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College of Science

Determination of Iodate in Iodised Salt by Redox Titration

Safety 0.6 M potassium iodide solution (10 g solid KI made


up to 100 mL with distilled water)
0.5% starch indicator solution
Lab coats, safety glasses and enclosed footwear must
(see below for preparation)
be worn at all times in the laboratory.
250 mL volumetric flask
Introduction 50 mL pipette (or 20 and 10 mL pipettes)
250 mL conical flasks
New Zealand soil is low in iodine and hence New
Zealand food is low in iodine. Until iodised salt was 10 mL measuring cylinder
commonly used (starting in 1924), a large proportion burette and stand
of school children were reported as being affected distilled water
by iodine deficiency as high as 60% in Canterbury
schools, and averaging 20 40% overall. In the worst
cases this deficiency can lead to disorders such as Method
goitre, and impaired physical and mental development. 1. Preparation of 0.002 mol L1 sodium thiosulfate
In earlier times salt was iodised by the addition of solution: Accurately weigh about 2.5 g of solid
potassium iodide; however, nowadays iodine is more sodium thiosulfate (NaS2O35H2O) and dissolve in
commonly added in the form of potassium iodate 100 mL of distilled water in a volumetric flask. (This
(KIO3). The Australia New Zealand Food Standards Code gives a 0.1 mol L1 solution). Then use a pipette to
specifies that iodised salt must contain: equivalent to transfer 10 mL of this solution to a 500 mL volumetric
no less than 25 mg/kg of iodine; and no more than 65 flask and dilute by adding distilled water up to the
mg/kg of iodine. mark; you will use this diluted thiosulfate solution
In this method we determine the amount of iodate in your titrations. The concentration of the diluted
(IO3) in iodised salt by first reacting the iodate with thiosulfate solution may be calculated as follows:
added iodide (I), under acid conditions, to produce [S2O32] (mol L1) = mass of NaS2O35H2O used (g)
iodine:
248.2 (g mol1) 0.1 (L) 50
IO3 + 5 I + 6 H+ 3 I2 + 3 H2O Alternatively, the concentration of thiosulfate
Then the resulting iodine is titrated with thiosulfate may be determined more accurately by titration
as follows: with a standard solution of iodate or potassium
permanganate (if either is available).
I2 + 2 S2O32 2 I + S4O62
2. Preparation of 0.5% starch indicator solution:
Weigh 0.25 g of soluble starch into a 100 mL conical
Equipment and Materials Required flask or beaker and add 50 mL of distilled water. Heat
iodised salt solution with stirring at 79 C for 5 minutes, being
careful not to exceed the stated temperature. Allow
0.002 mol L1 sodium thiosulfate solution solution to cool to room temperature.
(see below for preparation)
3. Accurately weigh about 50 g of iodised salt into a
1 mol L1 hydrochloric acid 250mL volumetric flask and add distilled water up to
the mark. Shake to dissolve salt.
4. Use a pipette to transfer a 50 mL aliquot of salt 4. Calculate the amount, in moles, of iodate in the salt
solution into a 250 mL conical flask. Then add 5 mL solution.
of 1 mol L1 hydrochloric acid and 5 mL of 0.6 mol L1 5. Calculate the concentration, in mol L1, of iodate in
potassium iodide solution. The solution will turn a the salt solution.
yellow/brown colour as iodine is produced, as shown
in Figure 1. 6. Calculate the number of grams of iodate in the salt
solution.
5. Titrate the solution with your 0.002 mol L1 sodium
thiosulfate solution until the yellow/brown colour 7. Based on the weight of the iodised salt you used to
of iodine becomes very pale (see Figure 1). Then add make your salt solution, calculate the iodate content
1 mL of starch indicator solution, which will produce of your salt, in mg of iodate (IO3) per kg of salt. NB:
a dark blue-black coloured complex with iodine as the molecular weight of IO3 is 174.9 g mol1.
shown in Figure 2 and continue your titration until 8. In order to see if your salt satisfies the Australia New
this colour completely disappears (see Figure 3). Zealand Food Standards Code, calculate the iodine
6. Repeat the titration with further aliquots of your content (in mg of iodine (I) per kg of salt) from your
salt solution until concordant results (titres agreeing result above as follows:
within 0.1 mL) are obtained. iodine (I) content = iodate (IO3) content x 126.9/174.9

Additional from your


Calculate
Notes
solution used from your concordant titres.
solution
3. used the concordant
amount, intitres.
moles, of thiosulfate
3. reacting.
Calculate the amount, in moles, of thiosulfate
Figure 1. Right flask: yellow/ 1. According
solution
reacting. to the titres.
used from your concordant specified limits for iodate in iodised
4. Calculate the amount, in moles, of iodate in the
3. Calculate
Calculatethe theamount,
amount,ininmoles,
moles,ofofiodate
thiosulfate
brown colour of iodine formed 4.
salt, the volume of 0.002
salt
reacting.
salt
solution.
solution.
in the
mol L1 sodium thiosulfate
from reaction of iodate from 4. required
5.Calculate
5. Calculate
Calculatethe in the inabove
the concentration,
amount,
the concentration, in moles, of iodate titration
in molinLthe
mol L , of iodate
1
, of iodate in
in
1
should lie between
the
saltsalt salt solution.
solution.
salt with acidic iodide solution. the
5.9
solution.
mL
6.5. 6.Calculate
Calculate
Calculate theand
the
15.4
the number
concentration,
number of grams
mL.
of
in grams
mol
of L Therefore,
iodate , ofiniodate
iodate
1
the salt
a rougher method
inin the salt
Left flask: pale yellow colour
for
the solution.
quickly
salt solution.
solution. determining whether or not your salt
left when nearly all iodine has 7.6. 7.Based
Calculate
Based
on thethe number
onweight ofof
the weight grams
the of the
iodisedof iodised
iodate
salt youinsaltthe you
used salt used
reacted with added thiosulfateFigure tosample
solution.
to make make
your salt conforms
yoursolution,
salt solution,
calculate theto
calculateiodatethese
the iodate limits
content content is to prepare the
reaction of 7. your salt, on
in mgtheinof iodate the) iodised
(IO per(IOkg )ofsalt
salt.
kgNB: the NB: the

sample
ofBased
your salt,
solution
mg ofofiodate
as above
per ofused
salt.
(adding hydrochloric acid
Figure
1. 1.Right
Rightflask:
flask:yellow/brown
yellow/brown colour
colourofofiodine
iodineformed
formedfrom reaction
from weight 3 you
during titration. of of iodatefrom
iodate
leftleft
fromsalt
whennearly
when
saltwith
nearlyall
with acidic
alliodine
acidic iodide
iodine has
iodide
hasreacted
solution.
solution.
reactedwith
withadded
Left
added
flask:
Left palepale
flask:
thiosulfate
yellow colour
yellow
during
thiosulfate during
molecular
colour weight
molecular
to make your of
weight
salt IO ofis 174.9
solution,

isg 174.9
moltheg iodate
IOcalculate
3
3

3
1.
mol content 1.

titration.
Figure 1. Right flask: yellow/brown colour of iodine formed from reaction
titration.
of iodate from salt with acidic iodide solution. Left flask: pale yellow colour and potassium iodide as described), but instead
8.of your
molecular
New
salt, in
8.In order
Zealand
tomg
Inweight
order
Foodof
of
seeto iodate
if your
see isifsalt
IO
Standards
your
174.9
3

Code,
) per kgthe
(IOsatisfies
gsalt
mol
of Australia
salt. NB: the
satisfies
1. the Australia
calculate the iodine
left when nearly all iodine has reacted with added thiosulfate during 3

Figure 2. Right flask: yellow/ titration. contentof titrating the solution simply add 1 mL of starch
New Zealand Food Standards Code, calculate the iodine
8. content (in mgtoofsee
In order iodine
if
(infollows:
(I) per
your salt kg of salt)the
satisfies from your
Australia
mg of iodine (I) per kg of salt) from your
result above as
New Zealand Food Standards Code, calculate the iodine
brown solution containing indicator, followed by 5.9 mL of thiosulfate solution,
result above as follows:
content
iodine (in mg of iodine
(I) content = iodate(I) per
(IO3kg of salt) from
) content your
x 126.9/174.9
last trace of iodine. Left flask: the blue-black
result iodine
above as
colour of starch-iodine should persist.
content = iodate (IO3) content x 126.9/174.9
(I)follows:

dark blue-black colour formed Additional Notes


iodine (I) content = iodate (IO ) content x 126.9/174.9

But when
1. Additional
According to the
a further 9.5 mL of thiosulfate solution is
Notes
3

specified limits for iodate in


when starch indicator is added Additional
1.added theNotes
iodised salt,
According the
volume colour
to of
the0.002 mol Lshould
specified sodium
limits
1
disappear.
for iodate in
to solution containing iodine thiosulfate required in the above titration should lie
1. iodised
Accordingsalt,tothe
thevolume
specifiedoflimits
0.002 formol
iodate in
L1 sodium
between
iodised 5.9 mL
salt,
thiosulfatetheand 15.4 mL.
volume
required Therefore,
ofin0.002 mol La1 titration
the above roughershould lie
sodium
near endpoint. method for quickly
thiosulfate required determining
in the above whether
titration
between 5.9 mL and 15.4 mL. Therefore, a rougher
orshould
not yourlie
Figure 2. Right flask: yellow/brown solution containing last trace of iodine.
Left flask: dark blue-black colour formed when starch indicator is added to Contact Us
salt sample
between
method
sample
5.9conforms
methodsolution
salt
mL
for
for quickly
and
as above
sampleiodide
to these
15.4
quickly mL. limits is toa prepare
Therefore,
determining
(addingwhether
determining
conforms to thesebut
rougher
whether
hydrochloric
or notacid
limits is to
the
or
your
not your
solution
Figure containing
2. Right iodine near endpoint.
flask: yellow/brown solution containing last trace of iodine.and salt potassium
sample conforms as
to described),
these limits is instead
to prepareofprepare
the
the
LeftFigure
flask:2.dark
Rightblue-black
flask: yellow/brown solution containing
starchlast trace ofisiodine.

Figure 3. A series of flasks


colour formed when
If you have any questions or comments relating to this
indicator
Left flask: dark blue-black colour formed when starch indicator is added to
solution containing iodine near endpoint.
sample
added to titrating
sample solution
solution
the solution as above
simply
as above add (adding
(adding 1 mL hydrochloric
of starch
hydrochloric indicator,
acid
acid
solution containing iodine near endpoint.
andand
followed potassium
by 5.9 mL
potassium ofiodide
iodide as described),
thiosulfate solution,
as described), but
the
but instead instead
blue-
of of
showing the colour change experiment, please contact us. Please note that this
blacktitrating
colour
titrating theof the solution
simplysimply
starch-iodine
solution should
add 1 mLadd of1starch
persist.mLButofindicator,
starcha indicator,
when
further 9.5by
followedmL5.9by
ofmL
thiosulfate
5.9ofmL solution
of thiosulfate is added thethe
solution, colour
the blue-
as the last remaining iodine service is for senior school chemistry students in
followed
should
black disappear.
black colour
colour
thiosulfate
of starch-iodine
of starch-iodine
solution,
shouldshould
blue-
persist.persist.
But when But
a when a
(with added starch indicator) New Zealand only. We regret we are unable to respond
further
further 9.5ofmL
9.5 mL of thiosulfate
thiosulfate solutionsolution
is addedistheadded the colour
colour
Contact
should Us
disappear.
should disappear.
is titrated with thiosulfate. to queries from overseas.
If you have any questions or comments relating to this
Contact
Contact Us Uscontact us:
The dark blue-black colour experiment,
Outreach
please
If you have any questions or comments relating to this
Outreach
disappears, leaving a colourless If you have any questions or comments relating to this
College
experiment,
College ofplease
please
of Science Science
contact us:
experiment,
Figure 3. A series of flasks showing the colour change as the last remaining contact us:
solution at the endpoint. University
Outreach of Canterbury
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iodine (with added starch indicator) is titrated with thiosulfate. The dark
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College of Science
blue-black colour disappears, leaving a colourless solution at the endpoint.

Calculations iodine (with added starch indicator) is titrated with thiosulfate. The dark
Figure 3. A series of flasks showing the colour change as the last remainingNew Private
Figure 3. A series of flasks showing the colour change as the last remaining Christchurch
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Zealand
University
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Bag
CollegeofofCanterbury
Science
4800
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blue-black colour disappears, leavingisa titrated
colourless solution at the endpoint.
iodine (with added
Calculations starch indicator) with thiosulfate.
blue-black colour disappears, leaving a colourless solution at the endpoint.
The dark
Christchurch
Private
Christchurch
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3 3644800
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Zealand
1. From the redox equations1.number
above,
Calculations determine the
From the redox equations above, determine the
of moles of thiosulfate required for reaction
Fax:
New
Email:
+64 3 364 2490
Zealand
Newoutreach@canterbury.ac.nz
Phone: Zealand
+64 3 364 2178
number of moles of thiosulfate
Calculations
with
1. eachFrommole therequired
of iodate
redox in thefor
equations reaction
original
above, salt solution.
determine the Phone:
Fax:Phone: +64
+64 3+64
364 36432178
32490
www.outreach.canterbury.ac.nz364 2178
number of moles theofaverage
thiosulfate required for reaction Email: outreach@canterbury.ac.nz
1. 2.
with each mole of iodatenumber
with
Calculate
in each
the
From theoriginal
mole
redox equations
of iodate in the
volume
salt of thiosulfate
solution.
above,
original
determine
salt solution.
the Fax:Fax: +64 +6433 364
364 24902490
2 of moles of thiosulfate required for reaction www.outreach.canterbury.ac.nz Email: outreach@canterbury.ac.nz
2. Calculate the average volume
with each mole of iodate in the original salt solution.of thiosulfate Email: outreach@canterbury.ac.nz
2. Calculate the average volume of thiosulfate solution www.outreach.canterbury.ac.nz
2 Calculate the average volume of thiosulfate
2. www.outreach.canterbury.ac.nz
used from your concordant
2
titres.
3. Calculate the amount, in moles, of thiosulfate
reacting.