Che 314; Analytical Chemistry

Names: BOKANG OBUSENG

Student no.: 201501174
WEEK: 8
Day: Friday
Date of submission: 7 May 2018
EXPERIMENT 2: SOLVENT EXTRACTION OF
METALS BY LIQUID - LIQUID EXTRACTION
AND ANALYSIS USING ATOMIC ABSORPTION
SPECTROSCOPY
AIM

This experiment was conducted with the aim of separating three metals (Cu, Pb and Mg) in a
sample mixture by liquid-liquid extraction and then use atomic absorption spectroscopy (AAS)
to determine their concentrations.

ABSTRACT
Separation of three metals ( cu, Pb,Mg) in a sample mixture by liquid-liquid extraction was
successfully carried out. The concentration of copper was found to be 0.057 mg/L in flask A and
0.044 mg/L in flask B, For magnesium the concentration was determined to be 0.1589 mg/L in
flask B and 0.1875 mg/L in flask C.

INTRODUCTION
In this experiment, liquid – liquid extraction is used to separate the metals copper, magnesium
and lead from a sample mixture. This technique employs the use of two immiscible liquids like
the aqueous and the organic liquids. The organic phase will float on top of the aqueous phase and
based on the principle ‘’like dissolves like’’ therefore, substances will dissolve on a certain phase
depending on how they interact with that phase. The substance of interest will then be identified
and quantified from that phase by a technique called Atomic Absorption Spectroscopy (AAS).
This technique is used principally for the quantitative determination of metal elements in
aqueous and solid samples from a wide range of fields including medicine, food and geology,
etc. The essential theory and principles of AAS as well as its applications and limitations for
chemical analysis will be investigated. This unit concentrates on atomic absorption based
on flames. Flame AAS is widely used, simple, effective and relatively low cost.
The technique makes use of absorption spectrometry to assess the concentration of an analyte in
a sample. It requires standards with known analyte content to establish the relation between the
measured absorbance and concentration of the analyte hence rely on the Beer-Lambert Law
which states that;
A = έbc
Where; A is the absorbance of the sample
έ is the molar absorptivity coefficient
b is the path length and
c is the concentration

The electrons of the atoms in the atomizer are promoted to higher orbital (excited state) for a
short period of time (nanoseconds) by absorbing a defined quantity of energy (radiation of a
given wavelength). This amount of energy, i.e. wavelength, is specific to a particular electron
transition in a particular element. In general, each wavelength corresponds to only one element,
and the width of an absorption line is only of the order of a few picometers (pm), which gives the
technique its elemental selectivity. The radiation flux without a sample and with a sample in the
atomizer is measured using a detector, and the ratio between the two values (the absorbance) is
converted to analyte concentration or mass using the Beer-Lambert Law. Applying the Beer-
Lambert law directly in AAS is difficult due to: variations in atomization efficiency from the
sample matrix, non-uniformity of concentration and path length of analyte atoms (in graphite
furnace AAS).
The chemical methods used are based on matter interactions, i.e. chemical reactions. For a long
period of time these methods were essentially empirical, involving, in most cases, great
experimental skills. In analytical chemistry, AAS is a technique used mostly for determining the
concentration of a particular metal element within a sample. Hence from this experiment,
copper, lead and magnesium are separated from a mixture by liquid-liquid extraction and
analysed using AAS.

METHODOLOGY

a. Reagents and apparatus

CHEMICALS APPARATUS
Cu/Pb/Mg ion mixture 125mL separation funnel
0.5 M Chloroacetate buffer (pH 3.00) 1mL pipette
0.10 M Oxine in CHCl3 3 x 50 mL volumetric flasks
2.0 M HCl 100 mL beaker
Dilute ammonia solution (1M) 100 mL Erlenmeyer flask
Distilled water AAS machine
Litmus paper

b. Procedure
1ml of the sample of Cu/Pb/Mg ion mixture was dilvered using a pipette into a 125ml separation
funnel containing 10 ml distilled water. 10ml of 0.5 ml chloroacetate buffer was added to the
funnel to extract Cu. Then 10ml of 0.10 M oxine was added CHCl 3. The mixture was then
shaken for 1 minute and the layers were allowed to separate. The CHCl 3 layer was extracted
through a smaller filter funnel with a small plug of cotton wool into a 100 ml conical flask. The
extraction of copper was repeated 2 times with two 5 ml aliquots of oxine solution and 3 oxine
extracts were combined and labelled “flask A”. The remaining aqueous solution was drawn off
into a 100 ml beaker then 3 drops of dilute ammonia solution were added. Then the solution in
the beaker was transferred back into the separating funnel and rinsed 2 times with distilled water.
Lead was extracted from the solution with 0.1M oxine in CHCl 3 using the same procedure used
for copper extraction. The extraction of Lead with 2 more 5ml aliquots of oxine solution was
done then the extracts were combined and labelled “flask B”. The top was drawn off to 50 ml
volumetric flask and then rinsed with distilled water and made up to the mark with distilled water
and the flask was labelled “flask C”. Copper was back extracted in the first CHCl 3/oxine extract
in flask 1 three times with 10 ml, 5 ml and 15 ml of 2 M HCl. The aqueous layer in a 50 ml
volumetric flask was collected and made up to the mark with distilled water and labelled “flask
A”. Lead was back extracted in the same way as copper and the resultant flask was labelled
“flask B”. The 5 ppm standards of Cu, Pb, and Mg were used to make a suitable range of
standards to bracket the expected concentration (1-5 ppm) in the extracts. Then the
concentrations of copper in flasks A and B, lead in flasks A, B, C and magnesium in flasks B and
C were determined using appropriate Atomic Absorption conditions.

RESULTS AND ANALYSIS OF DATA

Table 2: Concentrations of each component in each flask

FLASK [Cu] in mg/L [Mg] in mg/L
A 0.057 -
B 0.0474 0.1589
C - 0.1875

DISCUSSION
The calibration curves of 5 standards that were determined from this experiment for three metals
(lead, copper and magnesium) were used to calculate the concentration of the three metals in
solutions as seen from the attached results. The graphs were linear hence obeying the Beer’s law.
The concentration of copper was found to be 0.057 mg/L in flask A and 0.0474 mg/L in flask B,
For magnesium the concentration was determined to be 0.1589 mg/L in flask B and 0.1875 mg/L
in flask C. The liquid – liquid extraction method was successfully used in extracting the metals
before analysis using the AAS. Though the method is highly laborious, it is the best method to
use for separation and extraction of chemical species like metals [3].

The possible errors may include, Errors in pH adjustment: Since each of the three metals was
extracted at a specific pH, it might have happened that the pH of the solutions were not
accurately adjusted hence affecting the amount of a metal to be extracted. For instance, a pH
value below the required one for extraction will mean that little or nothing will be extracted from
the mixture. Human error: It could also have happened that not all the metal was extracted from
the separation funnel due to failure to run off all the desired solution containing the metal.
Instrumental error: Since the FAAS machine was used to analyse the amount of each metal in
each flask, it might have happened that the machine/instrument was not appropriately set or
calibrated. This has been observed from the deviations obtained from both the concentration and
absorbance values.

In order to correct or improve the results obtained in this experiment, one should ensure that pH
values for the solutions are accurately adjusted in accordance to the targeted metal to be
extracted. According to Ashall (2007), the efficiency of liquid-liquid extraction can also be
enhanced by adding one or more extractants to the solvent phase. The extractants interacts with
component to be extracted, increasing the capacity of the solvent.

CONCLUSSION
It was concluded that liquid – liquid extraction is the best method for separation and extraction of
metals in a sample. The concentration of copper was found to be 0.057 mg/L in flask A and
0.044 mg/L in flask B, For magnesium the concentration was determined to be 0.1589 mg/L in
flask B and 0.1875 mg/L in flask C.

REFERENCES

1. Skoog.W and Holler. D, (2007), Fundamentals of Analytical Chemistry, 7th ed., Wiley,
New York, p 759 – 789.
2. Walsh. A, (1955), The application of Absorption Spectra to Chemical Analysis,
Spectrochim, Acta 7, p 108-117.

3. Skoog, D.A., and James J.L, (1992), Principles of instrumental Analysis, 4th ed., Fort
Worth, Tex: Saunders College, p 800 – 831.

4. Welz. B and Sperling. M, (1999), Atomic Absorption Spectroscopy, Wiley-VCH,

Weinheim, Germany, p 445 – 476.