College of Science

Determination of iron by thiocyanate colorimetry

Use this method if you do not have access to a colorimeter
Safety • 1 mol L−1 sulfuric acid
• 0.15 mol L−1 potassium permanganate solution
Lab coats, safety glasses and enclosed footwear must (see below for preparation)
be worn at all times in the laboratory. • 100 mL beaker
Concentrated acids are highly corrosive − wear rubber
gloves and take care when handling. • 100, 200, 250 and 500 mL volumetric flasks
• 5 mL pipette
Introduction • 10 mL measuring cylinder
Iron is one of the many minerals required by the • 100 mL conical flask
human body. It is used in the manufacture of the • at least 6 boiling tubes (or large test tubes)
oxygen-carrying proteins haemoglobin and myoglobin.
A deficiency of iron in the body can leave a person • distilled water
feeling tired and listless, and can lead to a disorder
called anemia. Many of the foods we eat contain small Method:
quantities of iron.
1. Preparation of Fe3+ standard solutions: NB: It may
In this analysis the iron present in an iron tablet (dietary take several days to dissolve the Fe3+ salt used here,
supplement) or a sample of food is extracted to form so carry out this preparation well in advance of the
a solution containing Fe3+ (ferric) ions. To make the rest of the experiment. Weigh out about 3.0 g of
presence of these ions in solution visible, thiocyanate ferric ammonium sulfate (FeNH4(SO4)2•12H2O). Use a
ions (SCN−) are added. These react with the Fe3+ ions to mortar and pestle to grind the salt to a fine powder.
form a blood-red coloured complex: Accurately weigh 2.41 g of the powder into a 100
Fe (aq) + SCN (aq) → [FeSCN] (aq)
3+ − 2+ mL beaker and add 20 mL of concentrated sulfuric
acid (see safety notes). Leave powder to soak in
By comparing the intensity of the colour of this solution acid overnight. The next day, carefully pour the acid/
with the colours of a series of standard solutions, with powder slurry into a 500 mL volumetric flask, rinsing
known Fe3+ concentrations, the concentration of iron the beaker into the flask a few times with water,
in the tablet or food sample may be determined. This then make up to the mark with distilled water. Let
technique is called colorimetry. this solution stand for several days until the ferric
ammonium sulfate powder has fully dissolved. If
Equipment and Materials Required possible, insert a magnetic stirrer bar and stir the
solution to speed up this dissolving process.
• ferric ammonium sulfate FeNH4(SO4)2•12H2O standard
solutions: 2, 4, 6, 8 and 10 × 10−5 mol L−1 Use a pipette to transfer 20 mL of ferric ion solution
(see below for preparation) to a 200 mL volumetric flask and make up to the
mark with distilled water. This gives a solution with
• iron tablet (dietary supplement) or sample of iron- [Fe3+] = 0.001 mol L−1. To prepare a 2 × 10−5 mol L−1
containing food (eg: silverbeet, spinach, raisins.) standard solution pipette 10 mL of the 0.001 mol L−1
• 1 mol L−1 ammonium thiocyanate solution solution into a 500 mL volumetric flask, add 10 mL
(see below for preparation) of 1 mol L−1 sulphuric acid, and then make up to the
mark with distilled water. Repeat this procedure in
 separate 500 mL volumetric flasks, pipetting in 20, with distilled water. This diluted solution will be used
30, 40 and 50 mL of 0.001 mol L−1 Fe3+ solution in for colorimetric analysis.
turn, to obtain 4, 6, 8 and 10 × 10−5 mol L−1 solutions
respectively. Preparation of food sample for analysis:
(NB: if you do not have five 500 mL volumetric flasks
1. Accurately weigh a few grams (typically 2 − 5 g is
you can use one flask to prepare each standard in
required, depending on iron content of sample) of
turn. After preparing each standard, pour the solution
your food sample into a crucible.
into a labelled glass vessel which has a lid (eg: a
glass bottle). Then rinse your 500 mL volumetric flask 2. Heat the crucible over a bunsen burner (see Figure
thoroughly with distilled water before using it to 1) until the sample is reduced completely to ash,
prepare your next standard solution.) or (preferably) combust the sample directly in the
bunsen flame (as shown in Figure 2), reducing it to
2. Preparation of 1 mol L−1 ammonium thiocyanate
ash. NB: be very careful with the bunsen flame while
solution: Weigh 38 g of solid ammonium thiocyanate
heating/combusting your sample. Also beware that
into a 500 mL volumetric flask and make up to the
the crucible will become very hot during this process,
mark with distilled water.
so handle it only with crucible tongs − or preferably
3. Preparation of 0.15 mol L−1 potassium permanganate not at all − until it has cooled.
solution (only required for analysis of iron tablet):
3. When the sample and crucible have cooled, use a
Weigh 2.4 g of solid potassium permanganate into
stirring rod to crush the ash to a fine powder (see
a 100 mL volumetric flask and make up to the mark
Figure 3). Use a measuring cylinder to add 10 mL of
with distilled water.
1 mol L−1 hydrochloric acid and stir for 5 minutes,
making sure that all the ash is soaked.
Preparation of iron tablet for analysis: 4. Add 5 mL of distilled water and filter the solution into
1. Place iron tablet in a 100 mL beaker and use a a 100 mL conical flask to remove the ash. This filtered
measuring cylinder to add 20 mL of 1 mol L−1 sulfuric solution will be used for colorimetric analysis.
acid. Allow the tablet’s coating to break down and
its contents to dissolve. You may help this process by Colorimetric analysis:
using a stirring rod to carefully crush the tablet and
stir the solution. (NB: iron tablets sometimes contain NB: this analysis method applies to samples prepared
filler materials that may not fully dissolve in acid) using either of the two methods above (iron tablets or
food samples).
2. Once the iron tablet is dissolved, add 0.15 mol L−1
potassium permanganate solution dropwise, swirling 1. Accurately measure 10 mL of your sample solution
the beaker after each addition. Iron tablets usually into a clean, dry boiling tube/test tube. NB: this is
contain ferrous sulfate, with iron present as Fe2+ ions. most accurately done using a 10 mL pipette; however,
Since Fe2+ does not form a coloured complex with it is possible to do this accurately enough (and with
thiocyanate, permanganate ions are added to oxidise less hassle) using a clean 10 mL measuring cylinder if
all the Fe2+ to form Fe3+ ions. For the first few drops you measure carefully.
of permanganate, the purple colour will disappear 2. Next, measure 10 mL of each Fe3+ standard solution
immediately upon addition to the iron solution; into separate boiling tubes (one standard per tube) in
however, as further drops are added the colour order of increasing concentration, beginning with the
will begin to linger for a little longer. Stop adding 2 × 10−5 mol L−1 standard. It is a good idea to first rinse
potassium permanganate drops when the purple your pipette or measuring cylinder with a few mL of
colour persists for several seconds after addition the 2 × 10−5 mol L−1 standard). NB: Make sure you label
− usually no more than about 2 mL of 0.15 mol L−1 each boiling tube appropriately with the name of the
permanganate solution will be required. sample or standard it contain. A test tube rack is very
3. Transfer the iron solution to a 250 mL volumetric useful for holding and transporting your tubes (see
flask, rinsing the beaker with distilled water a Figure 4). Alternatively you can use a large beaker to
few times and transferring the washings to the hold them.
volumetric flask. Make up to the mark with distilled
water, stopper the flask and mix well.
4. Use a pipette to transfer 5 mL of iron solution to a
100mL volumetric flask and make up to the mark
 to the
your
zero when Fe3+ concentration is uh
zero
3. Now identify the point concen
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your
which corresponds to the absorbanc
concen
your unknown iron sample. 4.By draw
U
to the horizontal axis you will
iron
4. be(in
abl
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3. Using a 10 mL measuring cylinder, measure 10 mL concentration of Fe3+ in your unknow
of 1 mol L−1 ammonium thiocyanate solution into the
ironmo
(in
4. Use this concentration to calcu
each of six small clean vessels − six boiling tubes is iron (in mg) in your originalto
thetake
mo
tablet or
ideal. You should now have one measured portion of while
the molecular weight of iron is 55.8
to take p
to take into account any dilutions th
thiocyanate solution for each of your iron solutions. while preparing your sample while Ifp
5. solutio
4. As quickly as possible, pour 10 mL of thiocyanate 5. unknow
If the absorbance value
5.you me
If
Figure 2. Set up used for combusting a silverbeet sampleunknown
directly iron sample is greater tha
in the value
solution (the portions measured out above) into bunsen
bunsen 1. flame.
burner
burner Set flame.
up used for Figure
Figure 2. Set up used for combusting a silverbeet sample directly
Figure in the2. Set value
up usedfor your unknof
forhighest concentration
Figure 2. Set up used for combusting a silverbeet sample directly inmodify
the the above
will nee
each of your iron solutions. heatingburner
bunsen a silverbeet
flame. sample in
will
combusting a silverbeet need to value
procef
of an iron tablet, you should repeat
a crucible. sample directly in the bunsen of willanneir
5. Mix the solutions by swirling. A stable red colour will more
Figure 1. Set up used for dilute
heating solution
a silverbeet ofinthe
sample dissolved
a crucible.
burner flame.case of a food sample, youmore
of an dreir
should
appear over the next few minutes. using a smaller mass of your food.
case
moreofd
6. Allow the red colour to develop for 15 minutes. Then using
case ofa
estimate the concentration of Fe3+ ions in your iron Contact Us
using a
If you have any questions or comme
sample by identifying which of your Fe3+ standards Figure 3. Left photo: ash remaining after combustion of a silverbeet sample.
matches its colourmost closely. Figure 4 illustrates Right photo: silverbeet ash which has been ground to a fine powder using
a stirring rod.
experiment, please contact us:
Conta
Outreach
the range of colour intensities that you can expect College of Science IfCont
you h
from your set of Fe3+ standards. Tip: If you are using Figure 3. Left photo: ash remaining after combustion ofUniversity of Canterbury
a silverbeet sample.
experim
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Figure
Right 3. Left
photo: photo:ash
silverbeet ash remaining
which has been after combustion
ground to a Private
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boiling/test tubes all of identical sizes, the best way to Figure 3. Left photo: ash remaining after combustion ofChristchurch
a silverbeet sample.
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fineZealand
powder using Outrea
compare colours is by looking at your solutions from aground
stirring to
rod.a fine powder using a stirring rod.
New
above − looking down into the tubes (see Figure 5). Phone: +64 3 364 2178 College
Outrea
Fax: +64 3 364 2490 Univers
College
7. If the colour of your unknown iron solution Figure 4. Blood-red coloured solutions produced by the ferric thiocyanate
complex ion (Fe[SCN]2+). These solutions were prepared using the following
Email: [email protected]
Private
Univer
is stronger than the colour of your highest range of Fe3+ standards: 2, 4, 6, 8, 10, 12 × 10−5 mol L−1. Figure 2. Set up used for combusting a silverbeet sample directly in th
www.outreach.canterbury.ac.nz
Christc
3
bunsen burner flame. Private
concentration Fe3+ standard you will need to modify
New Ze
Christc
the above procedure. In the case of an iron tablet,
New Z
Phone:
you should repeat the analysis with a more dilute
solution of the dissolved iron tablet. In the case of a Fax:
Phone
Figure4.4.
Figure Blood-red coloured solutions produced bythiocyanate
the ferric
food sample, you should repeat the analysis using a Blood-red coloured solutions produced by the ferric Email:
Fax:
thiocyanate
complex ion complex
(Fe[SCN]2+). ion
These (Fe[SCN]
solutions 2+
).
wereThese solutions
prepared using were
the following
Figure 4. Blood-red coloured solutions produced3+by the ferric thiocyanate
smaller mass of your food. range of Fe3+ standards: 2, 4, 6, 8, 10, 12 × 10−5 mol L−1. Email:
www.o
complex ion (Fe[SCN]2+). These solutions were prepared using the 4,
prepared using the following range of Fe standards: 2, 6, 8,
following
Figure 3. Left photo: ash remaining after combustion of a silverbeet sa
10, 12 of
3 range × 10 −5
Fe3+ mol L−1. 2, 4, 6, 8, 10, 12 Right
standards: × 10−5 mol
photo: www.o
L−1. ash which has been ground to a fine
silverbeet powder u
a stirring rod.
Calculations 3
1. Assume that the concentration of Fe3+ in your
unknown iron solution is approximately equal to
that of the Fe3+ standard whose colour was the
closest match. Figure5. 5.
Figure TheThe same
same boiling
boiling tubes tubes as in4Figure
as in Figure (prepared 4 (prepared
using Fe3+ using
Fe3+ standard
standard solutions
solutions with concentrations
with concentrations of 2 −4.12Blood-red
Figure × 10−5 ofcoloured
2 −L−1)
mol 12 ×viewed
10produced
solutions
−5
by the ferric thiocyan
2. Use this concentration to calculate the mass of from above, looking directly down
mol L ) viewed from above, looking
−1 the length
complexofionthe
directly tube.
(Fe[SCN]2+).
down This
These
theview
solutions
length were prepared using the follo
range of Fe3+ standards: 2, 4, 6, 8, 10, 12 × 10−5 mol L−1.
iron (in mg) in your original tablet or food sample provides the most accurate “eyeball” comparison of the solutions’ colour
of the tube. This view provides the
intensities. 3 most accurate “eyeball”
(NB: the molecular weight of iron is 55.8 g mol−1). comparison of the solutions’ colour intensities.
Remember to take into account any dilutions Calculations
that you performed while preparing your sample
solution. 1. Using only the absorbance results obtained for
your Fe3+ standard solutions (not your unknown iron
sample), prepare a graph with [Fe3+] (in mol L−1) as the
Additional Notes horizontal axis and absorbance (at 490 nm) as the
1. If you
Figure 1. Set are using
up used a colorimeter
for heating a silverbeet instrument, it is not
sample in a crucible. vertical axis.
critical to have identical boiling/test tubes for
2. Draw a line of best fit for your data points that
each iron solution − any small vessels (eg: small
goes through the origin (because absorbance must be
beakers or glass vials) will do. However, if you are
zero when Fe3+ concentration is zero.
analysing the colour intensities by eye, as above, it is
important to have identical vessels in order to make 3. Now identify the point on your line of best fit
an accurate comparison − a set of identical boiling/ which corresponds to the absorbance measured for
test tubes is ideal. your unknown iron sample. By drawing a vertical line
(continued overleaf) to the horizontal axis you will be able to determine the
concentration of Fe3+ in your unknown solution.
4. Use this concentration to calculate the mass of
iron (in mg) in your original tablet or food sample (NB:
2. You may notice that even the standard giving Contact Us
the closest colour match to your sample is still
quite different − meaning that your estimated Fe3+ If you have any questions or comments relating to this
concentration is not very accurate. In order to obtain experiment, please contact us. Please note that this
service is for senior school chemistry students in
a more accurate result you may wish to try the
New Zealand only. We regret we are unable to respond
following procedure: to queries from overseas.
• Identify which two Fe3+ standards are the closest Outreach
colour matches to your unknown solution: one must College of Science
be slightly darker in colour and the other slightly University of Canterbury
lighter than your unknown. The concentration of Private Bag 4800
your unknown solution must lie somewhere between Christchurch
the concentrations of these two standards. For New Zealand
this example, let us pretend that the two closest Phone: +64 3 364 2178
standards are 4 × 10−5 and 6 × 10−5 mol L−1. Fax: +64 3 364 2490
Email: [email protected]
• Take 5 clean, dry boiling tubes. To the first tube we www.outreach.canterbury.ac.nz
add 10 mL of the 4 × 10−5 mol L−1 standard and 10 mL
of the 6 × 10−5 mol L−1 standard. We now have a new
standard that is 5 × 10−5 mol L−1.
• Next, we measure 5 mL of this 5 × 10−5 mol L−1
standard into a new tube and also add 5 mL of the
4 × 10−5 mol L−1 standard. We now have another new
standard that is 4.5 × 10−5 mol L−1.
• If we measure 5 mL of the 5 × 10−5 mol L−1 standard
into another new tube and add 5 mL of 6 × 10−5
mol L−1, we will make another new standard that is
5.5 × 10−5 mol L−1.
• We finish by measuring 10 mL of the 4 × 10−5 mol L−1
standard into one boiling tube, and 10 mL of the
6 × 10−5 mol L−1 standard into a different tube.
• We now have a set of five boiling tubes, each
containing exactly 10 mL of a different Fe3+ standard
solution, with concentrations of 4, 4.5, 5, 5.5 and
6 × 10−5 mol L−1. If we now repeat the colorimetric
analysis of our unknown iron solution using these
new standards instead of the original ones, we
should obtain a much more accurate value for Fe3+
concentration.