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FACULTY OF APPLIED SCIENCES

LABORATORY REPORT

CHEMICAL ANALYSIS OF FOOD


FST 556

TITLE OF PREPARATION AND STANDARDISATION OF BASE


EXPERIMENT AND ACID SOLUTION
NO. EXPERIMENT 1

NUR SYAZA HANI BINTI NICK HAMASHOLDIN


STUDENT’S NAME
(2018653554)

NURUL FAKHIRAH BINTI MAT AZAM


(2018660018)
HIEDAH NAPISA BT JUMAAT
GROUP MEMBERS
(2018238968)
NURUL SYAZWANI BINTI KASRIN
(2018414362)

GROUP AS246 4B
DATE OF
12/03/2020
EXPERMENT
SUBMISSION DATE 04/04/2020
LECTURER’S
DR SO’BAH AHMAD
NAME
INTRODUCTION
Standardization is the technique used to find the exact concentration of a solution. The most
commonly used technique for the standardization of a solution is titration. Titration is a
chemical technique that is used to measure the concentration of a certain chemical component
in a given solution. This is done using a solution which has a known concentration
(Madhusha, 2017). The point at which the reaction is complete in a titration is referred to as
the endpoint. A chemical substance known as indicator is used to indicate (signal) the
endpoint. The indicator used in this experiment is phenolphthalein. Phenolphthalein, an
organic compound is colorless in acidic solution and pink in basic solution. This experiment
involves two separate acid-base standardization procedures. In the first standardisation the
molarity of a sodium hydroxide solution (NaOH) with 0.1 M Potassium Hydrogen Phthalat
(KHP). Potassium hydrogen phthalate used to determine the concentration of sodium
hydroxide. Potassium hydrogen phthalate, often called simply KHP, is an acidic salt
compound. KHP is slightly acidic, and it is often used as a primary standard for acid-base
titrations because it is solid and air-stable, making it easy to weigh accurately. In the second
procedure the standardized NaOH will be used to determine the molarity of a hydrochloric
solution (HCl).

 From the volume and concentration of standard solution used in the titration, and the sample
size, the concentration of the constituent in the sample can be calculated. In the titration, a
standard solution of sodium hydroxide reacts with the organic acids present in the sample. A
standard acid such as potassium acid phthalate can be used to determine the exact normality
of the standard sodium hydroxide used in the titration. The phenolphthalein endpoint in the
assay for titratable acidity is pH 8.2, where there is a significant color change from clear to
pink. Nielsen, S. S. (2017) pg 179-184

As the best indicator for strong acid-strong base titration is chosen, the same solution of
standard base is used to titrate an unknown acid quantitatively using only the color change to
gauge the volumetric endpoint. Kooser, A. S., Jenkins, J. L., & Welch, L. E. (2001) p.1504

Application
Similar other findings…
From the volume and concentration of standard solution used in the titration, and the sample
size, the concentration of the constituent in the sample can be calculated. The assay for
titratable acidity is a volumetric method that uses a standard solution of sodium hydroxide
which reacts with the organic acids present in the sample, titrating to a phenolphthalein or pH
endpoint (Nielsen, S. S, 2017)

A standard solution is one whose solute concentration is accurately known. If a solute can be


in a very pure, stable weighable form a primary standard solution of it can be
prepared directly (Mudau, K. 200

OBJECTIVES
1. To prepare and standardised sodium hydroxide, NaOH solution and hydrochloric acid,
HCl solution by titration method.
2. To determine the concentration/molarity of NaOH and unknown HCl solution.

MATERIALS

Sodium hydroxide (NaOH), hydrochloric acid (HCl), phenolphthalein indicator, beaker,


volumetric flask, conical flask, pipette, burette, burette stand and clamp, small funnel, pipette
filler.

METHODS
a) Preparation of 1 M NaOH stock solution. (prepared by lab assistant)
A 500 ml of 1 M NaOH was first prepared by calculating the needed amount of
NaOH. The appropriate amount of NaOH pellet was weighed out and placed in a 250
ml beaker. Next, a 100 ml distilled water was added into the beaker and stirred until
all pellets are dissolved. The NaOH solution was then transferred into a 500 ml
volumetric flask and diluted to volume by using distilled water. The flask was
appropriately labelled and the solution was cooled at room temperature before used.

b) Preparation of 1M HCl stock solution. (prepared by lab assistant)


A 250 ml of 1 M HCl was first prepared by calculating the needed amount of HCl.
About 150 ml of distilled water was placed in 250 ml volumetric flask. The amount of
concentrated HCl needed was pipetted into the volumetric flask and diluted to the
mark with distilled water. The flask was labelled properly.

c) Dilution of NaOH and HCl from stock solution to 0.1 M


The amount of NaOH and HCL needed from the stock solution was calculated to
prepare 250 ml of 0.1M NaOH and 0.1 M HCl.

d) Standardisation of 0.1 M NaOH solution with 0.1 M potassium hydrogen


phthalate (KHP)
250 ml of 0.1M KHP was prepared by dissolving 5.1 g of dried KHP in 250 ml
volumetric flask. Next, 20 ml of KHP solution was pipetted into 250 ml conical flask.
Then, 2-3 drops of phenolphthalein were added as an indicator. The KHP solution
was titrated with 0.1 M NaOH until it turned into light and faint pink colour for 15
seconds. The volume of NaOH used was recorded. The titration process was repeated
until two close results were obtained.
e) Standardisation of 0.1 M HCl solution with standardised NaOH solution
20 ml of 0.1 M HCL solution was pipetted in 250 ml conical flask. The solution was
titrated with standardise 0.1 M NaOH using few drops of phenolphthalein as an
indicator for the endpoint. The volume of NaOH used was recorded. The titration was
repeated until two close results were obtained.

f) Determination the concentration of unknown HCl solution


20 ml portions of the unknown HCl was pipetted into 250 ml conical flask.Next, 2-3
drops of phenolphthalein were added as an indicator. The solution was titrated with
standardised 0.1 M NaOH until reach the end point. The titration was repeated
triplicate. The concentration of unknown HCl solution was calculated in terms of M
(mol/L) , mg/ml, as g/ml and as ppm.
DATA/RESULTS

Table 1.1 Titration of known molarity of 0.1 M NaOH


Trial #1 Trial #2
Initial burette reading NaOH (ml) 23.40 19.80
Final burette reading NaOH (ml) 45.50 42.00

Volume NaOH used (ml) (final-initial) 22.10 22.20

Molarity 0.0905 M 0.0901 M

Table 1.2 Titration of known molarity of 0.1 M HCl


Trial #1 Trial #2
Initial burette reading NaOH (ml) 22.00 22.00
Final burette reading NaOH (ml) 42.40 42.90

Volume NaOH used (ml) (final-initial) 21.40 20.90

Molarity 0.0966 M 0.0944 M

Table 1.3 Titration of unknown molarity of HCl


Trial #1 Trial #2
Initial burette reading NaOH (ml) 00.00 07.70
Final burette reading NaOH (ml) 29.30 37.30

Volume NaOH used (ml) (final-initial) 29.30 29.60

Molarity 0.1323 M 0.1336 M


*Figure 1.1 Titration of known molarity of 0.1 M NaOH was not taken because it was
discarded earlier.

Figure 1.2 Titration of known molarity of 0.1 M HCl

Figure 1.3 Titration of unknown molarity of HCl


CALCULATIONS

(Volume of KHP)(Molarity of KHP)


Molarity of NaOH =
Volume of NaOH

(Molarity of standardised NaOH )(Volume of standardised NaOH )


Molarity of HCl =
Volume of HCl

Standard deviation Coefficient of variance

To prepare 500 mL of 1 M NaOH stock solution;

n( mol)
Molarity, M=
V (Litre)

Molar mass NaOH = 40g/mol

1M = 40g

in case 1M NaOH 1 Litre needed 40g, then 500 mL needed 20g

For 500 mL, 402 = 20g NaOH needed to dilute with 500 mL distilled water.

To prepare 250 mL of 1 M HCl stock solution;

n( mol)
M= where; M=1, V= 250mL @ 0.25L, n=?
V (Litre)

n
1= hence, n= 0.25 mol
0.25

g
n¿ where mm HCl; 36.46g/mol
g /mol

g
0.25 =
36.46 g /mol

mass = 9.115 g
HCl conc. = 37%, density, = 1.2g/mL

  0.37 = 9.115g

 = 24.64 g

24.64 g
= 20.53 mL of HCl needed to dilute with 250 mL distilled water.
1.2 g/ml

To prepare 250 mL of 0.1M NaOH and 0.1M HCl;


M1V1 =M2V2
(1)V1 = (0.1) (250)
V1 = 25 mL
Therefore, 25 mL of NaOH and 25 mL of HCl needed from stock solution.

To calculate molarity of NaOH from Table 1.1;


( 0.02 L ) (0.1 M )
Trial #1 Molarity NaOH =
0.0221 L

= 0.0905 M

( 0.02 L ) (0.1 M )
Trial #2 Molarity of NaOH =
0.0222 L

= 0.0901M

(0.0905+ 0.0901)
Mean =
2

= 0.0903 M
2 2


Standard deviation = (0.0905−0.0903) +(0.0901−0.0903)
2

= 2 10−4

2.8284 10−4
Coefficient variance % =  100
0.0903

= 0.22 %
To calculate molarity of HCl from Table 1.2;

( 0.0903 M ) ( 0.0214 L)
Trial #1 Molarity HCl =
0.02 L

= 0.0966 M

( 0.0903 M ) (0.0209 L)
Trial #2 Molarity HCl =
0.02 L

= 0.0944 M

Mean = 0.0955 M

Standard deviation = 1.11 10−3

Coefficient variance % = 1.15 %

To calculate molarity of unknown HCl from Table 1.3;

( 0.0903 M ) (0.0293 L)
Trial #1 Molarity HCl =
0.02 L

= 0.1323 M

( 0.0903 M ) (0.0296 L)
Trial #2 Molarity HCl =
0.02 L

= 0.1336 M

Mean = 0.1330 M

Standard deviation = 6.50 10−4

Coefficient variance % = 0.49%

Concentration of unknown HCl in terms of mg/ml, g/ml and ppm.

0.1330 mol/L  mg/ml

mol 1L 36.46 g 1000 mg


0.1330 = = = = 4.8492 mg/ml
L 1000 mL mol 1g

4.8492 mg/ml  ppm (multiply by 1000) = 4849.18 ppm

4.8492 mg/ml  g/ml


mg 1000 g
4.8492 = = 4849.18 g/ml
mL 1 mg
DISCUSSION

The titrations had to be done with much care and precision because of its sensitivity. 

 It is important to note that the pink color in three titrations were all slightly different, some
being darker than others. It was crucial to make use of the half drop technique as well
because the endpoint was very sensitive to even 0.05 mL.
Also, each individual perceives color slightly differently, which affects the outcome of the
experiment. If the color has changed slightly, too much of the titrant, which comes from the
burette, can be introduced into the solution, overshooting results (Carpenter, M. E., 2018)

The average molarity of the sodium hydroxide solution was found to be 0.155 M after
standardization. Using that solution, the average concentration of potassium hydrogen
phthalate was found to be 27.99% in the #52 LO unknown solid. The standard deviation was
calculated as 2.411 which is acceptable yet a small cause of concern since the second
experimental trial yielded a KHP concentration of 25.31% which lies outside one standard
deviation away from the mean. Perhaps a better result could have been attained if equal
amounts of unknown mass were used for each trial.
Due to the simple nature of the experiment it was crucial to have accurate
measurements and clean equipments. 

According to Schoolworkhelper Editorial Team (2014), allowing the KHP solution to become
too pink. Due to excessive NaOH, there were accuracy issues in the calculation of the
concentration was inaccurate. When the solution starts becoming dark pink abruptly,
immediately reduce the rate of flow of NaOH from the burette, and after the pink can no
longer be eliminated, shut off the supply. This way, we avoid excess NaOH from being added

Allowing the KHP to flow along the inner walls of the conical flask. This would have
resulted in inaccuracies. The NaOH may not have reacted with the exact amount of KHP
expected. Make sure the conical flask is directly under the pipette, with no contact with the
inner walls, so as to get a more accurate measure of the volume.
It is a good idea to carry out titration in triplicate in order to make sure that the results would
not vary that much. This is done to minimize any errors done when titrating a sample.
must be carried out in the fume cupboard to prevent the smell of the compound to be
distributed in the laboratory. Moreover, NH4OH can lead to several irritation burn and also
vomiting and nausea. When handling it, do not contact directly to our hand, so use glove
when handle the substance.

A low standard deviation indicates that the values tend to be close to the mean (also called
the expected value) of the set, while a high standard deviation indicates that the values are
spread out over a wider range.
coefficient of variation (CV), also known as relative standard deviation (RSD), is a
standardized measure of dispersion of a probability distribution ratio of the standard deviation
to the mean.
The higher the coefficient of variation, the greater the level of dispersion around the mean.
The lower the value of the coefficient of variation, the more precise the estimate.

Standardization is the process of determining the exact concentration (molarity) of a solution.


Titration is one type of analytical procedure often used in standardization which two
solutions are introduced to form a reaction that once completed. reaches an identifiable
endpoint. In this experiment it involves two separate acid-base standardization procedures
containing primary and secondary standard. A primary standard is a reagent that is extremely
pure, stable, it not a hydrate/has no water of hydration, and has a high molecular weight. A
secondary standard is a standard that is prepared in the laboratory for a specific analysis. It is
usually standardized against a primary standard. In this experiment, for the first titration,
sodium hydroxide (NaOH) is the secondary standard and the primary standard is potassium
hydrogen phthalate (KHP). The molarity of NaOH is known. Based on titration of known
molarity of sodium hydroxide against potassium hydrogen phthalate (KHP), the average
concentration NaOH that had been calculated is 0.1 M. The actual molarity of Sodium
hydroxide in this experiment is 0.1 M. The molarity NaOH that had been calculated is same
with the actual molarity of NaOh.
In this experiment for second titration, sodium hydroxide (NaOH) is a secondary standard
that against with its primary standard which is hydrochloric acid (HCL). The molarity of
HCL is known, The average concentration of HCl that had been calculated is 0.082 M. The
actual concentration of HCl is 0.1 M. There is slightly difference in the value of the HCl duc
to the hygroscopic property Of secondary standard, NaOH which readily absorb moisture and
reacts with carbon dioxide in the Air. For third titration, it is to obtain the concentration of
unknown hydrochloric acid (HCI). The actual Concentration of unknown HCl is 0.15 M. In
this experiment, the average of unknown molarity of HCl that had been calculated is 0.1215
M. There is also a slightly difference with the actual Molarity. Again, this is due to NaOH
used which readily absorb moisture and reacts with carbon Dioxide in the air.
QUESTIONS & ANSWERS

1. Why is being careful towards the end of titration, as you reach the equivalent point, so
important?
Answer: The end point of a titration indicates that the equivalence point has been
reached. The equivalence point is the ideal point for the completion of titration. Titration
should be done carefully as it reached its equivalent point so it will give very accurate
and precise results. This precaution is to avoid from overshooting by adding too much
titrant and changes the colour solution into dark pink/purple. As this happens, the
titration needs to be repeated or by using back titration method.

2. Why did we use an indicator in our acid and not with the naoh in the burette?
Answer: Phenolphthalein is used as indicator in strong acid-strong base titration because
it changes color in a pH range between 8.3 – 10. It is a weak acid hence, it will appear
pink in basic solutions and clear in acidic solutions. That is why phenolphthalein is
added in the flask contains the acid solution and not in the burette that contains base
solution or else, the whole burette changes its colour into dark purple and the titration
will not succeeded.
CONCLUSION
In conclusion, the is determined. T

The titrations yielded an average concentration of

REFERENCES

1. Nielsen, S. S. (2017). Standard Solutions and Titratable Acidity. In Food Analysis


Laboratory Manual (pp. 179-184). Springer, Cham.

2. Kooser, A. S., Jenkins, J. L., & Welch, L. E. (2001). Acid-base indicators: a new look
at an old topic. Journal of Chemical Education, 78(11), 1504.

3. Kim, J. (2018). The Standardization of NaOH and KHP. Retrieved from


https://www.odinity.com/standardization-naoh-khp/

4. Madhusha. (2017). Difference Between Standardization and Titration. Retrieved from


https://pediaa.com/difference-between-standardization-and-titration/

5. Schoolworkhelper Editorial Team. (2014). Titration Lab: NaOH with Standardized


solution of KHP. Retrieved from https://schoolworkhelper.net/titration-lab-naoh-
standardized-solution-khp/

6. Eddy, D. (n.d). Chemistry 104: Standardization of Acid and Base Solutions. Retrieved
from http://www.chem.latech.edu/~deddy/chem104/104Standard.htm

7. Mudau, K. (n.d). Acid Base Titration – Preparation of standardization of NaOH and


the analysis of the unknown acetic solution. Retrieved from
https://www.academia.edu/28582165/Title_ACID_BASE_TITRATION_Preparation_
of_standardization_of_NaOH_and_the_analysis_of_the_unknown_acetic_solution

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