Experiment III

PREPERATION OF A STANDARD SODIUM HYDROXIDE SOLUTION, DETERMINATION

OF PURITY OF IMPURE KHP AND STANDARDIZATION OF HYDROCHLORIC ACID

4 October 2012

JACOB DONTON
 Donton 2

Introduction
Sodium hydroxide and Hydrochloric acid are common solutions in laboratories and are
often diluted to specific molar concentrations for practical use. Concentrated versions of these
solutions are extremely potent and dangerous, often unnecessary for conducting experiments.
Finding the true concentration of the diluted solution is a procedure called standardization,
where, in this case, a known substance, potassium hydrogen phthalate (KHP) is used for the
standardization of sodium hydroxide. KHP is used because it does not dissociate on its own, and
its purity can be achieved and stabilized at 99.99%. It reacts completely with sodium hydroxide,
in a monoprotic reaction, where phenolphthalein is used as an indicator to mark the neutral pH as
sodium hydroxide is added. This standardized solution is important because it can be used
accurately for many typed of experiments. However, a new standardization of this solution
should be done once every one or two weeks because it is known to collect carbon dioxide from
the atmosphere, creating hydrogen carbonate, changing the pH and concentration of the solution.

Discussion
Data and Calculations

Standardization of NaOH with Pure KHP

0.5106 g KHP
(1)Conc . NaOH ( M )= 0.0245 L NaOH =0.1003 M NaOH
g
204.23 ( )
mol

2 2 2
( 0.09930.1003 ) + ( 0.09930.0967 ) + ( 0.09930.1008 )
Standard Deviation ( s )= =0.00224
2

%RSD=0.00224 0.0993 100=2.26

The use of a known standard, KHP, to 99.99% purity ensured an accurate measurement
for the concentration of the NaOH solution. The weighing of the pure KHP error was reduced by
taking the difference of the emptied weighing glass and the weighing glass with the KHP, since
KHP stuck to the surface and left a slight residue. The volumes of NaOH added were the cause
of most of the error. This is because the endpoint is determined by the eye; the detection of the
pink hue. The shades of pink, from the indicator phenolphthalein vary and fade over timedue
 Donton 3

to the taking-in of carbon dioxide from the atmosphere. The absorption of carbon dioxide plays
a factor over time as well, which is why boiled DI water is used to dilute the concentrated NaOH,
to minimize this effect from the start.
The importance of the primary standard pure KHP is in the legitimacy of the results
obtained. The primary is standardized, usually, by the NIST, National Institute of Standards and
Technology, recognized ubiquitously. Since this a major source of standardized materials, most
laboratories will use the same KHP or other primary standard compounds, and the results will be
based on this standard. Having this type of standardization reduces uncertainty of
measurements. The only uncertainties are left to the weighing, volumes, and detection of the
indicator, and not having to find the purity of KHP as well.

Finding the Impurity of a Unknown KHP

0.0993 M NaOH
(1) Purity of KHP ( )= 100=42.29 Purity
0.8029 g Impure KHP
0.017 L NaOH
g
204.23 KHP
mol

2 2 2
( 41.5842.93 ) + ( 41.5841.49 ) + ( 41.5840.31 )
Standard Deviation ( s )( Purity )= =1.3121
2

1.3121
%RSD ( Purity ) = 100=3.16
41.58

With the standardized solution of NaOH using the primary standard of KHP, the impurity
of an unknown KHP can be found. Knowing that the pure KHP completely dissociates to the
endpoint, using the NaOH solution with a known concentration, this ratio of the false molar
concentration of NaOH and real NaOH denotes the impurity of the unknown KHP. Note, the
KHP is titrated to an endpoint, where it can no longer react, and has been permanently
dissociated. Equilibrium entails a balance of reactions, leaving it to react in either direction by
changing a number of factors such as concentrations, heat, and/or pressure.
 Donton 4

Standardization of and HCl Solution with Standardized NaOH

26.8 mL NaOH 0.0993 M NaOH

( 1 ) Conc . HCl ( M ) = =0.1064 M HCl
25.00 mL HCl

2 2 2
( 0.10660.1064 ) + ( 0.10660.1037 ) + ( 0.10660.1096 )
Standard Deviation [Conc . HCl ( M ) ]= =0.002953
2

0.002953
%RSD= 100=2.77
0.1066

The use of the standardized NaOH is seen in its basic nature, and standardized
concentration. It can standardize other solutions, such as unknown HCl solutions; given, a rough
molar concentration is known to be approximately 0.1M. Since this reaction consists of a strong
base and a strong acid, phenolphthalein is used to be an indicator for pH to detect when the
solution becomes just basic (pH greater than ~8.2). The reaction is also monoprotic so one-to-
one stoichiometric ratios can be used in calculations, as opposed to more complex calculations
associated with titrating polyprotic buffers.

Conclusion
Standardizing solutions with primaries greatly reduces uncertainty in general calculations
measurements. However, this does not dismiss the uncertainty of using glassware and eyesight
to perceive a given endpoint.
The relative standard deviation percentages
are considerably high, taking into account even,
the inaccuracy of the instrumentation. Even so,
more trials could have been conducted to reduce
these deviations to an acceptable percentage. Concurrently, the inaccuracy of using a visible
indicator to detect the endpoint of a reaction increases the uncertainty. An electronic pH detector
may be implemented to avoid using eyesight and perceived color for detection.
 Donton 5

References

Harris, C. Daniel, Quantitative Chemical Analysis, 8th Ed, W.H. Freeman & Company 2010, 22-
24, 206-212, 219-223, 225-226

Pratt, K. W., Evaluation of Independent High-Precision Assay Procedures for a High-Purity

Primary Standard Reagent, http://www.nist.gov/mml/csd/inorganic/highpurityreagents.cfm,
(accessed on 3 October 2012)