Analytical Chemistry Notes, Selected

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exp08 Gravimetric Richter Scale SASOL HT- HP ANALYTICAL- Sample Prob

Analysis Practic… Sept 00 CHEMISTRY-… Stoichiometr

Chemical and Physical Principles
ANALYTICAL CHEMISTRY
Analytical Chemistry
• Branch of Chemistry that deals with the analy
composition of matter
• Involves methods used to identify the substa
(qualitative analysis) and the exact amou
(quantitative analysis)
Quantitative Methods of Analysis

A. Classification of Methods of Analysis
1. Classical methods
a. Gravimetric method – measurement of th
chemically related to the analyte
b. Volumetric method – measurement of the vol
completely with the analyte
2. Modern methods
a. Spectroscopic method – measurement o
produced by the analyte or its interactions wi
b. Electroanalytic Method – involves measurem
the analyte such as current, potential or quant
3. Other methods – involves the measurement of
as heat of reaction (calorimeter ), index of r
activity ( polarimeter ) or mass-to-charge ratio (m
Related titles B. Typical Steps in Analysis

1. Selection of an appropriate method

• In the selection of method of analysis, it is
accuracy, complexity and component of the
and trained personnel and the time of analysi

• Standard procedures are usually available
Abstracts, Analytica Chimica Acta, Applie
exp08 Gravimetric Richter Scale
Association of Analytical
SASOL HT- HP
Chemists,Sample
ANALYTICAL-
etc. Prob
Analysis Practic… Sept 00 CHEMISTRY-…
2. Obtaining a representative sample Stoichiometr
• The American Society for Testing and Mate
y g
Standards (NBS) and Association of Official
 Search document
such a few organizations  st
that impose
analysis of some samples
• Three steps are generally followed in obta
sample, obtaining a laboratory sample and ob
• A gross sample is obtained from a bulk sam
that it is considered a representative of the bu
• A laboratory sample is a fraction of the gro
wherein further reduction to few milligrams r
114
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


3. Measurement of the sample

• First step in preparing a sample involves
volume
• Solid samples are dried in an oven usually
hours and cooled in a dessicator; analysis i
Samples that decompose upon heat treatmen
as-received basis
• Replicate samples are taken for analysis to en
and quality of the results. Results obtained
treated using various statistical tests to establ
Table 1. Classification of analysis based on s
Method Sample Ma
macro more than 100
semi-micro 10 mg – 100
micro 1 – 10 mg
ultra-micro less than 1 m
4. Preparation of a solution of the sample
• Most methods are designed to process liqu
since these samples are homogenous and are
• The following solvents are commonly emplo
of the sample:
a. Water . Samples of soluble salts read
temperature and heating may be done to f
b. Non-oxidizing acids. In many instances,
not dissolve in water and usually the ad
soluble. Hydrochloric acid is a typical no
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
sulfuric and perchloric acid.

c. Oxidizing acids. For more stubborn sa
acid, nitric acid and aqua regia are us
hydrochloric acid and nitric acid in 3:1 v
also used for dissolving silicate ores.

d. Fluxing agents. Samples which were not
usually fused with a molten solvent cal
classified as acidic
SASOL HT- HP
(K2S2O7, KHF
ANALYTICAL- Sample
and
2 Prob
Analysis Practic… NaOH
Sept 00 or KOH) CHEMISTRY-…
and oxidizing (Na 2O2).
Stoichiometr
ground sample with the solid flux in an
flux melts
flux melts.
• Reagents and chemicals used in the laborator
a. Commercial or technical reagents . R
purification and not directly used for ana
b. United States Pharmacopoeia (USP
Reagents. Reagents used by pharmacists
c. Chemical Pure (CP) reagents . Reagents
technical reagents
d. Reagent grade or analytical reagent (A
analyzed by the manufacturer with the a
container
e. Primary standard grade . Chemicals with
115
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


• There are several ways of expressing conce

solution. The following are most commonly
solutions:
a. Weight percent – usually used to expr
aqueous reagents
%
 wt  = weight

of

 wt  weight of s
b. Volume percent – commonly used to sp
liquid compound diluted with another liq
%
 vol  = volume

of

 vol  volume of
For alcoholic beverages, percentage of
terms of proof as follows:

proof = 2 %

c. Weight/volume percent – used to indic
reagent in a dilute aqueous solution
%
 wt  = weight of sol

  volume of sol
vol
d. Mole fraction (x) – commonly used

concentrations of solute present in a strea
mole of
Related titles x=

mole of solute + m

e. Molality (m) – temperature-indepen
conveniently in physicochemical measur
solutions
 sol
mole of
m =
kilogram of s
exp08 Gravimetric Richter Scalef. Molarity (M) – ANALYTICAL-

SASOL HT- HP most commonly used
Sample in
Prob
Analysis Practic… ofSept 00
solute, CHEMISTRY-…
in moles, dissolved inStoichiometr
a solven
1L in a volumetric flask
mole of sol
M =
 Search document of so
volume
Formality (F) – concentration term iden
for solutions of ionic salts that do not
solution
g. Normality (N) – once popular unit of
chemists
equivalent of
N =
volume of so
116
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


An equivalent represents the mass of

number of reacting units. The number
number of moles multiplied by the num
or atom.
=
equivalent of solute
where m = mass of solute [g], EW = equ

1
molar mass [g-mol – ] and f = molar equiv
Therefore, normality (N) is related to

following equation:
N = f × M = 
 eq  ×
 mol 
Table 2. Molar equivalents of s
Nature of solute Mo
acid numbe
base number
salt net
oxidant ga
reductant lo
h. p-function - used to express concentratio
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is any integer less than zero defined as fo
p[ f ( xto
Upload your documents )] =down
− l
Related titles where x = concentration of the species in

OR
5. Treatment of the sample
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• Some samples has to be reduced or oxidize
first 30 days are free.
treated to become colored or converted t
volatilized 
• More often, the accuracyContinue of an for Free
analysis
unwanted components called interferences
exp08 Gravimetric • Interferences
Richter Scale can be ANALYTICAL-
SASOL HT- HP eliminated by convertin
Sample Prob
Analysis Practic… Sept 00
process CHEMISTRY-…
called masking. TypicalStoichiometr
maskin
converting the interference into a stable com
th t dd d t th l
the reagents added to the sample
• Some separation processes
 Search  em
are commonly
document
the interferences such as precipitation, e
exchange, volatilization and chromatography
6. Measurement of the analyte
• Using classical methods of analysis, results
per thousand or better, requires relatively la
applied to measurement of major constituents
• Instrumental methods are generally more se
rapid, automated and capable of measuring
however, these techniques are more expensiv
117
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


Table 3. Classification of const

Component R
major g
semi-micro
micro
ultra-micro
7. Calculation of results and reporting of data

• Results of analysis can be expressed dependi
a. Solid Samples. Calculations on solid sam
common way of expressing results in a m
or % weight
 wt  = wt. anal
% 
 wt  wt. sam
Table 4. Concentrations of analyte in solid s
Unit Definiton
parts per  wt  = gram analyte
thousand
pt   ×10
 wt  gram sample
million
ppm  ×1
 wt  gram sample
ppb  ×1
billion  You're
wt  Reading a Previe
gram sample
b. Liquid SamplesUpload your documents

. Similarly, to down
concentratio
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liquid samples obtained fromORa macro a

weight by volume or % volume by volum
 wt  =Become
gram aanalyte

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%  first 30×days
100% or %
are free.
 vol  mL sample

Table 5. Concentrations ofContinue
analyte for
in liquid
Free s
(wt/vol and vol/vol)
Analysis Practic… Septper
parts 00
ppm
  =
CHEMISTRY-…
wt Stoichiometr
gram analyte
×1
million

 
vol mL sample
 
billion
ppb
Search 
 document  ×1
 
vol mL sample

trillion
ppb  ×1
 
vol mL sample
parts per  vol  = vol analyte
million
ppm  ×10
 
vol vol sample
parts per  vol  = vol analyte
billion
ppm  ×10
 
vol vol sample
118
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Gravimetric Methods of Analysis

A. Types of Gravimetric Analysis
1. Extraction method. The analyte in the sample
solvent and the residue from the solution, af
chemically related to the analyte
2. Precipitation Method. The analyte is convert
filtered, washed, dried or ignited and weighed
3. Volatilization Method. The sample is treated t
absorbing medium; the analysis is based upon th
B. Gravimetric Factor and Precipitating Agents
1. Calculation in gravimetric analysis
To calculate the amount of analyte in the sample
mass of final form
% analyte =
mass of sample
Gravimetric Factor (GF)
molar mass of analyte  x m
GF = × 
molar mass of final form  y m
2. Precipitating agent
• An ideal precipitating agent must give an
following properties:
can be easily filtered and washed free from


has very low solubility to avoid losses du

inert towards components

 of the atmosph
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

OR
Table 6. Precipitating agents used in precipit
Species Become a Scribd
Final Form
member for full ac
Precipitant
Precipitated
first 30 days are free. P
Cl AgCl
Br AgBr AgNO3 
I AgI Continue for Free
– 2
SO4 BaSO4 BaCl2
exp08 Gravimetric Richter Scale SASOL HT- HPAs2O3ANALYTICAL-
As Sample Prob
Bi Bi2S3 CHEMISTRY-… Stoichiometr
Cd CdSO4
H2S
H2S
Cu CuO
Sn 
SnO
Search
2 document 
Sb Sb2O3
Mg Mg2P2O7
(NH4)2HPO4
Zn Zn2P2O7
C. Theory of Precipitation
1. Properties of precipitates
a. Particle size. Solid particles formed from pre
• Colloidal – tiny particles with size ra
microns in diameter; these particles do
filtered easily
119
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• Crystalline – particles with size ranging f

particles settle readily and easily filtered
• Particle size is usually affected by tempe
solubility of precipitate and mixing rate
b. Appearance. Precipitates may appear to be
crystal (BaSO4), coarse crystal (PbCl2) or gel
c. Relative supersaturation (von Weimarn ratio

relative supersaturatio
where Q = concentration of the solute as prec

of the precipitate
• In order to obtain low relative supers
precipitate, Q must be minimized and S m
methods are done to accomplish such con
 increase the temperature during precip
 precipitate from dilute solution (to mi
 slow addition of precipitating agent w
2. Mechanism of precipitation
Precipitation is assumed to occur in two ways:
a. Nucleation
• Prevails at high relative supersaturation
• Results in the formation of large number
b. Particle growth
• Prevails at low relative supersaturation
• Results in the formation
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small number
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3. Colloidal precipitates OR
a. Electrical nature of colloidal suspensions
• Suspensions,Become
whicha are
Scribd member
stable for full
since thesac
negatively charged, hencefirst 30 dayseach
repel are free.
othe
• By heating, stirring and addition of elec
combine together and formContinuea readily filter
for Free
• This process of converting a colloidal su
solid is called coagulation
SASOL HT- HP ANALYTICAL-
or agglomerati
Sample Prob
Analysis Practic… Sept 00 of colloids
b. Adsorption CHEMISTRY-… Stoichiometr
• Ions are attached directly to the

solid surface and comprise the
primary adsorption layer
• The charge of this layer is
dependent on the charge of the
ion present in excess
• A charged primary adsorption
layer attracts excess oppositely
charged ions to form a secondary
layer or counter-ion layer
• These ions, held by electrostatic
forces have higher mobility compared to t
• The two layers, which constitute an elec
particles to come close thus inhibits the fo
120
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• The equilibrium constant and the standard

follows:
nε °
log K = (T = 298
0.05916 V
4. Oxidation-reduction titration methods

a. Auxiliary oxidants and reductants
• Pre-reductants
 Jones reductor - consists of zinc metal
(amalgamated zinc) and used to reduce
+2 +2 +3 +4
(Ti ), UO2 (U or U ) and Cr
 Walden reductor - consists of a colum
insoluble salt of silver and does not red
 Na2SO3, NaHSO3, or SnCl2
• Pre-oxidants
 NaBiO3, (NH4)2S2O8, K2S2O8, Br2, Cl2,
b. Permanganate titration
• Titration is carried out in acidic medium us
• In the presence of HCl, titrant is consumed
• Acidic and basic solutions of KMnO4 are
kept in dark-colored bottles to avoid decom
Titrant: KMnO4
Half-cell reactions: You're Reading a Previe
1
 acidic medium MnO4 – +
1
 MnOto4 – down
basic mediumUpload your documents +
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
Primary standards: OR
 As2O3 H3AsO3 +
2
 Na2C2O4 Become a Scribd memberC2Ofor4 – full
ac2
+2
 Fe metal first 30 days
Feare
free. Fe
FeSO4⋅(en)SO4⋅4H2O
+2 +
 Fe  Fe

Indicator: Continueself-indica
for Free
Endpoint: pale pink c
exp08 Gravimetric Richterc.Scale SASOL HT-
Dichromate HP
titration ANALYTICAL- Sample Prob
• Titration is carried out in acidic medium on
• Titrant is stable towards light and less e
Titrant is stable towards light and less e
organic matter compared to permanganate
Titrant:
K2Cr2O7
– 2
Half-cell reaction: Cr2O7 +
Primary standards:
+
 Fe metal Fe(s)  Fe
FeSO4⋅(en)2SO4⋅4H2O
+2 +
 Fe  Fe
Indicator: sodium dip
N-phenyla
Endpoint: first appea
133
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


d. Cerium (IV) titration

• Titration is carried out in acidic medium us
0.5 M or higher
• In the presence of HCl, titrant is consumed
Titrant: Ce(SO4)2 and (NH4
+4 – +3
Half-cell reaction: Ce + e  Ce
Primary standard: As2O3
Half-cell reaction: H3AsO3 + H2O  H
Indicator: ferroin / N-phenyla
End point: orange-red to pale b
e. Iodimetry: Direct titration with iodine
• Titration is carried out in neutral, weak alk
Titrant: I2 dissolved in conc
1 1
Half-cell reaction: I3 – + 2e –  3I –
Primary standard: As2O3
Half-cell reaction: H3AsO3 + H2O  H
Indicator: Starch solution
Endpoint: Formation of intens
f. Iodometry: Indirect titration with iodine
• The analyte is an oxidizing agent which re
in excess to liberate I2 equivalent to the am
Titrant: You're
Na2Reading
S2O3 a Previe
– 2 2
Half-cell reaction: 2S2O3  S4O6 – +
Related titles
Primary standard: KIO3 or K2Cr2O7

– 1 +
Half-cell reaction: 2IO3 +OR 12H + 10
Cr2O7 – 2 + 14H+ + 6
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Indicator: Starch solution
first 30 days are free.
Endpoint: Color change from
g. Summary of oxidants and reductants usedin tit
Continue for Free
Oxidants Half-cell reaction
– 1 + – +
exp08 Gravimetric Richter Scale KMnOSASOL
4 (acidic)
HT- HP MnO 4 + 8H + 5e
ANALYTICAL- Sample Mn
Prob
– 1 –
Analysis Practic… KMnOSept 00
4 (basic) CHEMISTRY-…
MnO 4 + 2H2O + 3e Stoichiometr
 MnO
–
MnO2 MnO2 + 4H+ + 2e  Mn+2
K Cr O Cr O – 2 + 14H+ + 6e –  2Cr+
K2Cr2O7 Cr2O7 + 14H + 6e  2Cr
Ce(SO4)2 Ce+4 + e –  Ce+3
I2 in KI I3 + 2e – 
 Search document – 1
3I – 1
I2 (satd) I2 + 2e –  2I – 1
I2(aq) I2 + 2e –  2I – 1
KIO3 2IO3 – 1 + 12H+ + 10e –  I2
Reductants Half-cell reaction
As2O3 H3AsO3 + H2O  H3AsO4 +

Na2C2O4 C2O4 – 2 2CO2 + 2e
Fe metal Fe  Fe+2 + 2e –
FeSO4 Fe+2  Fe+3 + e –
Na2S2O3 2S2O3 – 2  S4O6 – 2 + 2
134
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


5. Application of oxidation-reduction titration

a. Iodine number of oils and fats
• Measure of the degree of unsaturation of fa
• Expressed as the number of centigrams of
fat or oil
• Sample is dispersed in chloroform, t
monochloride in glacial acetic acid (Wij’s
the dark for 30 min
C C + IBr (excess) 
• KI is added to liberate the unreacted io

Na2S2O3 solution
IBr (unreacted) + KI
(V mL,sample
Na 2S2O 3
− VNa
mL, blank
S O
)( M
Iodine Number = 2 2 3
m
b. Peroxide value of oils and fats
• Measure of the extent of oxidative rancidity
• Expressed as the number of milliequival
kilogram of sample
• Sample is dissolved in a mixture of chlorof
with nitrogen gas to remove remaining oxy
liberate iodine You're Reading a Previe
1
2 I – + ROyour
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2H documents R
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(V

mL,sample
− VNa
Na 2S2OR
O3
mL, b
S
Peroxide Value = 2
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first 30 days
c. Dissolved oxygen (DO) – Winkler are free.
Method
• Measure of the amount of oxygen dissolved
• Measure of the ability toContinue
oxidize organic
for Free im
• Sample is treated with manganese (II) hy
brown precipitate of manganese (III) hydro
4 Mn(OH)
CHEMISTRY-…
2 + O 2 + 2H
Stoichiometr2
• Alkaline iodide-azide solution is added an
in concentrated H3PO4 to release the iodine
in concentrated H3PO4 to release the iodine
– 1 +
Mn(OH)3 + I + 3H  M
( mL
VNa 2S 2 O 3
)( M Na S
Dissolved oxygen = 2 2
volu
d. Chemical oxygen demand (COD)
• Measure of the amount of oxygen nece
material in a water sample
• Expressed as milligrams of oxygen required
• Sample is refluxed in the presence of HgS
known excess amount of standard K 2Cr2O
standard (NH4)2Fe(SO4)2 solution
135
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


(V mL,blank
Fe +2 2 )( M Fe + ) ×
− VFemL,+ sample 2
1m
COD = 6
volume sa
Molecular Absorption Spectrometry

A. Absorption Process and Beer-Lambert Law
• If a beam of light passes through a glass contain
radiation is always less powerful than that enteri
• Consider a block of absorbing matter where a be
radiant power, P0 strikes the surface perpendicul
of the material, b
• The emergent or transmitted radiation will
always have less radiant power, P than the
entering or incident radiation
• The fraction of incident radiation transmitted by
the solution, P/P0 is called transmittance and
related to absorbance according to the equation:
P
A = −log T = −log
P0
where A = absorbance, T = transmittance, P 0 =
incident radiant power [W], and P = transmitted
radiant power [W]
• Beer-Lambert’s law states that the absorbance
You're
is directly proportional to Reading a Previe
the concentration of
path length
P
Related titles A = −log T = −log

OR P0
where ε = molar absorptivity
– 1 – 1
Become a Scribd[L-mol
member for-cmfull ac
],
– 1
concentration [mol-L ] first 30 days are free.
B. Quantitative Analysis 
1. Standard addition method Continue for Free
• Involves addition of several increments of a
samples SASOL
of the HT- HP
same ANALYTICAL- Sample Prob
size and the resulting
development reagent is then diluted to a fixed
absorbance
• Assume several identical aliquots of the unkn
 Search
treated with several  s
document of standard
increments
concentration Cs and diluted to a fixed final volu
• If each of these solutions were assumed to obey
of each solution is described by:
εbVSC S εbVX C X
As = + = kVSCS
VT VT
where k = εb/VT, m = kVS and b = kCXVX
136
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exp08 Gravimetric Richter Scale SASOL HT- HP ANALYTICAL- Sample Prob

Chemical and Physical Principles

Quantitative Methods of Analysis

1. Selection of an appropriate method

exp08 Gravimetric Richter Scale SASOL HT- HP ANALYTICAL- Sample Prob

Chemical and Physical Principles

3. Measurement of the sample

sulfuric and perchloric acid.

exp08 Gravimetric Richter Scale SASOL HT- HP ANALYTICAL- Sample Prob

Chemical and Physical Principles

• There are several ways of expressing conce

d. Mole fraction (x) – commonly used

mole of solute + m

exp08 Gravimetric Richter Scalef. Molarity (M) – ANALYTICAL-

exp08 Gravimetric Richter Scale SASOL HT- HP ANALYTICAL- Sample Prob

Chemical and Physical Principles

An equivalent represents the mass of

where m = mass of solute [g], EW = equ

Therefore, normality (N) is related to

exp08 Gravimetric Richter Scale SASOL HT- HP ANALYTICAL- Sample Prob

Chemical and Physical Principles

Table 3. Classification of const

7. Calculation of results and reporting of data

b. Liquid SamplesUpload your documents

liquid samples obtained fromORa macro a

parts per  wt  = gram analyte

exp08 Gravimetric Richter Scale SASOL HT- HP ANALYTICAL- Sample Prob

Chemical and Physical Principles

Gravimetric Methods of Analysis

You're Reading a Previe

inert towards components

exp08 Gravimetric Richter Scale SASOL HT- HP ANALYTICAL- Sample Prob

Chemical and Physical Principles

• Crystalline – particles with size ranging f

where Q = concentration of the solute as prec

• Ions are attached directly to the

You're reading a preview 

Unlock full access (pages 8-19) by

exp08 Gravimetric Richter Scale SASOL HT- HP ANALYTICAL- Sample Prob

Chemical and Physical Principles

• The equilibrium constant and the standard

4. Oxidation-reduction titration methods

exp08 Gravimetric Richter Scale SASOL HT- HP ANALYTICAL- Sample Prob

Chemical and Physical Principles

d. Cerium (IV) titration

Reductants Half-cell reaction

As2O3 H3AsO3 + H2O  H3AsO4 +

exp08 Gravimetric Richter Scale SASOL HT- HP ANALYTICAL- Sample Prob

Chemical and Physical Principles

5. Application of oxidation-reduction titration

• KI is added to liberate the unreacted io

Become a Scribd member for full masac

exp08 Gravimetric Richter Scale SASOL HT- HP ANALYTICAL- Sample Prob

Chemical and Physical Principles

Molecular Absorption Spectrometry

where k = εb/VT, m = kVS and b = kCXVX

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exp08 Gravimetric Richter Scale SASOL HT- HP ANALYTICAL- Sample Prob

exp08 Gravimetric Richter Scale SASOL HT- HP ANALYTICAL- Sample Prob

exp08 Gravimetric Richter Scale SASOL HT- HP ANALYTICAL- Sample Prob

exp08 Gravimetric Richter Scale SASOL HT- HP ANALYTICAL- Sample Prob

exp08 Gravimetric Richter Scale SASOL HT- HP ANALYTICAL- Sample Prob