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Polymer Solutions

A traveling light wave can be described by the spatial and temporal

variations in its electric field vector, E:

(8.1.1)

direction of the light wave propagation

and magnitude k = 2/, with being

the wavelength. Appearance of

kr in the cosine means that the phase of the wave on all the points lying

on a given plane perpendicular to k is the same at any given time. is

the angular frequency and related to the frequency , speed of light c

and wavelength in free space 0 by:

(8.1.2)

1

Light Waves A Brief Review

Notice that the wavelength in a medium is generally not equal to 0 .

They are related by

(8.1.6)

light in the medium. For visible light, 0 3500-7000 . So, = c/ 0

1015 Hz. At such high speeds, typical photodetectors can only

measure the light intensity (energy per unit area per unit time), I,

integrated over time, where I is proportional to |EE| = E2. Such

detectors are called square-law detectors. In experiment, we usually

normalize the detector signal by the incident beam signal. This

cancels out the unknown proportionality factor between the detector

signal and I or E2.

It is more convenient to work with complex notations for E(r,t) and write:

(8.1.4)

3

(8.1.5)

As mentioned above, the wavelength and hence magnitude of k

depends on the refractive index, n. In turn, n depends on the

polarizability of the constituent molecules and their spatial

arrangement (density and orientation). Consequently, more

polarizable chemical moieties such as aromatic rings generally lead to

higher refractive indices. In the liquid state, all orientations of the

individual molecules are equally probable and we say that the liquid is

isotropic, and so do not need to worry about the fact that most

molecules are actually anisotropic. The magnitude of n usually lies

between 1.3 and 1.6 for polymers and aqueous or organic solvents.

According to the Lorentz-Lorenz equation for an ideal gas (or the

Clausius-Mosotti equation):

(8.1.7)

number of solute particles per unit volume. 4

2

The Basis What is Scattering?

Scattering is the re-radiation of a traveling wave due to a change in the

character of the medium in which the wave is traveling. For light,

scattering will be caused by local changes in refractive index or

polarizability, due to, e.g. a dust particle in the air or a polymer in the

solvent. Note that we assume nonabsorbing media here. So, the

incident light intensity will either be transmitted or scattered. If there is

no energy exchange between the medium and the wave, the incident

and scattered wave frequencies are the same and we call the

scattering process elastic. If very small differences in energy is

involved, the scattering is quasielastic. When there is large change in

the energy of the wave upon scattering, the process is inelastic.

Representative inelastic scattering in polymers include Raman and

Brillouin scattering. The former involves vibrational excitations and the

latter propagating density waves (i.e., sound waves or phonons) in the

medium. Lastly, scattering is incoherent if the intensity is independent

of scattering angle, and coherent if it depends on the scattering angle.

We will elaborate the concept of coherent scattering in this context

later. 5

If the scattering is due to randomly placed, noninteracting objects, the total scattered

intensity, Is, should be proportional to the number of scattering objects:

This should apply to the case of molecules in solution. We also anticipate larger

molecules to scatter proportionally more than smaller ones.

N.B. Suppose we scatter light from objects that are connected to one another, e.g.,

monomers within one polymer. Now the phases of the waves scattered from different

monomers should be related, because the distance rjk between any two monomers j

and k has some preferred value or range of values. This will lead to some

interference between these waves. Recall that interference between two waves is

constructive only if the difference in distance or path length difference (PLD) that the

two waves travel to the detector is some integral number of wavelengths, m, and

destructive if the PLD is an integer plus one half of . Because the PLD is on the

order of the distance between scatterers, we can therefore expect that in order to see

significant destructive interference we need the distance between scatterers to be a

significant fraction of , say a few percent. This will tum out to be the case. For visible

light with o 5000 , only for polymers that are larger than at least 100

(corresponding to polymers with Mn > ~ 105 g/mol) do we have to worry about this 6

kind of interference.

3

Basis Scattering from a Perfect Crystal

PLD =L -L = (/2)(k -k )r

1 2 s i

Consider a homogeneous array of

identical scatterers (e.g. atoms) that are k s ks

placed every 1 apart and shine light

with = 5000 on it. Every scatter will L1

re-radiate in all directions with the same L2 ki

amplitude and wavelength. For any

particular scatter and particular !

scattering direction k, we can always r Fig. 8.*

find another scatterer that produces a

scattered wave in the direction of k with path length difference (PLD)

exactly equal to /2 w.r.t. the first scatterer. This is possible because the

separation between scatterers is much less than so the array is

essentially a continuum. However, the above argument does not apply in

the forward direction (ki // ks) because the phase shift of the scattered

waves between two atoms is exactly canceled by the phase shift

between the incident waves arriving at the two atoms. Thus, the light

beam propagates through a homogeneous medium without any

scattering. 7

There are two ways by which we can generate scattering from our

hypothetical array. One would be to remove a few scatterers or add a few

scatterers with different scattering strengths than the medium molecules at

random. Then the "pairing-off" argument fails because each atom we

remove used to cancel a scattered wave from some other atom, but now it

cannot. Thus we conclude that random fluctuations in all otherwise

homogeneous medium give rise to scattering. This scattering is incoherent:

because the fluctuations are random by construction, on average there can

be no phase relation between them.

The second way of obtaining scattering from the hypothetical array would

be to make close to the distance between scatterers. Using x-rays with a

typical of 1.54, the pairing-off argument fails at specific incident angles

where the PLD between beams reflected from adjacent planes are

separated by integral multiples of , so the scattering from different atoms

will be in phase, i.e., coherent. This process is called Bragg diffraction (see

Fig. 8.3). In general, there will be coherent scattering when there is spatial

correlation between scattering objects on a distance comparable to . The

more spatial correlation between scatterers, the sharper the scattered peak

8

(scattering as a function of the scattering angle , see Fig. 8.3a) will be.

4

From Fig. 8.3b, one may see that the condition for Bragg diffraction is

(8.2.2)

(8.2.3)

cause the Bragg diffraction along ks, and that q = 2/D, where D is the inter-

planar separation.

!

ks

/2

!

ki

/2

9

Fig. 8.3 Fig. 8.4

(Rayleigh Scattering)

An incident light wave Ei will induce a dipole moment in an atom or

molecule, where

(8.3.1)

radiate an oscillating electric field that we will call the scattered E field Es.

The magnitude of this re-radiated wave depends on the direction of

observation (through the angle of detection, , as measured from Ei), the

distance from the dipole (r), the electron charge (e), and the acceleration

of the charge in the dipole (a):

(8.3.2)

10

5

Basis Scattering by an Isolated Small Molecule

(Rayleigh Scattering)

This shows that |Es* Es| ~ r- -2. Notice also that /e is the

displacement a charge e undertakes from the equilibrium position in

producing a dipole moment of . So we can write:

(8.3.3)

(8.3.4)

11

before, define to be the angle of detection measured from the polarization

direction of the incident wave or Ei. There is no angular dependence in the

x-y plane since sin = 1 along any direction in that plane. Along z, there is

no scattered wave since sin = 0 in this direction. Based on these, we

consider two cases.

Case 1: If the photodetector is in the horizontal (x-y) plane and is facing the

scatterer. At the same time, the incident Ei is polarized vertically (// z), we

expect

(8.3.5)

12

Fig. 8.5a Fig. 8.5b

6

Case 2: If the incident wave is unpolarized. We can view it as having

equal parts of vertically (// z) and horizontally (// y) polarized light.

Suppose again that the detector is in the x-y plane and is the

scattering angle as measured from the x direction (i.e., the propagation

direction of the EM wave). For the vertically polarized component (// z),

the scattered wave is the same for all . For the horizontally polarized

component (// y), is measured from the y-axis (see lower panel of

Fig. 8.5a). Clearly, sin can be written as sin(/2) = cos . So the

scattered field from the horizontally polarized part varies as cos , and

the scattered intensity as cos2. As a result, the total scattered

intensity varies as (1+cos2). Inserting this in (8.3.4), we get

(8.3.6)

13

14

7

15

Usually, the incident beam is smaller than the specimen. Its passage

through the specimen defines the illuminated or scattering volume.

Suppose we divide this volume into many cells of volume (n.b. this

volume is the same as the parameter in (8.1.7) if we consider each

cell as a scatterer particle) with the following properties:

1. 1/3 << , so each cell is effectively a point scatterer.

2. Each cell contains many monomers, with a concentration c that may

fluctuate statistically.

3. The cells are statistically independent, i.e., the fluctuations in one cell

is uncorrelated with that in other cells.

These assumptions require that Rg is smaller than 1/3. Each cell have

an instantaneous polarizability, containing an average value and a

fluctuation term:

(8.4.1)

16

8

Scattering from a Dilute Polymer Solution

Because Is/Io ~ <2> by (8.3.4), the scattering is determined entirely by

the mean-square fluctuations in polarizability,<()2>. Consider:

(8.4.3)

Assume that the scattering from the p and T fluctuations is the same in

the neat solvent as in the dilute solution. In the following discussions, we

will only consider the excess scattered intensity, Iex = Issolution - Issolvent. One

may perceive that only the fluctuation in c would affect Iex. Substituting

(8.4.2) in (8.3.5) gives Iex due to Rayleigh scattering from one cell. Since

there are 1/ number of cells per unit volume, the excess scattering due

to a unit-volume of specimen is:

equation (8.1.7):

(8.4.5) and (8.4.6), resp.

17

The key part is n/c, the refractive index increment (we drop the

reminder about constant T & P from now on), which can be measured or

looked up from tables. To find <(c)2>, write P(c) as the probability of a

given fluctuation c. So,

(8.4.7)

fluctuations, P(c) is symmetric about c = 0. Moreover, P(c) should be

related to the fluctuation in the free energy, G:

(8.4.8)

P(c) to evaluate <(c)2> by (8.4.7), one finds that 18

9

(8.4.9)

(8.4.11)

Recall that the condition for miscibility of a polymer solution is 2G/c2 > 0.

This can now be perceived from the Taylor expansion of G and the fact that

<c> = 0: For the solution to be stable, the energy change due to fluctuation

in c must be positive, so G > 0 2G/c2 > 0. With 2G/c2 > 0, the

quantity on the RHS of (8.4.11) is positive as required. Importantly, as the

spinodal is approached, 2G/c2 approaches zero. (8.4.11) implies that Iex

can get very large. Next, we relate 2G/c2 to a virial expansion. Suppose

that there are n1 moles of solvent and n2 moles of polymer in a solution that

has a volume of V (which we shall later set equal to the cell volume ):

(8.4.12a)

dV = 0 (8.4.12b)

19

(8.4.15b)

and

(8.4.16)

n1d1 + n2d2 = 0 at fixed T & P

So, (8.4.17)

But, (7.4.2)

So, (8.4.18)

20

10

and

(8.4.19)

as it fulfills the three conditions listed on p.16. By choosing V = and

substituting (8.4.19) in (8.4.11), we get:

(8.4.20)

So, (8.4.23) 21

(8.4.24a)

or (8.4.24b)

Note:

1. According to (8.4.24b), in the dilute solution limit c 0, Iex ~ R cM

which is proportional to (number of scatterers) x (scattering power of a

scatterer), as stated in (8.2.1).

2. In the dilute solution limit, light scattering measures M, and so does the

osmotic pressure. The two measurements are actually related: Light

scattering is determined by c, and their amplitude is related to the

associated osmotic cost (= [ (c + c) 0 ] / V ). One can imagine

semipermeable membranes around each of the fictitious cells. Any

fluctuations in a cells concentration will cause to change in such a way

that if c > 0, solvent in the neighboring cells wants to migrate there, and

vice versa. Essentially, thermal energy drives random fluctuations in c,

but the osmotic compressibility resists them.

22

11

3. The virial coefficient is obtainable from the

c dependence of (8.4.24b). Evidently, in a

good solvent where B > 0, the intensity will

Iex, a.u.

grow sublinearly when c is increased

sufficiently to make the second term of

(8.4.24b) significant. Conversely, for a bad

solvent with B < 0, the intensity will grow

faster than linear at large enough c. (see

c, a.u.

Fig. 8.6.)

4. There is an important difference between Fig. 8.6

light scattering and osmotic pressure

measurement. Consider the polymer to be a collection of i-mers. So,

(8.4.25)

So, (8.4.26)

24

12

Kc/R, mol/g

25

c, g/mL

Fig. 8.7

Here, we consider the finite size of a polymer. As discussed above, if the

distance, rjk, between two monomers j and k on a chain is not << , then

the waves scattered from each monomer will have a phase difference,

leading to variation in the scattered intensity with . Compared to a point

scatterer, an extended scatterer with the same content can incur some

destructive interference and hence a net reduction in the scattered

intensity. Operationally, it is convenient to define a form factor for a single

polymer, P(), as:

(8.5.1)

P() 1. Consider each (identical) monomer j to be a Rayleigh scatterer,

incurring scattered field Eo,s and a phase j in the scattered wave. The

electric field scattered by the chain, Es,tot, is given by the superposition of

the fields scattered by each monomer:

(8.5.2)

26

13

Form Factor of a Homopolymer Chain

(8.5.3)

(8.5.4)

(8.5.5)

27

So,

n.b. q = ks ki, and q =

(8.5.6)

2kisin(/2), where is the

scattering angle, equal to

the angle measured from

with (8.5.7) ki to ks.

ki ks

where P(rjk) is the probability of monomers j and k

being separated by a vector rjk. For a chain in a

theta solvent, this function is Gaussian given by

(6.7.1). Assume that the solution is isotropic, which applies in most

cases. Then it is convenient to work in spherical coordinates (r,,)

because P(rjk) has no or dependence. Observe that

(8.5.8)

(8.5.9)

28

14

Then we can write

By looking

up tables

of integral:

Since , we have

! ! q2 q4

< exp[iq rjk ] >= 1 < rjk2 > + < rjk4 > ...

6 120

(8.5.13)

29

the higher order terms on the RHS of (8.5.15), and Rg can be

determined from a simple plot of the scattering result as discussed

shortly below.

30

15

Zimm Equation

scattering of a dilute solution containing point scatterers. Here, we

attempt to modify it for the scattering of a dilute solution containing

extended, non-overlapping scatterers. The form factor, P(q) (or P())

we just derived provides the adjustment factor for the scattering power

of individual scatterers in going from being point-like to being

extended. As noted just beneath (8.4.24b), the scattering power of an

individual point-like scatterer is ~M. In a crude approach, we modify

(8.4.24a) by replacing M with P(q)M in (8.5.16) as shown below:

(8.5.16)

(8.5.17)

In the c 0 limit,

So,

making Zimm

plots 31

Zimm Plot

Recast (8.5.16) in the form of (8.4.24b). We get:

(8.5.19)

rigorous approach.

One common analysis of light-scattering data obtained from a

polymer solution is to make Zimm plots based on (8.5.18), as copied

below:

(chosen as discussed below). In practice, the data are obtained by

measuring R as a function of at several fixed concentrations, c. To

gain insight about how Zimm plots work, perceive the data as two series

of plots: One obtained by varying at several fixed c; another by varying

32

c at several fixed . (8.5.18) suggests that

16

Zimm Plot

both series should converge to the same

y-intercept of 1/Mw when q 0 and c c 0 extrapolations,

0. For the first series, the slope should slope = (4k2Rg2)/(3Mw)

be the same and ~Rg . For the second

2

Kc/R

choice of is to space out the curves in

the first series, which are separated by

c, where c is the incremental amount

of c employed in the experiment.

Accordingly, suitable choices of are 0

~1/c (with which the curves are extrapolations,

slope =

separated horizontally by amounts of 2B/3000

~1.) To analyze the plots, one first fits

the data, as functions of sin2(/2) at sin2(/2) + 3000c

various fixed c, to straight lines and find Fig. 8.8 Zimm plot for a sample of

the = 0 intercepts from the fits for each methyl cellulose in water.

c. Next, one fits the data as functions

of c at various to straight lines and find the c 0 intercepts for each .

The two procedures result in two sets of (extrapolated) points as shown in33

Fig. 8.8 by solid circles. These points would from two lines that intersect

Zimm Plot

the Kc/R axis at the same point. The value of that intercept is 1/Mw. It

can be shown that the slopes of the c = constant parallel lines are

(2kRg)2/(3Mw) and those of the = constant parallel lines are 2B/.

34

17

Example 8.3 on Zimm Plot

35

Fig. 8.9

36

18

Example 8.3 on Zimm Plot

For the c = 0 data in Fig. 8.9c, one finds that

c=0

=0

For the = 0 data in Fig. 8.9c, one finds that

Scattering Regimes

Based on (8.5.13), i.e.,

we can delineate four general regimes of behavior, depending on the value of qRg

P(q) 1. This is the Rayleigh regime and eqns (8.4.24a,b) apply.

2. If qRg 1, then only the next term in the expansion matters: P(q) 1

(q2/3)Rg2. In this regime, one can obtain Rg without knowing the shape of

the molecule. Alternatively, P(q) exp((q2Rg2)/3), and a plot of ln(Iex) vs.

q2 should be linear with slope -(Rg2)/3. This latter plot is termed a Guinier

plot and this regime is the Guinier regime.

3. If 1 qRg 10, more terms in the expansion of P(q) becomes important,

and these depend on the specific shape of the molecule. So, in this

regime the mathematical form of P(q) could help distinguish different

molecular shapes. We shall discuss some specific functional forms

below.

4. If qRg >> 1, the scattering is dominated by the internal structure of the

molecule, and one can extract no information about Rg or the shape of

the molecule.

Physically, q-1 is essentially a ruler in the sample. The choice of q dictates

38

that the scattering experiment will explore fluctuations on the length scale q-1.

19

39

40

20

Form Factor of Several Shapes

Here, we state the form factor for three particularly important shapes: the Gaussian

coil, the rigid rod, and the hard sphere.

(8.6.1)

This function applies to chains in a theta solvent and in a melt. Note that it

doesnt apply when q-1 is small and comparable to the persistence length or

statistical segment length.

2. For a rigid rod of length L and zero width, the form factor is:

(8.6.2)

(8.6.3) 41

Gaussian coils, hard spheres, and

very thin rods (a) as a funciton of

(qRg)2. (b) Inverse form factors as in

(a), showing the convergence to a

common slope of 1/3 in the small

qRg limit. (c) Form factors plotted on

a logarithmic scale, showing the

42

oscillations for the hard sphere.

21

Light Scattering Experiments

One common application of light scattering is in dynamic light scattering

(DLS) (to be discussed in the next chapter), which setup can also be

used to measure I(q). Another common application is in size-exclusion

chromatography as an absolute Mw detector, which is in routine use

nowadays.

Fig. 8.12 shows the schematic of a light scattering setup. The index

matching fluid (e.g. silicon oil and toluene whose refractive indices are

close to that of glass) serves to reduce reflection of the incident light from

the sample, which is enclosed in a glass container. The index matching

bath also provides an effective medium for controlling the sample

temperature.

Fig. 8.12 43

The scattering volume is determined by the intersection of the incident

beam and the collected beam (see Fig. 8.13). Assuming that both beams

are comparable in width, one can see that as deviates from 90o, the

volume of intersection increases by a factor of 1/sin. So the signal

should be multiplied by sin to correct for this variation.

Fig. 8.13

44

22

Samples and Solutions

Two main issues: (1) Choice of solvent (2) Need to prepare dust-free

samples.

For issue (1), one would like to have |n/c| as large as possible. It

may also be helpful to choose a solvent with a relatively small R of its

own, so that the polymer contribution to the excess scattering is

larger. (For pure solvent, scattering comes from density fluctuations,

which are determined by the isothermal compressibility of the solvent,

; the intensity is ~kT.) For issue (2), some solvents are easier to

make dust-free than others; for example, more polar solvents such as

water and THF are often trickier to clean than toluene or cyclohexane.

It is essential to remove dust, as stray particles that are significantly

larger than the polymer molecules will scatter strongly.

45

The two standard options are filtration and centrifugation, and the

former is usually preferred. Both are less than ideal, in that they may

change the concentration of the solution. There are two standard

diagnostics for the presence of dust in the sample. The first is to

examine the temporal fluctuations in the signal Ss (~Is). These should

be random, and have a root-mean-square amplitude close to

(<Ss>)1/2. If some dust is present, the signal is likely to increase

suddenly and then decrease suddenly some seconds later, as dust

particles drift in and out of the scattering volume. The second

diagnostic is to examine l0/I() versus sin2(/2) (or q2). According to

the Zimm equation this should produce a straight line. Dust will

increase I() selectively at low .

46

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