Open Journal of Soil Science, 2012, 2, 263-268
http://dx.doi.org/10.4236/ojss.2012.23031 Published Online September 2012 (http://www.SciRP.org/journal/ojss)
263
Comparison between Calcimetric and Titrimetric Methods
for Calcium Carbonate Determination
Pakhshan M. Maulood, Akram O. Esmail*, Mohammed S. S. Dohuki, Dalshad A. Darwesh
Soil and Water Department, College of Agriculture, Salahaddin University, Erbil, Iraq.
Received May 17th, 2012; revised June 20th, 2012; accepted July 5th, 2012
ABSTRACT
This study was conducted during 2008-2009 ,which included calcium carbonate determination from 84 locations (40
soil samples from Erbil, 24 samples from Sulaimani and Kirkuk in addition to 20 samples from Duhok) using calimetric
and titration method. The results indicated to significance correlation coefficient between the studied methods or it
means that the results of both methods are similar.
Keywords: Calcium Carbonate; Calcimeter; Calcareous Soil
1. Introduction
Most soils of agricultural areas are calcareous and have
an alkaline reaction. pH of calcareous soils is mainly
controlled by the amount of calcium carbonate in the soil
profile and often is fluctuating between 7.5 to 8.2. Exis-
tence or absence of calcium carbonate has an important
effect on soil pH and therefore, controlling many chemi-
cal reactions in relation to nutrient availability for plants
and mobility of these elements in soil [1]. Carbonate is a
natural constituent of many soil in the world, most car-
bonate minerals found in Iraqi soils are calcite (CaCO3)
and represent 90% - 95% of total soil carbonates [2]. The
distribution and amount of carbonates influence soil fer-
tility. The increase of calcium carbonate in soil usually
leads to many problems related to fertilization and nutri-
ent availability. The extent and rate are affecting by the
amount of carbonates in the soil, the chemical and
physical nature of the carbonates (e.g., particle size and
mineralogy) [3,4] Carbonates exert a major effect on soil
chemical properties of calcareous soils, like nutrient
availability and phosphorus fixation due to chemical fix-
ation of 70% - 90% of applied phosphorus fertilizer to
the soil [5]. Soil survey staff [6] indicated to increase in
soil pH with increasing soil CaCO3 content. Some at-
tempts have been done to evaluate methods of carbonate
determination in arid and semiarid soils including cal-
careous soils [7-10]. A suitable, accurate method of de-
termining limestone is required whenever quantitative
measurements are sought, such as in soil fertility prob-
lems where limestone dissolution rates are to be deter-
mined, or where lime recommendation procedures take
into account residual limestone [11]. The aim of this
study is to compare between two methods of CaCO3 de-
termination (Acid neutralization method and calcimetric
method).
2. Materials and Methods
The studied soil samples were taken from 84 locations
(40 soil samples from Erbil, 24 samples from Sulaimani
and Kirkuk in addition to 20 samples from Duhok), dur-
ing 2008-2009 (Figures 1-3). Soils were air dried ground
and sieved through 2mm sieve. The equivalent calcium
carbonate (E-CaCO3) was determined using 0.5 M HCl
for dissolution of CaCO3 and determined between the
two titration of the excess acid by using 0.2M NaOH as
mentioned by [12]. The second method of E-CaCO3 de-
termination was using calcimeter method as mentioned
by [13]. The simple correlation coefficient n (r) was de-
termined between the two studied methods [14].
3. Results and Discussion
The soils CaCO3 content of the studied locations were
ranged from (20 - 365.3 g·Kg−1 soil) for the soils of Erbil,
Sulaimani and Duhok respectively (Tables 1-3). The
statistical analysis indicated that the correlation co- effi-
cient values (r) between the studied two methods for the
three locations (Erbil, Sulaimaniya and Duhok) were
(0.993**, 0.998** and 0.994**) respectively (Figures
4-6). It means there is a significance correlation be-
tween calcimetric and titrimetrc method, or it means the
results of both methods are similar and both methods
*Corresponding author.

Comparison between Calcimetric and Titrimetric Methods for Calcium Carbonate Determination 264
Table 1. Shows determination of calcimetric and titrimetric methods of calcium carbonate in soil t of Erbil governorate.
Sites No. Locations Calcimetric Method Titrimetric MethodSites No.Locations Calcimetric Method Titrimetric Method
1 Kalak 287 274 21
Halgort
Mountain 20 25
2 Guwer 298.1 297.5 22 Akoyan 227.3 223
3 Yarmcha 312.9 316 23 Rosty 37.3 35
4 Mala-Qara 253 263 24 Hasarot 209.3 199.5
5 Erbil 246.4 239.2 25 Choman 64.7 64
6 Qushtapa 276.3 289 26 Rayat 41 53.5
7 Derband 137 128.5 27 Azadi 209.3 191.8
8 Degala 175.2 188 28 Haji-Omran 152 195
9 Koysenjaq 141.6 153.5 29 Haji-Omran 93.1 91
10 Koysenjaq 239.7 225 30 Chame-Beaje211.1 202
11 Qarasenj 140.8 140 31 Khalan 216.6 202
12 Bastora 290.9 292.3 32 Mergasor 201.4 193
13 Shaqlawa 209.1 198 33 Malman 291.2 292.3
14 Mama-Jelka 67.1 72.5 34 Soran Village108.3 112
15 Harer 193 187.5 35 Ashkafta 112 122
16 Spelek 79.1 71.5 36 Rezan 53.3 51.5
17 Jundeyan 220.3 231 37 Barzan 361.4 362
18 Zar-Gali 219.9 205.5 38 Maran 18.6 16
19 Rawndouz 138.1 131.8 39 Peran 15 18.5
20 Soran 55.9 55 40 Mandan 161 171
Table 2. Shows determination of calcimetric and titrimetric methods of calcium carbonate in soils of Sulaymani and Kirkuk
governorate.
Sites No. Locations Calcimetric Method Titrimetric MethodSites No.Locations Calcimetric Method Titrimetric Method
1 Ranya 44.5 43.5 13 Serwan 89.4 81.5
2 Ranya 63.4 65 14 Halabja 108.1 101
3 Qalat Dizah 16.8 18.5 15 Khormal 83.9 88.5
4 Haybat Sultan 163.9 170 16 Bayara 37.8 40
5 Kani Watman 164 170 17 Balkha 49 55.5
6 Kelka smaqa 137.9 132.5 18 Tawela 22.4 28.5
7 Dukan 294.9 292.5 19 Altun Kupri 201.6 199.9
8 Basneh 66 59 20 Kirkuk 153 156
9 Qalat Cholan 65.2 70.5 21 Kirkuk 192.2 192.3
10 Sulaymaniyah 190.4 193 22 Chemano 317.73 313
11 Said Sadek 145.3 151 23 Qara Hanjer 309.9 311
12 Derbandikhan 253.3 252.3 24 Chamchamal 242.6 253

Comparison between Calcimetric and Titrimetric Methods for Calcium Carbonate Determination 265
Table 3. Shows determination of calcimetric and titrimetric methods of calcium carbonate in soils of Duhok governorate.
Sites No. Locations Calcimetric Method Titrimetric MethodSites No.Locations Calcimetric Method Titrimetric Method
1 Qandil bridge 258.2 251 11 Duhok 246.1 251
2 Gawelan 365.3 360 12 Zaweta 203.1 192.5
3 Aqrah 160.3 172.8 13 Mam-Yazden339.4 329.6
4 Gali-Zanta 323.4 325 14 Swaratuka 185.5 192
5 Lalesh mountain 114.2 101.8 15 Solaf 196 192
6 Atrush 248.8 242.5 16 Serseng 193.6 192.2
7 Atrush mountain 304.4 306 17 Serseng 226.2 221.8
8 Baadrae 242.1 242.3 18 Kani Chnarkae163.9 170
9 Gali-Derkae 315.8 320 19 Qadash 201.7 192.3
10 Duhok 247.3 251 20 Zakho 251.3 250
Turke
y
Iran
Iran
Duhok
Nineveh
Sulaimani
y
a
Dokan lake
Erbil city
Ko
y
sen
j
a
Mergasor
Shaqlaw
Choman
Makhmour
Rawndouz
Soran
Bensalawa
Turke
y
Kirkuk
B
2
1
Kalak
4 3
6
578
9
10
12 11 13
14
16 15 19
17 18
20
30
37 36
35 32
40 39 38
34
33 31 24 23
21
26
25 27
28
29
26
22
Figure 1. Shows: (A) Map of northern governorate of Iraq; (B) Erbil governorate, sampling sites.

Comparison between Calcimetric and Titrimetric Methods for Calcium Carbonate Determination 266
A
B
1
2
3
4
5
6
7
8
9
11
10
12
13
14
15
16 18
17
Iran
Iran
Iran
19
20
21
22
23
24
Figure 2. Shows: (A) Map of Iraq; (B) Sulaymaniyah and Kirkuk governorates, sampling sites.
A
B
1
2
3 4
6
5
7
8
9
10
11
12
13
14 15
16 17
18 19
20
Figure 3. Shows: (A) Map of Iraq; (B) Duhok governorate, sampling sites.

Comparison between Calcimetric and Titrimetric Methods for Calcium Carbonate Determination 267
y = 0.981x + 3.059
r = 0.993
0
50
100
150
200
250
300
350
400
0 50 100 150200 250300 350 400
CALCIMETRIC
TITRIMETRIC
Figure 4. The relationship between titrimetric and calcimetric methods of calcium carbonate determination in soil of Erbil
governorate.
y = 0.9945x + 1.2715
r = 0.998
0
50
100
150
200
250
300
350
0 50 100 150 200 250 300 350
CALCIMETRIC
TITRIMETRIC
Figure 5. The relationship between titrimetric and calcimetric methods of calcium carbonate determination in soils of Sulay-
mani and Kirkuk governorates.
y = 0.9945x -0.2126
r = 0.994
0
50
100
150
200
250
300
350
400
0 50 100 150 200 250 300 350 400
CALCIMETRIC
TITRI ME TR IC
Figure 6. The relationship between titrimetric and calcimetric methods of calcium carbonate determination in soils of Duhok
governorate.

Comparison between Calcimetric and Titrimetric Methods for Calcium Carbonate Determination 268
Table 4. A comparison of equivalent calcium carbonate determination by two methods in soil samples of Kurdistan Region
governorate, data represented as (mean ± SE).
Governorate Calcimetric Method Titrimetric Method Differences
Erbil 169.62 ± 14.78 169.47 ± 14.61 0.15
Sulaimaniya and Kirkuk 139.90 ± 18.22 140.40 ± 18.15 –0.50
Duhok 239.33 ± 14.61 237.79 ± 14.60 1.54
have the same scientific base. The differences shown in
(Table 4) between mean values of E-CaCO3 content of
soil samples measured by the two mentioned methods are
non significance. A little difference observed between
two methods for soil samples of Erbil, Sulaimaniya-
Kirkuk governorates that reached to 0.15 and −0.5 re-
spectively. While the differences was 1.54 unit for Du-
hok soil samples. Generally, soil samples for E-CaCO3
content were increased gradually from Sulaimaniya-
Kirkuk, to Erbil toward Duhok governorate.
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