Saint Louis University

School of Natural Sciences

Department of Medical Laboratory Science

Activity 02

GROUP 06

MEMBERS:

MACHANUM, JORDAN M.

ANTONIO, MA. FELICIDAD S.

CASILDO, JOANNA MAE G.

DUQUE, ANNE KRYSSTELE A.

MANGLUGAY, LAINE DEONIBELLE P.

RAMOS, PAULENE ANDREA C.

ACTIVITY NO. 02

GROUP 06

EVALUATION

Above Below
Superior Average Poor
Criteria average average
5 3 1
4 2
Overall form and style
Title is clear and concise
Clear and concise report
All parts are properly related to each other
Referencing according to APA style
Introduction
Clearly stated problem/s
Significance of problem is established
Specific question/s is/are raised
Important terms defined
Adequate coverage of review of literature
Well organized review of literature
Studies critically examined
Literature are related to problem/s
Experimental procedures
Subjects and methods are described in detail
Variables are controlled
Appropriate data gathering procedures
Results and Discussion/Conclusions
Effective use of tables
Effective use of figures
Concise but complete report of findings
Appropriate statistical or other treatment of data
Logical analysis
Problem/s restated or addressed
Clear and concise discussion
Conclusion/s is/are based on results
Statement of practical or theoretical implications
Appropriate generalizations
Total
GRAND TOTAL

1
 ANALYSIS OF THE SOLUBILITY AND MELTING POINT
OF AN UNKNOWN COMPOUND

AUTHORS: MACHANUM1, J.M; ANTONIO1, M.F.S; CASILDO1, J.M.G; DUQUE1, A.K.A;

MANGLUGAY1, L.D.P; RAMOS1, P.A.C
1
– Department of Medical Laboratory Science, Saint Louis University, Baguio City, Philippines

ABSTRACT

The experiment was conducted to determine the physical properties of a given unknown
compound, assemble correctly the physical properties determination setups, and to utilize
physical properties data together with literature data in identifying compounds and determining
their purity. Laboratory experiment was the experimental approach used to identify the physical
properties of the unknown compound through the testing of its solubility and melting point
ranges. In terms of the results, the findings revealed that the unknown compound is slightly
soluble in distilled water. However, it was found to be insoluble in ethanol and cyclohexene. It
also showed that the final melting point range of the unknown compound is greater than 150℃.
As a conclusion based on the physical characterization, the group limited the identity of the
unknown compound to Copper(II) compounds such as Copper(II) sulfate pentahydrate (blue
vitriol)/nitrate/chloride due to its blue coloration and texture. Additionally, the unknown
compound is slightly soluble to water which is a good solvent for polar and ionic materials but
insoluble on cyclohexene and ethanol which is a non polar solvent. Lastly, the result in melting
point range suggests that the unknown compound has impurity due to the broadening of the
melting point range.

INTRODUCTION

Physical properties can be measured or observed without any changes of the

composition of its matter or its chemical composition is not affected. There are several ways in
distinguishing the physical properties but only two methods shall be performed namely:
Solubility and Melting Point. According to Kantz (2009), the solubility of a substance is usually
expressed because the mass of a substance, in grams, which will be dissolved in a fixed

2
amount of solvent (liquid), commonly a 100 g, at a given temperature. Relying at the molecular
shape of the substance, it's going to have exceptional solubility in exclusive solvents depending
on the character of the solvent. There are numerous factors influencing solubility such as
temperature, stirring, and the compounds themselves. These factors can speed up the solubility
rate or halt the solubility of certain substances. Temperature is a major factor when it comes to
solubility research findings because the level of solubility increases with temperature.
Temperature affects the solutions because it causes the molecules to speed up once they get
hotter or slow as they get colder and when the molecules move around swiftly they can quickly
merge into the molecules of the other solvent and vice versa. On the other hand, A solid's
melting point is the temperature at which it transitions from solid to liquid state at atmospheric
pressure. A substance's melting point depends on the pressure typically referred to as standard
pressure (Sandeep Kumar Reddy et.al, 2016). There are two factors affecting melting point:
Size of molecule and force of attraction between molecules.

The significance of this activity is to distinguish the unknown compound by performing

the two specific methods: Solubility and Melting Point. In addition to this, by means of physical
properties, the researchers would be knowledgeable enough in the solubility and melting point
of the unknown compound given. Solubility and Melting point play vital roles in identifying
compounds, Solubility determines how a substance dissolve into another type of substance
while Melting point can be used in identifying an unknown compound and as an indication of the
purity itself.

Thus, objectives of the determining the physical properties of the unknown compounds
are: Firstly, to distinguish the unknown compounds by means of performing physical properties
methods (Solubility and Melting Point). Secondly is to perform the physical properties correctly
including its setups. Lastly, in order to compare the results obtained with the literature data
which will be gathered in the determination of the unknown compounds.

3
 Methods

Solubility. To identify the solubility of the unknown solid the following materials were
used: 10 mL Pyrex® graduated cylinder, droppers for each solvent, Pyrex® test tubes, Denver
Model AA -0 analytical balance, watch glass, distilled water, ethanol, cyclohexane and 2mm
amount of the unknown solid. First, the test tubes were properly placed in the test tube rack.
After which 1mL of distilled water was measured using a graduated cylinder and transferred it
into the test tube. Unknown substance was measured gram by gram in the analytical balance.
Then, 1g of unknown substance was transferred to the first test tube containing distilled water
with constant agitation for the dissolution of the substance until such time that the substance will
dissolve. Using a different set of materials, to ensure the purity of the solvent, the same
procedures were done for ethanol and cyclohexane. Since ethanol is highly volatile it was
obtained only when the unknown solid is prepared to maintain the consistency of volume
between solvents. In addition, if 1 mg of the solute failed to dissolve in a 1 mL solvent it is
reported as insoluble for the specific solvent.

Melting point range. To observe the melting point range of the unknown solid the
following materials were used: three capillary tubes sufficient for three trials, matchsticks,
Bunsen burner, iron stand and iron ring, wire gauze, cork, mercury thermometer (-20ºC -
110ºC), ruler, rubber band to hold the capillary tube to the thermometer, iron clamp, watch
glass, 100mL Pyrex® beaker, glycerol and 2mm amount of the unknown. First, the capillary
tubes were sealed at one end by directly heating it over the flame of the Bunsen burner until the
exposed end was molten enough to be molded. After which the heated end of the capillary tube
was tapped on a flat surface to be completely sealed. Once the seal is secured it is marked at
2mm from its sealed end, then the open end is carefully filled with unknown sample contained in
a watch glass until the mark is reached. The capillary tube containing the sample is then
attached and aligned to the alcohol end bulb of the thermometer with a rubber band. Using the
iron clamp, iron stand and a cork the thermometer is stabled and submerged into the beaker
which contains a 40mL of glycerol. The beaker is placed on a wire gauze supported by the iron
ring slightly above the flame. Once all materials are properly prepared, the recording of the
temperature range of the thermometer was observed alongside with the unknown solid. As the
sample started to melt the temperature is recorded as well as the temperature at which the
sample is completely melt. After which the glycerol bath is allowed to cool down below the
recorded temperature of the starting range.

4
 RESULTS AND DISCUSSION

This chapter presents interpretation and analysis of the results gathered from the
experiment.

Color, odor and texture

The unknown compound, compound B, was observed by the students for its physical
characteristics. Compound B is blue in color and appeared to be in a combination of granular
and powdered form, rendering it coarse in texture. The unknown compound is odorless. The
students infer that is it Copper (II) sulfate pentahydrate based on the observations on the
physical properties of Compound B. Copper (II) sulfate pentahydrate has large, blue or
ultramarine, triclinic crystals or blue granules or light-blue powder (Budavari, 1996). Regarding
the odor of the compound, it is odorless (Farm Chemicals Handbook, 2000). There is a great
similarity between the physical properties of the unknown compound observed by the students
and the description based on the references.

Solubility

The result of the solubility of Copper (II) sulfate pentahydrate when it is mixed with
distilled water; cyclohexene and ethanol are the following:

Table 1. Solubility of 1g of Copper (II) Sulfate in Distilled Water, Ethanol and Cyclohexene
Distilled Water Ethanol Cyclohexene
Soluble but with a lot of residues Insoluble Insoluble

From the table above, it was observed that water is soluble to Copper (II) sulfate
pentahydrate but there were a lot of residues at the bottom part of the test tube and it was
observed that the water took the color of the compound which is blue. So it was noted that 1 ml
of distilled water cannot dissolve all 1 gram of copper (II) sulfate pentahydrate. While for the 1
gram of the compound placed in 1 milliliter of ethanol and in 1 milliliter of cyclohexane, the
compound did not dissolve and the liquid did not change in color, maintaining its clear form,
making it insoluble in ethanol as well as in cyclohexane.

5
Figure 1,2 &3: Solubility of 1g of Copper (II) Sulfate in Distilled Water, Ethanol and Cyclohexene

Copper (II) sulfate pentahydrate has a water solubility of greater than or equal to 100
mg/mL or 0.1g/mL and insoluble in ethanol and cyclohexane (National Oceanic and
Atmospheric Administration, n.d.). Water is a polar solvent and is considered to be effectively
responsible in dissolving other polar molecules such as sugars and ionic compounds such as
salts. (Solvent properties, 2015; Sandbox Networks, 2017). With the definitions stated
beforehand, the compound was dissolved because water is considered to be a universal solvent
and can dissolve substances that are polar and ionic in nature. With it being dissolved, it entails
that the compound is polar or an ionic compound.

A polar solvent is one where the molecules that make up the solvent have a charge that
is unequally distributed in the molecule. In the case of water, the oxygen atoms have a partial
negative charge and the hydrogen atoms have a partial positive charge.

Copper (II) sulfate pentahydrate is soluble in water primarily because the water is a
polar solvent. Knowing that the compound is ionic in nature, when it is combined with water, it
will dissociates into positively charged copper ions and negatively charged sulfate ions. In
addition, the polarity of the water will result into the attraction of positive ions to the oxygen
atoms of water having a partially negative charge and the sulfate ions attracted to hydrogen
atoms of water that have partial negative charge. So with that being said, water being a polar
solvent can dissolve ionic salts like Copper (II) sulfate pentahydrate (Enotes, 2011).

Ethanol is a polar solvent that can dissolve polar and non-polar substances but is less
polar than water (Ethanol as a solvent, n.d.). Cyclohexane is a nonpolar solvent and a volatile
inorganic solvent which can be good solvent for substances that have weak solute interactions
(Solvent properties, 2015; ChEBi, 2016). Copper (II) sulfate pentahydrate does not dissolve in
both ethanol and cyclohexane due to the reason that these substances do not have the ability to

6
hydrate copper and sulfate ions and also copper is insoluble in ethanol that has no impurities
(Trader China, 2009; Essays UK, 2018). Given that cyclohexane is an organic solvent, it was
stated that Copper (II) sulfate pentahydrate is practically insoluble in most organic solvents
(Toxnet, n.d.).

Melting Point

The result of the melting point are as follows:

Table 2. General details observed in the start and range of the Melting Point of the substance.
Trials ͦC
Trial 1 >150 ͦ C
Trial 2 >150 ͦ C
Trial 3 >150 ͦ C

Figure 4. Melting Point of Copper (II) Sulfate Pentahydrate

The equation of dehydration will shift to the right with regards to the Le Chatelier’s
Principle causing the residue obtained after heating, called the anhydrous compound, to have a
different structure and texture and may have a different color than the hydrate. (Santa Monica
College,n.d) Thus, producing an ashy white color for the Copper (II) Sulfate Pentahydrate

The first, second and the third trial measured 150 ͦ C The result of the test is nearly
similar to the boiling point of Copper (II) sulfate Pentahydrate provided by the National
Toxicology Program (1992) which is 297˚F or 147.2˚C. The Melting point of the Copper (II)
Sulfate Pentahydrate is above 110℃ with decomposition. (Lide, 1987-1988)

7
 The temperature the Copper (II) Sulfate Pentahydrate started to melt until it completely
melted was observed by the students. During the test of the Copper (II) Sulfate Pentahydrate,
the students observed that after submerging the capillary tube attached to the thermometer in
the Glycerol bath which was heated, there are some changes in the color of the compound that
indicates that it is starting to melt. Heating a hydrate leads to an endothermic reaction that
produces a residue known as the anhydrous compound. This compound is different in structure,
texture and even color in some cases, from its parent hydrate (Tresor, 2017).

CONCLUSION

Based on the physical characterization, the group limits the identity of the unknown
compound to Copper (II) compounds such as Copper (II) sulfate pentahydrate (blue
vitriol)/nitrate/chloride due to its blue coloration and coarse texture and is odorless. The findings
revealed that the unknown compound is slightly soluble in distilled water. However, it was found
to be insoluble in ethanol and cyclohexene. For the melting point, at greater than 150℃. of
glycerol bath, there is a visible discoloration of the material from blue to whitish hue which
indicates that the water from the substance is being removed from the hydrate. This changes
the copper (II) sulfate pentahydrate into an anhydrous compound. With all the established
results, the students were able to confirm that the material is indeed Cupric Sulfate.

REFERENCES:

Budavari, S. & Merck & Co (1996). The Merck index: an encyclopedia of chemicals, drugs, and
biologicals (12th ed). Merck & Co. Inc, Whitehouse Station, N.J

ChEBi. (2016). Cyclohexane. Retrieved from

hhtp://www.ebi.ac.uk/chebi/searchld.do?chebld=CHEBI:29005

Enotes. (2011). Why can copper sulfate dissolve in water easily?. Retrieved from
hhtps://www.enotes.com/homework-help/why-can-copper-2-sulfate-dissolved-water-
264071

Essays, UK. (November 2018). Importance of Solubility in Everyday First. Retrieved from
https://www.ukessays.com/essays/sciences/solubility.php?vref=1

8
Enotes. (2011). Why can Cupric Sulfate dissolve in water easily? Retrieved from:
https://www.enotes.com/homework-help/why-can-copper-2-sulfate-dissolved-water-
264071 (accessed June 10, 2019).

Essays UK. (2018). Mixing liquids and solids. Retrieved from

https://www.ukessays.com/essays/chemistry/mixing-liquids-and-solids.php?vrf=1

Farm Chemicals Handbook. (2000). (p. C104). Willoughby, Ohio: Meister.

Katz, D. (2009). Identification of a Substance by Physical Properties. Retrieved from

http://www.chymist.com/Identification%20of%20a%20Substance.pdf

National Toxicology Program (1996). National Toxicology Program Chemical Repository

Database. Research Triangle Park, North Carolina: NTP. Retrieved from:
https://cameochemicals.noaa.gov/chemical/20049?fbclid=IwAR1fArFEpLkdYgZRFC4Gy
8FsV0GqW4NNwFj8Vne0ZbMN_50rpoKRv2nB9mw (accessed June 10, 2019).

National Center for Biotechnology Information. PubChem Compound Database; CID=24462,

https://pubchem.ncbi.nlm.nih.gov/compound/24462 (accessed June 10, 2019).

Nedungadi P., Raman R. & McGregor M. (2013, October). Enhanced STEM learning with
Online Labs: Empirical study comparing physical labs, tablets and desktops. In Frontiers in
Education Conference, 2013 IEEE (pp. 1585-1590). IEEE. Retrieved from
https://amrita.olabs.edu.in/?brch=7&cnt=1&sim=33&sub=73

Properties of Hydrates for Chemistry Experiments (2017). Sciencing Database. 1655 26th
St Santa Monica, CA 90404. Retrieved from: https://sciencing.com/what-is-an-
endothermic-reaction-13712135.html (accessed June 10, 2019).

Sandeep Kumar Reddy et.al. (2016). Review on the Determination of Melting Point
Measurement System. Retrieved from
https://www.google.com/url?sa=t&source=web&rct=j&url=https://www.ijareeie.com/upload/2016/
february/59_A%2520Review.pdf&ved=2ahUKEwjwubSL1N7iAhWKdd4KHVg6DIgQFjAAegQIB
BAB&usg=AOvVaw1PaUrhmOzTEV3jBjQ2NQyw

Toxnet. (n.d.). Copper(II) Sulfate, Pentahydrate. Retrieved from https://toxnet.nlm.nih.gov/cgi-

bin/sis/search/r?dbs+hsdb:@term+@rn+@rel+7758-99-8

9
 APPENDICES

A. SOLUBILITY

Measuring 1g of the unknown Test tube filled with 1mL of water and
substance. watch glass containing the 1g of
substance.

An amount of1g of substance dissolves in

water, ethanol and cyclohexene.

An amount of1g of substance

dissolves in 1mL water.

10
B. MELTING POINT

Inserting the other end of the

The sealing of capillary tube by heating thermometer through a cork that serves
it directly over a flame. as a clamping area.

Submerging the alcohol bulb end of the

Attaching the capillary tube containing
thermometer into the glycerol bath.
the sample to a thermometer using a
rubber band.

11
 Recording of the temperature range at
Heating the glycerol bath. which the solid in the capillary tube
completely melts.

12