HANDBOOK

Chemistry
EXPERIMENT
FEST 2012
www.newcastle.edu.au
Experiment Fest
Page 2
CONTENTS
Introduction 3
Welcome 4

Studying Chemistry 6
Analysis of Nitrate Ion Concentration in Water 8
Determination of Phosphoric Acid in Cola 13
Determination of Sulfate in Lawn Food 20
Metal Analysis by Atomic Absorption Spectroscopy:
Concentration Of Sodium In Sports Drinks 25
Experiment Fest
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INTRODUCTION
ExperimentFest is an experiment program designed to provide enriching
educational experiences for senior high school students who are studying
Physics, Chemistry and Biology. ExperimentFest is supported by the
University of Newcastles Faculty of Science and Information Technology and
takes place at both the Callaghan and Ourimbah (Central Coast) campuses of
the University of Newcastle.

Callaghan Campus:
Physics - Mon 18 Thurs 21 June, 2012
Chemistry - Mon 18 Fri 22 June, 2012
Biology - Fri 15 - Fri 22 June, 2012

Ourimbah Campus:
Biology, Physics & Chemistry Mon 25 - Thurs 30 June, 2012
Tuncurry:
Physics - Saturday 23 June, 2012


The activities allow students to engage in a range of hands-on experiments
that are difficult to organise within a school setting, all under the supervision
of University Staff and Postgraduate students. Each experiment is chosen to
complement the NSW HSC syllabus for Biology, cementing classroom theory
and providing a good basis for examination preparation.

Experiments include:

Enzymes

Kidney Function

Measuring oxygen satration in the blood
All experiments are complemented by notes, follow-up discussions and
questions to enhance your learning experience.
For booking information contact:
Larry Milton on 49 469 159 or 0404 460 470; or
David Rushton on 4333 6965 or 0414 238 464
Experiment Fest
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WELCOME
Welcome to the Faculty of Science and Information Technology at the Univer-
sity of Newcastle. ExperimentFest is a wonderful chance to give you practical
experience which complements your classroom learning while giving you a
first hand look at University life and facilities. Science is an exciting field of
study, allowing you to move with the times and contribute actively and respon-
sibly to society. There are many education opportunities in science after high
school. Here in the Faculty we provide study and research programs in fast-
moving modern fields that make our world work.
The Faculty staff and students who will be taking you through the experiments
today are involved in contemporary science research. Please ask questions
and utilise your time with them.
Take this day to enjoy being out of the class room, exploring science with fel-
low students and participating in valuable experiments and discussions which
will help you in your HSC and beyond.
I wish you well in your studies. I hope you apply yourselves to the learning
process with enthusiasm and you enjoy your time at the University. We hope
to see you studying with us in the future!
Best wishes,

Prof. Bill Hogarth
Pro Vice-Chancellor Faculty of Science and Information Technology
University of Newcastle
CHEMISTRY
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STUDYING CHEMISTRY
Why study chemistry?
Chemistry is truly the central science. It is the science of the molecular scale, and it is at the molecular level where
major advances are being made in many diverse areas such as medicine, drugs, nanotechnology, new materials, and
the environment. A sound knowledge of chemistry is required to fully understand many other areas of science, and
this is why the study of chemistry is either compulsory or recommended by many other disciplines in the University.
Chemistry opens the door for many careers because training in chemistry is essential for many positions in industry, is
highly desirable for science teaching, and is useful for careers in the public service and management. Both the public
and the private sectors increasingly draw their higher management echelons from chemistry graduates.
But, most importantly, it is just so fascinating! If you want to understand the workings of the world around you - then
chemistry is for you!
Opportunities for further studies in Chemistry:
The Bachelor of Science degree program at the University of Newcastle provides a foundation of knowledge, skills
and attributes that allows graduates to be employable not just today but into the future and to contribute actively and
responsibly to society. Majoring in Chemistry, you have the opportunity to sample and/or specialise in any one of the
following:

Analytical Chemistry

Chemistry

Chemometrics (double major)

Environmental Chemistry

Forensic Chemistry

Geological Chemistry

Industrial Chemistry

Materials Chemistry

Medicinal Chemistry

Surface and Colloid Chemistry
Research in Chemistry at the University of Newcastle:
There are various groups here at the University which are committed to research in chemistry. Groups include:

Analytical and Environmental Chemistry

Battery Materials and Applied Electrochemistry

Coordination and Bioinorganic Chemistry

Marine Natural Products and Chemical Ecology

Polyoxymetalates and Catalysis

Surface and Colloid Group
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For me chemistry represented
an indefinite cloud of future
potentialities
- Primo Levi
Careers in Chemistry:
The Faculty of Science and IT care about our students and are interested
in giving as much direction as possible to those making career choices
and beyond. The possible career paths listed below include a range of
opportunities for graduates at degree, honours, and post graduate study
levels.

Analytical Chemist

Clinical Research Coordinator

Developmental Chemist

Environmental Chemist

Energy Technologist

Forensic Chemist

Geochemist

Industrial/Production Chemist

Laboratory Manager

Laboratory/Research Assistant

Meteorologist

Organic/Synthetic Chemist

Pharmaceutical/Medicinal Chemist

Reproductive Medicine / IVF Chemist

Research Scientist

Science Information/Education Officer

Science/Chemistry Teacher

Sciences Technician

Scientific Patent Attorney / Technical Advisor

Scientific Policy Officer

Scientific Writer
For more information on these career paths, please visit the Universitys
careers website: www.newcastle.edu.au/service/careers/majors/
For more information on the Faculty of Science and IT check out our website:
http://www.newcastle.edu.au/faculty/science-it/
Experiment Fest
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ANALYSIS OF NITRATE ION
CONCENTRATION IN WATER
SAFETY GLASSES MUST BE WORN AT ALL
TIMES DURING THE LABORATORY SESSION
RISK ASSESSMENT
Hazard Substance, Apparatus,
Procedure.
Precaution / Action
Burette filling: Use a plastic funnel to fill burette; remove equipment from retort
stand and fill over sink.
Pipette filling: Do not pipette by mouth. Use a pipette bulb to fill pipette.
Concentrated HCl Avoid skin contact, wash with copious quantities of water. Wear
safety glasses. Use in fumehood.

Extract from HSC Chemistry Syllabus:
Identify that water quality can be determined considering:
- concentrations of common ions
- total dissolved solids
- hardness
- turbidity
- acidity
- dissolved oxygen and biochemical oxygen demand
Perform frst-hand investigations to use qualitative and quantitative tests to analyse and compare the
quality of water samples
http://altura.speedera.net/ccimg.catalogcity.com/210000/21
1600/211630/Products/5673991.jpg
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Introduction
Nitrate and phosphorus are together known as nutrients when found in water
bodies. These two species, if present in sufficient quantities, allow excessive
plant growth and eventual stagnation of the water. This process is known as
eutrophication. Nitrogen is tied up in biological systems. Nitrate and nitrite
ions are important indicators of pollution by organic materials as nitrogen from
decomposing organic substances often ends up as nitrate or nitrite ions. The
determination of nitrate is often difficult because of the low levels found, and
the distinct possibility of interfering materials being present.
Spectrophotometry
When determining nitrate it is important to choose an analytical method
that suits both the interferences that are present and the level of analyte in
the solution. Spectrophotometry is an excellent analytical method. In visible
spectrophotometry, light impinges on a coloured substance causing certain
wavelengths of light to absorbed. The remaining wavelengths of light in the
visible spectrum are reflected and transmitted to the eye of the viewer. For
example, a purple dye absorbs wavelengths in the green-yellow parts of the
visible spectrum and reflects red and blue wavelengths of light.
Spectroscopy can also be carried .be carried out using other parts of the
electromagnetic spectrum such as the ultra-violet and infrared regions. The
principle of evaluation remains the same however, provided you have a device
for detecting the intensity of the radiation in the chosen region of the spec-
trum. In this experiment you will utilize UV radiation to quantify the amount of
nitrate ion in an unknown sample.
The Beer-Lambert Law.
The intensity of a coloured solution depends upon the concentration of the
coloured component and the path length through which the light travels. Laws
describing the absorption of light were originally formulated by Lambert (1760)
and Beer (1852), and today are combined to give a single law, which quanti-
tatively relates the extent of absorption of light to the concentration of absorb-
ing species in solution, known as the Beer-Lambert Law. Importantly this law
refers to a single wavelength and not to the absorption band as a whole.
Experiment Fest
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The Beer-Lambert Law states that, at a given wavelength,
the relationship between the intensity of the incident
and transmitted monochromatic light in terms of the
concentration of the absorbing species in solution and the
pathlength is given by:
where:
I
0
is the intensity of the incident light of definite
wavelength,
I
t
is the intensity of the transmitted light of the same
wavelength,
is the molar absorptivity (in units of L mol
-1
cm
-1
) at
that wavelength. It is a constant for a pure substance,
c is the concentration of the absorbing substance (in
mol dm
-3
, i.e. mol L
-1
),
d is the pathlength (in cm) of the absorbing substance.
Using mathematics (a log transformation) this equation
may be simplified to a linear form:
where:
Measurement of the absorbance of light by solutions
is accomplished using a spectrophotometer. In a
spectrophotometer a light source emits a range of
wavelengths which are passed into a monochromator.
The monochromator in turn selects a single wavelength of
light which is passed through the sample to be measured.
The incident light beam is absorbed to some extent by the
sample and the intensity of the transmitted light (of the
same wavelength as the incident light) is measured by a
photoelectric device.
The electrical circuit is so designed that the output of the
instrument is calibrated to read directly in absorbance or
percentage transmission.
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In this experiment you will use a spectrophotometer to determine the
concentration of an unknown nitrate containing solution in the UV region of the
electromagnetic spectrum. Good results may be obtained if the water contains
little or no organic matter (which also absorb in the UV). The method will involve
taking an absorbance spectrum of nitrate ion in the range 190- 300 nm to
select the strongest absorbance wavelength for your measurements. You will
then construct a calibration plot, otherwise known as a Standard Curve (see
below) from the absorbances of the nitrate samples of known concentration.
The concentration of the unknown NO
3
-
sample will then be determined by
measuring its absorbance and reading the concentration from the Standard
Curve.
Procedure
1. Prepare nitrate calibration standards for 0, 5, 10 and 15 mg/L by adding 0,
5, 10 and 15 mL, respectively, of the 100 mg/L stock nitrate solution, and
then making them up to the mark in a 100 mL volumetric flask with HCl
(i.e. 1mL of Conc HCl) and ultra-pure water.
2. Prepare your sample in a similar fashion by diluting 20 mL of the natural
water sample in a 100 mL volumetric flask with HCl and ultra-pure water.
3. Using your 0 mg/L standard record a background absorbance spectrum in
the range 190-300 nm.
4. Measure the absorbance spectrum of the remaining standards and sample
over the same wavelength range.
5. Prepare a calibration graph by plotting the absorbance maximum in each
spectrum and hence determine the concentration of nitrate ion in the
natural water sample.
NO
3
-
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Results
Solution Wavelength Maximum (nm) Absorbance at Maximum
0 mg/L standard
5 mg/L standard
10 mg/L standard
15 mg/L standard
Unknown
Unknown Concentration =
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Page 13
DETERMINATION OF
PHOSPHORIC ACID IN COLA
SAFETY GLASSES MUST BE WORN AT ALL
TIMES DURING THE LABORATORY SESSION
RISK ASSESSMENT
Hazard Substance, Apparatus,
Procedure.
Precaution / Action
Burette filling: Use a plastic funnel to fill burette; remove equipment from retort
stand and fill over sink.
pH electrodes Use with care. Remove electrode from solution when stirring.
Pipette filling: Do not pipette by mouth. Use a pipette bulb to fill pipette.
0.1 M NaOH solution. Avoid skin contact, wash with copious quantities of water. Wear
Safety Glasses
Extract from HSC Chemistry Syllabus:
The Acidic Environment Contextual Outline (extract)
Acids such as ascorbic acid (vitamin C) and citric acid occur in many foods. Many drinks
contain carbonic acid and some contain phosphoric acid. Other acids, such as benzoic
acid and acetic acid, are added to drinks and food to act as preservatives. Hydrochloric
acid is secreted into the human stomach to assist in the digestion of food, especially of
proteins to amino acids.
Extract from Chemistry Stage 6 Syllabus:
Perform a frst-hand investigation to determine the concentration of a domestic acidic
substance using computer-based technologies.
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Introduction
Determination of the concentration of acids or bases
is routinely carried out by titration using an acid / base
indicator such as phenolphthalein. Selection of the
correct indicator is important to ensure that the endpoint
(at which point the indicator changes colour) corresponds
with the equivalence point (the exact point where the
acid or base is neutralized) in the titration. In situations
where coloured solutions are involved, determination of
an end-point by a colour change is not practical. Under
these circumstances, a pH electrode (shown right) is
often used.
Given that cola is coloured, we will use a pH electrode to
determine the concentration of one of the components
of cola, phosphoric acid, by titration with dilute sodium
hydroxide. Titrations where a pH electrode is used are
often termed potentiometric titrations.
Principle
The electrical potentials of the electrode in the pH
meter (shown right) is dependent upon the hydrogen ion
concentration of the solution in which it is immersed. The
thin walled glass bulb at the end of the electrode which
contains a platinum contact immersed in a buffer solution
coupled to a reference electrode of fxed potential
(Ag/AgCl). The potential of this electrode can be directly
related to pH via an equation of the form:
E = E
glass
- 0.05915 pH
where E
glass
is a non-constant potential characteristic
of the glass electrode. The equation shows that the
electrical potential of the probe is therefore a function of
pH, consequently the electrode may be used to monitor
changes in solution pH. An incremental plot of the
observed pH readings against volume of titrant (NaOH
in this experiment) added, yields a curve with one or
more regions in which there is a rapid change in pH.
These infection points correspond to the completion of
proton-transfer equilibria for H
3
PO
4
; that is, they indicate
titration equivalence points. Further treatment of the data
with Excel permits a more accurate determination of the
equivalence points.
The frst infection point for H
3
PO
4
occurs at complete
conversion to dihydrogen phosphate ion (H
2
PO
4
-
).
Reaction complete at frst equivalent-point is thus:
H
3
PO
4
+ OH
-
H
2
PO
4
-
+ H
2
O (1)
www.seeinc.com/moreinfo/ AccumetXL25.html
Experiment Fest
Page 15
This point is significant, as there is a rapid increase in pH with only a small
addition of base. When the data is plotted, this first inflection point will be
obvious. As this is the first equivalence point (see plot below), it should be
approached carefully so that a precise measure of the volume of base
required can be obtained.
Continued addition of base results in the conversion of the dihydrogen
phosphate species to the mono-hydrogen form and a second infection point
appears on the titration curve. i.e.
H
2
PO
4
-
+ OH
-
HPO
4
2-
+ H
2
O (2)
Again, this second equivalence point will be obvious, as there is a rapid
change in pH with the addition of only a small volume of base. Further
addition of NaOH leads to the formation of phosphate ion:
HPO
4
2-
+ OH
-
PO
4
3-
+ H
2
O (3)
An animated graph showing the change in concentration of the species
present in a phosphoric acid titration can be viewed at the following website:
http://chemistry.beloit.edu/Rain/moviepages/phosphoric.htm. The
last infection point can be very diffcult to observe and we will not be trying
to detect it in this experiment. From the volume of titrant (OH
-
) consumed
between the frst and second infection points, the concentration of the
phosphoric acid component can be calculated.
Typical Titration Curve for Phosphoric Acid.
14
12
10
8
6
4
2
0
pH
0 0.5 1 1.5 2 2.5
Fraction Titrated
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Procedure: Phosphoric acid content of Coca-Cola
The beverage Coca-Cola contains significant amounts of phosphoric acid and phosphate salts and these can
be evaluated by titration. However, since beverages also contain carbonic acid, a necessary preliminary step is
elimination of this species. To shorten the lab, the Coke has been boiled already.

pH ELECTRODES ARE FRAGILE AND VERY EXPENSIVE!
They are easily damaged, so please take care when handling them !
1. Take a 100.0mL aliquot of the boiled beverage in a 250mL beaker.
2. Place the beaker on the magnetic stirrer, add the stirrer bug (more correctly a magnetic
follower) and carefully clamp the burette into position above the beaker (so that you can
comfortably add base) and the pH electrode into position. Turn the stirrer on and make sure that
it does not come into contact with the pH electrode. Stirring should be a steady, constant rate
not too rapid. This will help achieve effective mixing with each addition of the base.
3. With the pH electrode in place, titrate the solution with standard (approximately 0.10M NaOH
record the exact concentration) sodium hydroxide solution, recording the pH after each
addition. The first two additions of titrant volume (V
b
) can large (about 1 mL), as the pH change
at this point in the titration is only small (see diagram on page 15). The volume added should
however be decreased beyond this point the pH will begin to rise rapidly. You will need
to make adjustments to V
b
based on the change in pH / V. Make sure that you calculate
pH/V for each new V
b
addition as this will show when you are nearing the titration end-point
(by becoming large). When the pH is changing rapidly record the volume of addition should be
reduced to no more than 0.1mL - 0.2mL.
Drop-wise addition of NaOH in the vicinity of the equivalence point is essential to
create a satisfactory plot. Make sure that you calculate pH/mL as you go. This
permits precise determination of the end points.
4. Once you have passed through the first end point pH / V will fall off in magnitude. Have the
supervisor check your results at this point, then proceed to ascertain the second endpoint using
the same approach in step 3. The volume of NaOH may again be increased in the initial stages
(~5 mL) until you approach the second end point. The volume of NaOH added between the 1
st
and
2
nd
endpoints (V
2
) will be about the same as that observed for the first equivalence point (V
1
).
5. When the second inflection point has been reached, turn the magnetic stirrer off, remove the
pH electrode from the solution, wipe carefully with a clean tissue and place in the original flask
of distilled water. Leaving pH electrodes in solutions of high pH can damage them.
6. The titrated solution can be discarded down the sink.
DO NOT THROW THE BUG OUT WITH THE SOLUTION!
Replace it on the magnetic stirrer.
www.australianwinemakers.com.au
Experiment Fest
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Results: Concentration of NaOH solution M
mL NaOH added (Vb) Solution pH pH / mL
Example
0.00
5.10
2.55
2.75
2.75 - 2.55
5.10 - 0.00
= 0.04
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mL NaOH added (Vb) Solution pH pH / mL
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Data Handling / Calculations
8. Enter your results into an Excel spreadsheet under the column headings pH and V
b
mL, where V
b
is the volume of
base (NaOH) added (mL).
9. Generate a graph of this data, plotting pH (vertical axis) against V
b
volume of base added (mL). Label this plot pH
verses volume of NaOH added.
Results
10. From the graph, identify the volume of NaOH required for the titration of H
3
PO
4
-

the first equivalence point (V
1

on graph p15). Use this volume to calculate the concentration of the phosphoric acid present in the cola. Ex-
press your answer in moles per litre of cola (i.e. the molarity). Repeat this calculation using the volume of NaOH
required for the neutralisation of H
2
PO
3
-
(Eq. 2) - the NaOH volume between the first and second equivalence
points (V
2
on graph p15).
Follow-up activities:
1. Was there any difference between the volumes of NaOH required to achieve the first and second equivalence
points in the titration? What could account for this difference? Which of the NaOH volumes is likely to be the more
accurate? Explain your choice.
2. Why was the cola sample boiled prior to analysis?
3. A more accurate way to estimate the equivalence point is to perform a differential plot. Here a plot of pH/mL
verses volume of NaOH (V
b
) is prepared. The expression pH/mL shows the rate of change of slope along the
titration curve yielding a very accurate end point. (see below). Instructions on how to prepare a differential plot us-
ing Microsoft Excel may be found at.: A differential plot of a titration curve may be viewed at
http://facstaff.bloomu.edu/eschultz/chem%20116%20spring%2006/lab/Generating%20Titration%20Curve.pdf
7.00
6.00
5.00
4.00
3.00
2.00
1.00
0.00
12
10
8
6
4
2
0
pH
0 10 20 30 40 50 60
mL Base added
H 7
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Page 20
DETERMINATION OF
SULFATE IN LAWN FOOD
SAFETY GLASSES MUST BE WORN AT ALL
TIMES DURING THE LABORATORY SESSION
RISK ASSESSMENT
Hazard Substance, Apparatus,
Procedure.
Precaution / Action
Burette filling: Use a plastic funnel to fill burette; remove equipment from retort
stand and fill over sink.
Ammonia/Ammonium
Chloride solution
Toxic by inhalation. Causes burns. Risk of serious damage to eyes.
Use in fumehood
Pipette filling: Do not pipette by mouth. Use a pipette bulb to fill pipette.
BaCl
2
solution. Harmful by inhalation. Toxic if swallowed. Skin contact may produce
health damage. Avoid skin contact. Wash affected area well.
Eriochrome Black T
indicator
Cancer suspect agent. Cumulative effects may result following
exposure. Avoid skin contact. Wash affected area well.
Hot Plate: Burn risk. Avoid skin contact.
Extract from HSC Chemistry Syllabus:
Identify data, plan, select equipment and perform firsthand investigations to
measure the sulfate content of lawn fertilizer and explain the chemistry
involved
Analyse information to evaluate the reliability of the results of the above
investigation and to propose solutions to problems encountered in the
procedure.
http://altura.speedera.net/ccimg.catalogcity.com/210000/211600/211630/Products/5673991.jpg
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Introduction
The traditional method of determining sulfate is by precipitation as the barium
sulfate, filtering, ashing the filter paper (i.e. heating until the filter paper is turned
to ash with effectively zero weight) then weighing the residual matter. This is
termed a gravimetric method, as it relies on weighing. While not a particularly
complex procedure, it is time-consuming. The solution has to be boiled for nearly
1 hour to ensure that the barium sulfate precipitate forms particles large enough to
be successfully filtered. This process is termed digestion.
Titrations
In carrying out the titrations, use two samples (i.e. carry out the titrations in duplicate) and record your values to 2 deci-
mal places (that is, estimate between the graduations on the burette). Ideally, the two results should be within 0.2 mL to
be acceptable. Record your results in the Table below.
To simplify calculations, a blank titration is carried out first, where the volume of EDTA required to react with the Ba
2+

ions before the reaction with sulfate is determined. Record all titration values to second decimal point.
Interferences
This method will not give a meaningful result in the presence of phosphate, as the solid barium phosphate will also form,
leading to an incorrect estimation of the amount of barium ions which reacted with the sulfate.
In addition, the presence of other metal ions (such as copper, zinc, etc) will lead to low sulfate estimation, as these ions
also react with the EDTA. Their presence would lead to more EDTA being used than for the barium alone. As we are re-
lying on this value to determine the remaining barium, this figure will be artificially inflated. Thus when this inflated value
is subtracted from the initial moles of barium added, we would underestimate the actual sulfate concentration.
Supplied solutions:
Fertiliser solution of known concentration (6.6 g/L)
0.2 M Barium chloride BaCl
2
0.1 M EDTA solution
(Note: record the exact concentration 4 decimal points)
Concentrated ammonia solution NH
3

(CAUTION: see safety note above)
Eriochrome Black T indicator solution.
An alternative method, the one we will use, involves the addition of a known number of moles (excess) of barium ions
(added as a soluble barium salt), which then precipitates as barium sulfate. After removing the precipitate, the residual
barium in solution may be determined by titration with ethylenediamine tetraacetic acid (EDTA). This method is termed
a back titration. EDTA is a strong chelate - a species that reacts with metal ions to form a stable metal complex. It
reacts in a 1:1 ratio with barium forming a soluble complex (see equation). EDTA titrations are carried out under basic
conditions, often buffered to maintain a highly basic pH environment. This is to ensure that all of the OH protons in the
carboxyl units of EDTA have been deprotonated, thereby enabling the metal complex to form.
Experiment Fest
Page 22
Procedure:
Steps 1 and 2 should be carried out in duplicate (2 samples). Get steps 1 and 2 underway before
commencing the titration.
1. Pipette 1 x 50.0mL of the supplied ammonium sulfate solution into two separate beakers.
2. Pipette 25.0mL of 0.2M barium chloride into each beaker, then cover the solution with a
watchglass and place on the hotplate in the fume cupboard. These solutions will be used by
the group undertaking the experiment after you. Take two of the predigested samples from the
hotplate for your experiment.
3. Return the fertilizer solutions to your bench, place them in an ice bath to cool. While this is
taking place, carry out a blank titration on the 0.2M barium chloride solution as follows:
Pipette 25.00mL of 0.2M barium chloride into a 250 mL conical flask
Add 10mL of concentrated ammonia/ammonium chloride solution and 3-4 drops of
indicator
Titrate with 0.1M EDTA from red/purple to a blue endpoint.
Record the volume of EDTA required in the Results Table below as V
b
.
4. Repeat step 3 to obtain a duplicate result for the blank titration. Record the volume in the table
and average the two blank titration results.
5. Remove the now cooled fertilizer solutions from the ice bath and filter the BaSO
4
precipitate
from the first sample using the Millipore filtration apparatus on you bench. Make sure that you
place a 0.45m filter paper in the apparatus before commencing to filter.
This apparatus is very expensive. Take great care! Make sure that you use the filter
paper and not the separating paper! Check with the demonstrator if you are unsure.
6. Transfer the clear filtrate to a 250mL conical flask. Add 10mL concentrated ammonia/
ammonium chloride solution and 3-4 drops of the indicator solution.
7. Repeat steps 5 -7 for the second fertilizer sample.
8. Titrate sample 1 with 0.1M EDTA until the colour changes from red/purple to blue. Record this
volume to 2 decimal places as V
t
in the Results Table below.
9. Repeat step 8 with the second sample of the fertilizer solution.
10. Use the information in the Results Table to calculate the percentage of sulfate ion in lawn
fertilizer.
To assist the completion of the experiment, samples of the lawn fertilizer
pretreated with barium ion and predigested will be available. You will prepare
fresh samples for the group following you.
Experiment Fest
Page 23
Results:
Concentration of fertiliser (g/L) 6.6 g/L
Concentration of EDTA (exact concentration) M
Volume of EDTA required for blank (V
b
)
Titration 1 ...mL
Titration 2 ...mL
Average Titre: ...mL
Volume of EDTA required for test solution (V
t
)
Titration 1 ...mL
Titration 2 ...mL
Average Titre: ...mL
Difference in volume of EDTA (corresponding to Ba
2+
used, thus SO
4
2-
present) - V
b
- V
t
...mL
.
.
. moles of EDTA consumed. moles
.
.
. moles of sulfate moles
Initial mass of fertiliser in 50.0 mL sample ....g
Mass of sulfate determined experimentally ....g
% sulfate in the lawn food
Follow-up activities:
1. Calculate the percent of sulfate if the sample had been pure ammonium sulfate. Account for any differences.
2. Can you suggest any changes in the experimental procedure that may improve the accuracy?
3. What was the reason for adding the ammonium chloride?
4. Why is the concentration of the barium chloride not required in the calculations?
5. How could you minimise the interferences identified above?
Experiment Fest
Page 24
METAL ANALYSIS BY ATOMIC ABSORPTION SPECTROSCOPY:
CONCENTRATION OF SODIUM IN
SPORTS DRINKS
SAFETY GLASSES MUST BE WORN AT ALL
TIMES DURING THE LABORATORY SESSION
RISK ASSESSMENT
Hazard Substance, Apparatus,
Procedure.
Precaution / Action
Burette filling: Use a plastic funnel to fill burette; remove equipment from retort
stand and fill over sink.
Pipette filling: Do not pipette by mouth. Use a pipette bulb to fill pipette.
Extract from HSC Chemistry Syllabus:
Some foodstuffs are monitored for the presence of particular metals,
e.g. lead, to ensure that we are not consuming poisons that can accumulate
in our bodies.
Gather, process and present information to interpret secondary data from
AAS measurements and evaluate the effectiveness of this in pollution control.
AAS allows the detection of very small concentrations from samples of air,
water or food. This activity depends on your ability to manipulate data and
dilution factors. The absorbance values obtained using solutions of known
concentration enable you to draw a calibration graph. Use the specifc
absorbance data provided to read off the corresponding concentration for the
sample.
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Introduction
Atomic Absorption Spectroscopy (AAS) is a commonly
used technique for determining the concentration of metal
ions. This analysis of metals is important in a range of
applications from trace analysis of metals including
pollutants - in water and soil to quality control of materials
such as iron and special steels.
Quality control in products is an important commercial
tool. In this instance, the presence of salts such as
sodium in sports drinks is critical for their usefulness in
replacing the salt loss by athletes through perspiration.
Too little salt and the product will not be effective.
However, the addition of too much salt may diminish the
taste of the product, as well as slow the rate of absorption
of the liquid in the stomach.
The detection limits for metals vary considerably and
depends on the method used to atomise the sample. The
most common method for atomising samples is by fame
using an acetylene / air mixture. This produces a fame
temperature of about 2,500C, which is a relatively low
temperature for this technique. Under these conditions,
the detection limit for iron is 5 ng/L (or 5 parts per
billion, also expressed as 5 ppb), copper 1ppb; zinc
1.5 ppb and mercury 150 ppb. While these are the
detection limits, accurate quantitative analysis requires
concentrations 10 to 100 times greater than the
detection limit.
The basis of the method is that for a given metal ion, the
absorption is directly proportional to the concentration
(A [ ]) of the species present. We use this principle to
prepare a calibration curve and use this to determine the
concentration of the species in the unknown.
As with any analytical method, the determination of
metals by AAS can be affected by the presence of
other species. It is important that we are aware of these
and take steps to counter their effect. Any species that
changes the observed signal, while the concentration of
the metal remains unchanged, is termed an interference.
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Types of Interference
In this experiment we are primarily interested determining the sodium content of sports drinks by AAS. In addition,
we are interested in the possible interference from the presence of potassium in obtaining the correct reading for the
sodium. The sports drink sample you will analyse has both sodium and potassium present. In AAS, it is very important
that the standards we prepare are as close as possible to the sample under investigation.
Because alkali metals such as sodium have low ionisation potentials, they readily ionise in the fame, changing the
species responsible for the absorption and leading to errors in estimating the concentration. This is termed ionisation
interference. The simplest way to overcome this effect is to add another alkali metal that will ionise more easily than the
sodium, such as potassium. This is termed an ionisation suppressor. By having a high concentration of electrons in the
fame, ionisation of the sodium is suppressed.
Principle
Your analysis will determine the concentration of sodium present in a range of sports drinks. A series of standard
solutions of sodium will be prepared. Our selection of the range of these standards is based on our understanding of
the concentration of the unknown as well as the knowledge that high concentrations of substances cause deviations
from the linear relationship between absorption and concentration.
Preparation of the sample for analysis involves dilution of the initial sports drink sample. This is required to adjust the
concentration of sodium into the correct range for the operation of the instrument and to ensure that the absorption
reading is within the range of the standards.
Supplied solutions:
1,000 mg/L Sodium (NaCl) Stock
10,000 mg/L Potassium (KCl) Stock
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Procedure
Preparation of Standards
1. Prepare a series of four standard sodium solutions containing 0, 10.0,
20.0, 50.0mg/L (ppm) of sodium. To do this, measure out 0, 1, 2 & 5mL of
the sodium stock solution (from the supplied burette) respectively into four
separate 100mL volumetric flasks and make each flask up to the mark
with distilled water. Label them as as Na stds-1, 2, etc.
2. Prepare a series of sodium standards containing a constant amount of
potassium ions (as KCl).
3. Prepare the same series (i.e. 0.0, 10.0, 20.0 and 50.0 mg/L) as in Step 1
above by measuring out the same volume of sodium stock solution into
four new volumetric flasks. At this point, add 20mL of the 10,000 mg/L
potassium (KCl) stock solution (measured with a measuring cylinder) to
each volumetric flask and make up to the mark with distilled water. Label
this series as Na-K stds-1, 2,etc.
Preparation of Sports Drink Sample.
4. Pipette a 5mL aliquot (precisely known volume use a pipette) of
Gatorade into a 100.0 mL volumetric fask. Add 20mL of the 10,000 mg/L
potassium stock solution (measured with a measuring cylinder), then add
distilled water to the 100.0 mL mark. (What dilution factor have you just
introduced?).
5. Stopper all fasks and thoroughly mix the solutions by inverting the fasks
at least 6 times.
6. Analyse these solutions by AAS for sodium as described below.
Analysis
7. Measure the absorbance of the Na stds series (all 4 solutions). Solutions
are measured from lowest to highest concentration. Record these results
in the Table below. From the data, prepare a plot of Absorption Vs
Concentration Na stds.
8. Measure the absorbance of the Na-K stds series (all 4 solutions).
Solutions are measured from lowest to highest concentration. Record
these results in the Table below. From the data, prepare a plot of
Absorption Vs Concentration Na-K stds.
9. Measure the absorbance of the diluted sports drink. Record the
absorption value in the Table below.
10. From the absorption reading, determine the concentration of Na from
each calibration graph.
You must take the dilution factor into account when reporting the actual
concentration of sodium in the sports drink.
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Results
Table 1: Absorbance Values of Na standards
Concentration of Na stds
(mg/L)
AAS Absorbance
Na-stds Na-K stds
0.0
10.0
20.0
50.0
Table 2: Absorbance of Sports Drink.
Name of sports drink
Sodium concentration from bottle*
AAS Absorbance.
Concentration of sodium in sports
drink determined from Na stds
graph.
Concentration of sodium in sports
drink determined from Na-K stds
graph.
*Express all values in mg/L
Follow-up activity:
1. Which of the two values you have reported in the Table above would be
expected to be closer to the real value? Justify your choice.
2. If you were asked to determine the concentration of potassium in the
sports drink, what measures would you have to take to minimise ionisation
interference?
3. What is the actual concentration of potassium used in the Na-K stds
series (express your answer in mg/L or ppm)?
4. Draw a block diagram of an AAS unit and use this to briefy explain how
the system operates.
5. What procedure would you use to determine the amount of copper and
arsenic which could be leached from a Koppers log?
6. How could a high concentration of sodium in the sports drink slow down
water absorption by the stomach?