Oxygen flask combustion method ppt.pdf

Oxygen flask combustion method

1. HALIDE (SCHNOIGER'S OXYGEN FLASK
METHOD)
Presented By –
Shailesh S. Madbhagat.
Dr. Ghali College Gadhinglaj .

2. •CONTENTS -
1.INTRODUCTION
2.APPARATUS
3.PREPARATION OF SAMPLE
4.PROCEDURE OF DETERMINATION
5.APPLICATIONS

3. •INTRODUCTION-
1.Schnoigersoxygenflaskmethodisalsoknownas
oxygenflaskcombustionmethod.
2.Thismethod wasdeveloped bywolfgang
schnoigerin1955.
3.Oxygenflaskcombustionmethodisusedtoidentify
halogensthatareproducedbycombusting
organiccompound.
4.ThedefinitionofOFCMsaysthatthemethodis
usefulinidentifyingordeterminingifsulphuror
halogensareproducedwhenorganiccompounds
arecombusted.

4. 5. The compounds contain iodine, fluorine, chlorine,
bromine or sulphur in a flask that is filled with oxygen.
6. When these compounds are combusted they give
out inorganic products which are soluble in water.

5. •APPARATUS -

6. 1.Theapparatusconsistof500mlconicalflaskfitted
withacork(groundglassstopper)atthebottom
ofwhichisfixedplatinumwire.
2.Throughthisplatinumwireattachedaplatinum
specimencarrier.
3.Theupperpartoftheflaskismadelikesaucer.
4.Thegroundstopperismadeupofhardglass.
5.Forthedeterminationoffluorinetheflaskand
stopperusedshouldmadeupofquartz.

7. •PREPARATION OF TEST SOLUTION AND BLANK
SOLUTION -
Samples of test solution were prepared by the following method
below :
•PREPARATION OF SAMPLE -
1)Forsolidsamples-Weightaccuratelysuitable
quantityofsampleonhalidefreefilterpaper,
wrappeditandplaceditonplatinumguaze.
2)Forliquidsamples-Useagelatinecapsuleor
mixedwithmethylcellulosepowderandplacein
platinumgauze.

8. 3)Forointmentsandcreams-Placethesampleon
greaseproofpaper.Folditandplaceinsample
holder.

9. •Method of Combustion -
1)Theabsorbingliquidshouldbeplacedinflask.
2)Thentheflaskshouldbefilledwithoxygenandthegroundpartofthe
stoppershouldbemoistenedwithwater.
3)Thenthefusestripisignitedandtransferredtotheflaskimmediately.
4)Theflaskshouldbekeptairtighteninguntilthecombinationiffinished.
5)Theflaskshouldbeshakenoccasionallysothatthewhitesmoke
completelyvanishes.
6)Letitstandfor15to30minutesandresultingsolutionwouldbelabeled
asatestsolution.
7)Preparetheblanksolutioninthesamemannerwithoutsample.

10. •PROCEDURE OF
DETERMINATION -
1) Chlorine and Bromine-
1.Usingtheoxygenflaskmethod,burnthequantityofsubstance
specifiedinthemonograph.
2.Theabsorbingliquidconsistsof17mlofhydrogenperoxide(~60
g/l)TSand3mlofwater.
3.Whentheprocessiscomplete,rinsethestopper,platinumwire,
platinumgauzeandsideoftheflaskwith40mlofwater.
4.Add5dropsofbromophenolblueorethanolTSandthenby
drops,sodiumhydroxide(0.1mol/l)vsuntilthecolourchanges
fromyellowtoblue.
5.Thenadd1mlofnitricacid(3g/l)TSand5dropsof
diphenylcarbazoneorethanolTSasindicatorandtitratewith
mercuricnitrate(0.01mol/l)vsuntilthesolutionturnslight
violet.Performthetestwiththeblanksolutioninthesame
manner
Eachmlof0.01mol/lmercuricnitratevs=0.709mgofCl
Eachmlof0.01mol/lmercuricnitratevs=1.598mgofBr

11. 2)Fluorine-
1.Usingtheoxygenflaskmethod,burnthequantity
ofthesubstancespecifiedinthemonograph.
2.Theabsorbingliquidconsistsof15mlwater.
3.Whentheprocessiscomplete,rinsethestopper,
platinumwure,platinumgauzeandsideofthe
flaskwith40mlofwater.
4.Add0.6mlofsodiumalizarinsulfonate(1g/l)TS
andthenbydrops,sodiumhydroxide(0.1mol/l)
vsuntilthecolourchangesfrompinktoyellow.
5.Add5mlofacetatebuffer,pH3.0,TSandtitrate
withthoriumnitrate(0.005mol/l)vsuntiltheyellow
colourchangestopinkishyellow.Performthetest
withblanksolutioninthesamemanner.
Eachmlof0.005mol/lthoriumnitratevs=0.380mg
ofF.

12. •APPLICATIONS -
1.Oxygenflaskcombustionmethodhasbeenused
todetermineofsulphurandhalogeninmedicine.
2.Thismethodisusedfordeterminationofhalogen,
sulphur,phosphorus,argonandboroninorganic
compound.
3.Determinationofchlorineinpolymers.
4.Determinationoftotalfluorineincoal.
5.Determinationofmercuryinashandsoilsample.

13. The End
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