TITRATION

Scenario
Analysis of river water
Rivers throughout the UK are constantly monitored by the environment
and water standards agencies whose responsibility it is to ensure that
water quality is maintained. To ensure this, samples are regularly
collected and analysed by these agencies.
JEM Water is analysing the quality of its local rivers and streams and has
found that one of its rivers is showing high levels of acid present which
may be hydrochloric acid released from an industrial site upstream, and
investigates this further using titration.
It has also found a local stream contaminated with a coloured pollutant
(Copper (II) compound) that the agency thinks is caused by an industrial
plant further upstream in the next town. JEM Water has been tasked to
investigate the contamination and they will carry out the
investigation using colorimetric analysis. As a laboratory
technician working for JEM, you have been asked to carry
out the investigations.

Science Background
Volumetric analysis’ basic principle is that the known concentration of a
solution is added to an unknown concentration of a sample and when it
reacts you can then determine its concentration. The reaction taking
place when in progress with reaching its end-point is neutralisation.
Using an indicator in titration is important as it’s used for the detection
of the end-point in the reaction. This is because it detects the change in
the pH range and the end-point of titration is when the solution changes
colour so the indicator would make the solution change colour as it
shows us a colour change representing the pH change as well.
You would have to choose a suitable indicator when doing different types
of titration to ensure that the pH at the equivalence point on the titration
will fall within the range over which indicator changes colour. If not,
there would be an indicator error leading to invalid and inaccurate
results.
 Phenolphthalein is mainly used for acid-base titrations as it changes
colour in the 8.3-10 pH range. It will appear pink in basic solutions and
clear in acidic solutions making it useful as you see a clear colour change.
This would mean that the acid has to be a weak acid and the base would
have to be a strong base to get an equivalence point of 8.3-10 but can
also be used if there’s also a strong acid as well as a strong base. An
example of this is using hydrochloric acid and sodium hydroxide.
Another indicator for titration that can be used is methyl orange. Methyl
orange changes colour in the 3.1-4.4 pH range. It will appear yellow in
basic solutions but will change to red in acidic solutions. This would
mean that it would have a strong acid and a weak base to get the
equivalence point of 3.10-4.4. An example of this is using hydrochloric
acid and ammonium hydroxide for titration and you would then use
Methyl orange for the indicator.
Bromothymol blue is also another indicator for titration and it changes
colour in the 6.0-7.6 pH range. It will appear blue in basic solutions but
will appear yellow in acidic solutions. This would mean that you would
need a strong acid and a strong base. An example of this is using
hydrochloric acid and sodium hydroxide.
Determining the c
You would have to be precise when reading the volume of the sample in
the burette so your eye needs to be level with the meniscus and you
would have to read the lowest level of the meniscus to get an accurate
reading and results table and for when you’re doing the titration
calculations.
Repeating the experiment at least two times is essential to make sure
your results are reproducible and reliable and to get rid of any anomalies
that may have occurred. This also means the results should be
concordant with each other, at least 0.10cm3 of each other, anything
other than that is an anomaly.
The equipment needed to do the experiment is:
 Burette
 Conical flask
 Pipette
 Primary standard solution (hydrochloric acid)
 Sample of the unknown solution (sodium hydroxide)
 Volumetric flask
  Pipette filler
 Stand with clamp
 Funnel
 Phenolphthalein
 White tile
The standard procedure to obtain accurate and reproducible results of
titration is:
Preparation of a standard solution:
1. An estimation was used to get an approximate mass of the primary standard
to use to make up a known volume of hydrochloric acid.
2. Primary standard is weighed on a balance when it’s on a weighing boat.
3. Solid is then transferred to the volumetric flask and the weighing bottle rinsed
into the volumetric flask.
4. A volume of distilled water is added to the flask until the calibration line is
reached and it needs to be swirled around which makes it into a mixture until
the solute has been dissolved.
5. Volumetric flask is inverted several times to ensure the contents have been
mixed thoroughly.
6. Set to one side.

Procedure of volumetric analysis:

1. Wear an apron and goggles.
2. Use a pipette to transfer 25cm3 of sodium hydroxide. You do this by placing
the pipette filler onto the pipette and putting the pipette inside the solution
and then you use the pipette filler to fill the pipette up to 25cm3 (the
calibration line in the middle of the pipette) which you then proceed to squirt
it into the conical flask.
3. Carefully add 5 drops of phenolphthalein into the solution in the conical flask
and swirl so it gets mixed properly.
4. Place the conical flask on a white tile so we can see the colour change more
clearly.
5. Carefully pour the sample of hydrochloric acid that you have made through
your standard solution procedure of a set volume of 25cm3 into the burette
using a funnel so the solution doesn’t spill. Place the burette overhead of the
flask using a stand and clamp and the clamp is holding the burette.
6. Add the hydrochloric to the solution drop by drop by twisting the stopcock
whilst simultaneously swirling the flask until the solution is neutral (clear)
which is when you see the colour change and is also the end-point of the
reaction which you then need to stop immediately to get an accurate reading
of the volume in the burette.
7. Read the volume of the sample added from the burette to the nearest
0.05cm3.
8. Repeat the experiment at least three times until you get reproducible results
(titres within +/- 0.10cm3).
 9. Carefully and sensibly, put all the apparatuses and chemicals away in their
suitable locations and wash your goggles as there may be residue on it and
wash all the other apparatuses as well.
10. Record and present the data in a table format using correct units and being
precise with the results.
11. Do titration calculations to work out the unknown concentration of the
sample.

A primary standard is a standard that is sufficiently

accurate as the number of moles it contains is accurate and
easily weighed. Also, it’s a very pure reagent and provides a
reference to determine the unknown concentration of a
sample. It’s very stable when being used in titration and
when it’s stored, it has no water of hydration and has no
tendency to become hydrated and is of a high molecular
weight.
Evaluating the methodology:
 You would need a lot of practice when doing titration as human errors can
occur quite often. The practice of this would make your titrations more
accurate and reliable.
 When filling up the volumetric flask or pipette, make sure the meniscus lies
upon the calibration line because the titre would not be accurate and if you
put too much or too little alkali/acid, there would be less/more acid/alkali to
neutralise it making it inaccurate and that would mean you’re testing it at a
different set volume than your original one.
 Working on this with other people could mean that you see the colour changes
at different points of the experiment which could end up being an end-point
error as you’re not certainly sure when the end-point was leading to
inaccurate and unreliable results.

Vocational application