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ANALYTICAL INSTRUMENTATION
(INST-2135)
OBJECTIVE
Experiment-1
In this experiment, the spectrum of the background of the sample is first taken to
eliminate errors like peak of air (contaminants).The experiment is preceded by obtaining
spectrum of the standard Polystyrene film, followed by various plastic samples. The
functional groups present in the standard was identified and compared with samples.
Thickness of the samples was calculated.
Experiment-2
Inthisexperiment,NaClplateswerecleanedusingacetoneandtheliquidsampleswere
placedonthisplateusingPasteurpipette.SaltplateswereinsertedtotheIRinstrumentto
obtainpeaksoftheliquidsamples.Functionalgroupspresentintheliquidsampleswere
identified.
INTRODUCTION
Infrared spectrometer uses electromagnetic radiations to determine chemical compounds.
It allows us to determine functional groups present in the compound by just inserting a
sample into the instrument. IR instrument is used for solid as well as liquid and gas
samples. Solid samples are crushed in a mortar pestle using few drops of Nujol to obtain
paste. It can be used to detect alcohol present in blood. Forensic studies and criminal
analysis makes use of IR. IR instrument absorbs samples at their absorption wavelength
and helps us determine organic as well as inorganic compounds.
Experiment 1
OBJECTIVE
To calibrate the instrument using polystyrene standard film and to obtain the spectrum of
3 other types of plastic films and to measure its thickness from the absorption spectra and
detecting or identifying functional groups from the spectra.
PROCEDURE
FollowedasperANALYTICALINSTRUMENTATIONlabmanualDurhamCollegepg
3137.
MATERIAL
Polystyrenestandardfilm,polythenewrap,thickwrapper,plasticZiplockwrap.
OBSERVATION
Samples
Functionalgroups
Wavenumber(cm1)
Polystyrenestandardfilm
CH
3022.89
C=C
1601.60
CH2
1453.11
Aromaticring
1668.60
CCl
620.93
Polythenewrap
CH
2807.86
Thickwrapper
CH
2968.90
CH2
1465.57
CH
2965.94
CH2
1481.84
Plasticziplockbag
CALCULATION
ReferYellowpagessubmittedwiththisreport
DISCUSSION
Infraredspectrophotometerabsorbscompoundatcertainwavelengthproducingspectraof
thecompounds.Itabsorbsvariousfunctionalgroupspresentinthecompoundandthus
givingtheirspecificpeaks.Functionalgroupspresentinthestandardpolystyrenefilm
wascomparedwiththesamples(polythenewrap,thickwrapperandplasticziplockbag)
CHpeakwasobservedatwavelengthofaround3000inallthesamplesandCH2was
observedatthewavelengthofaround1450intwoofthesamplesexceptpolythenewrap.
ERROR
Duetosomehumanerrorsorchangesmadeinthesoftware,thepeaksobtainedwere
upsidedown.
CONCLUSION
Functionalgroupswereidentifiedinallthethreesamplesbycomparingthepeakswith
thatofthestandardpolystyrenefilmusingIRspectrophotometer.
Experiment 2
OBJECTIVE
To identify functional groups present in a liquid sample from the spectra obtained by
placing the liquid samples on a salt plates and inserting them to an IR instrument.
MATERIAL
NaClplates,acetone,octane,mxylene,methanol.
PROCEDURE
FollowedasperANALYTICALINSTRUMENTATIONlabmanualDurhamCollegepg
3137.
OBSERVATION
Sample
Functionalgroups
Wavelength(cm1)
Acetone
CH
2967.19
C=O
1593.28
C=C
1470.46
Metasubstitutedaromatic
ring
7707.16
Octane
CH
1470.46
Methanol
OH
33003500
CH
2967.48
mxylene
DISCUSSION
Inthisexperiment,liquidsampleswereplacedonasaltplatesusingPasteurpipetteand
plateswereinsertedtoanIRinstrument.Functionalgroupspresentinorganiccompounds
wereidentifiedfromthepeaks.Methanol,octane,acetoneandmxyleneshoweddistinct
peakoftheirfunctionalgroup.
ERROR
Duetosomesoftwareerrororhumanerror,thepeaksoftheliquidsampleswereupside
down.
CONCLUSION
Differentfunctionalgroupspresentintheliquidsampleswereeasilyidentifiedfromtheir
distinctpeaksusingInfraredspectroscopy.
REFERENCE
1) ANALYTICALINSTRUMENTATIONlabmanualDurhamCollegepg3137.
2) DurhamcollegeOrganicChemistryCheatsheet.