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# 1.

LAB 1
DETERMINATION OF THE CONCENTRATION OF ACETIC ACID IN VINEGAR
1.1 Introduction
Concentration of solution is the amount of solute in a given amount os solvent. A concentrated
solution contains relatively large quantity of solute in a given amount of solvent. Dilute solutions
contain relatively little solute in a given amount of solvent. There are 2 specifics term to express
concenrtation, which is molarity and percent by mass.
Molarity is the number of moles of solute per liter of solution.
Molarity ( M )

moles of solute
liter of solution

(Equation 1-1)

Percent by mass is the mass in grmas of solute per 100 grams of solution
Percent solute

grams of solute
x 100%
grams of solution

(Equation 1-2)

Vinegar is a dilute solution of acitic acid. The molecular formula for acetic acid is CH3COOH.
Both molarity and percent by mass of aceric acid in a vinegar solution can be determine by
performing a titration. A titration is a process in which small increments of a solution of known
concerntration are added to a specific volume of a solution of unknown concerntration until the
stoichiometry for that reaction is attained. Knowing the quantity of the known solution required
to complete the titration, calculation of the unknown solution ca be done. The purpose of titration
is to determine the equivalance point of the reaction. The equivalance point is reach when the
added quantity of one reactant is the exact amount necessary for stoichiometric reaction with
another reactant.

1.2 Objectives
To :
(a)

Determine the morality of a solution and the percent by mass of acetic acid in vinegar by

## titration with the standardized sodium hydroxide solution.

1.3 Theory
In the titration process, a burette is used to dispense a small, quantifiable increment of solution of
known concentration (Figure 1.1). A typical burette has the smallest calibration unit of 0.1mL
(Figure 1.2), therefore, volume dispense from the burette should be estimated to the nearest
0.01mL.

Figure 1-1: a) Depicts a typical 50-mL burette. b) Indicates smallest calibration unit, 0.1mL, on a typical 50 mL
burette

In this experiment, the equivalence point occurs when the moles of acid in the solution equals to
the moles of base added in the titration. For example, the stoichiometric amount of 1 mole of the
strong base, sodium hydroxide (NaOH), is necessary to neutralize 1 mole of the weak acid, acetic
acid (CH3CO2H), as indicated in equation 3.
NaOH (aq) + CH3CO2H(aq) NaCH3CO2 (aq) + H2O (l)

(Equation 1-3)

The sudden change in the pH of the solution shows that the titration has reached the equivalence
point. pH in an aqueous solution is related to its hydrogen ion concentration. Symbolically, the
hydrogen ion concentration is written as [H3O+]. pH is defined as the negative of the logarithm
of the hydrogen ion concentration.
pH = - log [H30+]

(Equation 1-4)

pH scale is a method of expressing the acidity or basicity of a solution. Solutions having a pH <
7 are acidic, pH = 7 are neutral, pH > 7 are basic. For example, a solution having [H 30+]= 2.35 x
10-2 M would have a pH of 1.629 and is acidic. Ph electrode will be used in this experiment. The
titration is initiated by inserting a pH electrode into a beaker containing the acid solution (pH
within 3-5). As sodium hydroxide, NaOH, is incrementally added to the acid solution, some of
the hydrogen ions will be neutralized. As the hydrogen ion concentration decreases, the pH of
the solution will gradually increase. When sufficient NaOH is added to completely neutralize the
acid (most of the H3O+ ions are removed from the solution), the next drop of NaOH added will
cause a sudden sharp increase in pH (figure 2-2). The volume of based required to completely
neutralized the acid is determine at the equivalence point of titration.

Figure 1-2: Acid-base titration curve of weak acid titrated with NaOH.

In this experiment, titration of vinegar sample with a standardized sodium hydroxide solution
will be done. To standardize the sodium hydroxide solution, of a primary standard acid solution
is initially prepared. In general, primary standard solutions are produce by dissolving a weighed

quantity of pure acid or base in a known volume of solution. Primary standard acid or bases have
several common characteristics:

## they must be soluble in the solvent of interest

Potassium hydrogen phthalate KHC8H4O4, and oxalic acid, (COOH)2, are common primary
standard acid. Sodium carbonate, Na2CO3, is the most commonly used based. Most acids and
bases (e.g. HCl, CH3COOH, NaOH, and KOH) are most available as primary standard. To
standardize one of these acid or based solutions, titration of the solution with a primary standard
should be done. In this experiment, NaOH solution will be titrated with potassium hydrogen
phthalate (KHP). The equation for this reaction will be:
KHC8H4O4 (aq) + NaOH (aq) KNaC8H4O4 (aq) + H2O (l)

(Equation 1-5)

Once the sodium hydroxide solution has beeb standardizes, it will be used to titrate 10.00mL
aliquots of vinegar. The equation for the reaction of vinegar with NaOH is
CH3COOH(aq) + NaOH(aq) NaCH3COO (aq) + H2O(l)

(Equation 1-6)

Knowing the standardized NaOH concentration and using equation 6, we can determine the
molarity and percent by mass of acetic acid in the vinegar solution.
Sample calculation for standardizing a based with KHP
Figure 3 depicts the titration curve of 1.523 grams of KHP dissolved in20.0mL of distilled water
titrated with NaOH. Determine the molarity of the NaOH solution.

Figure 1-3: titration curve of KHP with NaOH. The volume of NaOH used at the equivalence point is 15.3 mL of
NaOH.

## Calculate the moles of KHP used in the titration.

1.523 g KHC 8 H 4O 4 x

From equation 5, calculate the moles of NaOH required neutralizing the moles of KHP.

## 0.007458 mol KHP x

1 mol KHC 8 H 4O 4
0.007458 mol KHC 8 H 4O 4
204.2 g KHC 8 H 4O 4

1 mol NaOH
0.007458 mol NaOH
1 mol KHP

## Calculate the molarity of the NaOH solution.

15.30 mL NaOH x

1L
0.01530 L NaOH
1000 mL

mol NaOH
0.007458 mol NaOH 0.04875 mol NaOH

0.4875 M NaOH
L of solution
0.01530 L solution
L solution

Sample calculations for determining the acetic acid concentration in vinegar by titration with
standard base
A 10.00 mL aliquot of vinegar requires 16.95 mL of the 0.4875 M standardized NaOH solution
to reach the equivalence point of the titration. Calculate the molarity and the percent by mass of
CH3COOH in the solution. Assume the density of the vinegar solution is 1.00g/mL.

## Calculate the moles of NaOH that reacted.

16.95 mL NaOH x

1L
0.01695 L NaOH
1000 mL

0.01695 L NaOH x

0.4875mol NaOH
0.008263 mol NaOH
1 L NaOH solution

## Calculate the molarity of the CH3COOH solution

10 mL CH 3COOH x

1 mol CH 3COOH
0.008263 mol NaOH
1 mol NaOH

1L
0.010 L CH 3COOH solution
1000 mL

## mol CH 3COOH 0.008263 mol CH 3COOH 0.8263 mol CH 3COOH

0.8263 M CH 3COOH
L of solution
0.01 L solution
L solution

## Calculate the mass of acetic acid in the solution

10 mL CH 3COOH x

1L
0.010 L CH 3COOH solution
1000 mL

0.01 L CH 3COOH x

## 0.8263 mol CH 3COOH 60.06 g CH 3COOH

x
0.4963 g CH 3COOH
1 L solution
1 mol CH 3COOH

## Calculate the mass of the acetic acid solution

10 mL CH 3COOH solution x

1 g CH 3COOH solution
10.00 g CH 3COOH solution
1 mL CH 3COOH solution

## Calculate the percent by mass of acetic acid in the solution

g CH 3COOH
x100 %
g CH 3COOH solution
0.4693 g CH 3COOH
percent mass CH 3COOH
x100 % 1.963% CH 3COOH
10.00 g CH 3COOH
percent mass CH 3COOH

1.4 Procedure
1.4.1 Standardization of sodium hydroxide solution
1. Prepare 250 mL of approximately 0.6 M sodium hydroxide solution from NaOH
solid. The solution can be prepared in a beaker, and check the calculation with the
laboratory instructor prior to preparing the solution. Record your calculation.
2. Weight a 250 mL beaker and record the mass to the nearest 0.001g. Add 1.5 grams
of KHP to the beaker. Record the mass of the beaker and KHP to the nearest 0.001 g.
calculates the mass of KHP by difference and record the data. Add 30mL of distilled
water to the beaker. Stir the solution until the KHP has dissolved completely.
3. titrate this solution with NaOH and record the pH with 1 ml additions of NaOH
solution.
4. Repeat steps 1 to 3 to perform a second and third trial to standardize the NaOH
solution.
4. Plots the graph of pH versus NaOH. From the plots, determine the volume of
NaOH required neutralizing the KHP solution in each titration.
6. Calculate the molarity of sodium hydroxide for titration 1 and 2.
7. Calculate the average morality of sodium hydroxide solution for titration 1 and 2.
The resulting sodium hydroxide concentration will be used in part B of the
experiment.

## 1.4.2 Molarity of acetic acid and percent of vinegar

1. Transfer 10.00mL of vinegar to a clean, dry 250 mL beaker using a 10mL
volumetric pipette. . Add sufficient water, 75 to 100 mL, to cover the pH
electrode tip during the titration.
2. Add 1 ml of NaOH to the vinegar solution and record the pH
3. Repeat the above steps twice more
4. Plot the graph of pH vs volume NaOH added. And from the plots determine the
volume of NaOH required to neutralized vinegar in each titration. Record your data.
5. Calculate the molarity of acetic acid in vinegar for titration 1 and 2.
5. Calculate the average molarity of acetic acid fir each titration.
6. Calculate the percent by mass of acetic acid in vinegar for titration 1 and 2
7. Calculate the percent by mass of acetic acid in vinegar.

## 1.5 Result & Calculations

Standardization of sodium hydroxide solution

1.5.1

## 1. Calculations for preparing 150mL of approximately 0.6M sodium hydroxide

solution.
2.
Titration 1
Mass of beaker (g)
Mass of beaker + KHP (g)
Mass of KHP (g)
Volume of NaOH to neutralize
the KHP solution (mL)

Titration 2

## 3. Calculate the molarity of sodium hydroxide for each titration 1 and 2.

4. Calculate the average molarity of sodium hydroxide for each titration 1 and 2.

1.5.2

1.
Titration 1

Titration 1

Volume of
NaOH required
to neutralize
vinegar

## 2. Calculate the molarity of acetic acid in vinegar for titration 1 and 2.

3. Calculate the average molarity of acetic acid for each titration.
4. Calculate the % by mass of acetic acid in vinegar for titration 1 and 2.
5. Calculate the average percent by mass of acetic acid in vinegar.

## EXPERIMENT 2: DETERMINATION OF THE Ka VALUE OF A WEAK ACID

The relative acidity of a substance or a system is important in many situations, such as in the
quality of drinking water, food preservation, soil conditions for agriculture and physiological
functions. The strength of an acid is measured based on its ability to donate protons to base.
The acid ionization constant, Ka, is a quantitative measure of the strength of an acid. The Ka
value is a characteristic of an acid and can be used to identify an unknown acid. The Ka value
indicates the relative strength of an acid. The larger the Ka value, the stronger the acid and vice
versa.
You are given 10 ml of two unknown acid solutions and required to determine the acid ionization
constants, Ka of weak acid solutions by titration with 0.1 M sodium hydroxide, NaOH and by
measuring the pH of the weak acid. You are also required to identify the unknown weak acid
solutions from the calculated Ka values obtained during the experiment.
Based on the actual identity of the unknown weak acid solutions, you are required to evaluate
and compare which method is more accurate.

## EXPERIMENT 3: DETERMINATION OF CHROMIUM (VI) CONCENTRATIONS VIA

ABSORPTION SPECTROSCOPY

Many heavy metals, including chromium (Cr), are toxic even at low aqueous solution
concentrations. Chromium ions, Cr (III) or Cr (VI), are found naturally in rivers, lakes and
streams. Trivalent Cr (III) compounds are not usually considered as health hazards, but
hexavalent Cr (VI) compounds can be toxic if ingested or inhaled and have been established as
carcinogens.
You are required to determine the quantity of Cr (VI) present in a polluted water sample using
a spectrophotometer and a set of standard solutions. From your results you will conclude
whether the water sample is suitable for drinking and/or agricultural purposes.

## EXPERIMENT 4: BASIC WATER PROPERTIES 1

Oxygen saturation or dissolved oxygen (DO) is a relative measure of the amount of oxygen
dissolved in a medium. DO is naturally present in water and tends to be manipulated in
order to suit spesific applications; in drinking water a higher DO level improves the taste, but
at the expense of higher rates of pipe corrosion, consequently industry tends to minimise the
DO level to reduce maintenance costs.

You are required to determine the DO level in a series of water samples and ascertain
whether they comply with Malaysian Water Standards.

## EXPERIMENT 5: BASIC WATER PROPERTIES II

There are many chemicals present in water, not all of them are desirable. Chlorine is added
to water to kill bacteria which is good, but excessive quantities are hazardous to human
health. Iron from the degradation of pipes is inevitable and although its presence is not
hazardous to health, it does affect the taste of water and may discolour foods, which come in
contact with it. The presence of sulphates and phosphorous in water are a consequence of
using everyday items like cleaning products, which can pollute water supplies poisoning plant
and animal life.

You are required to determine the levels of chlorine (total and free), iron, sulphates and
phosphorous in a series of water samples and ascertain whether they comply with Malaysian
Water Standards.

2. LAB 6
SOAPS AND DETERGENT
2.1

Introduction

Soap is a generic term for the sodium or potassium salts of long-chain organic acids (fatty acids)
made from naturally occurring esters in animal fats and vegetable oils. All Organic acids contain
the RC02H functional group, where R is a shorthand notation for methyl, CH3-, ethyl CH3CH2-,
Propyl, CH3CH2CH2-, or more complex hydrocarbon chains called alkyl groups. Chemists use
the R shorthand notation because these groups can be very large and the hydrocarbon chain has
little effect on the compound's chemical reactivity. All esters contain the RC02R functional
group.
The R groups in soaps are hydrocarbon chains that generally contain 12 to18 carbon atoms.
Sodium fatty acids such as lauric (vegetable oil), palmitic (palm oil), and stearic (animal fat)
acids are just a few examples of soaps.
CH3(CH2)10COONa

sodium laurate

CH3(CH2)16COONa

sodium stearate

The hydrocarbon chain in soaps may contain saturated (no double bond) or unsaturated chains
(contains double bonds). Sodium salts are usually solid therefore; most bars of soap are of
sodium salts. Potassium salts are the basis of liquid soaps, shaving creams, and greases. Fats and
vegetable oils are triglycerides. Triglycerides in an ester derived from three fatty acids. A
triglyceride made from three lauric acid molecules is shown in Figure 6-1.
Saponification is the basic hydrolysis of an ester producing a carboxylic acid salt and an alcohol
(Eq.3-1) .A lone pair of electrons on the OH- is attracted to the partially positively charged C
atom in the C=O bond in the ester (Eq.6-1). The C-OR' bond breaks generating a carboxylic acid
(RC02H) and an alcohol (R'OH). In the presence of NaOH, carboxylic are converted to their
sodium salts (RCO2-Na+).

When a triglyceride is saponified, three fatty acid salts (soaps) and glycerol are produced as
shown in Equation 6-2. The R groups in the triglyceride may or may not have the same
chailength (same number of carbons).Thus, different types of soaps may be produced from the
saponification of a particular triglyceride.

Figure 6-1: A Triglyceride molecule made from lauric acid and glycerol

(Equation 6-1)

(Equation 6-2)

2.2 Objectives
To :
(a)

2.3

## Prepare soap and compare its properties to that of a synthetics detergent.

Theory

Soap is the salt of a weak acid. Most organic acids arc weak acids. Consequently, hydrolysis
occurs to some extent when soap dissolves in water. Soap solutions tend to be slightly alkaline
(basic) due to partial hydrolysis of the acid (Eq. 3).

(Equation 6-3)
The cleansing action of soaps results from two effects. Soaps are wetting agents that reduce the
surface tension of water, allowing the water molecules to encounter the dirty object. They are also
emulsifying agents. "Dirt" frequently consists of a grease or oil along with other organic species.
In general, organic compounds are nonpolar. Water is a polar species. These two substances will
not dissolve in each other because of their dissimilar characteristics (the "Like Dissolves Like"
rule). Soaps cross the boundary between polar and nonpolar because they contain a polar
hydrophobic (water- hating) end and a polar hydrophilic (water loving) end as shown in Figure
6-2.

Figure 6-2: Molecular structure, a) a line drawing, b) of sodium stearate. In a line drawing, all carbon and
hydrogen atoms are omitted at the intersection of each line as a shorthand method of drawing molecule. It is
understood that the C and H atoms are part of the molecule.

Because soaps have both polar and nonpolar region in the molecule, they are soluble in both
polar and nonpolar species. The hydrophobic
compound like grease

and

(nonpolar)

## oils. The hydrophilic (polar) end dissolves in water. Soap molecules

surround the grease and oils and break them up into microscopic droplets can remain suspended
in the water. These suspended microscopic droplets are called micelles (Figure 6-3). Micelles
contain very small amounts of oil or grease

in

## Figure 6-3: Formation of micelle

Water supplies in certain areas are acidic as a result of acid rain or pollution, or "hard" due to the
dissolved mineral content. Both acidic and "hard" water reduce the cleansing action of soap.
Soap is the salt of a weak acid. In the presence of a stronger acid, the sodium salt

is converted

to

(Equation 6-4)

3+

## , ions from the minerals that the water

passes over. Normally, soaps made from sodium and potassium fatty acid salts are soluble in

water. However, in the presence of these metal ions, the Na+ and K+ soluble salts convert to
insoluble Ca2+ , Mg2+ , and Fe 3+ salts (E q. 3-5).

(Equation 6-5)

In either acidic or "hard" water, the soluble soaps form insoluble salts that becomes a scummy
ring on bathtubs and black areas on shirt collars .The cleansing ability of soap is reduced because
soap molecules are removed from solution. There are several techniques used to circumvent the
problems generated by hard water. Water can be "softened" via removing hard water ions from
solution using ion exchange techniques or by adding water-softening agents, such as sodium
phosphate (Na3PO4) o rsodium carbonate (Na2CO3). Water-softening agents react with the Ca2+ ,
Mg2+ , and Fe 3+, removing them from water (Eq. 6-6 and 6-7) and preventing the reaction of these
ions with soap (Eq. 6-4 and 6-5).

(Equation 6-6)

(Equation 6-7)

Thus Syndets was design to overcome the soap problem with hard water. Syndets differ
from soaps in that the nonpolar fatty acids groups are replaced with alkyl or aryl sulfonic acids
(ROS03H). The alkyl or aryl sulfonic acids have long chains of carbon atoms giving the
hydrophobic (nonpolar) end. The salt of the sulfonic acid (sulfonate) group forms the hydrophilic
end of the molecule. The difference in polar groups is one of the key distinctions between a soap
and a synthetic detergent. Syndets form micelles and cleanse in the same manner as soaps. Two
examples of synthetic detergents are shown in Figure 6-4.

## Figure 2-4: Examples of synthetics detergents

Because sulfonic acid is a stronger acid than carboxylic acids, Syndets do not precipitate in
acidic solutions. Furthermore, alkyl and aryl sulfonates do not form insoluble salts in the
presence of the typical hard water ions. Thus, synthetic detergents remain soluble in both acidic
and "hard" water.

2.4 Procedure
2.4.1 Soap preparation
1. Place 25 mL of vegetable oil in a 250-mL Erlenmeyer flask. Add 20 mL of ethanol
and 25 mL of 6 M sodium hydroxide solution to the flask. Stir the mixture with d
stirring rod to mix the contents of the flask.
2. Heat the 250-mL flask in a boiling-water bath inside of a 600-mL beaker.
3. Stir the mixture continuously during the heating process to prevent the mixture
from foaming. If the mixture should foam to the point of nearly overflowing, remove
the flask from the boiling-water bath until the foaming subsides, then continue
heating. Heat the mixture for 20-30 minute or until the alcohol odor is no longer
detectable.
4. Remove the paste-like mixture from the boiling-water bath and cool the flask in an
ice bath for 10-15 minutes.

5. While the flask is cooling assemble the vacuum filtration apparatus shown in
Figure 3-5. Secure the vacuum flask to a ring stand with a utility clamp to pre-vent
the apparatus from toppling over.

## Figure 6-5: Vacuum Filtration apparatus

6. Weigh a piece of filter paper to the nearest 0.001 g and record the mass. Place the
filter paper inside the Buchner funnel. Moisten the paper with water so that it fits
flush in the bottom of the funnel.
7. Once the flask has cooled, add 150 mL of saturated sodium chloride (NaCl) solution
to the flask to "salt out" the soap.
8. Slowly turn on the water at the aspirator. Pour the mixture from the flask into the
Buchner funnel. Once all of the liquid has filtered through the funnel, wash the soap
with 10 mL of ice-cold water. Continue the suction filtration until

a11

of the water is

## removed from the soap.

9. Remove the soap from the funnel and press

it

## between two paper towels to dry it.

Weigh the filter paper and dried soap, and record the mass to the nearest 0.001 and
determine the mass of the soap by difference and record the mass.

## 2.4.2 Comparison of soap and detergent properties- precipitation and emulsification

1. Prepare a stock soap solution by dissolving 2g of your prepared soap in 100 mL of
boiling, distilled water. Stir the mixture until the soap has dissolved and allow the
solution to cool.
2. Repeat step 1 using 2 g of synthetic detergent (e.g., Dynamo). When both solutions
are cool, determine the pH of each solution using pH paper.
3. Label three test tubes as test tube 1, 2, and 3. Add 4 drops of mineral oil to each
test tube. Add -5 mL of distilled water to test tube 1. Add -5 mL of stock soap
solution to test tube 2. Add -5 mL of stock synthetic detergent to test tube 3.
4. Mix each solution by shaking and let stand for three to five minutes. Note which of
the solutions, if any, emulsifies the oil by forming a single layer.
5. Pour the mixtures into the Waste Container. Clean and dry the three test tubes.
6. Label three test tubes as test tube 1, 2, and 3. Place 2 mL of stock soap solution in
each of the three test tubes. Add 2 mL of 1% CaCl2 solution to test tube 1. Add 2 mL
of 1% MgC12 solution to test tube 2. Add 2 mL of l% FeCl2 solution to test tube 3.
Shake each test tube to mix the solutions. Record your observation.
7. Add 4 drops of mineral oil to each of the test tubes in Step 6. Shake each test tube to
mix the solutions and let the solutions stand for three five minutes. Note which of the
solutions, if any, emulsifies the oil by forming a single layer.
8. Repeat Steps 6-7 using -2 mL of stock detergent solution. Which solutions form a
precipitate?
9. Note which of the solutions, if any, emulsifies the oil by forming a single layer.
10. Pour the mixtures into the Waste Container. Clean and dry the test tube.
11. Place 5 ml, of stock soap solution in cine clean test tube and 5 rnL
detergent solution in a second test tube. Add 1 M HC1 one drop

at

of

stock

a time to both

## solutions until the pH in each test tube is equal to 3. (Use pH paper to

measure).Count the number of drops of acid added to each mixture. Does a precipitate
form in either mixture?
12. Add 1 drops of mineral oil to each test tube in Step

11.

## mix the solution. Is the oil emulsified in either mixture?.

2.4.3 Comparison of the cleaning abilities of a soap and detergent.
1. Clean, dry, and label three beakers. Place 20 mL of stock soap solution (from Step
1 in section 3.4.3) in the 1st beaker. Place 20 mL of stock detergent solution (from
Step 2 in section 6.4.4) in the 2nd beaker. Place 20 mL of a commercial liquid
Dynamo.
2. Obtain three cloth test strips that have been soaked in tomato sauce and place one
strip in each of the beakers. Place one cloth strip in beaker 1 (from above), one cloth
strip in beaker 2, and one cloth strip in beaker 3. Repeatedly stir each solution with a
stirring rod for 5 minutes.
3. Remove the cloth strips from the soap and detergent solution and squeeze out the
excess

## 2.5 Result & Calculations

2.5.1

Soap preparation
Mass of Filter (g)
Mass of filter paper
+ soap (g)
Mass

of

recovered (g)

soap

to

2.5.2

## Comparison of soap and detergent properties.

Brand name of
synthetics
detergent
pH

of

soap

solution
pH of synthetics
detergent
solution
Answer yes or no in the space provided below
System

Emulsification
Occurred

Distilled water
Soap
detergent

System

Precipitate
Soap

Oil emulsified
x

Soap

CaCl2
MgCl 2
FeCl3
Acidic

2.5.3

## Cleansing comparison of a soap and detergents

Visually compare each cloth strip to determine their relative cleanliness. Record your
observations.
Compare the cleansing ability of the two detergents.