge and the
effects of process changes on lime incorporation have not yet
been demonstrated.
Instead, techniques for assessing sludge treated using a variety
of processes, including postlime stabilization, have focused on
measures of sludge stability 共Bruce 1984; Switzenbaum et al.
2000兲. While lime incorporation and sludge stability are not
equivalent properties, they are related for post-lime-stabilized
sludge. In addition to pH and pH change during storage, Bruce
共1984兲 identified only methods that are related to sludge odor
production as being suitable for assessing the stability of lime-
stabilized sludge. More recently, Switzenbaum and co-workers
共Switzenbaum et al. 1997, 2000兲 reviewed various methods for
assessing biosolids stability. They concluded that selection of an
appropriate assessment method should be based not only on the
stabilization process, but also on the intended use of the biosolids
共e.g., as an amendment to agricultural soils, landfill cover, or for
use by homeowners兲. The pH, pH change during storage, mois-
ture, temperature, and ammonia evolution were listed 共in order of
preference兲 as appropriate stability assessment techniques for
alkaline-stabilized sludges, based on an analysis of current prac-
tice and the literature 共Switzenbaum et al. 1997兲. However, the
writers distinguished between assessment of Class A and B bio-
solids. Therefore, not all of the stability assessment methods
listed above, especially temperature and ammonia evolution, were
recommended for all combinations of biosolids classification and
intended use. In 2002, the list of recommended stability assess-
ment methods for alkaline-stabilized biosolids was narrowed to
pH and pH during storage 共Switzenbaum et al. 2002兲.
In this study, we used a bench-scale mixing system to system-
atically evaluate the usefulness of a suite of methods based on the
biological, chemical, and/or physical properties of lime-amended
sludge for quantitatively measuring the extent of quicklime 共CaO兲
incorporation into dewatered sludge. The pH was not a good in-
dicator of lime incorporation, but several useful quantitative as-
sessment methods were identified. The application of these new
methods in assessing the relationship between process parameters
and lime incorporation into sludge in a full-scale treatment system
is described in the companion paper 共North et al. 2008兲.
Materials and Methods
Experimental Approach
This paper focuses on evaluation of the following potential indi-
cators of lime incorporation 共Table 1兲: 共1兲 fecal coliforms; 共2兲
slurry pH; 共3兲 the distribution of calcium; 共4兲 NH3 evolution; 共5兲
the relative abundance of reduced sulfur compounds 共RSCs兲; 共6兲
net CO2 evolution or consumption; and 共7兲 adenosine triphos-
phate 共ATP兲 concentration. The rationale underlying the selection
of these seven potential measures of lime incorporation is de-
scribed below. Other potential measures of lime incorporation

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J. Environ. Eng. 2008.134:750-761.

 Table 1. Solids Content and Analyses Performed on Sludge Samples Collected on Different Sampling Dates
Percent
Sample solids Fecal Calcium Reduced CO2
date 共%兲 coliforms pH distribution NH3 ATP sulfur compounds evolution
July 31, 2001 25.9 3 3a
August 2, 2001 23.8 3 3
October 5, 2001 27.8 3 3
November 4, 2001 28.2 3 3a 3
January 3, 2002 27.5 3 3 3 3b 3
January 24, 2002 22.4 3 3 3 3 3a,b
April 10, 2002 27.1 3 3
Note: 3⫽analyses performed on a given sample.
a
Samples analyzed for reduced sulfur compound concentrations after incubation for a nominal 24-h period, as described in the text.
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b
Samples analyzed for reduced sulfur compound concentrations after incubation for a nominal 30-min period, as described in the text.

were evaluated as part of a larger study 共North 2003兲. For ex- cal and organic nitrogen 共Metcalf & Eddy 1991兲. NH3 evolution
ample, we were particularly interested in the possibility of using a was evaluated in this study in part because Switzenbaum et al.
flat-tip pH probe to measure the pH of lime-amended sludge 共1997兲 included it in a list of appropriate stability measures for
samples without first creating a slurry. However, reliable mea- Class A alkaline-stabilized biosolids used for purposes other than
surements were difficult to obtain with the flat-tip probe 共Orion application to agricultural lands or land reclamation or for Class
91-36 Combination Electrode兲, which is designed to measure the B biosolids used in landfill covers, although NH3 was subse-
pH of semisolid materials. The pH measured at the surface was quently dropped from the list 共Switzenbaum et al. 2002兲. Micro-
not stable and dropped quickly. More stable measurements could bial decomposition of organic nitrogen in unstabilized sludge
be made in the interior of a sludge sample, but accurate readings could increase its ammoniacal nitrogen content. Therefore, am-
could be obtained only by adding distilled water, which could moniacal nitrogen levels should decrease with improved lime in-
dissolve unincorporated lime. Therefore, the use of the flat-tipped corporation. On the other hand, the percentage of ammoniacal
pH probe was not explored further. Other potential measures of nitrogen released as NH3 by lime-treated sludge should increase
lime incorporation that were evaluated but, in the interest of brev- as incorporation and pH increase.
ity, are not reported here, include the available lime concentra-
tion, calcium speciation, and pH decay. Relative Abundance of RSCs
An increase in lime dosage has previously been shown to de-
Fecal Coliforms crease the production of RSCs from alkaline-stabilized sludge
Theoretically, as the incorporation of lime into dewatered sludge 共Hwang et al. 1994兲, presumably due to decreased microbial me-
increases, the inactivation of fecal coliforms in randomly obtained tabolism of sulfur-containing constituents of municipal waste-
subsamples should also increase. Fecal coliform levels are also water and microbial cells. Therefore, we were also interested in
routinely measured in stabilized sludge to assess compliance with evaluating whether the production of RSCs is influenced by,
the USEPA Part 503 rule 共USEPA 1993兲. Therefore, fecal and provides a measure of, lime incorporation. One challenge
coliform levels were used as a quantitative benchmark in the de- associated with the assessment of RSC production is that a large
velopment of the experimental mixing system for reproducibly number of reduced sulfur species with widely varying chemical
generating lime–sludge mixtures with varying degrees of lime compositions may be produced from unstable wastewater residu-
incorporation and in evaluating the usefulness of other potential
measures of lime incorporation.
Table 2. Relative Response of the Jerome 631-X Hydrogen Sulfide
pH Analyzer to Reduced Sulfur Speciesa
The pH of sludge following dilution and mixing with water was
included in the suite of lime incorporation assessment methods Response factor
evaluated in this study because it is used in the classification of Compound 共%兲
alkaline-stabilized biosolids 共USEPA 1993兲, and it is recom- Hydrogen sulfide 100
mended for the assessment of the stability of alkaline-stabilized Carbonyl sulfide 36
biosolids 共Switzenbaum et al. 1997; 2000, 2002兲. Dimethyl sulfide 7
Diethyl sulfide 25
Distribution of Calcium
Carbon disulfide 0.01
The distribution of lime in sludge should be a function of lime
Dimethyl disulfide 40
incorporation and was evaluated directly by calculating the
Diethyl disulfide 17
sample standard deviation and variance about the average calcium
Methanethiol 45
concentrations in randomly obtained subsamples from lime-
amended sludge. n-Propylthiol 40
n-Butylthiol 33
NH3 Evolution t-Butylthiol 35
Nitrogen is present in untreated primary and secondary municipal Thiophene 0.8
a
wastewater treatment sludges primarily in the form of ammonia- Information obtained from instrument manufacturer.

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J. Environ. Eng. 2008.134:750-761.

 als. The production of multiple reduced sulfur species and the
potential for these compounds to undergo further chemical and
biological transformations make the quantification of RSC pro-
duction using conventional analytical techniques, e.g., gas
chromatography, impractical for routine assessment of lime incor-
poration at wastewater treatment facilities. A much simpler ap-
proach for quantifying total reduced sulfur species was needed in
this study. Therefore, an analyzer that responds to a variety of
reduced sulfur species, including H2S 共Table 2兲, was used to
quantify the relative amount of total RSCs released by the sludge.
Absolute measurement of the abundance of RSCs was not pos-
sible because the response of the analyzer to different compounds
varies.
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Net CO2 Evolution or Consumption
CO2 is a product of microbial respiratory processes. Therefore,
CO2 evolution should decrease with the extent of microbial inac-
tivation and is widely used as a method for assessing the stability
of composted biosolids and solid waste 共Switzenbaum et al.
2002兲. However, interpretation of CO2 evolution data could po-
tentially be complicated, particularly in alkaline-stabilized sludge,
because CO2 can react with hydrated lime, according to
Ca共OH兲2 + CO2 → CaCO3 + H2O 共1兲
and it can be consumed through autotrophic microbial metabo-
lism in unstable sludge. Therefore, the usefulness of net CO2
evolution 共or consumption兲 as an indicator of lime incorporation
was also evaluated in this study.
ATP Concentration
ATP is potentially useful as a general measure of biomass because
it is the central molecule for storage of metabolic energy and
occurs in all living cells. It has been used to quantify viable bio-
mass in a wide variety of systems 共Karl 1980兲, including waste-
water 共Jorgensen et al. 1992兲 and lime-stabilized sludge 共Paulsrud
and Eikum 1975兲. Previous studies also showed that ATP levels
decreased due to the addition of lime and high pH 共Patterson et al.
1970; Paulsrud and Eikum 1975兲 and greater reductions in ATP
concentrations occurred as the lime dosage became larger 共Patter-
son et al. 1970兲. Therefore, ATP was evaluated as a potential
measure of lime incorporation in this study, and we expected that
as lime incorporation and microbial inactivation increased, sludge
ATP levels would also decrease.
Preparation of Lime–Sludge Mixtures with Different
Levels of Incorporation
To evaluate a potential measure of lime incorporation, dry granu-
lar lime was added to five 1-kg subsamples of freshly collected
sludge at a dose of 20% on a dry weight basis. The lime contained
92–94% CaO and was purchased from Chemstone 共Strasburg,
Va.兲 by DC WASA contractor K-F Environmental Technologies
共KF, Glen Burnie, Md.兲, which dewatered and postlime stabilized
a portion of the biosolids generated at the Blue Plains WWTP.
Approximately 90% of the lime particles passed through a No. 10
mesh 共2-mm nominal sieve opening兲 and approximately 8% of
the particles passed through a No. 60 mesh 共0.25-mm nominal
sieve opening兲 共North et al. 2008兲. To reproducibly achieve dif-
ferent levels of lime incorporation, each lime-amended subsample
was mixed at the lowest setting 共stir兲 in the bench-scale mixing
system, a Kitchen Aid K5SS Heavy Duty Mixer equipped with a
five-quart mixing bowl and flat beater mixing tool, for 10, 20, 30,
40, and 90 共or 100兲 s. The effectiveness of the bench-scale mixing
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J. Environ. Eng. 2008.134:750-761.
system at achieving different levels of lime incorporation at these
mixing times was evaluated by monitoring fecal coliform levels
in sludge samples that were collected on 22 different days be-
tween June 12, 2001, and April 10, 2002, and contained 22.4–
28.2% solids, as discussed below.
A minimum of 8 L of sludge was collected for analysis of
fecal coliform levels and one or more potential measures of lime
incorporation on each of seven different sampling days. Each as-
sessment method was tested using sludge obtained on at least two
dates. Sludge was collected from the outlet of one of seven cen-
trifuges in the sludge dewatering system at Blue Plains WWTP,
which is described in the companion paper 共North et al. 2008兲.
The sampling dates are summarized in Table 1, along with the
solids content and analyses performed on the sludge collected on
different days. Along with every set of lime-amended samples,
one or two unstabilized sludge controls that were not amended or
mixed with lime were maintained. Subsamples were randomly
collected from the lime–sludge mixtures that were mixed for dif-
ferent lengths of time or unstabilized sludge and apportioned on a
wet weight basis for analysis using one or more potential mea-
sures of lime incorporation.
Analytical Methods
Fecal coliforms were quantified in 1-g subsamples of unlimed
controls or lime-amended sludge obtained from the bench-scale
mixer using the membrane filter technique, according to Standard
Method 9222D 共APHA/AWWA/WEF 1998兲. The membrane fil-
tration technique was used in this study because it generated re-
sults more quickly than the multiple-tube fermentation technique,
which is required for classification of Class A biosolids 共USEPA
1993兲, and a comparison of fecal coliform levels in lime-amended
sludge samples measured using the two techniques yielded simi-
lar results 共North 2003兲. However, samples analyzed using the
membrane filtration technique had to be diluted at least 100-fold
to avoid interference from sludge solids. Each 1-g subsample of
sludge was blended with phosphate-buffered dilution water
共99 mL兲 in a commercial laboratory blender, before being serially
diluted and filtered.
The pH was measured at room temperature in slurries prepared
by adding 10 g of sludge 共measured on a wet weight basis兲 to
20 mL of DI water and occasionally mixing by hand for 30 min
共USEPA 2003兲. Calcium concentrations were determined using
1-g sludge subsamples that were diluted with 99 mL of dilution
water 共Hardy Diagnostics, Santa Maria, Calif.兲, mixed in a com-
mercial laboratory blender, and stored for less than a week at
4 ° C. Maryland Environmental Services 共Annapolis, Md.兲 per-
formed microwave-assisted acid digestion of the sludge samples
according to USEPA method 3051A 共USEPA 2007兲 prior to
analysis of calcium concentrations using inductively coupled
plasma atomic emission spectroscopy according to USEPA
method 200.7 共USEPA 2001兲.
ATP was extracted from 1-g samples of sludge in sterile
150-mL glass test tubes following the method of Webster et al.
共1983兲. Extraction solution 共9 mL兲 was added to each tube along
with the sludge and 0.67 mL of Antifoam A 共Sigma Chemical,
St. Louis兲. The extraction solution contained H3PO4 共0.67 M,
laboratory grade, J.T. Baker Inc., Phillipsburg, N.J.兲, urea 共2 M,
ultrapure grade, ICN Biochemicals, Aurora, Ohio兲, dimethyl sul-
foxide 共20%; protease/DNase/RNase free, Sigma兲, adenosine
共1.8 mg, laboratory grade, ICN Biochemicals兲, ethylene diamine
tetraacetic acid 共20 mM, laboratory grade, Fisher兲, and Zwitter-
gent 3–10 detergent 共1%; laboratory grade, EMD Biosciences,
 Darmstadt, Germany兲. The tubes were maintained at 4 ° C or on
ice for all remaining extraction steps. Microbial cell lysis was
accomplished by sonicating the test tubes using a Sonic Vibra
Cell 共Newtown, Conn.兲 for 30 s. Each test tube was then shaken
in a wrist-action shaker for 30 min before transferring the con-
tents to a sterile 15-mL centrifuge tube, which was placed on ice
and centrifuged at 1,500 rpm for 20 min. The supernatant was
transferred to another sterile 15-mL centrifuge tube. The 1-mL
aliquots of the supernatant were dispensed in duplicate or tripli-
cate to sterile 15-mL centrifuge tubes and diluted with 9 mL of
0.1 M Tricine buffer salts solution 共Sigma-Aldrich, St. Louis兲.
The amount of 1.02 g / mL ethanolamine 共Laboratory grade, ICN
Biochemicals, Aurora, Ohio兲 needed to titrate the samples to pH
7.6–7.8 was determined by adding phenol red to an aliquot that
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was not analyzed for ATP. The same amount of ethanolamine

solution was added to the remaining sample共s兲 共without phenol
red兲, which were stored for up to one week at −20° C or diluted
and analyzed immediately. A 10−3 dilution of each sample was
prepared using a 0.1 M Tricine buffer solution to eliminate inter-
ference caused by particles and analyzed in duplicate using a
luciferin–luciferase-based assay 共FLAAM ATP assay mix; Sigma,
St. Louis兲 and a TD20/20 Luminometer 共Turner Designs, Sunny-
vale, Calif.兲. The ATP concentrations in samples were determined
by comparison with a standard curve prepared by reacting serial
dilutions of an ATP standard 共Sigma, St. Louis兲 with the FLAAM
ATP assay mix.
For analysis of NH3, reduced sulfur compounds, or CO2, ap-
proximately 200-mg sludge samples were placed in 1-L Teflon
jars equipped with a screw-tight lid, two 1/4-in. gas-sampling
ports 共Savillex Corporation, Minnetonka, Minn.兲, and a gas inlet
check valve that made it possible to replace the volume of gas
removed for analysis with an equivalent volume of air. NH3 con-
centrations were measured by incubating samples for 30 min at
room temperature, inserting a NH3 gas detection tube 共0.2–200 or
50– 900 ppm, Sensidyne, Clearwater, Fla.兲 into a sampling port,
and then drawing a 100-mL headspace sample through the detec-
tion tube using a Sensidyne AP-1S pump.
The relative abundance of the total RSCs was measured by
incubating samples at room temperature for nominal periods of
30 min and/or 24 h before drawing a 25-mL headspace sample
through a Jerome 631-X hydrogen sulfide analyzer that was con-
nected to a sampling port on the Teflon jar via Teflon tubing. After
closing the incubation chambers, measurement of reduced sulfur
emissions was made within ⫾1 min of the nominal 30-min incu-
bation time and within ⫾0.5 h of the 24-h incubation time, except
on January 24, 2002. On January 24, 2002, sampling was delayed
slightly and the incubation times averaged 39 min 关⫾10 min, 1
standard deviation 共SD兲兴 and 27.6 h 共⫾33 min, 1 SD兲. Only con-
centrations that fell within the detection range reported by the
manufacturer 共3 – 50 ppm兲 are reported.
Net CO2 production or consumption was quantified using
a modification of a method developed for the analysis of soils
共Zibilske 1994兲. An 84-mL wide-mouth glass bottle containing
20 mL of CO2-free 1 N NaOH was placed in the center of a 1-L
Teflon incubation jar. The sludge sample was also placed in the
Teflon jar in a ring around the bottle containing the NaOH before
sealing the jar and incubating the sample for 30 min. 3 N BaCl
was added in excess to the NaOH, followed by three drops of
phenol red indicator. Unreacted NaOH was quantified by titration
with 0.2 N HCl. The mass of CO2 trapped by NaOH in the jars
containing sludge is reported relative to the amount of CO2 that
reacted with NaOH in jars that did not contain sludge.
Fig. 2. Geometric mean of fecal coliform concentrations in sludge
samples that were amended with lime and mixed for different lengths
of time. Geometric means were calculated based on concentrations
measured in: 艌21 samples collected on 艌12 different days for the
10-, 20-, 30-, and 40-s mixing times; four to six samples collected on
three different days for the 15- and 80-s mixing times; and nine
samples collected on six different days for the 60- and 100-s mixing
times. Error bars represent ⫾1 SD. Samples in which no colonies
were detected in any of the sample dilutions were not included in the
analyses. The censored data points were associated with samples
mixed for 20– 90 s and represented approximately 15% of the total
number of analyzed samples 共n = 162兲.
Results
Evaluation of Bench-Scale Mixing System
The first step in this study was to develop a bench-scale mixing
system for reproducibly generating samples with different degrees
of lime incorporation into dewatered sludge cake. Different levels
of incorporation were achieved by mixing lime-amended sludge
samples for varying amounts of time. Fecal coliform levels were
measured to evaluate the suitability of this approach and are
shown in Fig. 2. Overall, the geometric mean of the fecal
coliforms levels decreased with increased mixing time. The geo-
metric mean of fecal coliform levels in 26 unlimed control
samples collected from the full-scale sludge handling system on
17 different days was 107.40 CFU/ g dry sludge. Mixing lime and
sludge cake for 10– 20 s resulted in less than a 2 log reduction in
the geometric mean of the fecal coliform level. In contrast, a
3 – 4 log reduction in the geometric mean of the fecal coliform
level occurred when lime was mixed with sludge cake for
40– 90 s. The standard deviations about the geometric mean of
the fecal coliform levels in the lime-amended sludge also de-
creased with longer mixing times. These data provide clear evi-
dence that fecal coliform destruction during postlime stabilization
increases with the extent of mixing. To our knowledge, this has
been previously suggested 共e.g., WEF 1995兲, but not demon-
strated. The fecal coliform data also showed that operation of the
experimental mixing system for 10 to approximately 90 s could
be used to consistently produce samples that exhibited varying
degrees of lime incorporation for dewatered sludge cake contain-
ing 22.4–28.2% solids and were suitable for evaluation of other
potential quantitative measures of lime incorporation.

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Fig. 3. Fecal coliform concentrations 共䊐兲 and pH 共쎲兲 in
lime-amended sludge samples obtained on 共a兲 October 5, 2001;
and 共b兲 April 10, 2002, and mixed for varying lengths of time in a
bench-scale mixer. Fecal coliform levels were below the detection
limit in the October 5, 2001, samples mixed for 100 s and one sample
mixed for 60 s and in the April 10, 2002, samples mixed for 90 s.
For all other data points, the geometric mean of fecal coliform
concentrations in duplicate samples is shown. pH data points are
average concentrations in 共a兲 five or 共b兲 four replicates. Error bars
represent ⫾1 SD.
Sludge that was collected from the full-scale system on at least
two different days was amended with lime, mixed in the bench-
scale system for varying lengths of time, and then analyzed for
pH, calcium distribution, emission of ammonia, ATP, emission of
reduced sulfur compounds, and/or net CO2 production or con-
sumption 共Table 1兲. Fecal coliforms were also measured in all
lime-amended sludge samples and unstabilized controls.
Assessment of Measures of Lime Incorporation
The pH of slurries prepared from unstabilized controls was 6.4–
6.5. An average pH value of approximately 12 was measured in
homogenized slurries prepared from sludge that was mixed with
lime for 10– 100 s 共Fig. 3兲, suggesting that the slurry pH was not
influenced by the extent of lime incorporation in the original
samples. In contrast, fecal coliform levels in the same samples
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J. Environ. Eng. 2008.134:750-761.
Fig. 4. Fecal coliform and calcium concentrations in lime-amended
sludge samples obtained on January 24, 2002, and mixed for varying
lengths of time in a bench-scale mixer. 共a兲 Fecal coliform levels 共䊐兲
were below the detection limit in one 30- and 40-s sample and in both
samples mixed for 90 s. For all other data points, the geometric mean
of fecal coliform concentrations in duplicate samples is shown. 共b兲
Calcium concentration averages 共䉭兲 and variances 共쎲兲 were based
on analysis of 10 replicates. Error bars represent ⫾1 SD.
were affected by mixing times. Less than 1 log reductions in the
geometric mean of the fecal coliform levels were achieved when
undiluted sludge collected on either day was mixed for 10 or 20 s,
but approximately 4 log reductions were attained when mixing
times of 40 s or more were used.
The background calcium concentration in unstabilized sludge
was approximately 2% on a dry weight basis 共0.02 g / g dry sludge
solids兲. The average calcium concentration in randomly collected
subsamples of lime-amended sludge collected on a single day
remained relatively constant 共15–22% on a dry weight basis or
0.15– 0.22 g Ca/ g dry sludge solids兲 regardless of mixing time
共Fig. 4兲. These average concentrations compare well with the tar-
get dose of 20% CaO 共93% activity兲 on a dry weight basis.
However, the standard deviations of the calcium concentra-
tions measured in replicate samples that were mixed for a rela-
tively long period of time 共艌30 s兲 were much smaller compared
to the standard deviations in calcium concentrations in samples
mixed for only 10– 20 s. The trend in the distribution of calcium
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Fig. 5. Fecal coliform concentrations 共䊐兲 and NH3 共쎲兲 in
lime-amended sludge samples obtained on 共a兲 January 3, 2002;
and 共b兲 January 24, 2002, and mixed for varying lengths of time in a
bench-scale mixer. The January 24, 2002, fecal coliform data also
appear in Fig. 4. In the January 3, 2002, samples, fecal coliform
levels were below the detection limit in one sample mixed for 30 s
and in one sample mixed for 90 s. For all other data points, the
geometric mean of fecal coliform concentrations in duplicate samples
is shown, excepted as noted in Fig. 4 for the January 24, 2002,
samples. NH3 concentrations represent the averages in 共a兲 two or 共b兲
three replicates. NH3 concentrations in the January 3, 2002, samples
mixed for 90 s exceeded the range of the detection tubes. Error bars
represent ⫾1 SD.
as a function of mixing time is better illustrated by the variances
of the calcium concentrations in replicate subsamples 关Fig. 4共b兲兴.
Variances greater than 200 percent-squared are indicative of
lime that was unevenly distributed in poorly mixed samples,
i.e., samples mixed for 10 or 20 s, and variances of 20 percent-
squared or lower indicate that lime was homogeneously distrib-
uted in samples that were mixed for 30 s or more. The trend in
the variances was closely paralleled in the fecal coliform mea-
surements 关Fig. 4共a兲兴. The geometric mean of fecal coliform
concentrations in lime-amended samples mixed for 10 or 20 s
were similar to the concentration in unstabilized sludge, but de-
creased significantly in samples mixed for 30 or 40 s and were
not detectable in lime-sludge mixtures subjected to 90 s of mix-
756 / JOURNAL OF ENVIRONMENTAL ENGINEERING © ASCE / SEPTEMBER 2008
J. Environ. Eng. 2008.134:750-761.
Fig. 6. Fecal coliform concentrations 共䊐兲 and ATP 共쎲兲 in
lime-amended sludge samples obtained on 共a兲 January 3, 2002;
and 共b兲 January 24, 2002, and mixed for varying lengths of time in a
bench-scale mixer. The fecal coliform data represent the geometric
mean in duplicate samples, except as noted in Fig. 5. ATP
concentrations represent the averages in triplicate samples. Error bars
represent ⫾1 SD.
ing. Similar results were obtained with sludge collected on an-
other day 共Table 1兲, but are not shown in the interest of brevity.
A gas-phase NH3 concentration 艋0.2 ppm was measured in
the incubation chamber controls containing unstabilized sludge.
This relatively low level of NH3 production was expected because
the pH of the unlimed sludge was less than 7; therefore, any
ammoniacal nitrogen in the unstabilized sludge would primarily
have been present in the ionized, nonvolatile form. NH3 concen-
trations measured in all of the incubation chambers containing
lime-amended samples were higher than in the control chambers
and increased with mixing times of up to 40 s 共Fig. 5兲. The in-
crease in NH3 concentrations was mirrored by a decrease in the
fecal coliform levels when the mixing time was increased from 10
or 20 s to 30 s or more.
The geometric mean of the ATP concentrations in triplicate
unstabilized sludge controls was 1,418 and 7,617 ng ATP/ g sol-
ids on January 3, 2002, and January 24, 2002, respectively. ATP
concentrations in the lime-treated sludge samples were lower than
in the corresponding unstabilized controls 共Fig. 6兲, with one ex-
ception. The geometric mean of the ATP concentrations in the
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Fig. 7. Fecal coliform concentrations 共䊐兲 and CO2 共쎲兲 in
lime-amended sludge samples obtained on 共a兲 November 4, 2001;
and 共b兲 January 3, 2002, and mixed for varying lengths of time in a
bench-scale mixer. The January 3, 2002, fecal coliform data also
appear in Figs. 5 and 6. The fecal coliform concentrations represent
the geometric mean in duplicate samples, except as noted in Fig. 5.
CO2 concentrations represent the averages in triplicate samples. Error
bars represent ⫾1 SD.
January 3 lime-amended sludge samples mixed for only 10 s 关Fig.
6共a兲兴 was not significantly different than the average concentra-
tion in the unstabilized sludge, indicating that 10 s of mixing did
not incorporate lime enough to substantially decrease microbial
activity. Increasing the mixing time up to 30 s in lime-amended
sludge samples prepared on either day substantially decreased the
ATP concentrations. As discussed above, fecal coliform concen-
trations also decreased with mixing time in these samples 共Fig. 6兲.
CO2 levels measured in empty incubation chambers ranged
from 6.6 to 8.4 mg/ L. The CO2 levels measured in the control
chambers containing unstabilized sludge ranged from 46 to
58 mg/ L, indicating net CO2 production due to the high level of
microbial activity in these samples. The CO2 concentrations in
nearly all of the gas evolution chambers containing lime-amended
samples 共Fig. 7兲 were below the levels measured in the empty
chambers, indicating net consumption of CO2. The CO2 concen-
trations did not appear to be related to mixing time and lime
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J. Environ. Eng. 2008.134:750-761.
Fig. 8. Total reduced sulfur compounds 共RSCs兲 in lime-amended
sludge mixed for varying lengths of time in a bench-scale mixer. 共a兲
Average RSC concentrations in eight January 3, 2002, samples after
incubation for 30 min 共䊐兲, three July 31, 2001, samples incubated for
24 h 共쎲兲, and six November 4, 2001, samples incubated for 24 h
共䉱兲. 共b兲 Average RSCs measured in the January 24, 2002, samples
after a nominal incubation time of 30 min 共䊐兲 or 24 h 共쎲兲. Error
bars represent ⫾1 SD.
incorporation. In contrast, the fecal coliform levels in the lime-
amended samples decreased with increasing mixing time, as pre-
viously noted.
The suitability of nominal sample incubation periods of
30 min and 24 h for measurement of RSC concentrations was
evaluated. As shown in Fig. 8共a兲, the production of RSCs from
replicate samples during a given incubation period was very re-
producible, and similar RSC levels were observed for samples
that were collected on two different days and incubated for 24 h.
The amount of RSCs emitted from an unstabilized sludge control
increased from ⬃2 ppm after a 30 min incubation time to more
than 50 ppm after incubation of the sample for 24 h. Greater pro-
duction of RSCs was also observed in lime-amended samples that
were mixed for 艋20 s and incubated for 24 h compared with
those mixed for the same length of time and incubated for 30 min
关Fig. 8共a兲兴.
In samples incubated for 30 min, RSC concentrations in-
 creased with longer mixing times, i.e., with better lime incorpo-
ration 关Fig. 8共a兲兴. RSC concentrations measured after 24 h
decreased with increased mixing time. Variations in the properties
of sludge could conceivably have contributed to the different
trends in RSC concentrations as a function of mixing time ob-
served on different days. Therefore, RSC production in a single
set of lime-amended sludge samples was measured after approxi-
mately 30 min and again after slightly more than 24 h 关Fig. 8共b兲兴.
The amount of RSCs detected after the short incubation period
again increased with longer mixing times, while increased mixing
decreased RSC accumulation over a 24-h period.
Discussion
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The pathogen and vector attraction reduction requirements of the
USEPA Part 503 rule require elevated pH levels 共12 for 2 h, fol-
lowed by 11.5 for an additional 22 h兲 in Class B biosolids stabi-
lized with lime 共or other alkali兲. The USEPA provides guidance
on how to meet these regulatory requirements when the addition
of lime to dewatered sludge produces sludge masses that are not
entirely penetrated by the lime, i.e., the lime is not well incorpo-
rated 共USEPA 2003兲. Two alternatives are recommended. One
alternative is to mix thoroughly the sludge–lime composite before
preparing a slurry from a subsample of the composite and mea-
suring the slurry pH. The second option is to sample the interior
of a sludge mass when preparing the slurry used to analyze the
pH.
The slurry pH results obtained in this study suggest that ho-
mogenization of the sample before making pH measurements
may not provide an accurate assessment of biosolids quality.
Samples mixed for the shortest time periods 共艋20 s兲 in the
bench-scale mixing system contained regions of sludge that did
not react with lime. Nevertheless, homogeneous slurries prepared
from randomly obtained samples of these poorly mixed sludge–
lime composites attained high initial pH values that are consistent
with regulatory requirements, despite the fact that fecal coliform
levels were relatively high 共Fig. 3兲. Clearly, pH should be in-
cluded in protocols for assessing the stability and quality of lime-
treated biosolids, as previously recommended 共Switzenbaum et al.
1997, 2002; USEPA 2003兲. Measuring slurry pH using samples
obtained from regions of the dewatered sludge where little lime
seems to be present, e.g., in the interior of sludge masses, is a
conservative approach that can help ensure that the lime dose has
the potential to achieve adequate reduction of pathogens and vec-
tor attraction. However, the necessary levels of pathogen and vec-
tor attraction reduction will be realized only if sufficient contact
occurs between lime and sludge particles, which can be assessed
only by measuring the extent of lime incorporation.
This study identified several useful measures of lime incorpo-
ration that can be used to quantify the effects of process param-
eters on lime incorporation and complement assessment of lime
dose based on pH. The heterogeneous nature of samples mixed
for short periods 共艋20 s兲 was reflected directly in the large vari-
ability in the distribution of calcium 共measured as the standard
deviation or variance in calcium concentrations; Fig. 4兲. Because
large portions of the sludge in these samples did not contact lime
and attain an elevated pH, little ammoniacal nitrogen was re-
leased as NH3 from these samples 共Fig. 5兲, and they exhibited
high levels of microbial activity, which was reflected in the high
fecal coliform, ATP 共Fig. 6兲, and RSC concentrations 共Fig. 8兲.
Lime incorporation and sample homogeneity improved with mix-
ing in the bench-scale system. As a result, the variance in calcium
758 / JOURNAL OF ENVIRONMENTAL ENGINEERING © ASCE / SEPTEMBER 2008
J. Environ. Eng. 2008.134:750-761.
concentrations and the concentrations of ATP, RSCs, and fecal
coliforms diminished with increased mixing. NH3 levels in-
creased with mixing, and like the variance in calcium concentra-
tions and the concentrations of ATP, RSCs, and fecal coliforms, is
a good indicator of lime incorporation. In contrast, the concentra-
tion of CO2 in the incubation chambers, like pH, did not provide
useful information on the extent of lime incorporation.
Recommended Methodologies
It is important to note that in obtaining the NH3 data shown in
Fig. 5, special care was taken to prevent NH3 loss during collec-
tion of the samples. Most importantly, the size of the lime-
amended sludge samples was quickly determined on a volumetric
basis so that samples could be transferred to, and enclosed in, the
incubation chambers within 30 s of completing the mixing step.
We found that when we took the time to precisely weigh the mass
of lime-amended sludge being transferred, which resulted in a
somewhat longer period of time between the mixing and incuba-
tion steps, the NH3 levels did not increase with mixing time as
shown in Fig. 5. Instead, the NH3 concentrations measured in the
incubation chambers actually decreased somewhat with mixing
time 共data not shown兲. Apparently, NH3 release occurred very
rapidly in the samples mixed for the longest times; and, therefore,
substantial amounts of NH3 escaped before the samples were
placed in the incubation chambers. Thus, the wet weight of the
sludge added to a preweighed incubation chamber was deter-
mined by difference and converted to a dry weight using the
experimentally determined percent solids of the sludge. The
average dry weight of sludge samples used to measure NH3 con-
centrations following this approach was 42.3⫾ 7.9 g 共average
⫾standard deviation兲.
Another important implication of this study is that if RSCs are
used as a measure of lime incorporation, the measurements
should be made after 24 h to ensure that they reflect biological
activity. The release of RSCs within the first 30 min of incubation
共Fig. 8兲 is probably due to an increase in temperature because the
reaction between quicklime 共CaO兲 and water in sludge is exother-
mic 共Smith et al. 1998兲
CaO + H2O → Ca共OH兲2 ⌬H = − 65.23 kJ/mol 共2兲
The ambient temperature of the unamended sludge was, typi-
cally, 28° C. The addition of 20% lime 共dry weight basis兲 to
sludge with a solids content of 25% solids 共the average for sludge
used to assess reduced sulfur compound concentrations after
30 min; Table 1兲 would result in a temporary increase in sludge
temperature to 44.5° C if the lime was well incorporated, and thus
completely reacted 共Metcalf & Eddy 1991兲. As the sludge tem-
perature increases, the amount of volatile reduced sulfur com-
pounds measured in the headspace also goes up. The relationship
between temperature and the volatilization of a reduced sulfur
compound is reflected in the dimensionless Henry’s constant 共Hc兲
values, where Hc⫽ratio of the gas-phase concentration of a vola-
tile compound 共M / L3兲 to the aqueous concentration 共M / L3兲 at
equilibrium. Hc values were calculated from Przyjazny et al.
共1983兲 for two reduced sulfur compounds—dimethyl sulfide and
dimethyl disulfide—that were previously detected in emissions
from lime-stabilized biosolids at the Blue Plains WWTP 共Murthy
et al. 2002兲. Hc increases from 0.08 at 28° C to 0.16 at 44.5° C for
dimethyl sulfide and from 0.05 at 28° C to 0.10 at 44.5° C for
dimethyl disulfide. The volumes of gas and water in the gas evo-
lution chambers were estimated using the wet weight of sludge
added to each chamber, the sludge density, and the average per-
 cent solids, and were used along with the Hc values to estimate
the fraction of dimethyl sulfide and dimethyl disulfide that would
reside in the gas phase at 28 and 44.5° C. At 28° C, approximately
27% of the dimethyl sulfide in the sludge would partition into the
gas phase. At 44.5° C, the fraction of dimethyl sulfide residing the
gas phase would increase to approximately 46%. A similar shift in
the distribution of dimethyl disulfide would occur with an in-
crease in temperature. Smith et al. 共1998兲 found that a relatively
small fraction of the heat produced from the reaction of water
with CaO added to sludge at a 20% dose was consumed in water
evaporation 共rather than heating the sludge兲. Thus, it is possible
that the sludge temperatures following the addition of lime were
slightly lower than calculated above. Nevertheless, the temporary
increases in temperature resulting from the addition of lime would
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have been substantial and could have contributed to the relatively
high gas-phase concentrations of reduced sulfur species measured
at longer mixing times.
Biological processes, which generally exhibit longer time
scales compared with abiotic reactions, probably did not contrib-
ute substantially to the RSC concentrations measured during the
first 30 min after mixing. However, after the initial abiotic reac-
tions, substantial microbial activity, and thus biological produc-
tion of RSCs, presumably occurred in the unamended controls
and in unstabilized regions of the poorly mixed sludge. This prob-
ably explains why the concentrations of RSCs that accumulated in
the unamended sludge control increased from 12.5 ppm after ap-
proximately 30 min of incubation to ⬎50 ppm after incubation
for 24 h. In the sludge samples that were mixed with lime for the
longest periods of time, little microbiological activity and produc-
tion of reduced sulfur compounds occurred. As a result, the levels
of RSCs measured after 24 h were similar to those measured dur-
ing the first 30 min of incubation in the well-mixed samples.
The ATP assay is highly sensitive to experimental conditions
such as temperature and light and to the sample characteristics
and treatment methods. It is likely that variability in these factors
contributed to the large differences in the ATP levels measured
on different days. Paulsrud and Eikum 共1975兲 found that biologi-
cal municipal wastewater sludge contained nearly twice as much
ATP as primary sludge. In the current study, the percentage of
secondary sludge in the biosolids varied from day to day. For
example, the sludge collected on January 24, 2002, contained
56% secondary sludge, compared with 51% secondary sludge
on January 3, 2002. Greater amounts of biomass could help
explain why ATP levels were higher in the unstabilized sludge
and the lime-amended sludge mixed for the shortest times on
January 24, 2002, than in the analogous January 3, 2002, samples
共Fig. 6兲. The higher solids level in the January 3, 2002, samples
may also have contributed to lower measured ATP concentrations
by blocking or scattering the light that was produced by the reac-
tion of a luciferase enzyme with ATP, although the dilution of
samples 1,000-fold prior to the enzyme reaction step appeared to
minimize interference from the solids in this study. Because of the
cost and potential complexities associated with ATP measure-
ment, Bruce 共1984兲 recommended that the use of ATP in assess-
ing sludge stability should be restricted to research applications.
While we believe that ATP concentrations may also be a useful
measure of lime incorporation in more routine monitoring appli-
cations, we do recommend that the ATP concentrations measured
in the lime-amended samples should only be interpreted relative
to the levels measured in unstabilized sludge sampled on the same
day.
Although five different measures for assessing incorporation
of lime in post-lime-stabilization operations are recommended
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J. Environ. Eng. 2008.134:750-761.
here, some measures may be more suitable than others for use at
a particular plant. Fecal coliforms are recommended for routine
checks of lime incorporation at facilities that measure fecal
coliforms to assess compliance with the USEPA Part 503 regula-
tions. At these facilities, it would not require much extra effort to
use a bench-scale mixer to determine the benchmark level of fecal
coliforms that could be achieved in thoroughly blended sludge–
lime admixtures, as discussed below and by North et al. 共2008兲.
Quantification of NH3 and RSCs requires the purchase of special-
ized equipment, but the analytical methods described in this paper
are simple to carry out, and thus may also be appropriate at many
plants for routine assessment of lime incorporation or periodic
evaluation of the effects of process changes on lime incorpora-
tion. NH3 and RSC data may be particularly useful at facilities
that are concerned about sludge odors. The equipment and meth-
ods used to analyze many metals of interest in biosolids can also
be used in the quantification of calcium. However, the calcium
distribution is probably most useful for periodic evaluations of
lime incorporation because of the length of time required to ob-
tain the analytical results. Quantification of ATP is more labor
intensive and technically challenging than the other recommended
methods but may be appropriate for periodic assessment of lime
incorporation at some facilities, e.g., to corroborate the results
obtained using another measure of lime incorporation.
Practical Implications
If odors or fecal coliform counts suggest that the level of lime
incorporation being achieved at a post-lime-stabilization facility
is less than optimal or highly variable, investigators can use a
simple and inexpensive set of procedures based on the measures
of lime incorporation identified in this study to determine if lime
incorporation can be improved in the full-scale system, e.g., see
the companion paper by North et al. 共2008兲. If the evaluation of
lime incorporation will be based on the distribution of calcium, a
parameter that is not strongly influenced by the biological and
chemical properties of the untreated sludge, a benchmark value
that is characteristic of well-mixed sludge can readily be obtained
for comparison with the properties of sludge samples obtained
from the full-scale system. To determine the benchmark calcium
distribution in well-mixed sludge, at least 5 kg of unlimed dewa-
tered sludge should be collected from the full-scale system just
prior to the lime/sludge blender. A 1-kg sample of sludge should
be placed in a bench-scale mixer like the one used in this study,
amended with lime at the intended dosage, and operated at the
lowest 共stir兲 setting for 10 s before stopping the mixer and ran-
domly removing 10–15 1-g samples for analysis of calcium. The
procedure should be repeated four times using fresh subsamples
of the sludge collected from the full-scale system and a range of
mixing times that will result in different levels of lime incorpo-
ration. Although some variability among treatment plants is ex-
pected, based on the results of this study, it is likely that 10 s of
mixing will result in poor lime incorporation and 90 s of mixing
will thoroughly incorporate the lime.
The standard deviation 共or variance兲 in the calcium concentra-
tions should be calculated for each mixing time using standard
statistical methods, and the minimum standard deviation 共or vari-
ance兲 in calcium concentrations should be determined. The mini-
mum value will be attained at the longest mixing times 共as shown
in the plots of bench-scale mixing data in Fig. 4兲, but it is impor-
tant to note that the bench-scale mixing times are irrelevant to the
full-scale operation. The minimum standard deviation 共or vari-
 ance兲 in calcium concentrations can be used as a benchmark to
which measures of full-scale lime incorporation can be compared.
Full-scale lime incorporation can be measured by taking
10–15 samples of limed sludge from the full-scale system for
analysis of calcium concentrations. If the standard deviation 共or
variance兲 of the calcium concentrations calculated for the samples
mixed in the full-scale system is higher than the minimum value
achieved in the bench-scale system, then the amount of lime in-
corporation being achieved in the full-scale system is suboptimal.
In this case, it is possible that changes like those described in the
companion paper 共North et al. 2008兲 could be made to the sludge
stabilization process to improve lime incorporation. When this
approach was used to assess lime incorporation in the Blue Plains
post-lime-stabilization process before implementing several pro-
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cess changes, the standard deviation of calcium concentrations
measured in the limed samples obtained from the full-scale was
similar to that obtained after mixing unlimed sludge with lime for
10– 30 s in the bench-scale system 共North et al. 2008兲. These data
indicated that the level of lime incorporation being achieved in
the full-scale system was far from optimal. If, on the other hand,
the standard deviation 共or variance兲 in the calcium concentrations
calculated for the full-scale system is as low as the minimum
value achieved in the bench-scale system, then it is unlikely that
changes in the full-scale operation could improve lime incorpora-
tion and biosolids quality.
Assessment of lime incorporation in the full-scale system
using an approach similar to that outlined above for calcium con-
centrations can also be based on measurement of fecal coliforms,
ATP, NH3, or RSCs produced by the sludge. Because these pa-
rameters may be strongly influenced by the biological and chemi-
cal properties of the untreated sludge, which can vary daily,
measurement of fecal coliforms, ATP, NH3, or RSCs in limed
sludge collected from the full-scale system and lime/sludge mix-
tures prepared in the bench-scale mixer should be performed on
the same day.
Conclusions
Poor incorporation of lime into dewatered sludge can potentially
lower the quality of alkaline-stabilized biosolids. A bench-scale
mixing system was used in this study to generate samples with
varying degrees of lime incorporation. The pH of homogeneous
slurries prepared from post-lime-stabilized sludge provides im-
portant information on the lime dose, but was not influenced by
the extent of lime incorporation achieved in the bench-scale
mixer. Thus, the extent of lime incorporation in dewatered sludge
should be quantified to complement pH measurements and better
characterize the quality of post-lime-stabilized biosolids.
Several quantitative measures of lime incorporation in dewa-
tered sludge were identified in this study, including fecal
coliforms and the distribution of calcium, which was measured as
the standard deviation or variance in the calcium concentrations.
An advantage of measuring the calcium distribution is that it is
probably not substantially affected by day-to-day variations in
untreated sludge properties. The use of fecal coliform measure-
ments to assess lime incorporation is also appealing because
many utilities routinely measure fecal coliforms to demonstrate
that the USEPA Part 503 pathogen reduction requirements are
being met. NH3 emissions, RSCs, and ATP also appear to be
excellent measures of lime incorporation, provided recommended
procedures are followed. Meaningful information on lime incor-
poration can be obtained from NH3 data only if the lime-amended
760 / JOURNAL OF ENVIRONMENTAL ENGINEERING © ASCE / SEPTEMBER 2008
J. Environ. Eng. 2008.134:750-761.
sludge samples can be quickly sealed in appropriate incubation
chambers. An incubation of at least 24 h is recommended for
RSC measurements. Emission of these compounds immediately
following lime addition is probably largely due to physicochemi-
cal changes that result from the reaction of lime with water in the
sludge and may be influenced by the sludge properties. The char-
acteristics of the sludge also may influence the relative concen-
tration of ATP and other molecules such as NH3. Therefore, it is
recommended that levels of ATP and NH3 and their implications
with respect to lime incorporation should be interpreted relative to
their levels measured in unstabilized sludge on the same day.
Acknowledgments
Financial support for this project was provided by DC WASA.
Irina Y. Chikounova provided valuable technical assistance.
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