pISSN 2093-2332 eISSN 2287-5638

J. Korea Soc. Waste Manag., Vol. 37, No. 5, pp. 327-334, July 2020
https://doi.org/10.9786/kswm.2020.37.5.327 Original Paper

Evaluating Remediation Efficiency of Functional Oyster Shell Powder

for Organically Enriched Sediment

Md Akhte Khirul·Beom-Geun Kim·Daechul Cho*·Sung-Hyun Kwon**,†

Department of Ocean System Engineering, College of Marine Science, Gyeongsang National University
*Department of Energy and Environmental Engineering, Soonchunhyang University
**Department of Marine Environmental Engineering, Gyeongsang National University
(Received 10 April 2020 : Revised 29 June 2020 : Accepted 1 July 2020)

Abstract

Eutrophication is a serious environmental issue in coastal areas, caused by increased nutrient concentration from external
sources. Nutrients could augment in the bottom sediment and be released into overlying water, acting as an internal nutrient
source. Converted oyster shell powders were used to evaluate the suppression of nutrients release from bottom sediments.
Two kinds of oyster shell powder were applied into the sediment in the individual column with the control column. The
natural oyster shell powder (NOSP) was composed of calcium carbonate and the functional oyster shell powder (FOSP)
was composed of calcium peroxide. In the column where FOSP was applied, pH was increased due to hydrolysis of calcium
peroxide in the overlying water. The concentration of dissolved oxygen in the FOSP-treated columns was higher than that
of the control column. The FOSP could suppress the release of ammonia nitrogen and phosphates from the sediment into
the overlying water. It was proven that FOSP can effectively adsorb phosphates from organically enriched sediments.
Overall, the application of FOSP could effectively control nutrient release from the sediment to overlying water and help
reduce the eutrophication in the coastal areas.

Key Words : Marine sediment, Eutrophication, Remediation, Phosphate, Oyster shell powder, Nitrification

I. Introduction matter keeps on the bottom water and consumes dis-

The extensive eutrophication of coastal area is a most
serious problem. Marine eutrophication has been increased
due to agricultural, industrial wastewater, aquaculture
activities etc. Nutrients are deposited into sediments and
its released into water by the existing organic matter
decomposition in the sediment1). Several coastal regions
in South Korea has a lot of problems such as blue tide,
raw scum, the wideness of smelly gas and eutrophica-
tion. In consequence, input nutrients contain organic
First author : Md Akhte Khirul, Ph.D. student, Gyeongsang
National University
Co-author : Beom-Geun Kim, Master’s student, Gyeongsang
National University, Daechul Cho, Prof., Soonchunhyang
University
†
Corresponding author : Sung-Hyun Kwon, Prof., Gyeongsang
National University, shkwon@gnu.ac.kr, 055-772-9132
solved oxygen. Under reduced condition, generates
nutrients to overlying water from sediment for the
degeneration of organic matter2). Consequently, NH4+-N
and PO43-P are an important contributor to the enhance-
ment of hypoxia. It may reason, the dissolved oxygen
depletion in the water caused by its oxidation resulting in
the digression of marine ecosystems. On the contrary,
the depletion of oxygen is an enormous effect on aquatic
organisms and occasionally occur economic losses to
aquaculture activities. So, it is necessary to cut down the
sulfide concentration in the sediments wherein sustain
healthy ecosystems and keep up effective aquaculture
activities.
The southeastern coastal area in Korea is one of the
most productive oyster farming water in the world and it
contribute a large part of the local economy. Though,
annually about 250,000 tons of waste oyster shells are

327
328 Md Akhte Khirul·Beom-Geun Kim·Daechul Cho·Sung-Hyun Kwon
produced and most of the shells left untreated for long
time3). These oyster shells are consisting of 97% cal-
cium carbonate4). In fact, huge amounts of oyster shell
dumped into public water and reclaimed lands near the
seaside, causing odor problems because of the environ-
mental degradation5). Thus, recycling of waste oyster
shells has appeared as an essential issue in the maricul-
ture area. It is this important to find way to use oyster
shell which is reduce environmental problems. Several
studies on the application of oyster shells as a materials
filter in the food and chemical industries4), construction
materials6-7), soil conditioner8), sludge conditioner9), cement
clinker10), catalyst11), desulphurization sorbents12) and fil-
tering medium13) etc. Some of the waste oyster shells are
used for chicken feed and limestones in fertilizer14). The
Korean government has led to the investment of a fertil-
izer plant to enhance recycling of oyster shells15).
The purpose of the study are (1) the effects of pH, DO
on the release of nutrients into overlying water from sed-
iments, (2) to develop converting waste oyster shells and
to examined the remediation ability of functional oyster
shell powders application to organically enriched sedi-
ment-water column in terms of suppressing NH4+-N,
PO43-P concentration and sediment oxygen demand to
reduce eutrophication.
II. Materials and Methods
1. Sample collection and study area
In this study, marine sediment and water were col-
Fig. 1. The process of preparing functional oyster shell powder (FOSP).
lected in the mariculture sea area of Tongyeong bay, in
the southern part of Korea. The sediment sample was
collected from 0 to 15 cm below the sediment-water
interface using a grab sampler. The collected sediments
were packed in airtight polyethylene bags and stored at
4oC. Seawater samples were collected from 0.5-1.0 m
depth below the surface water. The sediment samples
were strained to remove debris and pebbles, followed by
homogenized before column packing and sediment char-
acterization.
2. Preparation of natural and functional oyster shell
powders (NOSP and FOSP)
The oyster shells are consisting of 97% calcium car-
bonate4). Natural Oyster shell powder dried in a drying
oven was ground for fine formation by using mortar. The
fine oyster shell powder passed through the 0.85 mm
sieve. One part of shell powder was sonicated with dis-
tilled water for 60 min (powder: water (w/w) = 1 : 2)
using an ultrasonicator (T18, Ultra-turrax, USA). The
dried powder was milled and then oxidized with hydro-
gen peroxide. The re-milled powder was used for exper-
iments, which is called functional oyster shell powder, as
oxygen releasing compound16). The involving chemical
reactions are shown in Eqs. (1), (2) and (3).
CaCO3 CaO + CO2 (1)
CaO + H2O Ca(OH)2 (2)
Ca(OH)2 + H2O2 CaO2 + 2H2O (3)
 Evaluation of the Remediation Efficiency of Functional Oyster Shell Powder Application to Organically Enriched Sediment 329
3. Experimental incubation
For laboratory-scale experiments was conducted in a
3-L transparent column (100 cm height × 6 cm diame-
ter). 300 gm sediment was added into the column to a
height of 20 cm from the bottom. Functional oyster shell
powder (FOSP) and natural oyster shell powder (NOSP)
were added in the sediment (0.5% w/w) and mixed to be
fully homogenized each column. While another column
prepared as control by the same quantity of natural sed-
iment. 2-L of filtered seawater was slowly added to the
column to avoid resuspension of sediment. The columns
were roofed by aluminum foil and stood in room tem-
perature (22ºC ± 2ºC). The overlying water samples
analysis were conducted on the days of 0, 3, 9, 12, 15
and sediment samples were analyzed before and at the
end of the experiments. Overlying water samples were
collected from three layers in the experimental col-
umns: top, middle and bottom layer from the sediment
surface by the distance of 70, 35, and 15 cm, respec-
tively.
4. Analysis of Physicochemical Property and Chemical
Analysis
Before analyzed, the water and sediment were sepa-
rated from the column and sediment was fully to be
homogenized. The pH and oxidation-reduction potential
(ORP) were measured using a multifunctional meter
(Orion 3 star, USA). Dissolved oxygen of the overlying
water was measured with a DO meter (YSI 550A,
USA). The supernatant pore water was collected from
the sediment by centrifugation (2000 rpm, 20 min). Before
analysis, the supernatant and overlying water samples
were filtered by microfiber filter (47 mm, GF/C). The
NO3N, NO2 -N and NH4+-N concentration were ana-
lyzed by potassium persulfate oxidation assays, indophe-
nol blue method, N-(1-naphthyl)- ethylenediamine
adsorption spectrophotometry and cadmium-copper col-
umn reduction method respectively according to the fol-
lowing previously described17). Phosphate (PO43-P) was
measured using the ascorbic acid reduction method.
For all experiments, overlying water and sediment were
conducted in triplicate and the average result were
used.
5. Sediment Oxygen Demand (SOD)
Before measurements, the distilled water was filtering
with glass microfiber filter paper (GF/C,What man, UK)
and aerated 8 h in a dark place. 2 grams sediment sam-
ple was placed into different BOD bottles. Then, the bot-
tles were filled with the aerated water. The dissolved
oxygen was continuous measured every 30 min in the
overlying water for a total duration of 5 h with a DO
meter (YSI 550A, USA). Mathematically, the incuba-
tion SOD rate can be formulated as following method18):
dC 1 100
SOD = -------  V   -----  -------------------- (4)
dt  M 100 – W
where dC/dt denotes change of DO (mg O2/L) per
time, and M is weight of a sample.
III. Results and Discussion
1. Effects of oyster shell powder on pH
The pH of the control, NOSP applied column and
FOSP applied column were 6.9-7.5, 7.0-7.9, and 7.2-8.1
for sediments and 7.6-7.8, 7.6-7.9, 7.6-8.0 for overlying
waters, respectively (Fig. 2). The FOSP applied column
pH was higher than NOSP applied column with control.
Because FOSP component is calcium peroxide which is
generate hydroxide. On the other hand, NOSP compo-
nent is calcium carbonate which is low soluble in water.
Generally, organically enriched sediment pH is weakly
acidic condition due to organic matter decomposition
and generate organic acid. So, appropriate amount of
FOSP application will not affect the pH value in the sed-
iment water column.
2. Effects of oyster shell powder on dissolved oxygen
and sediment oxygen demand
The organic matter mineralization in the sediments
consumes much amounts of oxygen, which is increase
anoxia problem in the coastal area. The deficiency of
oxygen in the water is a potential risk to aquatic ecosys-
tems, as a result release harmful gas and increases degree
of eutrophication. In this study, the concentration of DO
of the control, NOSP applied column and FOSP applied
column were 6.7-5.2, 6.7-6.2, and 6.7-6.6 mg/L in the
330 Md Akhte Khirul·Beom-Geun Kim·Daechul Cho·Sung-Hyun Kwon
Fig. 2. variation of pH in the overlying water (A) and
sediment (B) by addition of NOSP, FOSP (0.5% w/w) and
control for 15 days.
overlying water respectively (Fig. 3A). FOSP applied
column dissolved oxygen concentration was higher than
that of the NOSP applied column with control in the
overlying water. Because FOSP component is calcium
peroxide which is slowly generate oxygen and increas-
ing the DO level in the overlying water.
Sediment oxygen demand is a sink of oxygen, which
is defined as the oxygen consumption rate due to decom-
position of settled organic matter, chemically or biologi-
cally in the sediment17). SOD has been found to contribute
significantly to oxygen depletion. As shown in fig 3B,
the concentration of SOD of the control, NOSP applied
column and FOSP applied column were 0.04 ~ 0.09,
0.03 ~ 0.07 and 0.03 -0.05 mg/g in the sediment respec-
tively. This experimental result showed that, control col-
umn SOD was highly increased under experimental
period. Because highly degradation of organic matter in
the control column sediment, which was release of nutri-
ents, such as nitrogen, ammonium, phosphorus, phos-
Fig. 3. Variation of DO in the overlying water (A) and
sediment oxygen demand (B) by addition of NOSP, FOSP
(0.5% w/w) and control for 15 days.
phates etc. As a result, depletion of oxygen in the control
column overlying water (Fig. 3B). Sediment oxygen
demand (SOD) is a main cause of DO concentration. On
the other hand, FOSP applied column SOD was slightly
increased which indicates increased DO level in the
overlying water and reduce the nutrients release from
sediments to overlying water compared to others exper-
imental column.
3. Effects of oyster shell powder on nitrogen release
The transition and transportation of nitrogen concen-
tration at the sediment water interface is complicated,
containing the interconversion of different nitrogen spe-
cies. Some environmental factors may impact on nitro-
gen release from sediments such as DO, pH, redox
potential etc19). Nitrification-denitrification, ammonifica-
tion, and dissimilatory nitrate reduction to ammonium
(DNRA) action are important role in interconversion
 Evaluation of the Remediation Efficiency of Functional Oyster Shell Powder Application to Organically Enriched Sediment 331
Fig. 4. Variation of NH4+-N concentration in the overlying
water (A) and sediment (B) by addition of NOSP, FOSP
(0.5% w/w) and control for 15 days.
process. Under oxic condition, nitrification take place
spontaneously and NO3-N concentration becomes
higher. But under the anoxic condition, denitrification
was occurred, and nitrification restrained. In this experi-
ment, the concentration of nitrogen nutrients such as
NH4+-N, NO2-N, NO3-N release from sediment to
water were monitored by the effect of oyster shell pow-
der with control, where the sediment performed the lead
as a source. It was observed that, before the process,
NH4+-N concentration equilibrium in the overlying water
at all experimental column (Fig. 4). The concentration of
NH4+-N was rapidly increased with in the first 12 days
and the reached equilibrium in the NOSP applied col-
umn with control. On the other hand, FOSP applied col-
umn NH4+-N concentration was gradually increased until
experimental period in the overlying water. Therefore,
the NH4+-N concentration of the overlying water in the
FOSP applied column decreased compared to others col-
umn. The concentration of NH4+-N in the sediment pore
Fig. 5. Variation of NO3-N concentration in the overlying
water (A) and sediment (B) by addition of NOSP, FOSP
(0.5% w/w) and control for 15 days.
water was decreased in the all experimental columns.
On the other hand, the concentration of NO3−-N was
decreased in the overlying water and pore water of the
all experimental column until 15 days experimental
period (Fig. 5). However, the NO3−-N concentration in
the overlying water and pore water of the FOSP applied
column was higher than that of the other column. As
show in the fig 4 and 5, the concentration of NO3−-N
showed a mirror image of NH4+-N due to the diagenetic
reactions. The NH4+-N concentration in the main form of
inorganic nitrogen released into overlying water from
sediments. This experimental result may relate to the
mineralization into NH4+-N of organic nitrogen. It was
proved that, high pH may change the sediment proper-
ties and high dissolved oxygen concentration can inhibit
NH4+-N release from sediments20-21). In general, the
NH4+-N release rate decreased with the increasing pH. In
this experimental column, FOSP applied column sedi-
ment and water pH was comparatively higher than oth-
332 Md Akhte Khirul·Beom-Geun Kim·Daechul Cho·Sung-Hyun Kwon

ers column. On the other hand, the DO concentration

was decreased from 0 to 6 days in all column. After 6
days, FOSP applied column DO was increased due to
the oxygen releasing ability from peroxide. But NOSP
applied column DO was slightly increased and control
column DO was gradually decreased until experimental
period. Moreover, enough oxygen could help to catalyze
nitrification and denitrification processes22), so FOSP
applied column ammonium nitrogen concentration de-
creased and nitrate concentration increased compared to
others column. The concentration of nitrite nitrogen is
very low and continuously decreased, which became
negligible23). In summary, the nitrogen transformation
result indicates that the FOSP was blocked ammonium
release from sediment and increased NO3−-N in the over-
lying water compared to others column. This may be due
to decrease the nitrification rate and increase dissimila-
tory nitrate reduction to ammonium in the control and
NOSP applied column because the dissolved oxygen
concentration was lower than FOSP applied column.

4. Effects of oyster shell powder on Phosphorus release

The phosphorus release from sediments into overly-
ing water are affected by different environmental factors
including pH, oxidation reduction potential, tempera-
ture, physical process, intensity of light etc24). Under
anoxic condition, the phosphorus release from sediment
is highly increase is well documented. In this experi-
ment, sediment water column was not anoxic condition,
because the overlying water indicates the dissolved oxy-
gen was 6.7 to 5.2 mg/L in the control column.
At day 0, the oxidation reduction potential in the sedi-
ment was significantly negative (-211.9 mV), which indi-
cates the sediment was highly reduced condition. Under
reduced condition, phosphates release from sediments into
overlying water. As shown fig.6, the PO43-P concentra-
tion of the sediment pore water was decreased all experi-
mental column. At day 0, the concentration of PO43-P of
the FOSP applied sediment pore water was significantly
decreased due to the formation of calcium phosphates.
FOSP contains calcium peroxide and its surface is alka-
line, which is formation of phosphates salts with calcium.
3CaO2 + 2H2PO4 Ca3(PO4)2 + 2H2O + 2O2
(5)
Fig. 6. Variation of PO43-P concentration in the overlying
water (A) and sediment (B) by addition of NOSP, FOSP
(0.5% w/w) and control for 15 days.
In this way, the PO43-P in the sediment of the FOSP
applied column was adsorbed effectively onto the CaO2
with the precipitation of calcium phosphates. Because, P
forms in water body mainly include HPO42− and H2PO4 −,
which are in dynamic adsorption equilibrium to the sed-
iment25). So, the PO43-P concentration in the overlying
water highly increased in the NOSP applied column with
control column. But, the concentration of phosphates the
overlying water in the FOSP applied column decreased
compared to others column due to the suppression of
PO43-P releasing flux.
IV. Conclusions
The natural oyster shell powder (NOSP) and func-
tional oyster shell powder (FOSP) are mainly composed
of calcium carbonate and calcium peroxide. The func-
tional oyster shell powder is increasing the dissolved
oxygen level in the overlying water as a slow oxygen
 Evaluation of the Remediation Efficiency of Functional Oyster Shell Powder Application to Organically Enriched Sediment 333
releasing compound which could effectively improve the
anoxic condition in the sediment and overlying water. In
addition, obtained result suggested that, DO and pH at
sediment-water interface are closely associate with nutri-
ent release and their effect on nutrient migration is also
summarized in this study. The results of column experi-
ments proved that, FOSP can reduce NH4+-N and PO43-
P concentration and slightly increased NO3−-N concen-
tration in the sediment pore water and overlying water
effectively compared to control. According to obtained
results in this study, the application of FOSP to organi-
cally enriched sediments is effectively reduced NH4+-N,
PO43-P releasing flux and concentration of sediment
oxygen demand from the sediments.
Therefore, it can be concluded that converted oyster
shell powder can address two effective and environmen-
tal solution, namely the remediation of organic matter
enriched coastal sediment and the eliminating disposal
problems. In addition, the use of oyster shell powder
improving recycling perception and waste reduction
within the coastal area, which is environmentally and
economically beneficial.
Acknowledgments
This research was supported by Basic Science
Research Program through the National Research Foun-
dation of Korea (NRF) funded by the Ministry of Sci-
ence, ICT & Future Planning (2017R1A2B4008720) and
BK21 plus program, South Korea.
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