ENVIRONMENTAL ANALYTICAL CHEMISTRY

CHEM 301

EXPERIMENT 2 LAB REPORT

Ofentse Ramonnye
14000883
BSc Pure & Applied Chemistry
AIM

The experiment was done to extract the organic material from the waste water sample

INTRODUCTION

Extraction is a process that selectively dissolves one or more of the mixture components into
an appropriate solvent, the process of extraction with solvents is generally employed either for
the isolation of dissolved substances from solutions or from solid mixtures or for the removal
of undesired soluble impurities from mixtures[1]. Liquids which mix to form a homogeneous
liquid phase are said to be miscible, meaning that the two substances are mutually soluble in
all proportions, most organic liquid used as solvents for manipulations in an organic
chemistry laboratory are not soluble in water, since the organic liquid is not soluble in water it
separates into a separate phase hence organic liquids and water are said to be immiscible in
one another[1]. Solubility is the property of a substance, which describes the ability of the
substance to form mixtures with other substances, usually liquids, which are chemically and
physically homogeneous and in most cases, the solubility of a substance in another substance
increases with an increase in temperature, this property allows for purification of compounds
by recrystallization and the solubility of a substance in a liquid can be used to classify it, it
also can provide a method for separating a substance from other substances, this separation
technique is called extraction and will be used in many of your experiments to isolate the
organic product from a reaction mixture therefore the solubility of a substance is a vital piece
of information and before starting to work with a compound, it is necessary to know or to be
able to predict whether the substance will be soluble in water, aqueous acid, aqueous base, or
organic solvents such as ether[2]. In this experiment we extract organic matrices from the
waste water using solvent extraction method, the first requirement in this extraction process is
to select two immiscible solvents, one solvent, usually aqueous (water‐based), should be polar
in nature and the second solvent should be nonpolar and might be hydrocarbon, ether, or
chlorinated solvent, such as dichloromethane and when this two immiscible solvents are
placed into a container, two liquid layers are formed the more dense solvent is always the
bottom layer[3]. In our experiment we use hexane, which is nonpolar to extract the organic
matrices from waste water sample which is a polar solvent.

PROCEDURE

10ml of the prepared waste water sample from the last lab was transferred into a separating
funnel, then added the same amount of hexane to it and the mixture was shaken for further
mixing but opening the funnel at times to release pressure. The separating funnel was held
with the clamp to allow the mixture to settle after that the bottom phase was drawn off and the
remaining layer was kept ready for the next extraction.
DISCUSSION

A compound can be separated from impurities in a solution by extracting the compound from
the original (or first) solvent into a second solvent and for the process to be selective, the
compound must be more soluble in the second solvent than in the first solvent, and the
impurities must be insoluble in the second solvent, additionally, the two selected solvents
must be immiscible, or not soluble in one another, so that they produce two separate solvent
layers[4], therefore the choice of the extracting solvent is very critical in this protocol, in our
experiment the extracting solvent we used was hexane which is a nonpolar solvent which
when mixed with our waste water sample separated into two layers since they are immiscible,
this organic solution is less dense than water and in this case, the water layer was drawn off
through the stopcock, and the organic solution was retained in the funnel, ready for the next
extraction. After dissolving the mixture in the first solvent, the solution was added to a second
solvent. The two layers were vigorously mixed to maximize the surface area between them,
this mixing facilitates the transfer of a dissolved compound from one solvent layer to another.
Once the transfer process was complete, the layers were again allowed to form .Separation of
the two layers then completed, the separation of the desired compound from the impurities
was done.

The objective of a simple solvent extraction is to partition one or more substances between
two immiscible solvents and this is usually accomplished with the use of a separatory funnel,
if the separatory funnel has a glass stopcock, prepare the funnel for use by making sure that
the stopcock is lightly greased and will turn without difficulty but Teflon stopcocks need not
be greased[5]. With the separatory funnel supported in a ring,we checked to make sure that
the stopcock was closed and poured in the solution to be extracted, then added the extracting
solvent (the funnel was not filled to more than about three-fourths of its height), replaced the
stopper after wetting it with water (to keep the organic solvent from creeping out around the
stopper). With vigorous shaking, a total mixing period of ten to thirty seconds was considered
adequate to establish equilibrium, this allowed the separation of our mixtures.

When a volatile solvent is involved in an extraction, the establishment of the equilibrium

vapor pressure of the solvent will cause the pressure to rise inside the stoppered separatory
funnel[5], This pressure was best released by turning the funnel upside down (with the stopper
held in place with the palm of the hand) and cautiously opening the stopcock. Since a volatile
solvent (hexane) was used, the first mixing consisted only of a slow inversion of the
separatory funnel followed by release of the pressure. It is dangerous to try to extract a
solution if its temperature is near or above the boiling point of the extracting solvent[5]. Thus
because we used hexane the solution was cooled before extraction, When these solvents are
used, it is also a good idea to hold the separatory funnel by the ends so that the contents will
not be warmed by your hands.
CONCLUSION

The extraction of organic matrices from our waste water sample by solvent extraction was
successfully done and the desired matrix was ready for the next extraction.

REFERNCES

[1], Assessing solvent extraction approaches and methods, (2003). OECD, WHO.

[2], Manja, K.S., R. Sambasiva, K.V.Chndrashekara, K.J.Nath, S.Dutta, K.Gopal, L.lyenger,

S.S.Dhindsa and S.C.Parija, (2001). Report of study of Solvent Extraction, New Delhi.

[3], Chandrashekara, K.V., (2002).), Water Quality Management: South Asian Perspective,
Vision 2025. ILSI-India & UNICEF.

[4], Guidelines for removing Organic matrices from water- Water quality, 3rd Edition - vol 1:
Recommendations. WHO; 2004.

[5], Standard methods for the examination of water and wastewater; 20th Edition, Ed. Pub.
APHA, AWWA and WEF, 1998.