CH311 EXPERIMENT 4 ID: S11016863

TITLE:

Determining Calcium Carbonate content in the Marine Sediments using the

Gravimetric and Volumetric Methods

ABSTRACT

The marine sediments are of various classification, origins and sizes. And the biogenous sediment type
are as a result of the accumulation of hard parts of some marine organisms. For example, the calcareous
ooze that can be found above the calcium compensation depth. In this experiment, the methods of
gravimetric and volumetric are used to determine the calcium carbonate content in marine sediments.

AIM
The different gravimetric and volumetric methods are used to determine the calcium carbonate of marine
sediments

INTRODUCTION

The fluid environment is made up of the ocean and atmosphere. And the seawater/ocean in particular is a
chemical system that makes up about 75% of the water bodies that covers the Earth’s surface and known
to be ~97% water and 3% ions. The abundance of ion constituents in the seawater are further divided into
the four main components and are the major, minor, trace elements and gases. Calcium as one of the
major constituent is essential to marine organisms for physiological functions and also for the formation
of the exoskeleton. And the calcium exists in the seawater as calcium ions and calcium carbonate
(sediments).
The sediments accumulate in a loose, unconsolidated formed from the organic or inorganic matter that
originated from the weathering and erosion of rock, volcanic eruptions, the activity of living organisms
and chemical processes within the water itself and continues to rain down onto the ocean floor. It occurs
in a range of sizes and types from beach, mud, mix of silt and tiny shells, clays on the ocean floor,
biologically derived oozes and nodules and coatings of hard objects. The marine sediments are classified
into terrigenous, biogenous (siliceous and calcareous compounds), hydrogenous and cosmogenous.
However, this experiment focuses on the calcareous ooze that was formed mainly from shells of amoeba-
like foraminifera, small drifting molluscs (pteropods) & tiny algae (coccolithophores) and creatures living
nearly all surafec ocean water. On the other hand, the calcareous sediments dominates above the calcium
compensation depth (CCD) since at greater depths or below the CCD (~4500m) the pH decreases (more
acidic) dissolving the calcareous ooze.
And during this experiment, the calcium carbonate content was determined in the sediments by
gravimetric, volumetric, reaction with acid, titration and measuring the volume of carbon dioxide
produced.

METHODOLOGY:
CH311 EXPERIMENT 4 ID: S11016863

The method was divided into 5 different parts.

A. Qualitative Estimates
The marine sediments were collected from four different location, namely Tamavua River, My Suva Park,
Mosquito Island and Vunivadra River. Then, a small amount of each marine sediments were added into
four separate test tubes and a 2 ml of 2.0283M HCl was added separately into four test tubes each
containing marine sediments from the four different sites. The test tubes were shaken for a few seconds to
a minutes so that the sediments reacted with the acid and then unreacted sediments were allowed to settle
and were classified into three types.
Type 1: Almost all sediment dissolves
Type 2: Approximately half the sediments dissolves
Type 3: Very little sediment dissolves
B. Gravimetric Determination
The My Suva Park marine sediment was selected from the other marine sediment location to be used in
this gravimetric determination.
A 10.0018g of the My Suva Park marine sediment was weighted in a 250ml beaker. And 100ml of
standardized 2.0283M HCl was pipetted into the beaker. The beaker was then heated with continuous
stirring until no further effervescene was noticed. While letting the beaker to cool, a clean and dry
Buchner funnel and a filter paper were weighted together and the combined weight recorded. When the
beaker was cooled, the Buchner funnel, filter paper and gentle suction were used to separate the
supernatant solution from the undissolved sediment into a filtration flask in the fume board. Distilled
water was used to wash down the remaining sediments in the beaker. When conducting the filtration,
extra caution was taken as to avoid any loss of supernatant solution or sediment. After successfully
separating the solution from the sediment, the Buchner funnel and filter paper were dried in the oven and
then combined weight recorded. The supernatant filtrate was reserved to be used in part C and D of this
experiment.

C. Determination of Reacted Acid

The aqueous filtrate solution obtained in part B was transferred into a 500ml volumetric flask and
distilled water was added to make up the total volume up to the mark. Then, 10ml of this solution was
pipetted into a conical flask and titrated against a standardized 0.0987M NaOH. A colour change from
colourless to cloudy indicated the end point. The titration was repeated 3 more times and the results were
recorded.
D. Direct Titration of Dissolved Calcium and Magnesium Ions
A 10ml of the solution prepared in part C above was pipetted into a volumetric flask and was neutralized
with NaOH in the burette. After a 5ml of ammonia chloride buffer (pH = 10) and a small amount of
Eriochrome black-T indicator powder are added, the solution turns purple. Then it was titrated with the
standardized EDTA solution until the colour changes from purple to bluish green. The molarity of the
Ca²⁺ and Mg²⁺ ions in the solution prepared from the sediment filtrate was calculated

E. Determination of Carbon Dioxide produced

A 1g of the sediment was accurately weighed into a small two neck flask. The flask was equipped with a
dropping funnel with a pressure equalizing arm and a tube leading to an inverted 250cm3 measuring
cylinder. And the inverted measuring cylinder was filled with water and stand in a container of water.
Approximately 15ml of 2M HCl was filled into the dropping funnel and a stopper was fitted. While the
acid was slowly let to ran down the drooping funnel into the flask. The solution in the flask was warmed
gently until no further effervescene observed. The solution was allowed to cool to room temperature and
the volume of gas in the inverted measuring was recorded.
CH311 EXPERIMENT 4 ID: S11016863
RESULTS, CALCULATIONS, QUESTIONS AND DISCUSSION:

Results:
Room temperature = 27‫ﹾ‬C
Atmospheric Pressure = 101.2 kPₐ

A. Qualitative Estimates
Sediment Site Sediment Classification
Tamavua River Approximately half the sediment dissolves
My Suva Park Very little sediment dissolves
Mosquito Island Almost all the sediment dissolves
Vunivadra River Very little sediment dissolves
Concentration of HCl = 2.0283M

B. Gravimetric Determination
Mass of My Suva Park sediment = 10.0018g
Mass of filter + Buchner funnel = 161.5855g
Mass of filter + Buchner funnel + sediment (after placed in the oven) = 161.8977g
Mass of undissolved sediment = 0.3122
Concentration of HCl = 2.0283M

C. Determination of Reacted Acid

Titration Titre Volume Reading (ml)
Initial Final
1st 0 45
2nd 0 46.7
3rd 0 45.7
Average Titre Volume = 45.8ml
Concentration of NaOH = 0.0987M

D. Direct Titration of Dissolved Calcium and Magnesium Ions

Titration Titre Volume Reading (ml)
Initial Final
1st 1 6
2nd 6 12
3rd 12 16

Average Titre Volume = 5ml

E. Determination of Carbon Dioxide produced

Sediment Location Mass (g) Volume (cm³) of COₐ Produced
Mosquito Island Sand 1.0103 160
Vunivadra River 1.0105 15
Tamavua River 1.0069 35
My Suva Park 1.0139 14
CH311 EXPERIMENT 4 ID: S11016863

Calculation and Questions

B. Gravimetric Determination
Question 1: Calculate the percent of the sediment which has dissolved.
Mass of My Suva Park sediment = 10.0018g
Mass of undissolved sediment = 0.3122
Mass of dissolved sediment = 10.0018 – 0.3122 = 9.69g

% of dissolved sediment = (mass of dissolved sediment / mass sediment) X 100

= (9.69 / 10.0018) X 100
= 96.88%

Question 2: Assuming the dissolved sediment to be pure CaCO3, calculate the moles of CaCO3
dissolved.
CaCO₃: n = m/Mr = 9.69 / 100 = 0.097 moles

C. Determination of Reacted Acid

Question 3: Using the total moles of the HCI initially added to the sediment and total moles of the HCI
left unreacted, calculate moles HCI that has reacted with CaCO3. Supposing HCI has reacted only with
CaCO3 in the sediment also calculate the weight percent of CaCO3 in the sediment sample.
CaCO3 +2HCl CaCl₂ + CO₂ + H₂O

HCl: c = 2.02823M v = 0.1 L n = cv = 2.0283 X 0.1 = 0.2 mole HCl initially added to the sediment
n (HCl reacted) = 0.2 X (96.88 / 100) = 0.19 mole
n (HCl unreacted) = 0.2 – 0.19 = 0.01 mole
CaCO3: n = 0.2 / 2 = 0.1 mole m = n X Mr = 0.1 X 100g/mol = 10g
Weight % CaCO3 sediment sample = 10/10 X 100 = 100%

Question 4: Explain the chemical basis of appearance of the cloudiness during the titration.
The appearance of the cloudiness during the reaction indicated the unreacted HCl had been neutralized by
the addition of NaOH and also the formation of Ca(OH)₂.

D. Direct Titration of Dissolved Calcium and Magnesium Ions

Question 5: Calculate the moles of calcium + magnesium ions carbonate. Assuming all to be as CaCO 3
calculate its weight percent in the initial sediment sample.

Calcium ions: n = m/Mr = 10/100 = 0.1 mole

Magnesium ions: n = 0.1 mole
CaCO₃ % weight in initial sediment sample:
m = n X Mr = 0.1 X 100 = 10g
% weight = 10/10 X 100 = 100%

E. Determination of Carbon Dioxide produced

Question 6: Using the volume of CO2 released at room temperature and atmospheric pressure, calculate the
moles of CO2 produced and the weight percent of calcium carbonate in the sediment.
CaCO3 +2HCl CaCl₂ + CO₂ + H₂O
CaCO3 : n = m/Mr = 1 / 100 = 0.01 mole
CO₂ : n = 0.01 mole
% weight CaCO3 :
m = n X Mr = 0.01 X 100 = 1g
CH311 EXPERIMENT 4 ID: S11016863
% weight : 1/1 X 100 = 100%

Discussion
Form the results obtained in the above calculations, it was noted that by using the gravimetric
determination, there are some undissolved sediment and the mass was 0.3122 and the % of dissolved
sediment was 96.88. This showed that the HCl was not able to dissolve the 10.0018g of sediment.
However, in the determination of reacted acid, the weight % of calcium carbonate in the sediment sample
was 100%.
Similarly, in the direct titration of dissolved calcium and magnesium ions, the weight % if calcium
carbonate in the sediment sample was 100%.
Also, in the determination of carbon dioxide produced, the % weight of the calcium carbonate was 100%.
Thus, from these experiments, a majority of the tests proved that the sediment was composed of calcium
carbonate since the total % weight of calcium carbonate in the sediment was 100%. However, only the
gravimetric method showed that not all the sediment was able to dissolve in HCl. Only 96.88% of the
sediment was able to dissolve in HCl.

Conclusion
To conclude, the experiment was successfully carried out and that the aim of this experiment was
achieved. The different methods used was able to determine the calcium carbonate content in the
sediment.

References
Dr. Maata. M., 2020. Marine Chemistry. [Online]
Available at: https://elearn.usp.ac.fj/mod/resource/view.php?id=522414
[Accessed 1st 06 2020].