PRACTICAL EXERCISES MANUAL

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7.2 THEORETICAL BASIS

7.3 LABORATORYPRACTICAL EXERCISES

7 .3.1 Warnings, main instructions and precautions ... ................. 14
7.3.2 PRACTICE 0. Relationship between concentration and conductivity. ..................................... |5
7 .3.3 PRACTICE I . Application of Fick's Law for the determination of diffusivity. ....................... I7
7.3.4 diffusivity..
PRACTICE2. Effect ofthe concenrration in the ....................... l9
7.4 ANNEX r. CONDUCTIMETERMANUAL.................... .......................20

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7 PRACTICAL EXERCISES MANUAL

7.1 DESCRIPTION OF THE EQUTPMENT

The QDTL (QDTLC is QDTl-Computerised) is a didactic unit that allows

the learner to go into the theoretical knowledge that he may have about the unitary
operations of mass transfer; specifically, about the diffusion in liquids systems. The
student will obtain data and experimental results, which are very useful for an
optimum practical comprehension of the process and, therefore, for the technical
training of the learner.

7.1.1 Introduction

An irreversible flow originates from the high concentrations to the low

ones, when there is a gradient of concentrations in a multi-component
thermodynamic system. This flow is called dffision. The diffusion tends to give the
system back to its balance state, of constant concentration. 'lhe diffusion is described

by Fick's Law. Binary mixing will be only considered for the exposition of such law,

although similar developments are possible for multi-component mixings.

7.1.2 Description

The experimental determination of the diffusion coefficient, D.,n, for a

binary mixture, can be done using a device such as the one described below.

The user has a tube of small volume. A filtering cell with a determined
number of pores is put in one of its ends. A concentrated salt solution (sodium
chloride) is put inside. Such tube is put into a container that holds a pure solvent
(distilled water). Here starts the diffusion, which rvill be measured indirectiy from the
 PRACTICAL EXERCISES MANUAL

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conductiviw datum.

Besides, the equipment has a thermostatic bath. It let us to carry out the
experiments at different temperatures.

7.1.3 Practical possibilities

. Application of Fick's Law for the diffusivity determination.

o Effect of the concentration on the diffusiviW.

Other practical possibilities:

o Determination of the molar flow densitv.

o Simple analysis of an important unstable state process.

7.1.4 Specifications

Unit assembled in a structure for the diffirsiviW determination of a

component in a liquid. The unit consists of:

o A liquid tank.

o A magnetic stirrer and magnet.

o A conductimeter.

o A conductivity sensor.

o A diffrrsion cell.

Capillaries number (N)= 317

Capillary length (x)= 5mm

 PRACTICAL EXERCISES MANUAL

Capillary diameter (D)= lmm

o Thermostatic bath, compound of:

Water vessel

Element

Level switch

Temperature sensor

QDTL EQUIPMENT (MANUAL)

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4dib it ref.: QDTUQDTLC Date: March 2009 Pg:5/31

Conductivity
cell

Temperature
sensors

Thermostatic
bath

7.1.5 Accessories

o A chronometer.

7.1.6 Dimensions and weights

The structure dimensions are:

width: 400 mm.

Height: 450 mm.

Depth: 300 mm.

 PRACTICAL EXERCISES MANUAL

7.1.7 Required services

Power supply 220-240Y /monophasic / 50H2.

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dib Unit ref.: QDTUQDTLC Date: March 2009 es,7/ar I

7.2 THEORETICAL BASIS

An irreversible flow originates from the high concentrations to the low

ones, when in a multi-component thermodynamic system there is a gradient of
concentrations. This flow is called diffusion. The diffusion tends to give back the
system to its balance state, of constant concentration. The diffusion is described by
Fick's Law. Binary mixtures will be only considered for the exposition of such law,
although similar developments are possible for multi-component mixings.

7.2.1 Fick's Law for binary mixing

Consider the system represented on figure 1. In such system, a liquid A

evaporates through a pure not soluble gas ,8. At the same time, the liquid I goes out
slowly of the bottom part of the system, as it is shown on the figure, and vapours do
the same thing when they are removed by a gas current B that circulates through the
top part of the system.

Marins ot Fase$ A and B

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J

Figure 1. Diffusion of a vapour A in a gas.B, insoluble in the liquid phase

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A.

Given the differences of concentration of A between the gas in contact with

the liquid and the gas at the upper part, there will continuously exist a movement of
the vapours of A towards lower concentration parts (positive direction of the "2"
coordinate). On the other hand, the gases mixture will globally move towards the
negative direction of the "2" coordinate, because of the liquid emptying. If this
emptying is slow enough, the net movement of A will be rising. Fick's diffusion
experimental law establishes that, in a system in which there are concentration
gradients, the component I moves regarding the global movement of the mixture, in
the direction of the c l negative concentration gradients, according to next equation:

Jo=-DnoYcu (1)

where D# is a proportionality coefficient and Vcr represents the gradient

operator applied to the concentration ofl. The equation (l) is not the usual form of
Fick's law, since the coefficient D' depends on the system concentration. That is

why the following expression is preferred:

i^
J^=-cDnoYxo Q)

This equation represents the so-called Fick's Law of the diffusion. In this
case, the diffusivity D-,, is practically independent from the system's concentration.

The intemational system units for the diffusion kinetic coefficient are [m2 s-
11,
although they are often expressed in [cm2 s-'1. Th" diffusivity numerical values
vary a lot according to the system used. This variation is especially important when
the different aggregation states of the matter are considered. Thus, gases diffusivities
change usually in the interval of lo' to 10, [-t r-'], whereas for the liquids, the
variation is located in the interval covered between l0r0 and l0-e [m2 s-tl. The
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PRACTICAL EXERCISES MANUAL

Unit ref.: QDTUQDTLC Date: March 2009 Pg:9/31

diffusivity on solids changes from one system to the other, and their values are much
34 to
more lower; about 10 10-11 [rnt t-t]. The following table shows different
experimental values for the diffusion coefficient.

Gaseous systems (estimate pressure I Dnu 1m2ls1 at2g8 K

atm)

Air-water 2,6.101

Air-ethanol 1,35.10 5

Liquid systems (infinite dilution)

Water-benzoic acid 1,21.10 '

Water-chlorine 1,25.10 'g

Solid systems (at 293 K)

Bi in Pb 1,1.10-20

Al in Cu 1,3 . l0-34

Although gases kinetic theory is very simple, it is interesting to notice the

diffusivity dependence of a gas with pressure and temperature. The diffusion
coefficient increases with temperature and decreases with pressure.

Other very useful way to express the first Fick's law is:

N = x',(N u + N ,,) - cD.rnYxo (3)

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7.2.2 Liquids diffusivities

i

The theory of diffusion in liquids is not very developed and the

experimental data are less abundant than for gases. Liquids diffusivities are usually
of 4 to 5 orders of magnitude lower to those of gases at the atmospheric pressure.
Diffusion in liquids takes place due to the random movement of the molecules. But
the average distance travelled between the collisions is lower than the molecular
diameter, in comparison with what happens with gases, where the average free range
has higher magnitude order than the molecule size.

The diffusivities for diluted liquid solutions may be roughly calculated

from the equation:

(v oM T
D, -- 7.4a0- n-)'''
pV'

Where Du = Diffusivity, cm'ls

I= Absolute temperature, K
p: Viscosity of the solution, cP
Vt : Molar volume of^the solute as a liquid in its normal boiling
temperature, cm'/mol-g

V B : Parameter of association for the solvent

M s: Molecular weight of the solvent

The recommended values of ry o are 2,6 for water, 1,9 for methanol, 1,5 for
ethanol and I ,0 for benzene, heptano, etler and other solvents that are not associated.
They are only valid for low concentrations and are applicable to electrolytes.

For watery solutions with low concentration in electrolytes, an easier

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bcib Unit ref.: QDTUQDTLC Date: March 2009

t
equation can be used:

,-., 13.26x10-5
t',t'-
-
l;,rVI*
Where p6 : Water viscosity

Ve: Molar volume of the solute at its normal boiling temperature,

cm3/ mol-s

Notice that, contrary to the case of binary gases mixtures, the diffusion
coefficient for a diluted solution of A in B is not the same than the one corresponding
to a diluted solution of .B in l, since p, Ms and Va will be different when the solute
and the solvent are swapped. For medium concentrations, sometimes the user can
obtain an approximate value of D through the interpolation between the values of the
diluted solutions, but this method leads to important mistakes for the case of non
ideal solutions.

Example 2 1 .3. Estimate the diffusivity of benzene in toluene and of toluene

in benzene at I10"C. The physical properties are:

M Temp,oC Va at Temp p at 110'C,

cm3/mol cP

Benzene 78,11 80,1 96,5 0,24

Toluene 92,t3 I10.6 I 18.3 0.26
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QDTUQDTLC Date: March 2009 ,, Pg:12 131

SOLUTION:

The Equation (21 .26) will be used for benzene in toluene

Du _ 7.411 o{(92,13)r1'? 383

: 6,74 x l0-5 cm2ls
6
0,r 6(96,5)0

For toluene in benzene,

Dr= 7.411 0-8(78,1 l)r " 383 _ 5,95 x l0-5 cm2ls

0,240 18,3)06

7.2.3 Conductivitv

To know the diffusivity of the solute in the solvent, there is a possibility to

resort to indirect measures, that is to say, to calculate the diffusivity from another
known variable. In our case, since the used solute is a salt (NaCl for example), the
user will resort to measure the conductivity. Afterwards, from these data, the
diffusivity can be determined.

Conductivity is the capacity ofa solution to conduct the electric current. It

can also be defined as a measure ofthe total ionic concentration that a solution has.

7.2.3.1 Conductivity measurement

When the user knows the nature of the involved ion, it can be used to
determ i ne their concentration.

A full system to measure the conductivity is made up of:

{ A conductivity cell.
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{ A temperature probe.

{ A measure instrument.

The conductimeter measures the electric conductivity of the ions in a

solution. For this, it applies an electric field of the solution. To avoid changes in the
substances, effects of layer on the electrodes, etc., an altemating current is applied.

The usual measure units are S/cm. Other alternative ways to express the
conductivity of a solution are the Salinity and the Total Dissolved Solids (TDS).

7 .2.3.2 The temperature effect

The conductivity of a solution is highly dependent of the temperature. This

one has a double effect on the electrolytes: it has an influence on their solution and
on their ionic mobility.

The conductivity of a solution increases with temperature. This increase is

in yof .C
normally expressed , and it is called Temperature Coefficient (TC). In
general, watery solutions have a TC close to 2%l "C .

The temperature compensation consists in calculating from the C, the

conductivity value that a sample should have at a so-called reference temperature,
usually 25'C.
 PRACTICAL EXERCISES MANUAL

Pgz 14 l31

7.3 LABORATORYPRACTICALEXERCISES

7.3.1 Warnings, main instructions and precautions

o Follow security instructions at any moment.

. organic solvents solutions, such as; Iletc., must not be

used. It is due to the fact that the solution vessel and the diffirsion cell
are made of methacrvlate.
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4dib Unit ref.: QDTUQDTLC Date: March Pg: '15 / 31

7.3.2 PRACTICE 0. Relationship between concentration and conductivity.

7.3.2.1 Objective.

To find the ratio between the concentration of a saline solution and the
conductivity.

7.3.2.2 Necessary elements.

QDTL unit by Edibon

Sodium chloride

Distilled water

A precision scale

7 .3.2.3 P ractice development.

In this practice, a graph is going to be drawn, which will give the direct
ratio between conductivity and the saline concentration. This table will be very useful
for the following practices, where the user will need that ratio to know the
concentration from the conductimeter.

For this practice, it is necessary to prepare NaCl solutions at different

concentrations. For this, the user starts from a NaCl 2 M solution, which will dilute
in known concentrations. The conductivity cell is put in the different solutions and
the user writes down the conductivity value shown by the conductimeter.
 PRACTICAL EXERCISES MANUAL

Pg: l6 / 3l

This practice will have to be made for all the solutions with which the user
will use with the unit.
 PRACTICAL EXERCISES MANUAL

Unit ref.: QDTUQDTLC I ll"'rrra*r'zoog i@,ll

7.3.3 PRACTICE 1. Application of Fick's Law for the determination of
diffusivity.

7.3.3.1 Objective.

To study the diffusion of a solute in a liquid solvent (distilled water).

7.3.3.2 Necessary elements.

o QDTL unit by Edibon.

Sodium chloride.

A chronometer.

l
7.3.3.3 Practice development.

The cell is filled up with a NaCl 2M solution (1179/l). Fill up the cell
completely and clean any excess of solution from the cell outside and from the
capillary ends using filter paper.

Put the cell in its position within the vessel. Fill up the vessel of the
measurement unit with distilled water (approximately 1.5 L or 2 L). The distilled
water level must sufllass 5 mm the diffusion cell.

Afterwards, the magnetic stirrer will be tumed on at a not very quick

speed. Later, the conductimeter will be turned on and the user will start measuring
the conductivity, for example, every 30 seconds.
 PRACTICAL EXERCISES MANUAL

Pg:18/31

As it has been said before, the solution concentration will be determined

indirectly from the conductivity datum. The expression used will be the following
one:

dk _DA.N'1t.D2.M.CM
dt 4v.x

where:

dk
Conductivity variation speed regarding time
a
M Molarity of the saline solution

N Number of capillaries

x Capillary length

D Diameter of a capillary

V Distilled water volume

CM Conductivity variation

Thus, if it is represented the conductivity regarding time, it is possible to

obtain the diffusion coefficient or difhrsivity from the slope.
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Unit ref.: QDTUQDTLC Pg: 19 / 31

7.3.4 PRACTICE2. Effect of the concentration in the diffusivity.

7.3.4.1 Objective.

To study the influence of the concentration on the diffusivity.

7.3.4.2 Necessary elements.

o QDTL unit by Edibon.

Sodium chloride.

A chronometer.

7.3.4.3 P ractice development.

To study the influence of the concentration on the diffusivity, several

diffusion experiments will be made, changing from one to another the concentration
of the initial saline solution contained in the cell.
I

Make the previous practice starting from the saline solution 2M, 1.5M and
lM.

Represent graphically the concentration profiles in comparison with time.

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Unit ref.: QDTUQDTLC I Date: March 2009

7.4 ANNEX 1. CONDUCTIMETERMANUAL.

HAHS HELN
coNsusrlvlTY
METER

m{3t3
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B
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 PRACTICAL EXERCISES MANUAL

bdi Unit ref.: QDTL/QDTLC Date: March 2009 Pg:21 131

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 PRACTICAL EXERCISES MANUAL

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 PRACTICAL EXERCISES MANUAL

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 PRACTICAL EXERCISES MANUAL

Unit ref.: QDTL/QDTLC Date: March 2009

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PRACTICAL EXERCISES MANUAL
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Unit ref.: QDTL/QDTLC Date: March 2009 Pg:26 I 31

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PRACTICAL EXERCISES MANUAL

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t-3 &u &wrd("tf**:., l{il' Arcrq;r tcdtq#

" ?ke IIATA nEeERP frrnrtirn tliryltyn th
Esdfium! minimun lnd e*rege rcedin;r Tn run
thr FATA S.ECCIRl}futt*tbnn prc,*r tlw'Rsssr'd
Outtm'(3-6. HS. !!*nce- T'Ef, qffiill sdl app+ar
nn tlw I"CD di*plsy"

* Tfith ths-'RHf *yudb$l lndicatd*n thc diep[ay

{a} ftuh the'CAJJB$trnn'{}*?. Ftg, 1}nnra
thsn thc "ttstf f;lmhol with th* msieum ralus
rccr:rrled will rypeartntfir LCD dlsplay'
{hJ furh ths'CALL &lnnnn on** atnin, the'Min'
*ymtr**sith rhc minimua! vsluffi nessrded will
lppcs.oa &s LCtr di*P*uY-
 PRACTICAL EXERCISES MANUAL

di Date: March 2009 Pg: 28 / 31

{c} Push thc'CAIL Suur:n" $nc* Gh}rs, the'AVS-

r}$ot *ith thf **ETEEE ralucr *dJ a{rpesrd}*
rheLcDd$pliy.
{d}Tc dq*acdunle th*Datl Re**rd functk}e Ftss
the'Rccord Eulbn- i3-6, Fip l) oncc 'taln
All rsaoriNred uiurf,iat$rs lril! direppeir hsm the
dqrlnf.
**{ ftr gurnk ilE mnEDc,F[ ibllar ffir pmmdrrcr
rfiorm &abr -'

' FOWER tu drt$ 'glgg1

,gU ; Trmpcl$m
Cmp6r;atim;
Ftrtol if
mq$irtg..

ilElroty'RECffiO
-H$siifffir
*l$... l*tn. AlE

orffi--
mcht mgDofy lroftf llnctflr
 PRACTICAL EXERCISES MANUAL
.{,diba Unit ref.: QDTUQDTLC Date: March 2009 Pg:29 I 31

S. ABNfTISHAL FEATURES
{rlThe inctniercnt hex huiN! -in'Autu Ftwrcr $hut*nt'fl
in nrdsr t{r Frnl*mg tuttery [fe. Ths ft]etsr nrill snritch
(lfr aui$mf,tiea!$'if mrne rtf the butrrm er* pr*$s*rJ
rilithin I0 min-
To d*-aetivst* thls tbature., SeJecr th* mentrrry ft{,-sfd
functian during m,slsulgfil*nt. hy prc:ni*g thc
'REffiR.D" h*&*n{3 *s" Fi6- l i.
ltr) Th* inrtrument rl$r tratu,r*s ths ebifi:ry t{:t adj$fr thc
fl)ntrilst ut' thc dirylay,
Thls is ruhi*:rr*d hy cnnl.nrllang the "I-'C{} Crrntrnst
Adjust'prt (3 -5. tig. I l.

6, OAL!tsRATISH PROCEDURE
The mctcr ha* bcen crlilrrated during mtnulacturc.
Hnwcvcr, it may be nercrsrry m rr*calihrr* perirtdically.
Fartieularly if ths inrrrr,mcnt i$ u$*:rl fcr a krng period *r if
thc corductivity chctmde is ch*ngad"
Tn r*-calihr*R the lnstruF]ent, hllrrrv the prneedur*s
nhnffir hekrw:
*,
{1} Pnpar,c * " }"413 mS Calfhratinn $alutirxr
{?} $lidc th* " Rang* Select Switth'{3-9. Ftg, I } trr "! mS"
Prsiti$n.
{3, lmrncrrt, the " Cend*ctiyit}" ElErtrude '{3-5. Fig. 1 I
intn the s*lutiarn up tn thu immersinn lrrucl,
({} Adjus,l lhc " fauhratl.rn Arljux Pat'{vRtt, Fig. ?i,
lncEtrxl *ithin th* hett*ryerlmpartmsnt, until rht d&rpl*y
indi$atc$i *h* lalu* of thr rdihr*tinrx "rdllutii]n-

FOf'dT pAfxtfiL

l'fH * Frg.A
d bo Unit ref.: QDTUQDTLC
PRACTICAL EXERCISES MANUAL

Date: March 2009 Pg: 30 / 31

7. R$E3g PC II.ITERFAGE
l}te in*rurnsnl f*.et$r**,nn RS:33 {"}lltSut *'ia 3.5 mm
f rrminal t 3-t5. Fig, I l"
Thc ennmretnr nutFrt i* a l6 digit rlura s*rcam uihiah
{an hr utilitd ur fhs urcr'r rprritit npplieatrtn.

Aa RS!i|? tsd ndlb thc follqrrirg esenoction will bc

rcguircd ttl tint tbc iaslrumcat sith rhc FC *eriel
input.

Thc 16 digit d*tt strcrk xill b* dixplrynd in the

E+g& {!S! idic*le t{e fg-ltoralrg;!gl||-{._;

DO Ecdllllsrd
fl tp D4 ,, Drl=
D* rs B8
* !,1* &F, 1* 1 DP t x EOF,8 =$FF

O ,* lt*E1 DF 1* 1
p x fDF.S =SDP
 l
PRACTICAL EXERCISES MANUAL

Unit ref.: QDTL/QDTLC Date: March 2009 Pg: 31 / 31

- -"-"
00 tlo la +nE-
, 15 {ts
,fE?T-*" --tr184i,, 16 +i-cd
"w;{*_* l0=
It - ITKI

Ft+ iot
rpp*l & lorer stltJ* frr?'+'
=, l#pero:', Lourr '+1
|.e l-ersrgsili{-$rls !!:f :--:,

?. BATTEHY REPLACE]iIEFiT
{1} nft*n lhe kit rnrrlsr rf ll:tr dirplav *um'"I-H[*'
it indicatc r ftlrmilt ttattcry nutput of le*s than 6'-l V -
I*5 v. lt i* n****ary tu rep[a** thc ttet!*rt' H*u'xr*r"
io-ryec tneaflrre nr'rri mry *till trc made- fnr scwrrl
hcuri aftcr lrrw hettcry indratrir flppcar$ hcftrre thc
irrstrum*nt hesngrg i*lacru rnte.
{ll 5lide thr BaneryCrnrc'r{3* l}'Fig' I lat*tay hnm thc
instrumcnt and remow the hatleD'
f3I lru*all * 9V hanrry{FP3 typcland rrpla** l'h* s$'"sr