EXPERIMENT NO.

3
VOLUMETRIC TRANSFER

Abstract
The exact normality of NaOH was determined using KHP as primary
standard and the normality of HCl using NaOH as the secondary standard.
Phenolphthalein is used as the indicator in the titration process. It was found
out that after the experiment, the exact concentration of NaOH is 0.240N and
the exact concentration of HCl is 0.00N.

I. Introduction
Titration methods, often called titrimetric methods, include a large and powerful
group of quantitative procedures based on measuring the amount of a reagent of
known concentration that is consumed by an analyte in a chemical or electrochemical
reaction.

Titrations are widely used in analytical chemistry to determine acids, bases,

oxidants, reductants, metal ions, proteins, and many other species. Titrations are
based on a reaction between the analyte and a standard reagent known as the
titrant. The reaction is of known and reproducible stoichiometry. The volume, or the
mass, of the titrant needed to react completely with the analyte is determined and
used to calculate the quantity of analyte.

There are different types of titrations which include volumetric titrations which
involve measuring the volume of a solution of known concentration that is needed to
react completely with the analyte. In here, the given methods for volumetric analysis
involves primarily with the preparation of the standard acid and base solutions,
followed by neutralization titration, standardization of the acid solution against an
alkaline compound and the basic solution against an acid compound, and the
determination of the total strength of the acid and base.

It is important to note that before the titration process, the preparation of the
standard acid and base solutions are to be highly considered. It is because a
standard solution is that whose concentration has been determined to have a high
degree of accuracy and as well as it plays a central role in all titrations. Therefore, we
must consider the desirable properties for such solutions, how they are prepared,
and how their concentrations are expressed. The ideal standard solution for a

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titrimetric method will (1) be sufficiently stable so that it is necessary to determine its
concentration only once; (2) react rapidly with the analyte so that the time required
between additions of reagent is minimized; (3) react more or less completely with the
analyte so that satisfactory end points are realized; and (4) undergo a selective
reaction with the analyte that can be described by a balanced equation.

Few reagents completely meet these ideals.

The accuracy of a titration can be no better than the accuracy of the

concentration of the standard solution used. Two basic methods are used to
establish the concentration of such solutions. The first is the direct method in which a
carefully determined mass of a primary standard is dissolved in a suitable solvent
and diluted to a known volume in a volumetric flask. The second is by standardization
in which the titrant to be standardized is used to titrate (1) a known mass of a primary
standard, (2) a known mass of a secondary standard, or (3) a measured volume of
another standard solution. A titrant that is standardized is sometimes referred to as a
secondary standard solution. The concentration of a secondary-standard solution is
subject to a larger uncertainty than is the concentration of a primary-standard
solution. If there is a choice, then, solutions are best prepared by the direct method.
Many reagents, however, lack the properties required for a primary standard and,
therefore, require standardization.

Primary Standards

A primary standard is a highly purified compound that serves as a reference

material in titrations and in other analytical methods. The accuracy of a method
critically depends on the properties of the primary standard. Important requirements
for a primary standard are the following:

a. High purity. Established methods for confirming purity should be available.

b. Atmospheric stability.
c. Absence of hydrate water so that the composition of the solid does not
change with variations in humidity.
d. Modest cost.
e. Reasonable solubility in the titration medium.
f. Reasonably large molar mass so that the relative error associated with
weighing the standard is minimized.

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 Very few compounds meet or even approach these criteria, and only a limited
number of primary-standard substances are available commercially. As a
consequence, less pure compounds must sometimes be used in place of a primary
standard. The purity of such a secondary standard must be established by careful
analysis.

Objectives of the Experiment

State the general objective of the experiment in past tense.
Specifically, the experiment aimed to attain the following objectives:
1. To prepare standardized solutions of 0.25N HCl and 0.25N NaOH
to be used in Experiment 5 (Neutralization Titration) and
Experiment 6 (Determination of the Total Strength of Alkalinity of
Soda Ash, Anhydrous Sodium Carbonate) respectively

II. Materials
The materials used in the experiment were:
1. Five one-peso coins. These coins were the old BSP coin series
(1995-present) but are still in circulation. The coins were the 2003-
present version (5.35 g). The penny 1 was produced in 2012,
pennies 2 and 3 were produced in 2015 and pennies 4 and 5 were
produced in 2016.
2. State the apparatus/reagent. Describe the material in terms of
brands, conditions, and how it was used in the experiment.

III. Procedure
Preparation of Standard Solutions
Wash the volumetric glass wares first before performing the experiment using
distilled water. Fill the 2 1L-Erlenmeyer flasks up to the graduation mark and
heat to boil with the use of a hot plate. Afterwards, cover the flasks with an
inverted beaker and cool under tap water in a water bath. Wait until the water
inside the flasks has been cooled.
For 0.25N HCl solution

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 Add around 125 mL of boiled distilled water inside the 500-mL volumetric
flask. Measure 10.4 mL of concentrated HCl using the pipette and aspirator,
and then transfer it to the volumetric flask. Then, make a quantitative transfer
to the pipette Dilute the solution to 500 mL, and then shake the solution
vigorously to distribute evenly in the liquid. Do around 10 inversions if
necessary.
For 0.25N NaOH solution
Add around 250 mL of boiled distilled water inside the 1-L volumetric flask.
Weigh a watch glass and then measure on it 10 grams of solid sodium
hydroxide. Make a quantitative transfer to the pellets by transferring the
pellets from the watch glass to the beaker using a wash bottle. Afterwards,
dissolve the pellets in about 16mL of distilled water in a beaker. Transfer it
again to the 1L-volumetric flask and make a quantitative transfer to the
solution. Shake the solution and dilute the solution up to 1000mL or up to the
graduation mark. Do around 10 inversions if necessary to distribute evenly in
the liquid.

Standardization of NaOH solution

Weigh 0.5 g of Potassium Hydrogen Phthalate (KHP or C 8H5KO4) into a 250-
mL Erlenmeyer flask. Dissolve the primary standard in about 50 mL of distilled
water. Add two drops of phenolphthalein to the solution. Titrate the KHP
solution with the prepared NaOH solution to the faint pink endpoint. Record
the volume of NaOH used to titrate the KHP solution.

Comparison of Standard Solutions

Fill the burettes with their respective solutions. Run 25.00 mL of HCl
into a 250-mL Erlenmeyer flask. Add about 30mL distilled water and 3 drops
of phenolphthalein indicator. Titrate with the NaOH solution to the appearance
of a faint or light pink endpoint that persists for at least 15 seconds. Record all
volumes. Calculate the ratio of the strengths of the acid and base solutions.
Note: If the endpoint is overrun, back titrate by adding HCl (from the
burette) until the solution is just colorless, then, add NaOH drop wise to the
faint pink endpoint.
At equivalence point: meq NaOH = meq HCl
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IV. Results and Discussion
Introduce your results followed by a table with a heading. Do not cut
tables across pages.
Table 1. Table title
Mass (g)
Object
Method 1 Method 2

Table 4.1. Preparation of 0.25N HCl

Volume of concentrated HCl 10.4 mL
Weight of concentrated HCl 12.4 g
Equivalent weight 36 g/eq
Volume of solvent, distilled water 489.6 mL
Volume of solution 500.0 mL
Normality 0.25N

Table 4.2. Preparation of 0.25N NaOH

Weight of NaOH 10.0 grams
Equivalent weight 40 g/eq
Volume of solution 1000.0 mL
Normality 0.25N

A. Standardization of NaOH solution

Table 4.3. Titration of a 50-mL KHP solution with NaOH

Normality of
Trial MKHP VH2O VNaOH solution Remarks
NaOH
1 0.5 g 50 mL 12.8 mL Over titrated 0.191N
2 0.5 g 50 mL 10.4 mL Over titrated 0.235N
3 0.5 g 50 mL 10.2 mL Titrated 0.240N

Use the levels of interpretation to discuss your data. Level 1: What are
the important values present in your data? Level 2: What do those data imply?
Level 3: Is the data different from the theoretical or ideas from literatures?

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What are the probable sources of these deviations? Cite your sources. Level
4: Conclude and/or recommend to improve future similar or the same
experiments.
A. Preparation of Standard Solutions
The experiment was started by boiling the distilled water into the 2 1-L
Erlenmeyer flasks with the aid of a hot plate. The purpose of boiling the
distilled water is to eliminate the presence of carbonates in the solvent so that
the standard solution will be CO2 and CO3 free. Once these contaminants are
present, these may cause possible errors in determining the concentrations at
a high degree of accuracy. An example is Na 2CO3 which is a common impurity
in the solid NaOH used for the preparation of the alkali solution.
The purpose of covering the Erlenmeyer flasks with an inverted beaker
is to assure that there will be no impurity that will go through the water as it
boils. When it comes to removing the carbonates in the water, it has been
observed that at the moment that the water was boiling, water molecules
became water vapour and then water vapour molecules went up to the
beaker. And then the vapour will turn again to water that will run out through
the beaker.
On the other hand, the purpose of cooling the Erlenmeyer flasks
(containing distilled water) with a water bath is to lower its temperature until
the water inside the flasks reached room temperature. When the boiled
distilled water that has not been cooled is used in standardizing the solutions,
the tendency is that the solutions that will be produced will be very hot
besides the fact that the reactions between the water and the acid or the
water or the base will release heat that may contribute to the overall heat of
solution. And thus, it needs utmost carefulness to execute the procedures
properly. Moreover, too much heat of the solution may break the volumetric
glassware to be used and may lead to the repetition of the work or simply a
waste of time.
Afterwards, the computation of the concentrated HCl and reagent
graded solid NaOH was solved with respect to the availability of volumetric
glass wares, especially the volumetric flasks to which the solution was diluted
to volumes of 500mL and 10000mL respectively, provided by the laboratory.

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 Getting the exact amount of reagent to be used is very necessary in
getting the exact concentration of the solution. A quantitative transfer has
been also utilized for the goal of achieving a systematic process of the
experiment and so as to be accurate with the concentrations of the solutions.
Also, the dilution of the solution to volume is vital because once the volume is
less or more than of the graduation mark may lead to lesser concentration or
greater concentration compared to the calculated value of normality. Thus, the
proper execution of the procedures must be of high concern in order to
achieve better results (with the least error) not only in the concentrations of
the standard solutions but also in determining the volume to which that
analyte will completely react with the titrant (to be used to the succeeding
experiments).
B. Standardization of NaOH solution
Standardization is the process of determining the exact concentration
of a solution Titration is one type of the analytical procedure often used in
standardization. In a titration, an exact volume of one substance is reacted
with a known amount of another substance.
In calculating the normality of the NaOH solution, which will be
determined by titrating a 0.5g sample of potassium hydrogen phthalate (KHP;
HKC8H4O4) with the NaOH, has been computed by multiplying the weight of
KHP used and its molar weight, then multiplied by the stoichiometric of NaOH
and KHP, which is 1:1, and then divide it by the volume of NaOH used in the
titration. Or simply,
HKC8H4O4 + NaOH  NaKC8H4O4 + H2O
1 mol
( 204.23
( 0.5 g KHP )
g)
−3
=2.448 ×10 mol KHP

( 2.448 ×10 mol KHP ) ( 1 mol NaOH )=2.448 ×10

−3 −3
mol NaOH
1 mol KHP

2.448 ×10−3 mol NaOH

( Volume of NaOH added (mL))=C NaOH

C NaOH ×n=N NaOH

Where n is equal to 1

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 Curve for the Titration of 0.5 g KHP dissolved in
50 mL of water 0.25 N NaOH
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12
10
8
pH

6
4
2
0
0 2 4 6 8 10 12 14 16
Volume NaOH added (mL)

Figure 4-1 shows the change of pH versus the volume of NaOH added
in which after the addition of 10.2 mL of NaOH, the titration end point, the pH
of the solution is at 9.00. The titration process utilized a phenolphthalein
indicator to determine the end point. The indicator range for the
phenolphthalein indicator is from pH 8.00 up to pH 9.8. This means to say that
the phenolphthalein indicator is suitable for the titration of 0.5 g of KHP with
0.25N NaOH since the pH at the equivalence point is at 9.00 and is included
in the pH rage of the said indicator.

V. Conclusion
Conclude by answering your objectives. You may include some salient
recommendations.
The exact normality of NaOH was determined using KHP as primary
standard and the normality of HCl using NaOH as the secondary standard.
Phenolphthalein is used as the indicator in the titration process. It was found
out that after the experiment, the exact concentration of NaOH is 0.240N and
the exact concentration of HCl is 0.00N.

VI. Answers to Questions

VII. References

Harris, D. (2010). Quantitative Chemical Analysis, 8 th Ed. New York: W. H.

Freeman and Company. ISBN-13: 978-1-4292-1815-3.

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Skoog, D. A., West, D. M., Holler, F. J. & Crouch, S. R. (2014). Fundamentals
of Analytical Chemistry, 9th Ed. CA, USA: Brooks/Cole, Cengage
Learning. ISBN-13: 978-0-495-55828-6.
Sciencing. (2018, March 13). Retrieved March 23, 2019, from Why Must a
Burette & Pipette Be Rinsed With the Appropriate Solution Before a
Titration?: https??sciencing.com/must-appropriate-solution-before-
titration-8745281.html
LibreTexts, C. (2015, September 17). Instrument Calibration. Retrieved March
23, 2019, from
https://chem.libretexts.org/Bookshelves/Analytical_Chemisty/Suppleme
ntal_Modules_(Analytical_Chemistry)/Data_Analysis/Instrument_Calibr
ation_over_a_regime
Walker, J. P. (2012). Volumetric Glassware. North Carolina, United States.

Follow the APA format. Research their format. Arrange the references
alphabetically. Include all that you have cited.

Appendices

Appendix A
Table 4. Mass of pennies and the standard deviation of the masses in the trials
using method 1
Penny Mass of penny in grams Standar
numbe d
r Deviatio
n
Trial 1 Trial 2 Trial 3 Trial 4 Trial 5 Trial 6 Mean
1 5.998 5.998 5.998 5.998 5.998 5.998 5.998 0.00007
4 4 3 2 4 4 4 6
2 5.402 5.402 5.402 5.402 5.402 5.402 5.402 0.00010
8 9 8 6 9 9 8 7
3 5.402 5.402 5.402 5.402 5.401 5.401 5.402 0.00011
9
 0 0 0 1 8 8 0 2
4 5.436 5.436 5.436 5.436 5.436 5.436 5.436 0.00007
8 8 9 9 9 7 8 4
5 5.424 5.424 5.424 5.424 5.424 5.424 5.424 0.00011
5 4 6 7 6 4 5 1

You may include sample computations on how the data in the tables were
calculated.

Insert the rubric after this page.

The pagination of the next lab report shall continue from here but do not place
the page number of the first page of the next report.

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Experiment 1. Using the Analytical Balance
LABORATORY REPORT RUBRIC

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 Criterion 1 2 3 4 Scor
 Does not clearly identify  Rudimentary problem  Clearly identifies main  Clearly identifies the
the problem; identification; problem and includes main problem and
 Identifies an  Identifies main problem some of the subsidiary subsidiary, embedded
inappropriate problem but does omits relevant issues; or implicit aspects of the
Problem
or represents the issue issues;  Some discussion or problem;
Identification
inaccurately  Does not identify the relationships between  Clearly addresses the
(3 points) relationship between subsidiary issues relationship among
different aspects or subsidiary issues;
issues within the  Identifies not only the
problem. basics of the issue but
also recognizes subtle
nuances of the issue

 Fails to question data;  Identifies some  Asks insightful  Analyzes insightful

 Ignore bias; questions; questions; questions;
 Misses major content  Notes some bias;  Detects bias;  Refutes bias;
Interpretatio
n areas;  States some  Categorizes content;  Critics content;
(7 points)  Detect no inconsistencies;  Identifies  Examine
inconsistencies;  Selects sources inconsistencies; inconsistencies;
 Chooses biased adequately.  Recognizes context.  Values information
sources.

 Fails to draw  Identifies some  Formulate conclusions;  Examines conclusions;

conclusions; conclusions;  Recognizes arguments;  Uses reasonable
 Sees no arguments;  Sees some arguments;  Notices differences; judgment;
Analysis and
Evaluation
 Overlooks differences;  Identifies some  Evaluates data;  Discriminates rationally;
(10 points)  Repeats data; differences;  Seeks out information  Synthesizes data;
 Omits research  Paraphrases data;  Vies information
 Assumes information critically
valid.

 Omits argument;  Misconstruction  Argues clearly;  Argues succinctly;

 Misinterpret issues; arguments;  Identify issues;  Discusses issues
 Excludes data;  Generalizes issues;  Attribute sources; thoroughly;
Presentation 13
(5 points)  Draws fault conclusions;  Cites sources;  Suggest solutions;  Shows intellectual
 Shows intellectual  Presents few options;  Incorporates honesty;
dishonesty  Overlooks some information.  Justifies decisions;
information  Assimilates information
Rater: ________________________________

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