Experiment No.

Preparation and Standardization of Reagents

Group No. 4 Date Due: December 11, 2014

Group Members: Date Performed: November 20, 2014

Asjali, Seagal

Paden, Lucen Jane

Resando, Sheena Mae A.

Name:

Sheena Mae A. Resando

BS Chemistry II
 Abstract

This activity aims to demonstrate the most common method for obtaining standard
solutions for titrimetric analysis, prepare solution that has the approximate concentration
desired to ± 0.5% of its actual value, determine the concentration of sodium hydroxide to the
standard solution by direct titration against a primary standard, and to test the accuracy of the
determined concentration by comparison with a known standard.

The calculated concentration of the standardized NaOH for the three trials has an
average of 0.0987 M. It has standard deviation of 0.0011 and a percent error of 1.29%. This
indicates that the data obtained shows a high degree of precision since its standard deviation
is less than 1 but do not possess a high degree of accuracy since it percent error exceeds to 1.
On the other part, the calculated concentration of the standardized HCl for the three trials has
an average of 0.0972 M. It has a standard deviation of 0.0002 and a percent error of 2.79%.
Thus, the data obtained is a precise one but less accurate since its percent error is more than
one.

From the activity, we’re able to demonstrate the most common method for obtaining
standard solutions for titrimetric analysis, prepare solution that has the approximate
concentration desired, and determine the concentration of sodium hydroxide to the standard
solution by direct titration against a primary standard. The concentration of sodium hydroxide
is 0.0987 M in which it has a percent error of 1.29%. This error might be due to the possible
errors encountered upon doing the dissolving part.
 Chapter I

Introduction

The accuracy of many analytical measurements is dependent upon the manner in

which the standard solutions are prepared and stored, and the accuracy with which they are
standardized. Combining the methods recommended for the preparation and handling of such
solutions into one practice eliminates the necessity for covering such details in all of the
methods wherein the solutions are used. Chemical reagents are manufactured and marketed in
different grades of purity. The purest reagents are marketed as “analytical reagent”. Other is
“laboratory reagent” and “chemically pure”. The strength of chemicals is expressed as
normality or molarity. Hence, it is useful to be informed about the strength of the acids and
alkalis most commonly used in chemical laboratories.

In this activity, the concentration of NaOH analysis is determined by using the NaOH
solution to titrate an exactly known mass of primary standard potassium hydrogen phthalate
or KHP. When sodium hydroxide reacts with potassium acid phthalate, it yields to water and
NaKC8H4O4. The end-point is mark by using phenolphthalein as indicator. Sodium carbonate
(anhydrous) is a suitable chemical for preparing a standard solution as a primary standard.
The molarity of the given HCl can be obtained through titrating it against the standard
sodium carbonate solution prepared. Hydrochloric acid when reacts with sodium carbonate
will gives sodium chloride, carbon dioxide and water. The end-point is marked by using
methyl orange as an indicator.

This activity aims to demonstrate the most common method for obtaining standard
solutions for titrimetric analysis, prepare solution that has the approximate concentration
desired to ± 0.5% of its actual value, determine the concentration of sodium hydroxide to the
standard solution by direct titration against a primary standard, and to test the accuracy of the
determined concentration by comparison with a known standard.
 Chapter II

Methodology

A. Preparation of approximately 0.1000 M NaOH Solution

About 4.2 grams sodium hydroxide was weighed in a 150-mL beaker. To

dissolved sodium hydroxide, 50-mL of carbon-free distilled water was added into the beaker.
The solution was then transferred into a 1000-mL volumetric flask. The beaker was rinsed
thoroughly and the washings were transferred to the flask. More carbon-free distilled water
was added to the flask up to the mark. After that, the solution was transferred to a plastic
container with well fitted suitable stopper which prevents access to atmospheric carbon
dioxide. The solution was then stored at the locker which will be titrated against KHP to
determine its exact molarity.

B. Preparation of approximately 0.1000 M HCl Solution

1000-mL bottle was obtained for storage. It was washed with liquid detergent first
then rinse with tap water and then distilled water. 1000-mL of distilled water was measured
unto the beaker. The water was heated to boiling and then cooled at room temperature. After
that, about 500 mL of boiled water was transferred to the 1000-mL volumetric flask and then
the 8.0 mL concentrated HCl was slowly added into the flask.

C. Standardization of 0.10 M NaOH solution against Potassium Acid Phthalate (KHP) using
Direct Titration

Dried samples of 0.50-0.60 grams of KHP were weighed duplicately into a 250-
mL Erlenmeyer flask. Each sample was dissolved in 100-mL boiled distilled water and then
cooled at room temperature. Two drops of phenolphthalein indicator was added to the
solution in the flask. The cleaned buret was rinsed with NaOH and was discarded. The buret
was then filled with NaOH solution and it was allowed to stand for 30 seconds before reading
the exact position of the meniscus. The initial reading was recorded. Sodium hydroxide
solution was slowly added to the flask of KHP solution while swirling its content. As NaOH
was added, a pink color appeared. The color disappears with swirling. As the endpoint was
approached, the color disappears more slowly, at which time NaOH solution was added drop
by drop. The end point was reached when one drop of NaOH solution turned pink from
colorless. The solution was then discarded and the flask was washed with plenty of tap water
and was rinsed with distilled water. The titration was repeated two more times.
D. Standardization of 0.1000M HCl solution against Sodium Carbonate using Direct Titration

About 2.0 grams of Na2CO3 was dried in a weighing bottle for two hours at105-
110° C, was cooled and stored in a dessicator. About 1.3 grams of dried Na2CO3 was
weighed. The weighed carbonate was transferred to a beaker and 100 mL of distilled water
was added into it to dissolve completely. After it was dissolved, the solution was transferred
to a 250-mL volumetric flask. The beaker was rinsed thoroughly to transfer all the washes to
the flask and was filled with water up to the mark. 25 ml of the sodium carbonate solution
was pipet to a clean erlenmeyer flask. This was then titrated with the given dilute
hydrochloric acid until the color of solution just changes from yellow to orange. The titration
was repeated two more times.
 Chapter III

Results and Discussion

The following tables below showed the results and data on the direct titration of
standardized NaOH against KHP and also the standardized HCl against Na2CO3.

Table1.1 Results and Data on the Direct Titration of Standardized NaOH against KHP

Titrations
1st 2nd 3rd
Final buret reading (ml) 28.90±0.01 ml 28.35±0.01 ml 31.17±0.01 ml
Initial reading (ml) 3.65±0.01 ml 2.81±0.01 ml 2.75±0.01 ml
Volume of titrant (ml) 25.25±0.01 ml 25.54±0.01 ml 28.42±0.01 ml
Color of analyte after Faint pink Faint pink Faint pink
titration
Weight of KHP sample (g) 0.5152±0.0001 g 0.5140±0.0001 g 0.5670±0.0001 g
Moles of NaOH (mol) 2.523 × 10-3 2.517 × 10-3 2.776 × 10-3
Molarity of standardized 0.09991 M 0.09854 M 0.09769 M
NaOH (M)
Mean and standard deviation 0.0987± 0.0011 M
Percent error (%) 1.29 %

The table above shows the results and data obtained on the direct acid-base titration of
standardized NaOH against the KHP. The color of the analyte which is the potassium
hydrogen phthalate or KHP after it was being titrated with NaOH is faint pink caused by the
addition of phenolphthalein as an indicator since end-point is mark by using the said
indicator. Equivalence point was reached as faint pink solution was observed.

The number of moles of NaOH was obtained through the use of KHP sample’s
weight. The following are the calculated or obtained number of moles of NaOH for each trial:
2.523 × 10-3, 2.517 × 10-3 and 2.776 × 10-3 moles. The calculated volume of titrant is the
volume of NaOH needed to neutralize the KHP solution. The following are the volumes of
titrant for the three trials: 25.25 ml, 25.54 ml and 28.42 ml.

The molarity or the concentration of the standardized NaOH was obtained through the
use of the number of moles of NaOH and the volume of titrant. The average molarity of
standard NaOH calculated is 0.0987 M. It has a standard deviation of 0.0011 and a percent
error of 1.29 %. The obtained data therefore has a high degree of precision since its standard
deviation is <1 but don’t have a high degree of accuracy since its percent error is >1. This
might be due to some personal error encountered upon doing the dissolving part.
Table 1.2 Results and Data on the Direct Titration of Standardized HCl against Na2CO3

Weight of Na2CO3 (g) 1.3098±0.0001 g

FW of Na2CO3 (g/mol) 105.988 g/mol
Molarity of Na2CO3 (M) 0.04945 M
Volume of Na2CO3 solution (ml) 250.00±0.08
Volume of Na2CO3 solution used (ml) 25.00±0.01 ml
Titrations
1st 2nd 3rd
Final buret reading (ml) 26.40±0.01 ml 27.50±0.01 ml 26.70±0.01 ml
Initial reading (ml) 0.90±0.01 ml 2.10±0.01 ml 1.30±0.01 ml
Volume of titrant (ml) 25.50±0.01 ml 25.40±0.01 ml 25.40±0.01 ml
Color of analyte after titration Orange Orange Orange
Moles of Na2CO3 used (mol) 1.2363×10-3 mol 1.2363×10 mol-3
1.2363×10-3 mol
Moles of HCl used (mol) 2.4725×10-3 mol 2.4725×10-3 mol 2.4725×10-3 mol
Molarity of std HCl (M) 0.09696 M 0.09734 M 0.09734 M
Mean and standard deviation 0.0972±0.0002 M
Percent error (%) 2.79 %

Table 1.2 shows the results and data obtained on the direct acid-base titration of
standardized HCl against Na2CO3. The color yellow analyte (Na2CO3 solution) which is
caused by the addition of methyl orange indicator, turned to color orange after it was being
titrated with HCl. Equivalence point was reached as orange-colored solution was observed.

The following are the calculated molarities of HCl for three trials: 0.09696, 0.09734
and 0.09734 M. It has an average or mean of 0.0972 M. Its calculated standard deviation is
0.0002 and has a percent error of 2.79 %. Thus, the obtained data has a high degree of
precision considering its calculated standard deviation which is <1, but a less accurate one
since its percent error falls to more than 1. The possible source of its error may be on the
dissolving part.
 Chapter IV

Summary and Conclusions

The concentration of NaOH analysis is determined by using the NaOH solution to

titrate an exactly known mass of primary standard potassium hydrogen phthalate or KHP.
When sodium hydroxide reacts with potassium acid phthalate, it yields to water and
NaKC8H4O4. The end-point is mark by using phenolphthalein as indicator. Sodium carbonate
(anhydrous) is a suitable chemical for preparing a standard solution as a primary standard.
The molarity of the given HCl can be obtained through titrating it against the standard
sodium carbonate solution prepared. Hydrochloric acid when reacts with sodium carbonate
will gives sodium chloride, carbon dioxide and water. The end-point is marked by using
methyl orange as an indicator.

The calculated concentration of the standardized NaOH for the three trials has an
average of 0.0987 M. It has standard deviation of 0.0011 and a percent error of 1.29%. This
indicates that the data obtained shows a high degree of precision since its standard deviation
is less than 1 but do not possess a high degree of accuracy since it percent error exceeds to 1.
On the other part, the calculated concentration of the standardized HCl for the three trials has
an average of 0.0972 M. It has a standard deviation of 0.0002 and a percent error of 2.79%.
Thus, the data obtained is a precise one but less accurate since its percent error is more than
1.

From the activity, we’re able to demonstrate the most common method for obtaining
standard solutions for titrimetric analysis, prepare solution that has the approximate
concentration desired, determine the concentration of sodium hydroxide to the standard
solution by direct titration against a primary standard. The concentration of sodium hydroxide
is 0.0987 M in which it has a percent error of 1.29%. This error might be due to the possible
errors encountered upon doing the dissolving part.
 Appendix

Solving for the Moles of NaOH:

Given: wt KHP = 0.5152 g; FW KHP = 204.2283 g/mol

Solution:
1 𝑚𝑜𝑙 𝐾𝐻𝑃 1 𝑚𝑜𝑙 𝑁𝑎𝑂𝐻
mol NaOH = 0.5152 g KHP × ×
204.2283 𝑔 1 𝑚𝑜𝑙 𝐾𝐻𝑃

= 2.523 ×10-3 mol NaOH

Solving for the Concentration of Standardized NaOH:

Given: mol NaOH= 2.523 ×10-3 mol; volume of titrant = 25.25 ml

Solution:
2.523 ×10−3 mol
MNaOH =
0.02525 𝐿

= 0.0999 M NaOH

Solving for the Moles of HCl:

Given: wt Na2CO3= 0.131035 g; FW Na2CO3= 105.99 g/mol

Solution:
1 𝑚𝑜𝑙 Na2CO3 2 𝑚𝑜𝑙 𝐻𝐶𝑙
mol HCl = 0.131035 g × ×
105.99 𝑔 1 𝑚𝑜𝑙 Na2CO3

= 2.47259 ×10-3 mol HCl

Solving for the concentration of Standardized HCl:

Given: mol HCl= 2.4725×10-3 mol; volume of titrant = 25.50

Solution:
2.4725×10−3 mol
MHCl =
0.02550 𝐿
 = 0.09696 M HCl

Reference

http://dramarnathgiri.blogspot.com/2012/06/preparation-and-standardization-of.html

http://www.chem.sc.edu/analytical/chem321l/labs/expt4.pdf

http://www.studymode.com/essays/Solution-Preparation-And-Standardization-1390691.html

http://www.yahooanswers.com/Preparation-and-standardization.html