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Experiment 4

This experiment determines the percentage of ammonia in household ammonia solution through back titration. [1] Ammonia solution is reacted with excess hydrochloric acid. [2] The excess HCl is then back titrated with a standardized sodium hydroxide solution. [3] Calculations using the titration data allow the moles and mass of ammonia originally present to be determined, from which the percentage of ammonia in the solution can be calculated.

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Tèddy Ñawå
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238 views

Experiment 4

This experiment determines the percentage of ammonia in household ammonia solution through back titration. [1] Ammonia solution is reacted with excess hydrochloric acid. [2] The excess HCl is then back titrated with a standardized sodium hydroxide solution. [3] Calculations using the titration data allow the moles and mass of ammonia originally present to be determined, from which the percentage of ammonia in the solution can be calculated.

Uploaded by

Tèddy Ñawå
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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EXPERIMENT 4: DETERMINATION OF PERCENT AMMONIA IN HOUSEHOLD

AMMONIA - BACK TITRATION

1. Introduction

Volumetric titration is an analytical method of measuring the volume of a solution of


known concentration required to react completely with an analyte (solution being
analyzed). In normal (forward) titration, the concentration of the analyte is
determined from the titration reaction, In Back titration method the analyte (which is
the limiting reagent) is not determined from the titration reaction, but by working
back to the original reaction, hence the type of titration method is called back
titration.
In volumetric usually primary and secondary standards are used. The concentration of
the primary standards are accurately known as it is prepared from compounds of high
purity and the solution is stable over a reasonable time. The secondary standards
usually used in volumetric analysis are standardized using primary standards.

In this experiment, ammonia solution, which is the limiting, reacts completely with
HCl (excess reagent) in reaction:

NH 3 (aq )  HCl(aq )  NH 4 Cl(aq )


analyte excessreagent
Thee titration reaction is
HCl(aq )  NaOH (aq )  NaCl (aq )  H 2 O(l)
excess s tan dard

n NaOH n HCL, excess



1 1
where n NaOH  M NaOH VNaOH .

Working backward in the originalreaction, number of moles of HCl that reacted


completely withNH3in 1:1 mole ratio is

1
n HCl, reacted  n HCl, initial  n HCl, titrated

From the above equation the concentration, mass, and percent by mass of ammonia in
ammonia solution assuming density of ammonia solution is 1.00 g/cm3.

In titration, indicators, which are organic weak acids are used. The indicator,
HIn,partially dissociate into ion, in an equilibrium reaction:

HIn (aq )  H 2 O(l) H 3 O  (aq )  In  (aq}


⇌
Colour1 Colour 2
According to Le Chatelierprinciple,In an acidic medium ( H+)the equilibrium
composition shifts to the reactant side and we observe colour 1 of HIn. Atthe
stoichiometric point, adding one –two drops of the basic medium (OH-) we reach the
end-point. At the end-point onwards the equilibrium composition shifts to the product
side, we observe colour 2 of In-., Therefore determining the end-point is very crucial
in volumetric titration analysis.

2. Materials

25 cm3 pipette, 10 cm3 pipette, 50 cm3 burette, 250 cm3 conical flasks 250 cm3
volumetric flask , small funnel
Chemicals: Aqueous HCl. And NaOH solution, Household ammonia solution,
phenolphthalein indicator
3. Procedure

Part 1:StardardizedHCl and NaOH solutions


The technicians will provide to you the concentrations of HCl and NaOH solutions

Part 2: Determination of the concentration of Ammonia in household ammonia

(a) Pipette 5.00 cm3 of the ammonia solution into a 250 mL conical flask, and pipette
25.00 mL of 0.1000M HCl and add it to ammonia solution.

2
(b) Allow the mixture to react for about 5 minutes by shaking the flask slightly.
(c} Add 2-3 drops of phenolphthalein indicator.
(d) Clean the burette with distilled water and finally rinse it abo 10.00 mL of 0.1000
M NaOH solution
(e) Close the stop coke of the burette and clamp it to the stand gently, and fill it with
NaOH solution.
(f) Perform a trial titration until you reach the end point (the point when the colour of
the indicator just turns purple). Record your as shown below in the Results and
Data Section.

Tabe 1: Titration of HCl with 0.1000 NaOH


Accurate titration
Trial 1 2 3
mL mL mL
Final volume of NaOH
Initial volome of NaOH
Titre volume of NaOH
Mean titrevolune

(g) Repeat steps (a) – (f) to obtain 3 accurate titrations


(h) Clean thoroughly the conical flask with water then with distilled after each
titration.

Some additional notes on the use of volumetric glassware and titrations:

(1). All volumetric glassware (pipettes, burettes and volumetric flasks)


should be thoroughly rinsed b after use, first with tap water, then with distilled
water.

(2). When pipetting, always keep the tip of the pipette immersed in the

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liquid, otherwise air will be sucked in and the liquid will enter the pipette filler.

(3). Taking the reading on the burette:

(i). Use the bottom of the meniscus for volume readings. The
bottom is often more clearly seen when an opaque piece of paper is held
behind the graduation marks.
(ii). The eye must be level with the liquid when taking a reading,
Otherwise an error due to parallax will arise. (If the eye is above the
liquid level, too small a volume reading will be made; if the eye is below
the liquid level, too large a volume reading will result.)

(iii). If the volume reading cannot be made comfortably while


standing on the floor, do not climb on a stool (as you may fall). Instead,
bring the burette stand down to the seat of the stool before taking the
reading.

(4). Volumes smaller than a normal drop can be added from the burette:
allow a small volume of solution to form on the burette tip, and then touch the tip
to the wall of the flask. Rinse this drop into the bulk of the liquid by using a
wash bottle with distilled water. Note that this does not affect the titration, as the
addition of distilled water will not change the no. of moles of solute in the flask.
(Note that a drop formed at the tip after the end point has been reached will
introduce an error.)

4. Results and Data Analysis

(1) Calculate moles NaOH titrated. Use the mean titre.


(2) Determine excess mole of HCL.
(3) Find moles HCl that reacted with NH3.

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(4) Calculate mass of NH3 and percent NH3 in ammonia solution.

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