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DEPARTMENT OF
CHEMISTRY
PHYSICAL CHEMISTRYLABORATORY
CHEMISTRY 444/544LABORATORY MANUAL:
WINTER, 2011
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CONTENTSPage No
Occupational Health and Safety 3
Laboratory Rules and Regulations 4General ire Orders !"c#no$ledge%ent or% &"rrange%ents for Laboratory Sessions 'Reading References 1(Plagiaris%1)Laboratory Reports or%at13
Expe!"e#$%
1 *inetics of reaction bet$een e+,,,- and SN/ by the stopped 0o$
techniue 12
2 &!'($!)#(*+R)$($!)#(* %pe$( )- HC* (#. DC*
2
Te").#("!% )- 3(*(#! e**%
4 eter%ination of heats of solution fro% solubility %easure%ents
3!
5 Te p($!$!)# )e!e#$ 6 Te e78!*!'!8" I+9 I2 I+
; M(3#e$! %8%ep$!'!*!$ )- %)*!. $(#%!$!)# "e$(* )"p)8#.%
41
& he dipole %o%ent of chloroben5ene44
' 6iscosity7 8olar %ass of a poly%er
4'
2 9nthalpy of %i:ing of acetone and $ater
;3
1( 6iscosity of gases ;&
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11 issociation constant of H3OOH fro% electrical conducti
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1; Ce"!(* O%!**($!)#%: Te Be*)8%)+>(')$!#%?!! Re($!)#
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OCCUPATIONAL HEALTH AND SAFETY
YOUare $arned that all substances handled and all operations perfor%ed
in a laboratory can be ha5ardous or potentially ha5ardous. "ll substances
%ust be handled $ith care and disposed of according to laid do$n
procedures. "ll operations and %anipulations %ust be carried out in an
organised and attenti
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LABORATORY RULES AND RE@ULATIONS
1 Students %ust be present ten %inutes before the start of each
scheduled laboratory session. Lateco%ers $ill be refused entry to
the laboratory.
) No student $ill be per%itted to $or# in the laboratory outside of
laboratory hours e:cept by e:press per%ission of the staB
%e%ber+s- responsible for the session. Ne
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%ust be returned to its proper place= clean and dry= and in $or#ing
condition= unless other$ise indicated or instructed.
11 "ll solids %ust be discarded into the bins pro
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)1 he use of reagent bottle caps as $eighing receptacles is forbidden.
)) Liuids @ $hether corrosi
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O# e(!#3 ( e e(8($!)# (*("
1 Stop nor%al $or# i%%ediately.
) 8a#e safe any apparatus= and %aterial in use= shutting oB as
necessary any local gas taps?
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9P"R89N O H98,SR>
PORL"N S"9 EN,69RS,>
ACNOWLED@EMENT FORM
,= the undersigned +please print full na%e-
..........................................................................
Student No. ........................................
,dentity No. .......................................
do hereby ac#no$ledge ha
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ARRAN@EMENTS FOR LABORATORY SESSIONS
D($e% (#. T!"e% -) P($!(* Se%%!)#%
Practical sessions $ill be held only on the speciAc ti%etabled day during
the $inter uarter.
Laboratory sessions $ill co%%ence pro%ptly. Students are e:pected to
report punctually for each laboratory session. hose arri
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they can still ha
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des#- and utilise the full area of the sheet of graph paper= adKusting the
scales on the a:es to %a:i%i5e the space a
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Garland= Nibler and Shoe%a#er= Experiments in Physical Chemistry=
Se
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L(')($) Rep)$%:
Lab reports %ust be $ritten INDI&IDUALLY= %ust be of Kournal uality=
and %ust follo$ the M"S for%at. Online you can also And guidelines onhttp7??$$$.rose@hul%an.edu?tilstra?.
I"p)$(#$ D($e%: o be ad
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o ecide $hich
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iscussion
onclusion
References
he follo$ing pages include a %ore detailed description of each of thesections. Ce a$are that this is a li
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literature= and identify ho$ this $or# is diBerent or related to the citedliterature.
he concepts and their related euations %ust be de
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practice constructing one fro% scratch. he construction of a good datatable reuires #no$ing $hat the i%portant features are.
,. We# $) 8%e T('*e%
ables are to be used $hen the data are precise nu%bers= $hen there aretoo %any to be presented clearly in the narrati
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Often the %ost concise and precise $ay to present data is to plot it. hechallenge is #no$ing $hat to plot on $hich a:is. "n understanding of thetheory behind the e:peri%ent should pro
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,n the discussion section= it should be clearly stated $hether or not theproble% has been resol
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EPERIMENT 1
THE INETICS OF REACTION BETWEEN IRONIII AND
THIOCYANATE IONS BY THE STOPPED FLOW TECHNIGUE
Re-ee#e7 "t#ins= Physical Chemistry= &th 9d.= pp. '!4@'!!.
he rates of reaction of %etal auo ions $ith ligands ha
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+*OHZ 1.'! : 1(@3 8 *OHZ !.; : 1(@; 8 *c Z #1)?#)1Z 123 8@1 all
%easured at ); -
V*cZ #34?#43X
Note that the reaction+s- that $e are studying are the for$ard paths of the
euilibria. Note also that there are t$o substitutions to consider in the%echanis%= that is= of the auo ion and of the %onohydro:y auo ion= and
further= that the euilibria are connected by hydrolysis constants. 6alues
for these euilibriu% constants can be obtained fro% the literature.
his leads to the second factor to be considered in the e:peri%ent. De
need to #eep the ionic strength constant +(.; 8 here-. ,t is usual to
%aintain ionic strength $ith salts such as NalO4and LilO4= and to adKust
the acidity $ith an acid such as HlO4. Ob
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(.1( 8 HlO49 1.( 8 NalO4
he accurate concentrations of these solutions are gi
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igure ) sho$s the positions of the
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On the S"@)( Rapid *inetics "ccessory the dead
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F!38e 1: Sche%atic of the Hi@ech S"@)( Rapid *inetics "ccessory.
);
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!#e$! (#(*%!%
Since the position of the euilibriu% connecting the eSN)W and
e+OH-SNWspecies lies far o
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Rate of destruction of eSNW Z ][][
1 3412 FeSCN
H
Kkk
K
OH
c
+
he nett rate of for%ation of eSN)W
is gi
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V!eXeV"CNXe Z ec
FeSCNK
][1
leading to cancellation of the Arst and third ter%s abo
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9:peri%ent ).
&IBRATIONAL+ROTATIONAL SPECTRA OF HC* (#. DC*
Expe!"e#$ < p(3e 41; !# S)e"(?e, e$ (*, $ e.!$!)#
9uip%ent +in )11C-7lecture bottles of Hl and l,R sa%ple cellglass
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+to a dis#ette or to the H98 Aleser
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,nstructions7
he FSpectru% for Dindo$sF +SD- soft$are pac#age controls the Per#in@9l%er %odel 1!(( ,R and is running on a P connected to theinstru%ent.
he data collection co%puter should be po$ered on and SD $ill startauto%atically after Dindo$s2; is loaded. Other$ise= SD can be startedby double clic#ing on the FSpectru%F des#top icon. he user log in dialogbo: $ill be displayed. Log in to the progra% as F144F= $hich can beselected fro% the list of users in the pull do$n %enu. he pass$ord isFpche%F. ,f the progra% is already running= go to the FSetupF %enu= selectFhange loginF and select F144F fro% the users %enu.Place the e%pty ,R cell into the sa%ple co%part%ent by sliding the endplate of the cell into the %ount inside the co%part%ent. lose the sa%pleco%part%ent door.
he Spectru% %ain $indo$ loo#s li#e7
"fter the e%pty cell is properly positioned in the instru%ent sa%pleco%part%ent= clic# on the FC#GrdF button +on the upper toolbar- to collecta bac#ground spectru%. he scan para%eters ha
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the bac#ground spectru%. Must use the default na%e and selectFOou can then FloseF the selected spectru% fro% the FileF%enu. +Note7 if you FhaltedF a pre
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H98 net$or# Aleser
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Expe!"e#$
her%odyna%ics of Gal
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( ) ( ) ( ) ( ) ( )3 4 2
6 62 2Zn Fe CN aq Fe CN aq Zn aq
++ +
or this reaction the Nernst euation +euation 1- beco%es
( )
( )
2 4
6
3
6
2
2ln
Zn Fe CNo
Fe CN
A ART
nFA
+
=
,f $e assu%e that the acti
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he 5inc electrode is a 1@c% $ide strip of 5inc sheet and theplatinu% electrode should be constructed by attaching a s%all piece ofplatinu% foil to the tip of the electrode. ,nterface the t$o electrodes to theco%puter
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Expe!"e#$ 4
HEAT OF SOLUTION FROM MEASUREMENTS OF SOLUBILITY
Re-ee#e%: "t#ins and de Paula= pp. 42@;4= )1)@)14.
Ma%es and Prichard= pp. !)@!4.
I#$).8$!)#:
One of the best #no$n and %ost useful ther%odyna%ic for%ulae is the
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he ther%ostat should be set at about 4( $hen you enter the
laboratory. " bottle containing a saturated solution of ben5oic acid and
e:cess solid ben5oic acid $ill be supplied. Sha#e the bottle and transfer
about 1;( c%3to the conical 0as# supplied. he solution should contain a
fe$ gra%s of undissol
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,s the signof1Hoin accord $ith Le hateliers principleQ iscuss.
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he *, and *,3are insoluble in he:ane. he purpose of the e:peri%ent is
to deter%ine the euilibriu% constant of the abo
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+ii- he tip of the pipette %ust pass throughthe he:ane layer to reach
the aueous layer. o pre
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EPERIMENT ;
MA@NETIC SUSCEPTIBILITY OF SOLID TRANSITION METAL
COMPOUNDS
Re-ee#e%7 . Nicholls= Complexes o the !irst/6o8 Transition
Elements= pp. 1((@111.
.P. Shoe%a#er= .D. Garland= M.D. Nibler= Experiments in
Physical Chemistry= 'th 9d.= pp. 3!1 @ 3&(.
,f a substance is placed in a %agnetic Aeld= the %agnetic Aeld strength
$ithin the substance $ill either be greater or s%aller than that in the
surrounding space. ,f the intensity is greater= the substance is said to be
p(("(3#e$! $hile if it is s%aller the substance is .!("(3#e$!.
ia%agnetis% is uni
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%o%ent= =of the substance by Lange
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also=
$here $# and $u represent the $eights of the #no$n and un#no$nsubstances respecti
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the hole through the bench= call the lecturer or de%onstrator= $ho $ill
attend to this.
4 Re%o
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EPERIMENT ENE
Re-ee#e7 "t#ins= Physical Chemistry= &th 9d.= pp. !'!@!2!.
" dipole is produced $hen there is an asy%%etric distribution of charge
o
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%olar polari5ability= P= is gi
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he theory of ebye assu%es that polar %olecules are suciently separated
so that the interaction a%ong their dipoles is negligible. his condition can
only be obtained in the gas phase or in dilute solutions in a non@polar
sol
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and of pure cyclohe:ane. Note the a%bient te%perature.
I#%$8"e#$($!)#
9ach student is pro
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EPERIMENT
&ISCOSITY: THE MOLAR MASS OF A POLYMER
Re-ee#e%7 Ma%es and Prichard= Practical Physical Chemistry= 3rd 9d.=
pp. )3@);= pp. ;2@!(.
"t#ins= Physical Chemistry= &th 9d.= pp. &4'@&;(.
,f a shearing force is applied to a liuid= the liuid $ill 0o$= but at the sa%e
ti%e a resistance to this 0o$ $ill be set up. onsider a liuid 0o$ing along acapillary tube. ,t has been fairly $ell established that= if the rate of 0o$ is
not too great= the liuid in i%%ediate contact $ith the $all of the capillary is
stationary. he rate of 0o$ increases $ith the distance fro% the $all. Let
the distance fro% the $all be 5 and the
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radius r in a ti%e t. P is the pressure diBerence across the t$o ends of the
tube= $hich causes the 0o$.
,n practice the capillary tube is incorporated in a
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%olecules %a#e a relati
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$here m and a +see abo
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since P depends only on the density of the liuid.
,n this case the densities can all be ta#en as that of $ater and $e ha
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EPERIMENT
ENTHALPY OF MIIN@ OF ACETONE AND WATER
Re-ee#e7 "t#ins= Physical Chemistry= &th 9d.= pp. 1&3@1&4.
he %olar enthalpy of %i:ing= H%:g?+n"W nC- of t$o liuids " and C to for%a liuid %i:ture= can be deAned as the enthalpy change acco%panying the
for%ation of 1 %ole of the liuid %i:ture fro% the reuisite a%ounts of the
t$o pure liuid co%ponents at the sa%e te%perature and pressure as the
%i:ture.
,n this e:peri%ent the %olar enthalpies of %i:ing of
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upon $hether the %i:ing process is e:other%ic or endother%ic=
respecti
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as abscissa. Moin the plotted points. he Agure obtained %ay loo#
%ore or less as follo$s7
Note that= in contrast to the situation encountered in the heat of
%i:ing e:peri%ent described in part +a-= the electrical heating
e:tends o
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C(*8*($!)#%
+a- Calculations o heat capacity
,f the potential diBerence applied to the heater is denoted F6F= the
current FiF= and the ti%e for $hich the heater $as acti
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EPERIMENT 10
&ISCOSITY OF @ASES
Re-ee#e%7 .P. Shoe%a#er= .D. Garland= M.,. Steinfeld= M.D. Nibler=
Experiments in Physical Chemistry= 'th 9d.= pp. 1)'@13;.
"t#ins= Physical Chemistry= &th 9d.= pp. '3(@'3).
,n this e:peri%ent= the
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rises fro% a lo$er Aducial %ar# ato an upper Aducial %ar# bis denoted as
tab. or any such apparatus of gi
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R*74
1' =
+3-
Since euation +1- does not apply accurately $ithin this transition region=it is necessary that < should be s%all in co%parison $ith
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9:a%ination of the apparatus to deter%ine the nature of the
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D($(
1 Poise Z (.1 N s %@)
L Z 1;.( c%
r Z (.(&; %%
EPERIMENT 11
DISSOCIATION CONSTANT OF ACETIC ACID FROM
MEASUREMENTS OF ELECTRICAL CONDUCTI&ITY
Re-ee#e%: "t#ins and de Paula= pp. &!1@&!4.
Ma%es and Prichard= pp. )32@)43.
De#!$!)# )- Te"%:
Resistance +R-
,f a potential diBerence= 6= is applied bet$een t$o points in a conductor=
and an electric current= i= 0o$s through the conductor= the electrical
resistance is deAned as R Z 6?i.
Enits7 oh%=
onductance +G-he conductance is deAned as the reciprocal of resistance= i.e. G Z l?R.
Enits7 sie%ens= S
Resisti
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c$
=
$here c is the concentration $hich %ust be e:pressed in %ol % 3in order
to obtain
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electrodes and " the area of the electrodes. his can be $ritten Z G$here is called the cell constant since it depends on the di%ensions ofeach indi
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concentration c and at inAnite dilution= respecti
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increases.
Expe!"e#$(* P)e.8e:
8a#e up solutions of (.() %ol d% @3= (.(() %ol d%@3and (.((() %ol d%@3
acetic acid fro% the (.1 %ol d% @3acid. his is %ost con
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Expe!"e#$ 12
THE RATE OF HYDROLYSIS OR IN&ERSION OF SUCROSE,
BY POLARIMETRY
Re-ee#e%: "t#ins and de Paula= pp. &21@'(3.
Ma%es and Prichard= pp. ''@'2 and 122@)((.
I#$).8$!)#:
irst@Order Reactions
he hydrolysis of sucrose occurring in aueous solution can be $ritten as
the reaction
1)H))O11 W H)O +& !H1)O! W !H1)O!sucrose @glucose @fructose
$hich proceeds
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.....+3-
9uations +)- and +3- are
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facing the light source= the light is said to be right circularly polari5ed light.
,f it rotates countercloc#$ise= it is left circularly polari5ed light. Dhen left
and right circularly polari5ed bea%s of eual intensity are co%bined= they
yield plane polari5ed light. on
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" liuid or a solution sho$s optical acti
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$here k= 6 and l are as deAned pre
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place at roo% te%perature. Record the te%perature.
3. ill the polari%eter tubes by using a pipette. ry the tube carefully
before inserting into the polari%eter. 8a#e sure that no air bubbles
are present in the tube.
4. Since solid sucrose is rather hygroscopic= close the reagent bottle
after use.
;. lean the polari%eter tube after use by rinsing it three ti%es $ith
distilled $ater. ry the tube on the outside.
G8e%$!)#%:
1. Dhat is the role of HWin this reactionQ Dhat is the
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EPERIMENT 1
A COMPLE REACTION 6 THE BROMINATION OF ACETONE
Re-ee#e: . aniels= M.D. Dillia%s= P. Cender= R.". "lberty= ..
orn$all= M.9. Harri%an= Experimental Physical Chemistry= &th
edition= pp. 1;)@1;;.
I#$).8$!)#:
he purpose of this e:peri%ent is to deter%ine the rate la$ and the rate
constant for the bro%ination of acetone. ro% rate data collected at t$o
or %ore te%peratures the acti
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e:tent of reaction. he s%all a%ount of bro%ine is co%pletely consu%ed
$hile the other reactants re%ain at an essentially constant concentration.
Since the reaction (*atep III=
+!-
he e:ponent r is deter%ined fro% t$o runs= say , and ,,,= in $hich
VH3OH3X, Z VH3OH3X,,,and VHWX,,,Z $VHWX,. hese conditions lead to
()lo>
)8*ate(*atelo>* IIII=
+&-
he rate constant is then deter%ined according to euation +)- fro% the
e:ponents= reaction rate= and the concentration data for $hich the rate
applies.
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he acti
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absorbance. Repeat this procedure by using Arst !.( c%3and then 3.( c%3
of (.() %ol d%@3Cr)diluted in each case $ith 1(.( c%3of 1 %ol d%@3Hl
and sucient distilled $ater to gi
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ion. "n analogous euation is used along $ith the data on solutions
nu%ber 1 and 4 to calculate the order $ith respect to bro%ine.
Ese euation +3- and the e:peri%ental results obtained to calculate the
rate constant # for each of the #inetic runs. eter%ine an a
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Expe!"e#$ 14
DISSOCIATION CONSTANT OF AN INDICATOR
BY SPECTROPHOTOMETRY
Re-ee#e%: Ma%es and Prichard= pp. 23@2&.
Expe!"e#$(* P)e.8e:
onsult the de%onstrator about the operation of the spectrophoto%eter.
>ou are pro
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+iii- he pH %eter should be calibrated using the t$o standard buBer
solutions pro
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Expe!"e#$ 15
DIFFERENTIAL SCANNIN@ CALORIMETRY DSC
OBECTI&ES
his e:peri%ent has the follo$ing three obKecti
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igure 17 iBerential po$er P
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he soft$are of the S instru%ent gi
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PROCEDURECefore beginning a fe$ points are $orth noting. Sa%ple $eighings are
carried out using a %icrogra% balance $ith an uncertainty no greater than afe$ hundredths of a %g@@ta#e the uncertainty to be (.(1( %g. "lso= inrunning soft$are $ith the Per#in@9l%er S& tas#s $ill be acco%plishedthrough using function #eys 1@2.
". S Run $ith 4=4@di@n@he:ylo:ya5o:yben5ene1. irst %a#e three +3- $eighings of a pan and a co
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onditions+other ,nitial 6alue )(.( %D
3. Place the e%pty sa%ple pan W coOER "" O ,L9S "N G9N9R"9PR,NOES OR 9"H REN.
C. S run $ith indiu% %etal
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1. Si%ilarly $eigh a sa%ple= about 1( %g= of ,n %etal in analu%inu% sa%ple pan. "gain place a sa%ple co
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4. or the liuid crystalline solid deter%ine S +in M *@1 %ol@1- for each
phase transition. Dhy should there be a large diBerence in S for the
) phase transitions7 s n and n iQ
;. or the ,n sa%ple= calculate Sfus +in M *@1 %ol@1- for ,n and for each%etal in
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EPERIMENT 1;
Ce"!(* O%!**($!)#% (#. W(e%: Te Be*)8%)+>(')$!#%?!!
Re($!)#
he study of oscillating che%ical reactions and other syste%s that e:hibit
e:otic dyna%ics has been a
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caused by the periodic concentration changes is %ore than co%pensated by
the entropy increases fro% other processes also conco%itantly proceed in
the reaction %i:ture. Hence a syste% already at euilibriu% is unli#ely to
sho$ any oscillatory beha
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+a- in the redo: potential of the syste%= $hich is controlled by the ratio
of the concentrations of the reduced to the o:idi5ed for% of the
%etal ion catalyst V8+nW1-WX?V8nWX=
+b- the concentrations of the bro%ide ion= VCr@X and
+c- the colors= based on the concentrations of the colored %etal ion
co%ple:. or e:a%ple= if ceriu% is used= the color $ill alternate
bet$een faint bro$n to colorless= and if ferroin is used= the color
$ill alternate bet$een deep read and blue.
A%%8"e. Me(#!%" )- $e B> e($!)#.
he Arst accepted %echanis% $as by Richard ields= 9ndre *oros and
Richard Noyes at the Eni
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+3- )e+,6- W H)+OOH-)W CrH+OOH-) x fCr@W other products
P)e%% A Re($!)#% R1 6 R
he o
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VCr@XcriticalZ 1(@;VCrO3@X(
Dhen VCr@X ` VCr@Xcritical process " do%inates= leading to a decrease in VCr@X.
Ho$e
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$hile
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,nduction period 1 @@hange@1 ) )w 1hange@) 3 3w )
etc etc nw n@1