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 Bioresource Technology 95 (2004) 53–59

Evaluating heavy metal contents in nine composts using

four digestion methods
Zeng-Yei Hseu *

Department of Environmental Science and Engineering, National Pingtung University of Science and Technology,
Pingtung 91201, 1 Hsieh-Fu Road, Nei-Pu, Pingtung 91201, Taiwan, ROC
Received 10 February 2003; received in revised form 16 May 2003
Available online 11 March 2004

Abstract
The production and application of compost potentially contaminate the environment with heavy metals. The heavy metal
contents of composts must be exactly determined. Therefore, this study aims to understand the heavy metal contents in composts,
using different digestion methods and to recommend the most appropriate digestion method making this measurement. Nine
composts from different sources, including swine manure, poultry litter, food waste, municipal sewage sludge, soybean meal, wood
residues, flesh-bone dust, fish-bone meal and guano, were selected to be digested by four methods to determine the contents of Cd,
Cr, Cu, Mn, Ni, Pb and Zn by AAS. The four digestion methods were nitric acid, dry ashing, nitric–perchloric acid and sulfuric acid
methods. Analytical results indicated that the nitric acid procedure was the most efficient for recovering Cd, Mn and Ni from most
compost samples. The sulfuric acid procedure yielded the lowest recovery of Pb from the certified reference material (BCR 146) and
the compost samples, especially from the composts with high pH and EC values potentially high in Ca. The nitric acid procedure
was recommended as the method for digesting the composts herein, based on recovery analysis, cost and time taken. Dry ashing was
recommended as a flexible method. Nitric–perchloric acid procedure was not recommended because perchloric acid is potentially
hazardous during digestion and it recovers relatively little heavy metal.
Ó 2004 Elsevier Ltd. All rights reserved.

Keywords: Heavy metal; Compost; Digestion method; Nitric acid

1. Introduction the heavy metals either in solution or in a form that is

The production of compost from agricultural and
industrial wastes, and municipal by-products is an
important means of recovering organic matter and an
essential method of disposal. Compost is applied to
cropland to maintain and improve soil structure and
plant nutrition (Gigliotti et al., 1996). However, the
presence of heavy metals in composts is the main cause
of adverse effects on animal and human health, trans-
mitted through the food chain from soil, groundwater
and plants (Senesi et al., 1999). Consequently, exactly
analyzing the contents of heavy metal in composts is
very important for the routine monitoring and risk
assessment and regulation of environment.
Elemental analysis of a compost sample requires that
the organic fraction of the sample be destroyed, leaving
*
Tel.: +886-8-7740253; fax:+886-8-7740320.
E-mail address: zyhseu@mail.npust.edu.tw (Z.-Y. Hseu).
readily dissolved. The approaches for destroying organic
material and dissolving heavy metals fall into two
groups-wet digestion by acid mixtures prior to elemental
analysis and dry ashing, followed by acid dissolution of
the ash (Zarcinas et al., 1987). Various methods have
been presented for digesting plant tissue and soil sam-
ples for metal analysis. However, composts have very
different physical, chemical and biological properties
from those of soils and plants. Gorsuch (1959) discov-
ered that methods of digestion that involved mixtures of
nitric, sulfuric or perchloric acids were satisfactory for
digesting mineral elements in organic and biological
materials. Rodushkin et al. (1999) used two digestion
methods, including open-vessel digestion with concen-
trated nitric acid and microwave digestion with a mix-
ture of concentrated nitric acid and hydrogen peroxide,
to analyze heavy metals in cereal and coniferous tree
samples by ICP-AES. They found that both procedures
supported the fast preparation of numerous samples,

0960-8524/$ - see front matter Ó 2004 Elsevier Ltd. All rights reserved.
doi:10.1016/j.biortech.2004.02.008
54 Z.-Y. Hseu / Bioresource Technology 95 (2004) 53–59

matching the high through-put of samples by ICP Some standard reference materials, similar to a
techniques, but the open-vessel digestion procedure compost matrix, have been used to elucidate the recov-
provided the advantage of low equipment cost and less ery of heavy metals by different digestion methods
need for pretreating the samples. Most wet oxidation (Zarcinas et al., 1987; De Abreu and Berton, 1996;
procedures require the use of a combination of acid and Moral et al., 1996). However, little attention has been
oxidant, of which the most commonly used are nitric, paid to samples of popularly used composts. No stan-
sulfuric and perchloric acids and hydrogen peroxide dard official methods of digestion of composts exist in
(Hoenig, 1995). However, perchloric acid is potentially Taiwan to measure amounts of heavy metals. Therefore,
hazardous during the digestion of biological materials the aims of this study are to (1) evaluate the contents of
and can cause the loss of potassium and boron (Zarcinas Cd, Cr, Cu, Mn, Ni, Pb and Zn in nine composts using
and Cartwright, 1983). Dry ashing may cause some different digestion methods; (2) explain the dissolution
elements to be lost by the volatilization or adsorption of by the digestion methods, using inorganic acid mixtures,
elements on the walls of the furnace, such that As, Cr of composts, and (3) recommend the most appropriate
and Pb may be lost at ashing temperatures of 500–550 digestion method for determining the seven heavy met-
°C (Azcue and Mudroch, 1994). als in the various composts.
Previous studies have established good procedures for
measuring the total metal concentration in soil and sedi-
ment samples dissolved by concentrated mixtures of
2. Methods
inorganic acids at high temperatures (Agemian and Chau,
1976; Ammons et al., 1995; Hossner, 1996; Chen and Ma,
2.1. Compost samples
1998; Hseu et al., 2002; Sastre et al., 2002). Less is known
about the relative recovery of heavy metals from com-
Nine mature composts from different sources in
posts by the widely used digestion methods (Zheljazkov
Taiwan were used in this study. They were swine man-
and Warman, 2002). Many methods for digesting com-
ure, poultry litter, food waste, municipal sewage sludge,
post have been described in previous studies; they include
soybean meal, wood residues, flesh-bone dust, fish-bone
concentrated nitric acid digestion, dry ashing, nitric–
meal and guano. Swine manure was obtained from the
perchloric acid digestion and sulfuric acid digestion.
Livestock Farm of National Pingtung University of
These methods are considered to be appropriate for
Science and Technology (NPUST). Food waste, from
pseudo-total analysis. However, they do not completely
typical Chinese food and tropical fruit residues, was
dissolve silicate, but they are sufficiently good to attack
collected and composted from the restaurant of
and dissolve heavy metals bound to important compost
NPUST. Municipal sewage sludge was obtained from
constituents (Zheljazkov and Warman, 2002). Heavy
the Min-Seng Wastewater Treatment Plant in Taipei
metals in the silicate mineral require digestion with
City. The other composts were commercially available
hydrofluoric acid (HF) and strong acids. However, the
and purchased from markets. All composts were air-
use of HF in routine laboratories is not recommended, as
dried and ground to pass through a 1 mm stainless sieve;
it is highly corrosive and difficult to handle. Sastre et al.
they were then stored in the plastic bottle prior to
(2002) stated that nitric acid digestion was an optimum
analysis. The selected properties of the composts were
method for estimating heavy metal content in soil samples
determined as follows: the pH of the compost/distilled
with high organic matter content, being superior to
water mixture (2.5:1) was determined using a glass
microwave-assisted and aqua regia digestions. De Abreu
electrode (McLean, 1982); the organic matter content
and Berton (1996) presented statistically higher values for
was measured by the Walkley-Black wet oxidation
Cd, Cr, Cu, Fe, Mn, Ni, Pb and Zn concentrations in
method (Nelson and Sommers, 1982); the total nitrogen
municipal waste compost, sewage sludge and swine
amount was determined by the regular Kjeldahl method
manure obtained by an aqua regia method than were
(Bremner and Mulvaney, 1982); electrical conductivity
obtained by nitric acid and nitric–perchloric acid meth-
(EC) was measured from the extract of a saturated paste
ods. Zheljazkov and Warman (2002) used nitric acid, ni-
of compost (Rhoades, 1982).
tric and perchloric acids and dry ashing digestion methods
to analyze 17 elements in six composts from Canada. They
found that nitric acid digestion provided the highest 2.2. Methods of digestion
recovery of As, Mo, Ni and Se; that nitric and perchloric
acids provided the highest recovery of Co, and dry ashing Before digestion to analyze heavy metals, each
recovered most Mn. Both nitric acid and nitric–perchloric compost sample was dried at 65 °C for 48 h. Four
acid provided similar levels and better recovery of Cd and digestion methods were applied herein, involving nitric
Pb, than dry ashing. Inhat and Fernandes (1996) found acid, dry ashing, nitric–perchloric acid and sulfuric
that nitric acid effectively recovered 21 elements from acid. All methods were performed in triplicate for each
composted poultry manure, excluding Mn. sample.
 Z.-Y. Hseu / Bioresource Technology 95 (2004) 53–59
2.2.1. Nitric acid digestion
This approach was partly modified from that of
Zheljazkov and Nielson (1996). One gram of sample was
placed in a 250 ml digestion tube and 10 ml of concen-
trated HNO3 was added. The sample was heated for 45
min at 90 °C, and then the temperature was increased to
150 °C at which the sample was boiled for at least 8 h until
a clear solution was obtained. Concentrated HNO3 was
added to the sample (5 ml was added at least three times)
and digestion occurred until the volume was reduced to
about 1 ml. The interior walls of the tube were washed
down with a little distilled water and the tube was swirled
throughout the digestion to keep the wall clean and
prevent the loss of the sample. After cooling, 5 ml of 1%
HNO3 was added to the sample. The solution was filtered
with Whatman No. 42 filter paper and <0.45 lm Milli-
pore filter paper. It was then transferred quantitatively to
a 25 ml volumetric flask by adding distilled water.
2.2.2. Dry ashing
One gram of sample in a crucible was placed in a
preheated muffle furnace at 200–250 °C for 30 min, and
then ashed for 4 h at 480 °C. Then, the sample was re-
moved from the furnace and cooled down; 2 ml of 5 M
HNO3 was added and evaporated to dryness on a sand
bath. Next, the sample was placed in a cool furnace and
heated to 400 °C for 15 min, before being removed (from
the furnace, cooled and moistened with four drops of
distilled water). Next, 2 ml of concentrated HCl was
added and the sample was evaporated to dryness, re-
moved, and then 5 ml of 2 M HCl was added and the
tube was again swirled. The solution was filtered
through Whatman No. 42 filter paper and <0.45 lm
Millipore filter paper, and then transferred quantita-
tively to a 25 ml volumetric flask by adding distilled
water (Issac and Kerber, 1971).
2.2.3. Nitric–perchloric acid digestion
Nitric–perchloric acid digestion was performed, fol-
lowing the procedure recommended by the AOAC
(1990). One gram of sample was placed in a 250 ml
digestion tube and 10 ml of concentrated HNO3 was
added. The mixture was boiled gently for 30–45 min to
oxidize all easily oxidizable matter. After cooling, 5 ml
of 70% HClO4 was added and the mixture was boiled
gently until dense white fumes appeared. After cooling,
20 ml of distilled water was added and the mixture was
boiled further to release any fumes. The solution was
cooled, further filtered through Whatman No. 42 filter
paper and <0.45 lm Millipore filter paper and trans-
ferred quantitatively to a 25 ml volumetric flask by
adding distilled water.
2.2.4. Sulfuric acid digestion
This method is the wet digestion procedure described
by Jones and Case (1990). 0.5 g of sample was placed in
55
a 250 ml digestion tube and 3.5 ml of concentrated
H2 SO4 was added. The mixture was allowed to stand for
30 min at room temperature. About 3.5 ml of 30% H2 O2
was added to the digestion tube and the sample was then
heated at 250 °C for 30 min. Thereafter, the digestion
tube was removed from the digestion block and cooled
down. 1 ml of 30% H2 O2 was added until the digest was
clear upon cooling. When the solution was clear fol-
lowing cooling, it was filtered through Whatman No. 42
filter paper and <0.45 lm Millipore filter paper and
transferred quantitatively to a 25 ml volumetric flask by
adding distilled water.
2.3. Heavy metal analysis
The concentrations of Cd, Cr, Cu, Mn, Ni, Pb and Zn
in the final solutions were determined by an atomic
absorption spectrometer (AAS) (Hitachi Z-8100,
Japan).
2.4. Quality assurance and quality control
Two standard reference materials, including SRM
1573a (tomato leaves) from the National Institute of
Standards and Technology (NIST), USA, and BCR 146
(sewage sludge) from the Commission of European
Community, Belgium, were digested in triplicate and
analyzed using the four methods to support quality
assurance and control (QA/QC). Table 1 shows the
recoveries of heavy metals in the two standard reference
materials by four digestion methods. The recoveries of
seven elements by the four methods ranged from 63% to
111%, respectively. A blank was run for each digestion
procedure to correct the measurements. For sets of every
ten samples, a procedure blank and spike sample,
involving all reagents, was run to check for interference
and cross contamination. Table 2 lists the method
detection limits (MDL) of the four digestion procedures.
2.5. Statistical analysis
Significant differences between concentrations of
heavy metals, following different digestion methods were
analyzed by ANOVA (SAS Institute, 1982). Statistical
significance was defined as p < 0:05.
3. Results and discussion
3.1. Characteristic of compost
Table 3 presents the selected characteristics of all
composts. The pH values ranged from strongly acidic
(5.2) for municipal sewage sludge to slightly alkaline
(8.3) for soybean meal. All of the composts include large
amounts of organic matter, ranging from 17.7% to
56 Z.-Y. Hseu / Bioresource Technology 95 (2004) 53–59

Table 1
The recovery analysis of heavy metal content (mg kg 1 ) in two certified reference materials
Cd Cr Cu Mn Ni Pb Zn
SRM 1573a (Tomato leaves)
Certified 1.52 1.99 4.70 246 1.59 –a 30.9
Nitric acid 1.38 (91%)b 2.15 (108%) 4.18 (89%) 210 (85%) 1.25 (79%) – 25.6 (83%)
Dry ashing 1.42 (93%) 1.83 (92%) 4.32 (92%) 232 (94%) 1.38 (87%) – 26.4 (85%)
Nitric–perchloric 1.30 (86%) 1.78 (89%) 4.27 (91%) 253 (103%) 1.13 (71%) – 24.2 (78%)
acid
Sulfuric acid 1.34 (88%) 1.52 (76%) 3.87 (82%) 224 (91%) 1.25 (79%) – 27.5 (89%)
BCR 146 (Sewage sludge)
Certified 77.7 – 934 588 280 1270 4059
Nitric acid 52.5 (68%) – 683 (73%) 445 (76%) 201 (72%) 1135 (89%) 3678 (91%)
Dry ashing 56.3 (72%) – 672 (72%) 492 (84%) 208 (74%) 1215 (96%) 3415 (84%)
Nitric–perchloric 49.3 (63%) – 711 (76%) 474 (81%) 215 (77%) 983 (77%) 4132 (102%)
acid
Sulfuric acid 65.7 (85%) – 651 (70%) 380 (65%) 310 (111%) 942 (74 %) 3024 (75%)
a
Not certified.
b
Number in the parentheses is recovery (%).

Table 2 faunal composts including swine manure, poultry litter,

Method detection limits (mg kg 1 ) for different digestion methods of flesh-bone dust, fish-bone meal and guano.
AAS in this study
Nitric acid Dry Nitric–per- Sulfuric
ashing chloric acid acid 3.2. Comparison of different digestion methods
Cd 0.002 0.007 0.004 0.004
Cr 0.08 0.08 0.07 0.10 3.2.1. Cadmium
Cu 0.02 0.04 0.03 0.04 The concentrations of Cd in the soybean meal and the
Mn 0.05 0.04 0.06 0.06 flesh-bone dust were not detectable by any of the four
Ni 0.03 0.02 0.02 0.03 digestion methods; the concentration of Cd was higher
Pb 0.10 0.08 0.05 0.06
in the poultry litter than in all other composts (Table 4).
Zn 0.02 0.03 0.03 0.07
No significant (p < 0:05) differences existed between
four digestion methods in terms of the recovery of Cd
from swine manure. Of the four digestion methods, ni-
Table 3 tric acid was the most efficient in recovering Cd from all
Selected characteristics of the composts in this study composts, except for the guano. However, less Cd was
Compost pH OMa (%) C/N ECb (dS/m) recovered from most composts digested by nitric–
Swine manure 7.6 61.3 18.4 3.10 perchloric procedure was less than that recovered by
Poultry litter 7.9 40.4 10.0 1.69 nitric acid alone. Dry ashing yields a similar recovery
Food waste 6.2 49.6 15.3 2.34 rate to nitric–perchloric acid for swine manure, poultry
Municipal 5.2 25.4 14.0 0.21
sewage sludge
litter, food waste, wood residue and guano. The sulfuric
Soybean meal 8.3 22.8 15.1 0.20 acid procedure always recovered the least Cd from all
Wood residues 7.2 17.7 20.7 0.10 composts, except guano.
Flesh-bone dust 5.4 87.9 10.7 0.61
Fish-bone meal 6.9 69.3 10.4 2.31
Guano 8.1 24.5 6.92 1.35 Table 4
a
Cadmium contents (mg kg 1 ) in 9 composts by four digestion methods
Organic matter.
b
Electrical conductivity. Nitric Dry ash- Nitric–per- Sulfuric
acid ing chloric acid acid
Swine manure 1.31a 1.22a 1.11a 1.10a
Poultry litter 7.01a 6.84ab 6.38ab 6.04b
87.9%, respectively. The C/N values, ranging from 6.92 Food waste 0.49a 0.43b 0.40bc 0.36c
Municipal 2.42a 2.09ab 1.99b 1.87b
to 20.7, were within the normal range for mature com-
sewage sludge
post (Zucconi and de Berttoldi, 1987). The differences Soybean meal ND ND ND ND
between floral and faunal composts were clearly re- Wood residues 0.35a 0.26ab 0.23b 0.19b
flected by their respective EC values. However, the EC Flesh-bone dust ND ND ND ND
values of the floral composts, including soybean meal Fish-bone meal 1.80a 1.64a 1.39b 1.38b
Guano 0.20c 0.28b 0.33b 0.73a
and wood residues, were much lower than those of the
 Z.-Y. Hseu / Bioresource Technology 95 (2004) 53–59 57

Table 5 Table 6
Chromium contents (mg kg 1 ) in 9 composts by four digestion Copper contents (mg kg 1 ) in 9 composts by four digestion methods
methods Nitric Dry Nitric–per- Sulfuric
Nitric Dry Nitric–per- Sulfuric acid ashing chloric acid acid
acid ashing chloric acid acid Swine manure 511b 481b 626a 510b
Swine manure 4.18c 10.3a 7.83b 2.40d Poultry litter 112b 90.0b 139a 136a
Poultry litter 6.00bc 15.2a 4.94c 6.93b Food waste 488a 459a 512a 477a
Food waste 90.3b 95.7a 44.7c 44.4c Municipal 179a 172a 165a 182a
Municipal 4.17b 81.7a 26.0c 25.6c sewage sludge
sewage sludge Soybean meal 13.5b 10.9b 40.0a 34.0a
Soybean meal 5.17b 9.28a 8.74a 3.66c Wood residues 10.5c 17.2b 22.7a 20.5a
Wood residues 45.2b 56.0a 35.3c 29.3c Flesh-bone dust 15.0a 11.0ab 13.5a 7.65b
Flesh-bone dust 4.09a 3.03b 1.42c 3.39ab Fish-bone meal 4.55c 21.0a 17.4ab 13.8b
Fish-bone meal 3.86c 14.3a 3.67c 9.74b Guano 128b 76.5c 144ab 172a
Guano 11.3a 9.47a 9.98a 3.64b

3.2.4. Manganese
3.2.2. Chromium Manganese is relatively abundant in the composts
The highest concentration of Cr was found by all used in this study (Table 7). The recovery of Mn in the
digestion methods in the food waste (Table 5). Dry composts is affected not only by the digestion method,
ashing recovered significantly more Cr from all com- but also by the type of compost. For example, the nitric
posts except flesh-bone dust, than did any the digestion acid procedure may recover more Mn from municipal
method. Chromium exists in a number of oxidation sewage sludge and soybean meal than from swine
states, and the most stable and common forms are manure and guano.
Cr(VI) and Cr(III). These two forms have very differ-
ent chemical properties, and Cr(VI) is more toxic and 3.2.5. Nickel
more readily extracted from solid particles, while The four digestion methods did not significantly differ
Cr(III) is less mobile and adsorbed tightly onto sili- in terms of the recovery of Ni from the swine manure
ceous materials (McGrath and Smith, 1990). The and the fish-bone meal (Table 8). The nitric acid pro-
digestion power of dry ashing is related to the high cedure showed more Ni in the composts, except in
temperature and the reactivity of free chlorine formed poultry litter and soybean meal, than any other proce-
in the final solution; dry ashing is thus a better means dure. However, dry ashing was more efficient in recov-
of extracting refractory metals, such as Cr. The sulfuric ering Ni than were nitric–perchloric acid and sulfuric
acid procedure still recovered the least Cr from most acid procedures. Sulfuric acid exhibited the highest
compost samples. The nitric acid and nitric–perchloric recovery only from the guano sample.
acid procedures did not significantly differ in terms of
recovering Cr from the swine manure, fish-bone meal 3.2.6. Lead
and guano. The sulfuric acid procedure showed poor recovery
from the composts with higher pH and EC values, such
3.2.3. Copper as swine manure, poultry litter and guano (Tables 3 and
The Cu content was highest in swine manure and 9), probably because of the precipitation of Pb and the
food waste, regardless of the digestion method used. potential interference of PbSO4 during the subsequent
However, nitric–perchloric acid and sulfuric acid pro-
cedures were more efficient than nitric acid and dry Table 7
ashing procedures in recovering Cu from all compost Manganese contents (mg kg 1 ) in 9 composts by four digestion
samples (Table 6). During the nitric–perchloric acid methods
procedure, adding HClO4 accelerated the digestion. Nitric Dry Nitric–per- Sulfuric
Copper has a high affinity for organic compounds acid ashing chloric acid acid
(McBride, 1989), so using a digestion agent with a Swine manure 666c 840b 1044a 859b
stronger oxidizing capacity results in the more complete Poultry litter 237d 624a 551b 494c
decomposition the compost. Therefore, more Cu was Food waste 204a 189a 206a 211a
Municipal 212a 179b 139c 154c
recovered in digestion procedures in which stronger
sewage sludge
oxidants, such as HClO4 and H2 SO4 were involved. Soybean meal 351a 263b 262b 263b
However, HClO4 , when hot, is a strong oxidant and can Wood residues 318a 342a 320a 324a
react with explosive force when brought into contact Flesh-bone dust 49.5b 25.0d 40.0c 53.0a
with easily oxidizable compounds, especially if the Fish-bone meal 103ab 92.7c 98.5bc 107a
Guano 598c 1536b 1808a 193d
digestion mixture is almost dry.
58 Z.-Y. Hseu / Bioresource Technology 95 (2004) 53–59

Table 8 Table 10
Nickel contents (mg kg 1 ) in 9 composts by four digestion methods Zinc contents (mg kg 1 ) in 9 composts by four digestion methods
Nitric Dry Nitric–per- Sulfuric Nitric Dry Nitric–per- Sulfuric
acid ashing chloric acid acid acid ashing chloric acid acid
Swine manure 20.0a 19.3a 19.5a 22.6a Swine manure 1382b 1240c 1506a 836d
Poultry litter 14.5b 14.6b 34.2a 14.6b Poultry litter 670bc 628c 693b 781a
Food waste 64.3a 58.3a 28.7c 43.8b Food waste 623ab 577b 628ab 673a
Municipal 49.4a 51.3a 11.5b 18.8b Municipal 1056ab 1265a 974b 1118ab
sewage sludge sewage sludge
Soybean meal 7.13b 9.99a 8.20ab 3.57c Soybean meal 74.4a 35.3c 53.5b 55.3b
Wood residues 54.7a 55.4a 45.4b 27.0c Wood residues 135ab 128b 139ab 177a
Flesh-bone dust 1.60a 1.85a 1.06b 0.99b Flesh-bone dust 62.3b 48.0b 60.0b 97.4a
Fish-bone meal 15.9a 15.5a 14.4a 16.7a Fish-bone meal 103a 24.2b 22.0b 87.9a
Guano 4.55ab 4.19bc 3.71c 5.24a Guano 190a 111b 206a 222a

analysis. Relatively insoluble CaSO4 may be formed,
lowering Pb by coprecipitation from the compost sam-
ple with higher Ca content, as identified from pH and
EC values. However, better dissolution is exhibited by
the other methods, especially nitric acid digestion, which
is associated with the lowest costs of reagents and
equipment.
3.2.7. Zinc
Zinc was the most abundant heavy metal in swine
manure and municipal sewage sludge, according to all
digestion methods. However, the methods clearly
determined widely different Zn contents (Table 10). No
digestion method recovered the most Zn from all com-
posts, but nitric acid and sulfuric acid procedures were
recommended for recovering more Zn from most com-
post samples than the other methods.
procedures in recovering Cu in all compost samples. As
determined the certified reference material (BCR 146),
the sulfuric acid procedure recovered the least Pb (Table
1). However, the sulfuric acid procedure recovered least
Pb from most of the composts with high pH and EC
values, and potentially high levels of Ca. Consequently,
the sulfuric acid procedure should not be used to
determine the Pb content in compost with a high Ca
content obtained by precipitation. The observed total
Zn contents in all composts, determined by these four
methods, differed greatly, implying the wide range of
amounts of metals in the collected compost samples.
HNO3 was used to prevent explosive reactions of the
organic matter with HClO4 prior to the sample was di-
gested. In summary, the nitric acid procedure is rec-
ommended as the method for digesting composts, based
on recovery analysis and cost and time effectiveness. Dry
ashing is a flexible method, especially for recovering Cr.

3.3. Recommended digestion method

4. Conclusion
The nitric acid procedure was the most efficient
method for recovering Cd, Mn and Ni from most Although all the composts showed different pH and
compost samples herein. Dry ashing was the most effi- EC values, nitric acid digestion was the most efficient in
cient in recovering Cr, and was not the least efficient terms of the recovery of the heavy metals in this study,
poorest method for recovering any of the other six ele- especially for Cd, Mn and Ni. Based on cost and time
ments. Nitric–perchloric acid and sulfuric acid proce- effectiveness, the nitric acid procedure was recom-
dures were more efficient than nitric acid and dry ashing mended as the standard method for digesting composts
in a traditional open-vessel digestion system. Dry ashing
Table 9 is recommended as a flexible method. The sulfuric acid
Lead contents (mg kg 1 ) in 9 composts by four digestion methods procedure typically recovered least of the seven heavy
Nitric Dry Nitric–per- Sulfuric metals and should not be used to determine the Pb
acid ashing chloric acid acid content in compost. Nitric–perchloric acid procedure is
Swine manure 3.35b 2.27c 7.07a 2.44bc not recommended because perchloric acid is potentially
Poultry litter 8.11b 9.23b 15.9a 6.00b hazardous during digestion and recovers relatively little
Food waste 77.2a 66.7b 71.9ab 50.9c heavy metal.
Municipal 71.0b 83.0a 65.5c 17.8d
sewage sludge
Soybean meal 6.78a 9.10a 8.74a 8.90a
Wood residues 27.3a 27.5a 22.5a 10.8b Acknowledgements
Flesh-bone dust 13.9a 14.0a 11.8a 8.19b
Fish-bone meal 4.71b 12.2a 3.16b 2.10b The authors would like to thank the National Science
Guano 10.7a 6.55b 6.26b 5.28c
Council of the Republic of China for financially sup-
 Z.-Y. Hseu / Bioresource Technology 95 (2004) 53–59
porting this research under Contract No. NSC91-2313-
B-020-023.
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