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Week 5 to 7 1211 Equivalent Weight Determination

Dr. Urmi Doshi

Determination of the Equivalent weight of the Unknown acid RCOOH


3 PARTS (Performed over 3-week period, i.e. 1 part in each of the three labs)

Useful Definitions
Acid: A compound that ionizes in water to produce H+ (hydrogen) ions. OR A compound that
increases the concentration of H+ ions that are present when added to water.
Examples
[Note - aq: aqueous phase; (s): solid phase; (g): gas phase]

HCl: Hydrochloric acid


HCl(aq) H+(aq) + Cl-(aq)
___________________________

Carboxylic acid
RCOOH(s)

RCOO-(aq) + H+(aq)

______________________________

H2SO4 : Sulfuric acid


H2SO4(aq) 2H+(aq) + SO4-(aq)
______________________________

Examples of common household acids : Vinegar (Acetic acid); Lemon & Orange Juice (Citric acid);
Aspirin (acetyl salicylic acid)
Base: A compound that ionizes to produce OH- (hydroxide) ions. OR A compound that increases
the concentration of OH- ions that are present when added to water.
Examples
NaOH: Sodium Hydroxide
NaOH(s) Na+(aq) + OH-(aq)
_______________________________________

Week 5 to 7 1211 Equivalent Weight Determination

Dr. Urmi Doshi

Mg(OH)2: Magnesium Hydroxide


Mg(OH)2(s) Mg2+(aq) + 2OH-(aq)
___________________________________________

Examples of common household bases : Windex (ammonia); Baking powder (sodium carbonate),
Milk of magnesia (magnesium hydroxide)

Neutralization: It is a reaction in which when an acid and a base are added together, they react
with each other to form salt and water. The properties of the acid and base are neutralized, i.e. no
net increase in H+ or OH- ions.
HCl(aq) + NaOH(aq) NaCl(aq) + H2O(l)
ACID

BASE

SALT

WATER

Neutralization reaction is quantitative, i.e. the amount of acid and base that react with each other
depends on the balanced equation (equal number of each type of atoms on either side of the
equation).

Acid-Base Titration: A method to determine the concentration of an acid or base by neutralizing it


with a base or an acid, respectively of known concentration.
Acid
+
Base

Salt
+
Water
For example, the concentration of the acid is known, volume of acid used is known, concentration
of the base is not known and the volume of the base needed to neutralize the acid is obtained from
titration.

Standard in acid-base titration: A compound that can be measured accurately (so that its
number of moles or concentration can be calculated accurately) and thus help in determining the
number of moles (or concentration) of another compound with which it reacts in an acid-base
titration.

Equivalence point: Equivalence point or stoichiometric point is the point in titration when the
amount of acid ( or base) added is enough to completely neutralize the base ( or acid). OR when
chemically equivalent quantities of acid and base are added.
Indicator: A compound that is added in the beginning of titration. It changes color in response to a
chemical reaction. The change in color of the indicator helps in visualizing the end-point of titration.
Example: phenolphthalein is colorless in acidic and neutral conditions but changes to fuchsia (pink)
color in basic conditions
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Week 5 to 7 1211 Equivalent Weight Determination

Dr. Urmi Doshi

End-point: When the indicator changes color, the end point of the titration is reached.
Equivalence point can be different from end-point, as the former is determined from the
stoichiometry of the reaction.

Molarity:
1. Molarity = weight in grams / Molecular weight
2. Molarity = number of moles of solute/ 1 liter of solution

Equivalent Weight: Equivalent weight of an acid is the mass of acid required to generate 1 mole
of H+ ions in aqueous solution. Equivalent weight of a base is the mass of the base required to
generate 1 mole of OH- ions in aqueous solution.
Example
HCl(aq) H+(aq) + Cl-(aq)
1 mole of HCl (i.e. 36.5 g[1.01 + 35.45]) generates 1 mole of H+ ions
Equivalent weight of HCl = 36.5 g / 1 = 36.5 g
__________________________________________
H2SO4(aq) 2H+(aq) + SO4-(aq)
1 mole of H2SO4(i.e. (1.01x2)+32.07+(16x4) = 98.1 g) generates 2 moles of H+ ions
Equivalent weight of H2SO4 = 98.1 g / 2 = 49.05 g

Week 5 to 7 1211 Equivalent Weight Determination

Dr. Urmi Doshi

Part I: Standardization of NaOH

Theory: KHP is
or KHC8H4O4 is the monopotassium salt of phthalic acid. It is solid and
can be weighed accurately. Therefore, it is used as a primary standard in acid-base titrations.
NaOH solution cannot be prepared by measuring exact mass because solid NaOH is highly
reactive. Using a known concentration of KHP, we will titrate NaOH of approximate concentration.
From the volume of KHP required to neutralize NaOH and its known concentration, the actual
concentration of NaOH will be determined (i.e. NaOH solution will be standardized). This
standardized NaOH solution will be used to determine the exact molarity of HCl in Part II.
KHC8H4O4 + NaOH KNaC8H4O4 + H2O
Chemicals: NaOH (Sodium hydroxide), KHP (Potassium hydrogen phthalate), Deionized (DI)
water, Indicator (phenolphthalein)
Materials: 1 1-L(1000ml) bottle with cap, Erlenmeyer flask, Burette
Procedure:
1. Prepare NaOH solution (900 ml of approximately 0.1 M)
1 mole of NaOH has a mass of 40 g. 1 M NaOH solution contains 40 g of NaOH in 1 liter of
water. To prepare 0.1 M NaOH, one will need 4 g of solid NaOH in 1 liter of DI water. Therefore
for 900 ml, one will need 3.6 g of NaOH. Weigh 3.6 g of solid NaOH using one-place electronic
balance and place in a clean and dry 1-liter bottle. Add around 500 ml of DI water, put the cap
on and shake well to completely dissolve the solid NaOH. Make the volume to 900 ml by
adding the remaining 400 ml DI water. Shake well. Keep the cap on to avoid evaporation of
water and thus change in concentration. Shake the bottle well before each use. Do not waste
the NaOH solution as you will need to perform several titrations with this 900 ml in subsequent
labs.
2. Prepare KHP solution
Weigh by difference 0.3 g of dried KHP (solid acid in the oven cooled to room temperature)
using analytical balance and place in a clean Erlenmeyer flask. Rinse out the weighing boat
with DI water into the flask to get all of the KHP in the flask. Pour 20 ml of DI water and dissolve
KHP. If necessary, use a hot water bath to dissolve KHP and add more 20 ml of water (No
boiling, only gentle heating). Cool to room temperature before you use KHP solution for
titration. Add 1 drop of phenolphthalein indicator.
Note: Prepare KHP solutions 3 times in a clean dry flask by repeating the above procedure.

Week 5 to 7 1211 Equivalent Weight Determination

Trial 1

Dr. Urmi Doshi

Trial 2

Trial 3

Mass of Weighing
Dish (g)
Mass of Weighing
Dish + KHP (g)
Mass of KHP (g)

3. Titrate NaOH with KHP


Rinse a well-cleaned burette with about 5ml of the prepared NaOH solution three times. Fill the
burette with NaOH solution using a funnel. Make sure the burette is not leaking and to remove
any air bubbles. Record the initial reading to 2 places after the decimal (e.g. 5.75 ml, the
markings on the burette lets you read 5.7 ml, the number in the 2 nd decimal place is estimated).
Titrate the KHP solution in the Erlenmeyer flask with the NaOH solution in the burette as
follows:
Open the tap and add a small amount of NaOH solution to the flask.
Swirl the flask or Use a magnetic stirrer in the flask to mix the KHP and NaOH
solutions.
Continue adding small amounts (around 0.5 ml) of NaOH with constant stirring until
the color of the solution changes to pink momentarily and becomes colorless after 10
seconds. When after adding NaOH the drop in the flask turns pink, SLOW DOWN the
speed of adding NaOH because you are near the end-point. Now add NaOH drop wise
and touch the tip of the burette with the flask so that the drop of NaOH falls in the
flask. Rinse with a small amount of DI water using a dropper (or pipettor) to wash the
drop down the flask. Sometimes you will need to further slow down the speed of
adding NaOH such that you add half a drop at a time. When the color of the solution
remains pale pink for more than 20 seconds the end-point is reached. If the solution
turns dark pink, it indicates you overshot the end-point and you will need to repeat the
titration. Figure 1 illustrates the different stages during the titration. Once the end point
Figure 1. Titration of an acid and a base
using phenolphthalein indicator

is reached (pale pink colored solution), record the final reading and the color of the
solution in the flask.
Record all your readings in the DATA TABLES
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Week 5 to 7 1211 Equivalent Weight Determination

Dr. Urmi Doshi

Repeat Steps 2 and 3 until you get 3 GOOD trials [i.e. % deviation (see
Calculations below) should be less than 0.75%]
Only if needed

Trial 1

Trial 2

Trial 3

Trial 4

Trial 5

Initial Reading
Final Reading
Volume of
NaOH (ml)
used
Calculations:
KHC8H4O4 + NaOH KNaC8H4O4 + H2O
1 mole of KHP reacts with 1 mole of NaOH to generate 1 mole of salt and 1 mole of water
Therefore, the stoichiometric ratio of acid to base is 1:1 in this reaction.
Molecular weight of KHP = 202.24 g/mol
1.
2.
3.
4.

Calculate the moles of KHP titrated


Determine the moles of NaOH that reacted
Calculate the volume of NaOH required to titrate KHP
Calculate the exact concentration of NaOH solution in Molarity (you know the number of
moles and volume of NaOH from 2 and 3)
5. Error analysis: Calculate % deviation in Molarity of NaOH

Trial 1
Molarity of NaOH
Average Molarity:
M or mol/lit

Trial 2

Trial 3

Deviation from
Average

Average deviation in Molarity of NaOH = (|


| + | | + | |)/3
% Deviation in Molarity of NaOH = (Average Deviation / Average Molarity) X 100
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Week 5 to 7 1211 Equivalent Weight Determination

Dr. Urmi Doshi

Part II: Determination of accurate Molarity of HCl


Theory: Titrate a base NaOH) of known concentration with an acid (HCl) of approximate /
unknown concentration.
HCl(aq) + NaOH(aq) NaCl(aq) + H2O(l)
HCl reacts with NaOH in a 1:1 stoichiometric ratio
Chemicals: Standardized NaOH solution (From Part I), HCl solution, Deionized (DI) water,
Indicator (phenolphthalein)
Materials: 1 500ml bottle with cap, Erlenmeyer flask, Burette
Procedure:
1. Obtain HCl:
Deliver 10.00 ml of HCl solution of unknown concentration using an automatic pipettor into a
clean and dry Erlenmeyer flask. Record in your notebook the number of the container from
which you pipetted HCl.
2. Titrate HCl with standardized NaOH (from Part I)
Add 20 ml of DI water into the flask. Add a drop of phenolphthalein indicator. Fill the burette
with standardized NaOH and follow the steps of titration as given in Part I.3 (i.e. titrate
NaOH with KHP). Please note, here the acid in the flask is HCl, unlike KHP in Part I. Note
your readings in the data table below. Perform three trials and more, if needed.
Only if needed

Trial 1

Trial 2

Trial 3

Trial 4

Trial 5

Initial Reading
Final Reading
Volume of
NaOH (ml)
used
3. Calculate the ratio Volume of NaOH/ Volume of HCl. Calculate the average ratio and
average deviation. The % average deviation should be less than 0.5%. If not, repeat
titrations until you get consistent results.
4. Calculate molarity of HCl and perform error analysis (i.e. calculate % deviation). % deviation
should be less than 0.75%.
Molarity of HCl = (Average Molarity of NaOH * Volume of NaOH used for titration) /Volume
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Week 5 to 7 1211 Equivalent Weight Determination

Dr. Urmi Doshi

of HCl [i.e.10.00 ml]

Part III: Determination of equivalent weight of the unknown acid RCOOH


Theory: Titrate a base NaOH) of known concentration with an unknown acid (RCOOH) of
unknown concentration.
RCOO-Na+(aq) + H2O(l)

RCOOH(aq) + NaOH(aq)

Chemicals: Standardized NaOH solution (From Part I), RCOOH (Pure, dry, unknown acid you
obtained), Deionized (DI) water, Indicator (phenolphthalein)
Materials: Erlenmeyer flask, Burette
Procedure:
1. Prepare RCOOH solution
Weigh by difference 0.3 g of solid, dry RCOOH using analytical balance and place in a clean
Erlenmeyer flask. Rinse out the weighing boat with DI water into the flask to get all solid acid in
the flask. Pour 50 ml of the solvent that dissolves your RCOOH acid (you identified the solvent,
for example 25%, 50%, 75%, or 100% ethanol, in the previous experiment (Section V.C of the
lab manual)). If necessary, use a hot water bath to dissolve RCOOH (No boiling, only gentle
heating). Cool to room temperature before you use RCOOH solution for titration. Add 1 drop of
phenolphthalein indicator.
2. Titrate RCOOH with the standardized NaOH
Fill the burette with standardized NaOH and follow the steps of titration as given in Part I.3 (i.e.
titrate NaOH with KHP). Please note, here the acid in the flask is RCOOH, unlike KHP in Part I.
Note your readings in the data table below. Perform three trials.
Only if needed
Trial 1

Trial 2

Trial 3

Trial 4

Trial 5

Initial Reading
Final Reading
Volume of
NaOH (ml)
used
3. Calculate Equivalent weight of RCOOH
Equivalent weight of acid = Weight of acid in grams / (Molarity of NaOH x Volume of NaOH
used in liters)
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Week 5 to 7 1211 Equivalent Weight Determination

Dr. Urmi Doshi

4. Perform error analysis (% deviation should be less than 0.75%)


5. Submit completed Report Sheets on NaOH molarity, HCl molarity on page 87 and
Equivalent weight on page 89 NO LATER THAN MARCH 10.

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