INTRODUCTION

There are a number of methods for testing the iodine

content of salt, ranging from qualitative “spot” tests
which are useful in field settings (see Chapter 10,
Rapid Salt Testing Kits, for details), to more quantita-
tive methods, such as iodometric titrations performed
in laboratories for validation purposes.
The technical information on salt iodine titration Information regarding the testing of salt
provided in this chapter should assist those wishing to fortified with potassium iodate (KI03), which is
establish laboratories for salt monitoring purposes. recommended in developing countries due to its
While iodine titration methods are reasonably simple, greater stability than potassium iodide (KI), is
they are still quantitative chemical tests, and therefore detailed below. Information includes the chemical
demand a certain degree of analytical skill, as well basis for the titration-method, reagent preparation and
adequate funds to setup and maintain a modest stability, step by step procedure and precautions, and
laboratory. In addition, the analyst will need some cost details.
expertise in order to maintain quality assurance The second part of this chapter provide details
records for method and result validation. regarding quality control practices necessary for
For the above reasons, these guidelines on salt laboratories to ensure that reliable data are generated.
iodometric titration will primarily be aimed at- This includes steps required for the initial method
validation, with worked examples, as well as more
• Medium to large scale salt producers (e.g.> general routine quality control and quality assurance
1,000 tonnes per year), as part of their issues.
factory quality control. Appendices are also provided with information
• Government agencies responsible for about laboratory water requirements, a listing of all
quantifying the iodine content of salt necessary equipment, and information about an
obtained from producers, and perhaps other alternative titration method which can be used if salt
sites, such as households, markets, ware- is known to be fortified with potassium iodide instead
houses and importers. of potassium iodate.
The technical requirements of iodine titration
TITRATION METHOD FOR IODATE
analysis may limit its use for some, such as small
CONTENT
scale producers or field workers who also need to
verify salt iodine content. In these situations, use of Description of Reaction
simpler semi-quantitative, or qualitative spot tests, as The iodine content of iodated salt samples is
described in Chapter 10, would be much more measured using an iodometric titration, as described
appropriate. by DeMaeyer, Lowenstein, and Thilly, (1979). The
A person with experience in laboratory reaction mechanism can be considered in two steps
chemistry techniques would be preferable for (See Box 1):
performing these tests and maintaining adequate
quality assurance records. Such a person could be Reaction 1: Liberation of free Iodine from salt
trained in less than a week. Less experienced persons • Addition of H2SO4 liberates free iodine
could be considered to perform the actual titration from the iodate in the salt sample.
procedure, but would require a longer training period
• Excess KI is added to help solubilise the
and greater levels of routine supervision.
free iodine, which is quite insoluble in pure
Different salt iodine test methods need to be water under normal conditions.
used depending on the form of iodine (iodate or
iodide) used in fortification. The iodometric method Reaction 2: Titration of free Iodine with
for iodate will not detect the iodine content of a salt thiosulfate.
sample fortified with potassium iodide, and vice • Free iodine is consumed by sodium
versa. If the form of iodine in the salt sample is thiosulfate in the titration step. The amount
unknown, a simple spot check method can be of thiosulfate used is proportional to the
employed for verification (see Chapter 10 for amount of free iodine liberated from the salt.
relevant details).
86
Titration Methods for Salt Iodine Analysis
• Starch is added as an external (indirect) REAGENT PREPARATION
indicator of this reaction, and reacts with
free iodine to produce a blue colour. When Water Requirements for Reagent Preparation
added towards the end of the titration (that
Water required for this method should be boiled, dis-
is, when only a trace amount of free iodine
tilled water, which requires provision of a distillation
is left) the loss of blue colour, or endpoint,
unit. As a simpler alternative, regular tap water
which occurs with further filtration,
treated with a mixed bed deionizing resin can be
indicates that all remaining free iodine has
used, thus avoiding the need for an expensive
been consumed by thiosulfate.
distillation unit (See Appendix 11-2 for further
details on preparation of this water.)
• 0.005M Sodium thiosulfate (Na2S203):
Dissolve 1.24g Na2S203-5H20 in 1000mL
water. Store in a cool, dark place. This
volume is sufficient for 100-200 samples,
depending on the iodine content of samples.
The solution is stable at least 1 month, if
stored properly.
• 2N Sulfuric acid (H2SO4) Slowly add
6mL concentrated H2SO4 to 90mL water.
Make to l00mLwith water. This volume
is sufficient for 100 samples. The
solution is stable indefinitely.
Note: Always add acid to water, not water to acid, to
avoid excess heat formation and spitting of acid. Stir
solution while adding acid.
• 10% Potassium iodide (KI): Dissolve l00g
KI in 1000mL water. Store in a cool, dark
place. This volume is sufficient for 200
samples. Properly stored the solution is
stable for six months.
• Starch indicator solution: Make l00mL of a
saturated NaCl solution, by adding NaCl to
approximately 80mL water in a beaker, with
stirring and/or heating, until no further solid
will dissolve. This solution is stable for at
least one year. Weigh 1g soluble starch into a
l00mL beaker, add l0mL water, heat to
dissolve. Add saturated NaCl solution to the
hot starch solution to make up to l00mL
Store in a cool, dark place. This volume is
sufficient for 50 samples. The solution is
stable for up to one month, and should be
heated (not boiled) each day it is used to re-
suspend any solids.

Monitoring Universal Salt lodization Programmes 87

Figure 11-1: Weighing salt sample

Procedural Steps
Step 1. Weigh l0g of the salt sample into a 250rnL Erlenmeyer flask with a stopper.

Step 2. Add approximately 30mL water, swirl to dissolve salt sample.

Step 3. Add water to make volume up to 50mL.
Step 4. Add 1mL 2N H2SO4.
CAUTION - Do not pipette by mouth.
Step 5. Add 5mL 10% KI. The solution should turn yellow if iodine is present.
CAUTION - Do not pipette by mouth.

Figure 1 1-2: Addition of 10% potassium iodide

solution
Step 6. Stopper the flask and put in the dark
(cupboard or drawer) for 10 minutes.
Step 7. Rinse and fill burette with 0.005M
Na2S203, and adjust level to zero.

Figure 11-3: Filling the burette with sodium thiosulfate

solution.

Step 8. Remove flask from drawer, and add Stop 10. Record the level of thiosulfate in the
some Na2S203 from the titration burette until the burette and convert to parts per million (ppm) using
solution turns pale yellow (Flask B shown in the conversion table in Appendix 11-3.
Figure 11.4). NOTE: Analysis time is approximately 20 minutes
per sample.
Step 9. Add approximately 2mL of starch indicator
solution (the solution should turn dark purple) and Precautions
continue titrating until the solution becomes pink, • The reaction mixture should be kept in the dark
and finally colourless. (Colour sequence of titration before titration because a side reaction can occur
is shown in flasks C, D and E, figure 11.4) when the solution is exposed to fight that causes
iodide ions to be oxidized to iodine.
Figure 1 1-4: This photo shows the various color • Inaccurate results may occur if starch solution is
changes that will be seen during the titration. used while still warm.
Flask A - after addition of KI (Step 5); • If starch indicator is added too early, a strong
Flask B -just prior to addition of starch (Step 8); iodine-starch complex is formed, which reacts
Flask C - after starch has been added (Step 9); slowly, and gives falsely elevated results.
Flask D -just prior to titration end-point (Step 9), • The reaction should be performed at mild room
Flask E - titration end-point (step 9). temperature (<30oC), since the iodine is volatile, and
the indicator solution loses sensitivity when exposed
to high temperatures.
 SALT IODINE METHOD VALIDATION AND
QUALITY ASSURANCE
It is of the utmost importance that salt iodine test
results be reliable, accurate and timely. This is
especially the case if the salt iodine test data is to be
used for iodine deficiency programme evaluation and
monitoring.
Establishing a salt iodine monitoring system
that gives information about how well the salt is
fortified is the “first level” in salt iodine quality
assurance. However, we must also be sure that the
information derived from the monitoring system (i.e.,
the actual salt iodine test results) is also of good
quality. This can be considered the “second level” of
salt iodine quality assurance.

Laboratory Quality Assurance and Quality

Control
Quality “assurance” typically takes a broader
approach, and deals with certain management and
organisation concepts that influence the operation of
the entire laboratory. The minimum requirements
needed to assure the quality of all laboratory salt
iodine testing are discussed in detail below, and
practical working examples are provided. Figure 11-
5 details some of the key elements of salt iodine
laboratory quality assurance.

Figure 11-5

Key elements of
Total Laboratory Quality
Assurance for Salt Iodine
• Salt Sample Recording
• Reagent inventory/batch Checks
• Equipment Checks
• Method Validation
- Sensitivity, recovery, cross-
checks
• Internal Quality Control
- Establish QC materials
- Routine QC testing
- Monitor test Precision
• External Quality Control
- Establish laboratory network
- Link industry and Government
labs

90 Titration Methods for Salt Iodine Analysis

VALIDATION Sensitivity
During the initial set-up phase of salt iodine titration Establish an estimate of the lowest iodine level that
methods, these four performance characteristics can be reasonably detected by the test method used
should be thoroughly validated: precision, (i.e., its operational sensitivity). An example of the
sensitivity, recovery, and comparison and cross- criterion that might be used to calculate this is the
checking. Each is briefly described below. point at which the mean salt iodine concentration
(ppm) of samples consistently yields results with a
Precision CV >20%.
Calculate the percentage Coefficient of Variation Recovery
(%CV) for repeat analysis of the same sample (at An initial percent recovery should be made to ensure that the test
least ten separate estimates). If possible, this should system is capable of detecting all iodine present. This can be
be done on a number of different salt samples that done by analysing a series of salt solutions to which known
have a range of iodine concentrations, e.g., 25, 50 concentrations of iodine have been added. The following is a
and 100 ppm. With good technique, and reliable worked example:
methodology, the precision should be <15% CV. IODINE
The following gives a worked example:
ADDED OBSERVED MEASURED* %RECOVERY**
____________________________________________________
NONE 15
SALT IODINE TITRATION (ppm)
SALT SAMPLE NUMBER 20 32 17 85
40 53 38 95
#1 #2 #3 60 77 62 103
RESULT No.

1 AVERAGE 94*
18 48 75

2 20 52 68
MEASURED = OBSERVED value corrected for BASELINE
(i.e., value obtained with NO iodine added)
3 19 50 73
** % Recovery = (MEASURED ppm/ADDED ppm) * 100%
4 16 47 67
As a guideline, the average recovery, allowing for
expected test imprecision, should be between 85
5 22 55 70
and 115 percent.
6 17 48 72 Comparison & cross-checking
If possible, an initial sample cross-check should be per-
7 21 43 75
formed with others as a means of assessing method bias.
This could be done either with a laboratory using the same
8 23 51 66 method or compared to alternative techniques e.g.,
correlation between titration method and
9 19 55 72 spectrophotometric method.

10 20 49 78
NOTE: PAMM (Program Against Micronutrient
Malnutrition) provides a service for those
M EAN 19.5 49.8 71.6 laboratories wishing to cross-check samples for
their initial validation. For further information,
STD DEV 2.17 3.68 3.86 please contact:
PAMM Laboratory
%CV* 11.1 7.4 5.4
Centers for Disease Control
Mailstop F20
Standard deviation
4770 Buford Highway Ne
* % CV= _____________________ Atlanta, Ga, 30341-3724, USA
mean Phone: 1 404 488 4088
Fax. 1 404 488 4609
 ROUTINE QUALITY CONTROL Example: A known iodized salt sample was analysed
Once the laboratory method has been validated as by titration twenty times. For the 20 result values
above, it must establish and maintain ongoing obtained, the calculated sample mean was 32 ppm,
quality control (QC) data, both internally (or 'in- and the standard deviation was 2.5. The operating
house') and externally (inter-laboratory), as control range (OCR) for this example can be
described below. established as:
Internal or "in-house" Quality Control
Known positive iodized salt sample(s) should be
OCR = 32 + 2 (2.5)
obtained by the laboratory and stored in sufficient 32 + 5
quantity for analysis every time salt titrations on
unknown samples are run e.g., daily or weekly. By
(27, 37)
performing multiple analyses on these positive salt Therefore, the lower control limit is set at 27 ppm,
samples, a concentration range can be established the upper control limit is 37 ppm, and the control
and used for operational quality control purposes. range is 27 to 37 ppm. Subsequent test results
The following provides a description and worked falling between 27 and 37 ppm are to be considered
example of how to calculate and establish a quality in control, while any results <27, or >37 ppm are
control range and a quality control chart. outside the control range, and therefore out-of-
control.
Establishing and Interpreting a Quality Control
Range: Quality Control Charts
Multiple salt iodine analyses on a known positive salt Once the above operating control range has been
sample should be performed until approximately 15 established, standard quality control charts and rules
to 20 titration results have been obtained. To establish should be used to interpret these control values,
the control range, it is best if these results are decide acceptability of test results, and be kept as a
obtained over a period of time (e.g., three to four tests permanent record to verify all unknown sample
per day), rather than all at once (e.g. twenty tests in results.
one day), as this will give a more realistic estimate of The quality control chart is prepared as follows:
true day-to-day and analytic variability. •Use regular linear graph paper to prepare these
Once a sufficient number of these test results plots.
have been obtained, use a hand calculator or standard •Enter the salt iodine concentration (in ppm) scale for
statistical formulae to calculate the sample mean con- the control on the Y-axis. Make sure the concentra-
centration (X) in ppm, and standard deviation (SD). tion range plotted on this axis extends from less
The 95% confidence interval can then be calculated than the lower limit (i.e., <L), to above the upper
and used as the operating control range, as follows: limit (i.e., >U). For the example given above, which
_ has a calculated range of 27 to 37 ppm, the Y-axis
Sample Mean (X) +2 x SD could be scaled from 20 to 40 ppm.
•Find the sample mean concentration value (i.e., ) on
The X - 2 (SD) = the lower confidence limit (L), the Y-axis scale, and draw a continuous horizontal
and X + 2 (SD) = the upper confidence limit (U.) The line across the entire graph paper at this point For
operating control range is (L, U). the example this would be at 32 ppm.
Unless serious technical or performance errors •Find the lower limit concentration value (i.e., L) on
occur during these initial analyses, the above range the Y-axis scale, and draw a continuous horizontal
should reasonably reflect the normal amount of varia- line across the entire graph paper at this point For
tion expected when using this method over time. the example this would be 27 ppm.
Therefore, any future analysis of the same sample •Find the upper limit concentration value (i.e., U) on
should produce a result between the lower and upper the Y-axis scale, and draw a continuous horizontal
limits (i.e., the L - U range), for 95% of test results. line across the entire graph paper at this point For
Values falling within this range are considered to be the example this would be 37 ppm.
'in control." Only 5% of subsequent test values for • The X-axis is used to plot time, i.e., the date on
this sample should fall outside the established range, which the control sample is analysed.
provided the method (and technician) is operating
Once prepared, this chart is used to plot the
normally. Results falling outside the established
specific analysis date, and salt iodine concentration
range are considered potentially suspicious and
obtained for the control every time it is tested. If the
therefore classed as 'out-of-control.'
control point obtained is between the two limit lines,
then the test is deemed in control, and all results are
accepted. Any control values that are plotted outside
the two limit lines should be considered as out-of-
control, and the results of any corresponding
unknown salt samples tested at the same time should
also be rejected as unacceptable due to possible
method error.
92 Titration Methods for Salt Iodine Analysis
 When an out-of-control value is obtained, steps 81.6 ppm. (Note: The computer software used to
should be taken to identify the possible reason for generate this chart plots the y-axis in units of
this event (e.g., use of old reagent, incorrect standard deviation, as opposed to ppm units, but this
procedure used or reagent mix-up), and correct the will not change the general overall shape of the
problem. Once resolved, and control values have chart.) As can be seen, such charts are very useful in
returned to normal, repeat the previously rejected identifying when problems occur within the test
unknown salt samples to obtain acceptable results. system, and allow corrective action to be taken. In
Figure 11-6 gives a real example of a typical Figure 11-6 the extremely high values above the
salt iodine quality control chart for a control with a upper limit (called outliers) were due to a
mean salt iodine concentration of 74 ppm, a standard deterioration in the sodium thiosulfate solution which
deviation of 3.8, and an operating control range of give falsely elevated test results.
66.4 to

Figure 11-6: Example of a Salt Iodine QC Chart

Monitoring Universal Salt lodization Programmes 93

 External or Inter-laboratory Quality Control These 'external' comparisons should occur at regular
External cross-checking of samples is the best way intervals (e.g., two to three times per year). Each
for each laboratory to assess its own performance time participants in the QC programme are sent
compared to other laboratories, and detect potential unknown salt samples for analysis, and test results
method bias or inaccuracy. This type of inter- should be returned to the QC programme coordinator
laboratory exchange should be seen as a supplement by a specific date, collated, reviewed, and reported to
to internal QC, not as its replacement! Each salt each participant as soon as possible. Feedback
iodine testing laboratory (government and industry) should show how results from each laboratory
should be encouraged to form or participate with compare to all others participating in the same
others in an on-going salt sample exchange network programme. However, it is most important that the
(see Figure 11-7). results be presented anonymously. This is easilv
achieved by giving all laboratories a special code
Figure 1 1-7: Extemal Salt Iodine QC Network number known only by the coordinator and
participating laboratory.

LAB -
MANUFACTURER 2 INTERNATIONAL
LABS

CENTRAL
TESTING LAB

94 Titration Methods for Salt Iodine Analysis

 The reported results are best presented graphi- An alternative approach is to have all
cally, as shown in figure 11-8. The value of external participating laboratories send salt samples along
comparisons can be seen in this example. While with their test results to some central coordinating
most laboratories yielded similar salt iodine results laboratory for analysis and comparison. However
(20 to 30 ppm), Laboratory 2 showed consistently this approach will increase the work load at the
lower values, while Laboratory 4 had greater coordinating laboratory.
imprecision compared to the other laboratories. Also Coordination of the external QC programme is
note that laboratory 6 had generally satisfactory probably best done by an independent agency (e.g.,
results, except for one obvious outlier. Government), and every effort should be made to
encourage voluntary participation by all salt testing
Figure 11-8: Example of Salt Iodine laboratories, especially industry and producers. Use
External QC Chart of awards or certificates sent to regular participants
in the programme can be a helpful motivational tool.

Salt Iodine QC Program

Sample A

Laboratory Code Number

Monitoring Universal Salt lodization Programmes 95

 OTHER ELEMENTS OF QUALITY Instrument Calibration
ASSURANCE The exact details depend on the type of test method used,
but these should be performed in some routine fashion
Salt Sample Recording (e.g., calibrate balance every month). For each calibration
Each laboratory must maintain a logbook with sample keep a record of the following details:
details recorded in ink, such as: • Instrument tested
• Date/time collected • Date calibrated
• Date/time received • Calibrated by whom?
• Outcome (pass/fail, specific reading.)
• Sample specific details (code #, brand, batch, expiry
date)
• Date analysed
REFERENCES
• Technician performing test
• Test result
1. De Maeyer EM, Lowenstein FW, Thilly CH. “The
• Supervisor's signature
control of endemic goiter.” World Health
• Date result is reported Organization, Geneva, 1979.
An example of a format that could be used in a salt
sample analysis logbook is given at the end of the
chapter, which could be copied and adapted for use as
a “master” form.
Reagent Inventory Details
The laboratory supervisor should ensure all relevant
details regarding test chemicals are recorded:
• Chemical brand, quantity, grade and batch/lot
number
• Date ordered and received
• Date each “working” reagent is prepared, and by
whom
• Give each working reagent an “in-house” lot
number
An example of a salt iodine reagent inventory
form is given at the end of the chapter, which
could be copied and adapted for use as a “master”
form.

96 Titration Methods for Salt Iodine Analysis

 SALT SAMPLE ANALYSIS LOGBOOK

SAMPLE
ID'*

SALT IODINE REAGENT INVENTORY

CHEMICAL:_________________________________

*DATE DATE BRAND, BATCH/LOT

ORDERED RECEIVED QUANTITY NUMBER

Monitoring Universal Salt lodization Programmes 97

 APPENDIX 11-1

Equipment and Reagents Required to Establish a

Salt Iodine Laboratory
Many items on the following list of equipment and reagents can be procured
through UNICEF Copenhagen Supply Division, or various scientific supply companies.
QUANTITY UNICEF QUANTITY UNICEF
CODE CODE
NOTE: If distilled water is to be used, the
1 Balance, Four-beam pan following equipment is required:
Sensitivity = 0.01g,
Capacity = 410g 1 Water Still 4L/day electric 220V 01 676 00
(e.g., Fisher Scientific Cat. No. 02-020-411)** 1 Hot plate 220V 20 004 02
1 Rod, stirring, flint glass assorted 09 686 00
1 Set of weights for above pkt
(e.g., Fisher Scientific Cat. No. 02-314) OR
4 Flask. volumetric, 1000mL NOTE: If tap water treated with deionizing resin is
(e.g., Fisher Scientific Cat. No. 10-210G) to be used (see Appendix 11.2), the following
equipment replaces the 3 previously listed items:

2 Flask, volumetric, l00mL 2 Flask, Erlenmeyer, 4L

(e.g., Fisher Scientific Cat. No. 10-119-10D) (e.g., Fisher Scientific Cat. No. 10-040P)
1 Whatman Filter Paper, 15cm diameter
2 Measuring cylinder, l0mL
(e.g., Fisher Scientific Cat. No. 09-805G)
(e.g., Fisher Scientific Cat. No. 08-552-4H)
1 4L Polyethylene carboy for water storage
12 Measuring cylinder with stopper, l00mL 09 374 30 (e.g., Fisher Scientific Cat. No. 02-963AA)
12 Beakers, Pyrex 09 160 00 1 kg Mixed bed deionizing resin
Flasks, Elenmeyer (conical) with stopper, 250mL 1.5meq/mL, 300-1,180µm, mesh size 20-50
(e.g., Fisher Scientific Cat. No. 31038, 0.1 cubic
(e.g., Fisher Scientific Cat. No. 10-098E)
feet - this should be enough to provide sufficient
4 Pipette, volumetric, 1mL 09 676 00 water for at least one year).

4 Pipette, volumetric, 5mL 09 679 05 1 Hotplate/stirrer, 220V

(e.g., Fisher Scientific Cat. No. 11-501-7SH)
4 Burette w/straight stopcock l0mL 09 239 00
3 Magnetic stirring bars
4 Burette stand 09 767 00 (e,g., Fisher Scientific Cat. No. 14-511-70)
2 Laboratory safety glasses REAGENTS REQUIRED
(e.g., Fisher Scientific Cat. No. 17-286-1C) Sodium Thiosulfate Pentahydrate, ANALAR, 500g
1 Parafilm, for covering beakers (e.g., Fisher Scientific Cat. No. S445-500)
(e.g., Fisher Scientific Cat. No. 13-374-12) (Sufficient for 50,000 samples)

12 Glass bottles with stoppers Sulfuric Acid, concentrated, 2.5L

09 194 50 (e.g., Fisher Scientific Cat. No. A298-212)
for reagents, 250mL
(Sufficient for 40,000 samples)
4 Funnel, lab, plain, diam. 65mm 09 450 00
Potassium Iodide, 500g
4 Watch glass, 75mm diam. 09 888 00
Sodium Chloride, 3kg
6 Spatula Lab single blade (e.g. Fisher Scientific Cat. No. S271-3)
150mm SS lenqth 09 699 10 (Sufficient for 3,000 samples)

4 Dropper bottle, glass 25-60mL 09 190 00 Soluble starch, 500g

(e.g. Fisher Scientific Cat. No. S516-500)
1 Desiccator plain Scheibler l50xl50mm 09 374 60 (Sufficient for 25,000 samples)

** Fisher Scientific, 50 Fadem Road, Springfield, NJ, 07081, USA Fax: 201-379-7415,
ATTENTION: Jackie Dubeau

98 Titration Methods for Salt Iodine Analvsis

 APPENDIX 11-2

USE OF TREATED TAP WATER

WITH DEIONIZING RESIN AS
AN ALTERNATIVE TO
DISTILLED WATER
The resin required (as per Appendix 11-1) is a mixed
bed resin, containing cation and anion exchange
beads. Deionization occurs by exchanging cations
with hydrogen, and anions with hydroxyl on the
resin. In this way, all ionic species are removed from
the water.
e.g., Resin-H + Resin-OH + NaCl → Resin-Na +
Resin-Cl + H20

The resin contains a colored dye (e.g. purple)

irreversibly bound to the anion exchange resin, which
turns from purple to gold when the exchange capacity
is exhausted.
To deionize water for use in the laboratory, follow
these steps:
Step 1. Add resin to a conical flask or beaker,
covering the base with approximately 1.5cm of resin.
Usually a 2 - 5 L flask is used; the bigger the flask,
the more resin needed.
Step 2. Fill the flask with good quality tap water
(distilled water can also be used if available) and mix
Figure 11-9 Mixing resin procedure
on laboratory stirrer for approximately one to three
hours. Alternatively, water can simply be left in the
flask with the resin for a longer period of time (24
hours), with occasional stirring and then let resin Regenerate the cation exchanger using three
settle. times the volume of 3N HCl and rinse with four
Step 3. Decant the water from the resin, making sure volumes of deionized water. Check that the pH is <5.
not to leave the resin dry. ALWAYS LEAVE AT Regenerate the anion exchanger with at least ten
LEAST 1cm OF WATER ON THE RESIN. If the volumes of 3N NaOH and rinse with deionized water
resin is allowed to dry out it must be discarded, since until the pH <9. Mix the resins thoroughly by
the ion exchange capability may be greatly reduced. agitating with a stirring rod.
Step 4. To ensure complete removal of resin The mixed bed resin has a shelf life of two
years at room temperature. This shelf life may be
particles that may float on the surface, simply pass
extended by storing in the refrigerator.
resin-treated water through standard laboratory-
grade filter paper.

Mixed bed resins are not normally regenerated

after exhaustion because of the difficulty of
separating the two resin components, and proper re-
mixing. However, if you wish to regenerate the
resin after it has changed colour, you must separate
the anion and cation exchange resin beads. Shake
the resin in twice its volume of water, let it settle,
and decant the top layer containing the less dense
anion exchanger. Repeat until separation is
complete.

Monitoring Universal Salt lodization Programmes 99

 APPENDIX 11-3

CONVERSION TABLE :
IODINE CONTENT IN PARTS
PER MILLION
BURETTE PARTS PER BURETTE PARTS PER
READING MILLION (ppm) READING MILLION (ppm)

0.0 0.0 5.0 52.9

0.1 1.1 5.1 54.0
0.2 2.1 5.2 55.0
0.3 3.2 5.3 56.1
0.4 4.2 5.4 57.1
0.5 5.3 5.5 58.2
0.6 6.3 5.6 59.2
0.7 7.4 5.7 60.3
0.8 8.5 5.8 61.4
0.9 9.5 5.9 62.4
1.0 10.6 6.0 63.5
1.1 11.6 6.1 64.5
1.2 12.7 6.2 65.6
1.3 13.8 6.3 66.7
1.4 14.8 6.4 67.7
1.5 15.9 6.5 68.8
1.6 16.9 6.6 69.8
1.7 18.0 6.7 70.9
1.8 19.0 6.8 71.9
1.9 20.1 6.9 73.0
2.0 21.2 7.0 74.1
2.1 22.2 7.1 75.1
2.2 23.3 7.2 76.2
2.3 24.3 7.3 77.2
2.4 25.4 7.4 78.3
2.5 26.5 7.5 79.4
2.6 27.5 7.6 80.4
2.7 28.6 7.7 81.5
2.8 29.6 7.8 82.5
2.9 30.7 7.9 83.6
3.0 31.7 8.0 84.6
3.1 32.8 8.1 85.7
3.2 33.9 8.2 86.8
3.3 34.9 8.3 87.8
3.4 36.0 8.4 88.9
3.5 37.0 8.5 89.9
3.6 38.1 8.6 91.0
3.7 39.1 8.7 92.0
3.8 40.2 8.8 93.1
3.9 41.3 8.9 94.2
4.0 42.3 9.0 95.2
4.1 43.4 9.1 96.3
4.2 44.4 9.2 97.3
4.3 45.5 9.3 98.4
4.4 46.6 9.4 99.5
4.5 47.6 9.5 100.5
4.6 48.7 9.6 101.6
4.7 49.7 9.7 102.6
4.8 50.8 9.8 103.7
4.9 51.9 9.9 104.7

100
Titration Methods for Salt Iodine Analysis
APPENDIX 11-4: REAGENT PREPARATION
Water preparation is the same as for procedures
ALTERNATIVE TITRATION
described in section on “Titration Method for
FOR IODIDE CONTENT
Iodate content,” page 86.
Description of Reaction 1. Methyl Orange lndicator - Dissolve 0.0lg methyl
While use of potassium iodide (KI) is not common in orange in l00mLwater.
many developing countries for salt fortification, basic
2. 2 N Sulfururic Acid - Add 5.56mL concentrated
details of a titration method (De Maeyer EM,
H2SO4 to 90mL water, make to l00mL with water.
Lowenstein FW, Thilly CH, 1979) suitable for
analysing salt iodized with KI are provided here. 3. Bromine Water - Place 5mL in a small flask,
The reaction mechanism for this iodometric (keep in fume hood due to dangerous fumes)
titration is as follows:
4. Sodium Sulfite Solution - Dissolve lg sodium
Reaction 1: Potassium iodide is dissolved from the sulfite in l00mLwater
salt.
5. Phenol Solution - Dissolve 5g phenol in l00mL
Reaction 2: Bromine water oxidizes iodide ions to water
free iodine. Sodium sulfite and phenol are added to
6. Potassium Iodide Solution - Dissolve l0g potassium
destroy excess bromine so that no further oxidation
iodide in l00mL water
of I- can occur before KI solution is added.
Reaction 3. : The titration reaction with thiosulfate 7. Sodium Thiosulfate Solution (0 005N - Dissolve 0.124g
is the same as that described in the iodate method sodium thiosulfate pentahydrate in l00mL water
earlier. 8. Starch Solution - Dissolve 1g soluble starch in l00mL
water, with heating

(All the above need stoppered flasks and should

be stored in the dark)
Procedure
Step 1. In a 250mL Erlenmeyer flask place l0g of
salt sample and 50mL water. Swirl to dissolve.
Step 2. Add 6 drops of methyl orange indicator
(solution turns pale orange). Add 2N H2SO4
dropwise (1 drop or until a pink colour change).
This is done to neutralise the reaction mixture.
Step 3. Add 0.5mL bromine water (solution changes
to yellow).
Step 4. Add sodium sulfite solution, dropwise, until
solution turns pale yellow. Wash down the flask
sides with H20.
Step 5. Add 3 drops phenol solution (solution turns
clear).
Step 6. Add 1mL 2N H2SO4
Step 7. Add 5mL potassium iodide solution. (Turns
yellow).
Step 8. Add sodium thiosulfate solution from the
titration burette until solution turns pale yellow. Add
1mL starch solution, leading to a dark purple colour.
Continue titration until solution becomes colourless.
Step 9. Note the burette reading and convert to ppm
using the table in Appendix 11-3.

Precautions - Please refer to precautions listed in

the iodate method described earlier.

101
Monitoring Universal Salt lodization Programmes