Chapter 1

Basic Tools and Operations of Analytical Chemistry

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 1

Learning Objectives
How to use the analytical balance.
Volumetric glassware and how to use it.
Common laboratory apparatus for handling and
treating samples.
How to filter and prepare precipitates.
Laboratory safety.

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 2

Borosilicate
Borosilicateglassware
glassware(Pyrex,
(Pyrex,Kimax)
Kimax)isisnormally
normallyused
used
because it is thermally stable.
because it is thermally stable.

KNC2133 Analytical Chemistry

Dr Md Rezaur Rahman 3
Modern
Modernbalances
balancesare
areelectronic.
electronic. They
Theycompare
compareone
onemass
massagainst
againstanother
anothersince
sincethey
theyare
are
calibrated
calibratedwith
withaaknown
knownmass.
mass. Common
Commonbalances
balancesare
aresensitive
sensitiveto
to0.1
0.1mg.
mg.

Electronic analytical balance.

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 4
Electronic
Electronicbalances
balancesoperate
operate
on
onthe
theprinciple
principleof
of
electromagnetic force
electromagnetic force
compensation
compensation––the the
compensation
compensation currentto
current to position
bring the pan back to its
bring the pan back to its
original
scanner
originalposition
positionisis
proportional
proportionaltotothe
thesample
sample
weight.
weight.

hanger

coil
temperature
sensor
Operating principle of electronic balance.

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 5

Mechanical
Mechanicalbalances
balancesoperate
operateas
asfirst
firstclass
classlevers.
levers.
MM1LL1 ==MM2LL2
1 1 2 2

Principle of analytical balance.

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 6

The
Thesingle-pan
single-panbalance
balanceisisas
asaccurate
accurateas
as
electronic balances, and almost as fast.
electronic balances, and almost as fast.
But
Butititcan’t
can’tbe
beinterfaced
interfacedto
toaacomputer
computerto
to
collect
collectand
andprocess
processdata.
data.
And
Andyou
youhave
haveto
toread
readaascale
scaleinstead
insteadof
ofaa
digital
digitalnumber.
number.

Typical single-pan balance.

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 7

Weighing
Weighingbottles
bottlesare
areused
usedfor
fordrying
dryingsamples.
samples. Hygroscopic
Hygroscopic(ability
(abilityof
ofaasubstance
substance
to
toattract
attractand
andhold
holdwater
watermolecules
moleculesfrom
fromthe
thesurrounding
surroundingenvironment,
environment,through
through
absorption
absorption or adsorption) samples are weighed by difference, keeping thebottle
or adsorption) samples are weighed by difference, keeping the bottle
capped except when removing the sample.
capped except when removing the sample.

Weighing bottles.

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 8

AAweighing
weighingdish
dishor
orboat
boatisisused
usedfor
fordirect
directweighing
weighingof
ofsamples.
samples.

Weighing dish.

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 9

Volumetric
Volumetricflasks
flasksare
arecalibrated
calibrated
to
tocontain
containan
anaccurate
accuratevolume.
volume.

See
Seethe
theinside
insideback
backcover
coverof
ofthe
the
text for tolerances of Class A
text for tolerances of Class A
volumetric
volumetricglassware.
glassware.

Volumetric flask.
KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 10
Volumetric
Volumetricpipets
pipetsaccurately
accuratelydeliver
deliveraafixed
fixedvolume.
volume.
AAsmall
smallvolume
volumeremains
remainsininthe
thetip.
tip.

Transfer or volumetric pipets.

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 11

Measuring
Measuringpipets
pipetsare
arestraight-bore
straight-borepipets
pipetsmarked
markedat
atdifferent
differentvolumes.
volumes.
They
Theyare
areless
lessaccurate
accuratethan
thanvolumetric
volumetricpipets.
pipets.

Measuring pipets.
KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 12
Syringe
Syringepipets
pipetsprecisely
preciselydeliver
delivermicroliter
microlitervolumes.
volumes.
They
Theyare
arecommonly
commonlyused
usedtotointroduce
introducesamples
samplesinto
intoaagas
gaschromatograph.
chromatograph.

Hamilton microliter syringe.

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 13

Syringe
Syringepipets
pipetscan
canreproducibly
reproduciblydeliver
deliveraaselected
selectedvolume.
volume.
They
Theycome
comeininfixed
fixedand
andvariable
variablevolumes.
volumes.The
Theplastic
plastictips
tipsare
aredisposable.
disposable.

Single-channel and multichannel digital displacement pipets and

microwell plates.

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 14

AA50-mL
50-mLburet
buretisismarked
markedinin0.1
0.1mL
mLincrements.
increments.
You
Youinterpolate
interpolateto to0.01
0.01mL,
mL,good
goodto
toabout
about±0.02
±0.02mL.
mL.
Two
Tworeadings
readingsare
aretaken
takenfor
forevery
everyvolume
volumemeasurement.
measurement.

Typical buret.
KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 15
 Position
Positionthe
theblack
blackfield
fieldjust
justbelow
belowthe
themeniscus.
meniscus.
Avoid
Avoidparallax
parallaxerror
errorby
byreading
readingatateye
eyelevel.
level.

Meniscus illuminator.
KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 16
 Place
Placethe
theflask
flaskon
onaawhite
whitebackground.
background.
Place
Placethe
theburet
burettip
tipin
inthe
theneck
neckof
ofthe
theflask
flaskwhile
whileyou
youswirl.
swirl.

Proper technique for titration.

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 17

Use
Useaadesiccator
desiccatorto
tocool
coolaadried
driedor
orignited
ignitedsample.
sample.
Cool
Coolaared
redhot
hotvessel
vesselbefore
beforeplacing
placingininthe
thedesiccator.
desiccator.

Desiccator and desiccator plate.

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 18
CaCl
CaCl2 2isiscommonly
commonlyused.
used.
ItItneeds
needsperiodic
periodicreplacement
replacementwhen
whenwet
wetor
orcaked.
caked.

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 19

Used
Usedto
toignite
ignitesamples
samplesat
athigh
hightemperatures,
temperatures,e.g.,
e.g.,to
todry
dryash
ashorganic
organicmatter.
matter.

Muffle furnace.
KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 20
 Used
Usedto
todry
drysamples
samplesbefore
beforeweighing.
weighing.
Usually
Usually110
110oCCused.
o
used.

Drying oven.
KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 21
AAfume
fumehood
hoodisis“dirty”
“dirty”since
sinceititdraws
drawsin
in
laboratory air.
laboratory air.
AAlaminar-flow
laminar-flowhood
hoodfilters
filtersair (0.3mm
air(0.3 mm
HEPA
HEPAfilter)
filter)and
andflows
flowsititout
outinto
intothe
the
room.
room.
Use
Useititas
asaaworkstation
workstationfor
fortrace
traceanalysis.
analysis.

Laminar-flow workstation.
KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 22
 Use
Usethese
thesefor
forquantitative
quantitativetransfer
transferof
ofprecipitates
precipitatesand
andsolutions,
solutions,
and
andfor
forwashing
washing precipitates.
precipitates.

Wash bottles: (a) polyethylene, squeeze type; (b) glass, blow type.
KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 23
 Use
Usefor
forfiltering
filteringnon-gelatinous
non-gelatinousprecipitates.
precipitates.

Filtering crucibles: (a) Gooch crucible; (b) sintered-glass crucible; (c)

porcelain filter crucible.

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 24

Mount
Mountthethefiltering
filteringcrucible
cruciblein
inaacrucible
crucibleholder
holder
and
and connectthe
connect the
filtering flask to a water aspirator.
filtering flask to a water aspirator.

Crucible holders.

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 25

These
Theseare
areashless
ashlessfilter
filterpapers.
papers.
They
Theyare
areignited
ignitedaway
awayafter
aftercollection
collectionof
ofthe
theprecipitate.
precipitate.
Use
Usefor
forgelatinous
gelatinousprecipitates.
precipitates.

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 26

This
Thisprovides
providesaagood
goodseal
sealand
andprevents
preventsair
airbubbles
bubblesfrom
frombeing
beingdrawn
drawnin.in.
Suction
Suctionfrom
fromthe
theweight
weightof
ofthe
thewater
waterin
inthe
thestem
stemincreases
increasesthe
thefiltration
filtrationrate.
rate.
Let
Letthe
theprecipitate
precipitatesettle
settlein
inthe
thebeaker
beakerbefore
beforebeginning
beginningfiltration.
filtration.

Properly folded filter paper.

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 27
Decant
Decantthe
thesolution
solutionby
bypouring
pouringdown
downthe
thestirring
stirringrod.
rod.
After
Afterdecantiing
decantiingthe
themother
motherliquor,
liquor,add
addwash
washwater
waterto
tothe
theprecipitate
precipitateand
anddecant
decantagain,
again,
repeating 2-3 times.
repeating 2-3 times.
Then
Thenwash
washthe
theprecipitate
precipitateinto
intothe
thefilter.
filter.

Proper technique for transfer of a precipitate.

KNC2133 Analytical Chemistry 28
Dr Md Rezaur Rahman
Use
Usethis
thisto
toscrub
scrubthe
thewalls
wallsof
ofthe
thebeaker
beakerand
andcollect
collectall
allthe
theprecipitate
precipitate(by
(bywashing).
washing).

Rubber policeman.

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 29

Heat
Heator orignite
ignitethe
thecrucible
crucibleto
toaaconstant
constantweight
weight(to
(to0.3-0.4
0.3-0.4mg)
mg)before
beforeadding
addingthe
the
filtered
filteredprecipitate.
precipitate.
Fold
Foldthe
thefilter
filterpaper
paperover
overthe
theprecipitate.
precipitate.
Drive
Driveoff
offmoisture
moistureatatlow
lowheat.
heat. Then
Thengradually
graduallyincrease
increaseheat
heattill
tillthe
thepaper
paperbegins
beginsto
tochar.
char.
After
Afterthe
thepaper
paperisisgone,
gone,ignite
ignitethe
theprecipitate.
precipitate.

Crucible and cover supported on a wire triangle for charring off paper.
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Dr Md Rezaur Rahman 30
Obtaining
Obtainingaarepresentative
representativesample
sampleisisthe
thefirst
firststep
stepof
ofan
ananalysis.
analysis.
The
Thegross
grosssample
sampleisisseveral
severalsmall
smallportions
portionsofofthe
thesample.
sample.
This
Thisisisreduced
reducedtotoprovide
provideaalaboratory
laboratorysample.
sample.
An
Analiquot
aliquotofofthis
thissample
sampleisistaken
takenfor
forthe
theanalysis
analysissample.
sample.

KNC2133 Analytical Chemistry

Dr Md Rezaur Rahman Sampling 31
Microwave
Microwaveovens
ovensprovide
providerapid
rapiddrying.
drying.
Acid
Aciddecomposition
decompositiontimes
timesare
arereduced
reducedfrom
fromhours
hoursto
tominutes.
minutes.

Schematic of a microwave system.

KNC2133 Analytical Chemistry
Dr Md Rezaur Rahman 32
Use
Usethese
thesefor
foracid
aciddigestions.
digestions.
They
Theyare
aretilted
tiltedwhile
whileheating
heatingto
toavoid
avoidlosses
lossesfrom
from“bumping”.
“bumping”.

KNC2133 Analytical Chemistry Fig. 2.28. Kjeldahl flasks.

Dr Md Rezaur Rahman 33
 Laboratory
Laboratorysafety
safetyisisaamust!
must!
Learn
Learnthe
therules.
rules.
See
SeeAppendix
AppendixD.
D.

KNC2133 Analytical Chemistry

Dr Md Rezaur Rahman 34
GOOD LAB PRACTICES
Standard Operating Procedure (SOP): a specific set
of instructions for a task (i.e., safety protocol, how to
calibrate a balance, etc.)
Safety in the Lab: proper components (i.e., eye wash,
shower, fire extinguishers, etc.)
Chemical Hazards: explosive, highly reactive,
flammable, toxic, corrosive, can cause other health
problems
Handling: minimize exposure, understand proper
storage and disposal

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 35

MINIMIZE YOUR EXPOSURE: breathing, skin and
eye contact, ingestion, injection
USE PROPER STORAGE: metal cabinets for
flammables, ventilated for volatiles, separate reactives
PROPER DISPOSAL: know in advance your disposal
plan (OSHA & EPA guidelines)

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 36

Material Safety Data Sheet
Required for every chemical produced
Contains information about the following:
Chemical and physical properties
Health hazards
Interactions with other chemicals
Disposal instructions

msds.pdf

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 37

THANK YOU

KNC2133 Analytical Chemistry Dr Md Rezaur Rahman 38