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# 1.

LAB 1

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.

moles of solute
Molarity ( M )  (Equation 1-1)
liter of solution

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

grams of solute
Percent solute  x 100% (Equation 1-2)
grams of solution

Vinegar is a dilute solution of acitic acid. The molecular formula for acetic acid is CH 3COOH.
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 mol KHC 8 H 4O 4
1.523 g KHC 8 H 4O 4 x  0.007458 mol KHC 8 H 4O 4
204.2 g KHC 8 H 4O 4

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

1 mol NaOH
0.007458 mol KHP x  0.007458 mol NaOH
1 mol KHP

##  Calculate the molarity of the NaOH solution.

1L
15.30 mL NaOH x  0.01530 L NaOH
1000 mL

## mol NaOH 0.007458 mol NaOH 0.04875 mol NaOH

M    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.

1L
16.95 mL NaOH x  0.01695 L NaOH
1000 mL

0.4875mol NaOH
0.01695 L NaOH x  0.008263 mol NaOH
1 L NaOH solution

##  Calculate the moles of CH3COOH neutralized by the moles of NaOH

1 mol CH 3COOH
0.008263 mol NaOH x  0.008263 mol NaOH
1 mol NaOH

##  Calculate the molarity of the CH3COOH solution

1L
10 mL CH 3COOH x  0.010 L CH 3COOH solution
1000 mL

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

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

##  Calculate the mass of acetic acid in the solution

1L
10 mL CH 3COOH x  0.010 L CH 3COOH solution
1000 mL

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

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

##  Calculate the mass of the acetic acid solution

1 g CH 3COOH solution
10 mL CH 3COOH solution x  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
percent mass 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

1.4 Procedure

## 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.

## 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 average molarity of acetic acid fir each titration.

6. Calculate the percent by mass of acetic acid in vinegar for titration 1 and 2

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

solution.
2.
Titration 1 Titration 2

## Volume of NaOH to neutralize

the KHP solution (mL)
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 Standardization of sodium hydroxide solution

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, K a, is a quantitative measure of the strength of an acid. The K a
value is a characteristic of an acid and can be used to identify an unknown acid. The K a 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 K a 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.