Volumetric Analysis - The Dublin School of Grinds...Volumetric Analysis No part of this publication...

6th Year Chemistry

Higher Level Sinéad Nolan

Volumetric Analysis

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@Dublin School of Grinds Page 2 Sinéad Nolan

Table of Contents

Volumetric Analysis Procedures .................................................................................................. 3

Determination of the amount of water of crystallisation in hydrated Na2CO3 .................. 7

Determination of the concentration of ethanoic acid in vinegar ......................................... 9

Estimation of iron in an iron tablet ........................................................................................... 11

Iodine – thiosulphate titration ................................................................................................... 13

Determination of the percentage of hypochlorite in bleach ............................................... 15

Estimation of the total hardness of a water sample .............................................................. 17

Estimation of dissolved oxygen by redox titration ................................................................ 19

Past Exam Question 1’s ............................................................................................................... 21

Past Exam Solutions to Question 1’s ......................................................................................... 49


Volumetric Analysis Procedures

Primary standard

pure / stable / anhydrous (not hydrated) / no water loss (no efflorescence) / not

deliquescent / not hygroscopic /does not sublime / high molecular (molar) mass (Mr)

from which solutions of known concentration (molarity) can be made / no need to

standardise by titration / water soluble

NB Primary standard for acid-base reactions = anhydrous sodium carbonate (Na2CO

3)

[Allow (3) for sodium carbonate.]

[OTHER POSSIBILITY: sodium tetraborate (disodium tetraborate]

Primary standard for redox reactions = ammonium iron(II) sulphate

A standard solution is a solution whose concentration (molarity) is known

A standardised solution is a solution whose concentration (molarity) known (found, got,

etc.) by another titration (colorimetry, u.v. spectroscopy)

Making up a solution starting with a solid solute

rinse from clock glass into beaker containing deionised water //

stir // dissolve //

pour (add) through funnel into volumetric flask //

add rinsings of beaker //

add deionised water until bottom of meniscus on (level with) mark /

read at eye level //

stopper and invert* several times

[* Do not allow “shake” for “invert”]


Making up a solution with iron tablets

tablets crushed with mortar and pestle //

washed into beaker //

stirred to dissolve //

transferred into flask using funnel / glass rod //

rinsings of beaker added to flask //

flask on level surface / mark at eye-level //

add drop-by-drop / add using dropper (pipette, wash bottle) / top up carefully //

until bottom of meniscus level with mark //

invert / mix / shake [“swirl” not acceptable]

Diluting a solution of bleach or vinegar

pipette (burette) vinegar/bleach (3) can be shown on diagram

into volumetric flask (3) can be shown with diagram provided line on neck present

add deionised water (3)

when near mark, add dropwise (using dropper/pipette/wash bottle) / until bottom of

meniscus on (at) mark / read bottom of meniscus

Procedure for preparing the burette

rinse with deionised water

rinse with reagent (solution)

clamp vertically

use funnel when adding reagent / remove funnel after filling

open tap to fill below tap (tip, jet, nozzle) / remove air bubbles [Allow ‘tap is full’]

set bottom of meniscus on mark / read bottom of meniscus


Importance of filling the part below the tap

air will be displaced by the solution (reagent) / some of measured volume replaces air /

some of measured volume not delivered / some of measured volume goes to fill space /

causes (gives) wrong (inaccurate, too high, too low) reading (result, titre) / air will be

displaced (removed, got rid of) during the titration / will be filled during the titration /

affects result / burette only works properly when it (part below tap) is full / burette

designed to work properly when it (part below tap) is full / distorts result (reading)

Description of how the level of the liquid in the burette was adjusted to the zero mark

fill above mark and adjust with tap / fill to below mark and add dropwise

Procedure for preparing the pipette

rinse with water followed by the solution it is going to contain //

fill pipette using a pipette filler to above the mark (graduation line) //

adjust to have bottom of meniscus on mark / read at eye level (vertically)

remove droplets adhering to outside //

drain under gravity into titration flask //

touch tip of pipette against side of flask to add droplet adhering to outside tip // do

not blow out drop inside pipette

Importance of using a pipette filler

safety / avoid solution getting into mouth / hygiene

Explanation of operations involving the conical flask and its contents during the titration

swirl to mix //

allow time after addition from burette for reaction //

On white surface //

Wash down sides with deionised water (NB this does not affect number of mols of

reactants in the flask)


Importance of placing the conical flask on a white tile

so that colour-change (end-point) clearer (more easily seen)

Precautions (and explanation of how this precaution would have contributed to the

accuracy of the titration result) that should have been taken as the end point of the

titration was approached.

Precaution Explanation

add drop by drop (slowly) add dropwise so that end point will be

precisely (accurately) detected (correct

end point not passed) / one drop of

solution would change colour near

end point

wash down inner sides of conical flask wash sides so that all reagent(s) (acid)

in the reaction mixture

swirl (shake) flask contents swirl to ensure thorough mixing of

reactants


Determination of the amount of water of crystallisation in hydrated Na2CO3 (2006)

1Na2CO3 = 2HCl

1

25 x M =

2

26.05 x 0.11

M = 25 x 2

1 x 26.05 x 1 0.1

(i) M = 0.05731 mol L–1 (molarity of the Na2CO3 solution)

x 106 (Mr of Na2CO3)

(ii) = 6.075 g L–1 (concentration of the Na2CO3 solution in g L–1)

2 (solution only made up to 500 cm3)

= 3.0375 g of Na2CO3 in 500 cm3

Mass of water of crystallization in the crystals = mass of crystals – mass of Na2CO3 in 500

cm3

= 8.20 – 3.0375

= 5.1625 g

% by mass of water of crystallisation = crystals theof mass total

solution theof cm 500in water of mass 3

= 8.2

5.1625x

1

100

= 62.9 % (% by mass of water of crystallisation in

crystalline Na2CO3)

106

3.0375:

18

5.1625(divide by Mr)

0.0287 : 0.287

0.0287

0.0287:0.0287

0.287(divide by smallest number)

1 : 10


Notes

Indicator: methyl orange

Colour change at the end-point: yellow (base) to pink (acid)

Example of a strong acid – weak base titration

Methyl orange suitable as an indicator as the pH at the end point passes through the

indicator range

Not more than 1 – 2 drops of indicator should be used as indicators themselves are

weak acids or weak bases and may affect titration results if added in larger quantities


Determination of the concentration of ethanoic acid in vinegar (2008)

1CH3COOH = 1NaOH

1

22.65 x M =

1

25 x 0.1

M = 22.65 x 1

1 x 25 x 0.1

M = 0.11 mol L–1 (molarity of the diluted vinegar)

x 60 (Mr of CH3COOH)

= 6.6 g L–1 (concentration of the diluted vinegar in g L–1)

x 10 (dilution factor 25 cm3 to 250 cm3)

= 66 g L–1 (concentration of the original vinegar in g L–1)

x 10 (g L–1 to g 100 cm–3 = % (w/v))

= 6.6 % (w/v) (concentration of original vinegar in % (w/v))


Notes

The vinegar is diluted because it is too concentrated and there would have been a

very large volume of NaOH needed to get a reasonable titration and also it would

have required a very concentrated solution of NaOH for neutralisation

Indicator: phenolphthalein

Colour change at the end-point: pink (base) to colourless (acid)

Example of a weak acid – strong base titration

Phenolphthalein suitable as an indicator as the pH at the end point passes through

the indicator range

Ethanol in white wine is oxidised to ethanoic acid in vinegar

Methanoic acid is the acid which occurs in nettles and stinging ants

Benzoic acid and it’s salts are used as food preservatives, disinfectants, antiseptics,

biocides and fungicides

Not more than 1 – 2 drops of indicator should be used as indicators themselves are

weak acids or weak bases and may affect titration results if added in larger quantities


Estimation of iron in an iron tablet (2009)

5Fe2+ = 1MnO4-

5

25 x M =

1

18.75 x 0.1

M = 25 x 1

5 x 18.75 x 0.1

(i) M = 0.0375 mol L–1 (molarity of the Fe2+ solution)

4 (solution only made up to 250 cm3)

= 0.009375 mol 250 cm–3

x 56 (Ar of Fe)

(ii) = 0.525 g 250 cm–3 (total mass of iron in 250 cm3 of the solution)

5 x 0.325 = 1.625 g (mass of the 5 tablets)

% by mass of iron in the tablets = tablets theof mass total

solution theof cm 250in iron of mass 3

= 1.625

0.525x

1

100

(iii) = 32% (% by mass of iron in the tablets)


Notes

KMnO4 is a secondary standard as it decomposes in strong sunlight and so must be

standardised immediately prior to use.

KMnO4 is an oxidising agent and is easily reduced. It does not dissolve easily in water.

The titre reading is taken from the top of the meniscus when KMnO4 is in the burette

as the bottom of the meniscus is difficult to see due to the opaque nature of the

KMnO4

Iron tablets are prescribed to prevent anaemia

H2SO4 added when making up tablet solution to prevent Fe2+ being oxidised to Fe3+

by oxygen in the air

H2SO4 added before each titration to ensure complete conversion of MnO4- to Mn2+

and to prevent formation of Mn4+, a dirty brown precipitate

Neither HCl or HNO3 can be used to acidify the solution in the conical flask as the Cl-

ions in the HCl would be oxidised to produce Cl2 which is poisonous, and HNO3 is a

strong oxidising agent itself and will take part in the reaction

Self indicated: no indicator required

Colour change at the end-point: colourless to first permanent pink colour

Reaction is autocatalysed, i.e. Mn2+ which is a product of the reaction catalyses

reaction. Rate of reaction increases as reaction proceeds


Iodine – thiosulphate titration (2007)

2S2O3 = 1I2

2

20 x M =

1

25x 0.05

M = 20 x 1

2x 25x 0.05

M = 0.125 mol L–1 (molarity of the Na2S2O3.5H2O solution)

x 248 (Mr of Na2S2O3.5H2O)

= 31 g L–1 (concentration of crystalline Na2S2O3.5H2O in g L–1)


Notes

KI is added to bring/keep the I2 in solution; pure I2 is insoluble in water, as water is

polar and I2 is non-polar and hence cannot form hydrogen bonds with water

molecules

Indicator: starch

Colour change at the end-point: blue-black to colourless

Colour changes from the start of the titration:

KMnO4 + KI /

H2SO4 Na2S2O3 + starch + Na2S2O3

purple reddy/

brown

straw

yellow

blue-

black colourless

Starch is only added once the solution turns straw yellow. If the starch was added

before this stage then the blue-black complex that is formed is too concentrated and

too stable to decompose fast enough to give an accurate end-point


Determination of the percentage of hypochlorite in bleach (2011)

1ClO- = 1I2

1I2 = 2S2O3

1ClO- = 2S2O3

1

25 x M =

2

16.1 x 0.1

M = 25 x 2

1 x 16.1 x 0.1

(i) M = 0.0322 mol L–1 (molarity of the diluted bleach)

x 20 (dilution factor 25 cm3 to 500 cm3)

(ii) = 0.644 mol L–1 (molarity of the original bleach)

x 74.5 (Mr of NaClO)

(i) = 47.978 g L–1 (concentration of NaClO in g L–1)

10 (g L–1 to g 100 cm–3 = % (w/v))

(i) = 4.7978 % (w/v) (concentration of NaClO in % (w/v))


Notes

The bleach is diluted because it is too concentrated and there would have been a very

large volume of Na2S2O3 needed to get a reasonable titration

KI added for two reasons (i) to ensure all the bleach reacted and that the maximum

amount of iodine was liberated and (ii) to bring/keep the I2 in solution; pure I2 is

insoluble in water, as water is polar and I2 is non-polar and hence cannot form

hydrogen bonds with water molecules

Indicator: starch



bleach + KI /

H2SO4 Na2S2O3 + starch + Na2S2O3

colourless reddy/

brown

straw

yellow

blue-

black colourless





Estimation of the total hardness of a water sample (2010)

1M2+ = H2Y2-

1

50 x M =

1

9.20 x 0.01

M = 50 x 1

1 x 9.20 x 0.1

(i) M = 0.00184 mol L–1 (moles per litre of calcium and magnesium ions (M2+))

x 100 (Mr of CaCO3)

(ii) = 0.184 g L–1 (grams per litre expressed in terms of CaCO3)

x 1000 (g L–1 mg L–1 ppm)

(iii) = 184 ppm (ppm in terms of CaCO3)


Notes

EDTA = ethylene diamine tetraacetic acid

Indicator: Eriochrome Black T or Solochrome Black T, a grey-blue solid

Colour change: wine-red to blue

Complexiometric titration – EDTA forms a complex with the Ca2+ and Mg2+ ions that

are present in the hard water

Indicator complexes with Ca2+ and Mg2+ ions at the start of the experiment = wine-red

colour

Add the EDTA, Ca2+ and Mg2+ ions will form a complex with the EDTA

Indicator without the Ca2+ and Mg2+ ions = blue colour

Buffer pH = 10 is added as the indicator only works accurately at pHs greater than 9

Not using a buffer may lead to a poor endpoint, incomplete complexing or EDTA

complexing with other ions

The general purpose of buffers is to resist changes in pH or to stabilize the pH

EDTA is stored in a plastic bottle as it may extract metal ions from glass if left in a glass

container for long periods of time


Estimation of dissolved oxygen by redox titration

1O2 = 4Mn(OH)3

4Mn(OH)3 = 2I2

2I2 = 4S2O3

1O 2 = 4S2O3

1

100 x M =

4

5.7 x 0.02

M = 100 x 4

1x 5.7x 0.02

M = 0.000285 mol L–1 (molarity of the dissolved oxygen in the water)

x 32 (Mr of O2)

= 0.00912 g L–1 (concentration of the dissolved oxygen in the water in g L–1)

x 1000 (g L–1 mg L–1 ppm)

= 9.12 ppm (concentration of the dissolved oxygen in the water in ppm)

NB 1:4 ratio if asked to calculate O2 concentration directly; 1:2 ratio if asked to calculate

I2 concentration first


Notes

Indicator: starch



white ppt brown ppt reddy/brown straw yellow blue-black colourless




The following precautions should be observed when collecting water for B.O.D.

analysis (i) fill the bottle under the surface of the water to prevent atmospheric

oxygen being trapped and, thus, giving an artificially high oxygen level (ii) fill the

bottle completely to ensure that no air is trapped between the top of the water and

the stopper of the bottle and (iii) the second bottle is stored in the dark for 5 days at

20 oC to prevent photosynthesis leading to an increased oxygen content or to prevent

respiration which will lead to a decrease in the oxygen content

Concentrated solutions of MnSO4 and alkaline KI are used to minimise the amount of

the water sample that is displaced, to minimise the change in the oxygen dissolved in

the sample and to ensure that a small volume of solution supplies an excess

The additions were made well under the level of the water, using a dropper, making

sure not to bubble air into the water in the process

Water samples that may have high B.O.D.s should be diluted by a fixed amount with

well-oxygenated water in order to ensure that dissolved oxygen will be present

during the 5 day period and that a measurable amount of oxygen will be present at

the end of the test period

It can be concluded that no dissolved oxygen is present had a white precipitate been

observed instead of the brown precipitate after the first two additions of reagents to

the bottle filled with river water?

Kits, designed for use in the field, allow the dissolved oxygen concentration to be

measured immediately on collection of the sample. The immediate determination of

dissolved oxygen is considered best practice as biochemical (biological) reactions

(photosynthesis, respiration, metabolism) may occur which will alter the dissolved

oxygen concentration


Past Exam Question 1’s

LC 2015 – Question 1

Solution


Solution (cont’d)



Solution


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Solution


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Solution (cont’d)


Past Exam Solutions to Question 1’s

LC 2015 – Question 1 Solution

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