Intrinsic Viscosity: Chain Linkage in Polyvinyl Alcohol
The intrinsic viscosity of polyvinyl alcohol solutions was used to determine its molecular mass.

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Intrinsic Viscosity: Chain Linkage in Polyvinyl Alcohol
The intrinsic viscosity of polyvinyl alcohol solutions was used to determine its molecular mass.

© All Rights Reserved

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Polyvinyl Alcohol

Bea Lorraine S Acosta

Department of Chemistry

Xavier University-Ateneo de Cagayan

Corrales Avenue, Cagayan de Oro, Philippines

Abstract The experiment aimed to calculate the intrinsic where Rh is the hydrodynamic volume. The hydrodynamic

viscosity of PVOH solutions at different concentrations, volume is related in some way to the physical size of the

which was then used to determine the molecular weights of chain, given by the mean square radius of gyration as

both cleaved and uncleaved PVOH solutions using Flory

and Leutner method. Prior to calculation of intrins ic (Eq 2)

viscosity, the viscosity of the solutions was first calculated

and this was used to calculate for s pecific viscosity. where is the hydrodynamic coil expansion factor. (1)

Specific viscosity is the fractional increase in the viscosity

over that of the pure solvent caused by the addition of a Intrinsic viscosity, [], is defined as the ratio of the specific

polymer. The intrinsic viscosity was determined by viscosity to the weight concentration of solute, c, in the limit

plotting specific viscosity over concentration as a function of zero concentration:

of concentration and extrapolating at zero concentration.

The intrinsic viscosity of uncleaved and cleaved PVOH

[ ] ( ) ( ) (Eq 3)

solution was found to be 0.9434 and 0.0195 100mL g -1 ,

respectively. Using Flory and Leutner method, the average

viscosity molecular weight (M v) of both uncleaved and c is usually expressed in grams of solvent per 100 mL of

cleaved solutions were found to be 7.03710 4 and 420.4 g solution yielding [] with units of 100 g/cm3 . [] can be found

mol -1 , respectively. Moreover, the fraction of reverse by plotting either vs. c or vs. c and extrapolating to

linkages () was also calculated. The obtained delta was

zero concentration (the y-intercept of the best-fit line). (2)

found to be 0.1967; the inverse of this value is 5.086. This

implies that after cleaving the PVOH, 1 reverse link in

every 5 monomer units is formed; this large value signified

that the formation of head-to-head linkages was more II. EXPERIMENT AL SECT ION

favored during the polymerization process.

Keywords- Intrinsic Viscosity, Specific Viscosity, Polymer, The viscometer was thoroughly cleaned with chromic

Flory & Leutner Method acid cleaning solution and rinsed copiously with water, and

dried with acetone and air. The viscometer was immersed in a

water bath at 25C to equilibrate. The viscometer was

calibrated with distilled water.

I. INT RODUCT ION

Preparation of Stock Solution. A stock solution of the

polymer was prepared by weighing out accurately 4.0 to 4.5 g

The viscosity of even dilute polymer solutions is usually far

of dry polymer. It was slowly added with stirring to about 200

larger than just the viscosity of the background solvent, due to

mL of hot distilled water in a beaker. The powder was sifted

the large differences in size between the polymer and solvent

onto the surface and stirred gently to prevent bubbles and/or

molecules. In the non-free draining limit, we consider the

foam. When the entire polymer has dissolved, it was cooled

polymer chain to move as an equivalent impermeable particle

and then transferred carefully and quantitatively into a 250-

with an associated hydrodynamic volume that produces the

mL volumetric flask. The flask was filled with distilled water

same drag as the polymer chain. The friction coefficient is

up to the mark and was slowly inverted a few times to miss the

given by Stokes law as

contents.

(Eq 1)

Preparation of Uncleaved Solution. From the stock

solution, 50 mL was pipetted into 100-mL volumetric flask,

and diluted to the mark with distilled water, observing

precautions to prevent foaming. where and 0 are the viscosity of the solution and the

solvent, respectively. The calculated specific viscosities sp

Preparation of Cleaved Solution. To cleave the were 0.2798 and 0.2631.

polymer, 50 mL of the stock solution was pipetted to a 250-

mL flask; added with 25 mL distilled water and 0.25 g of solid The specific viscosity is dependent on the amount of

KIO4 . The flask was heated to about 70C and the solution PVOH in the solutions. However, it is more desirable to obtain

was stirred until all the salt was dissolved. The flask was then a viscosity independent to the concentration of PVOH

placed in a water bath and stirred until the solution was at solution. This is done by defining the viscosity of the solution

25C. The solution was transferred to a 100-mL volumetric at infinite dilution as shown in Eq 3. The intrinsic viscosity []

flask and diluted to mark with distilled water. was obtained by plotting vs. c or vs. c and

A second concentration of each material was extrapolating it to . The calculated intrinsic viscosity []

prepared by transferring 50 mL of the initial solution into a of the uncleaved PVOH solution was 0.9434100 mL g -1 .

100-mL volumetric flask and diluted to the mark with distilled Table 1 shows the summary of results while Figure 1 shows

water. All solutions were placed in water bath to equilibrate. the graph for the uncleaved solution. In Figure 1, the blue

graph represents vs. c while the red graph represents

The viscosities of the polymer solutions were vs. c; the value of the intrinsic viscosity [] is the value of the

measured using the viscometer. In between uses, it was y-intercept, where .

thoroughly rinsed with distilled water to remove the polymer,

and then dried with acetone and air. Table 1. Summary of obtained results for the uncleaved

PVOH solution.

c sp []

(g/100 mL) (g/cm3) (cP)

III. RESULT S AND DISCUSSION

0.8192 0.9980 1.144 0.2798

In this experiment, a stock solution of polyvinyl 0.4096 0.9980 1.129 0.2631 0.9434

alcohol (PVOH) was prepared and then used to produce

cleaved and uncleaved polymers. The intrinsic viscosities of

the cleaved and uncleaved PVOH solution was calculated, and

then used to calculate for the molecular weight of the

polymers.

solutions, the viscometer was calibrated to obtain its apparatus

constant B; water was used as the reference liquid. The

following equation (Eq 4) was used

(Eq 4)

g/cm3 , of the reference liquid. The calculated value of B was

0.02909.

of intrinsic viscosity of the uncleaved PVOH solution. Two Figure 1.The extrapolated graphs for the uncleaved PVOH

concentrations of this solution were prepared; 0.8192 and solution.

0.4096 g/100 mL. Using Eq 4, the calculated viscosity, ,

were 1.144 and 1.129 cP, respectively. This property is The second part of the experiment involves cleaving

dependent on the molecular properties of PVOH such as the PVOH with KIO4 . From the structure of PVOH, it can be

molecular size, molecular shape, and structure. Since it is in inferred that ts monomer unit can link to other monomer unit

solution form, it is dependent on the PVOH concentration, in a head-to-tail and head-to-head manner. The frequency of

molecular weight, and structure. The specific viscosity sp of head-to-head linkage depends on the relative rates of the head-

PVOH was calculated using the equation below (Eq 5). to-tail growth-step reaction and the head-to-head growth step

reaction.

(Eq 5)

The addition of KIO4 at 70C to the PVOH solution molecular weight known as the viscosity average molecular

causes the cleavage of 1,2-glycol linkages, which will then weight .

produce smaller chains. The size of the smaller chains depends

on the number of head-to-head linkages in the PVOH. Two kinds of averages are not equal but can be

related using the following expression (Eq 7):

In a similar manner with the first part of the

experiment, the viscosity, specific viscosity, and intrinsic

(Eq 7)

viscosity of the cleaved PVOH were calculated to be 1.160

and 0.9637 cP, 0.2975 and 0.0784, and 0.0195 100 mL g -1 .

The equation above is specific to the polydisperse PVOH.

Table 2. Summary of obtained results for the cleaved PVOH Rearranging Eq 7, was calculated to be 3.723104 and

solution. 222.4 g mol-1 for the uncleaved and cleaved PVOH,

c sp [] respectively.

(g/100 mL) (g/cm3) (cP)

By comparing the values of viscosities and average

0.8192 1.0978 1.160 0.2975 molecular weights of both uncleaved and uncleaved PVOH

0.4096 0.9980 0.9637 0.0784 0.0195 solution, it is concluded that the cleavage caused a decrease in

value of the said parameters.

was calculated using the obtained values of viscosities and

molecular weights of the uncleaved and cleaved polymer. The

fraction was calculated using the following equation (Eq 8)

(Eq 8)

uncleaved and cleaved polymer, and M 0 is the molar mass of

the monomer which is 44.0 g mol-1 . Substituting the previous

value to Eq 8 and combining it with Eq 7 gives an expression

that makes use of the viscosity average molecular weight M v

to calculate for directly (Eq 9).

( ) (Eq 9)

Figure 2.The extrapolated graphs for the cleaved PVOH

solution.

The obtained value of delta was 0.1966; the inverse

of this value is the ratio of head-to-head linkages for a number

In the molecular level, PVOH contains many single

bonds which make rotations in the structure pos sible. The of monomer units of PVOH, in this case that value is 5.086. In

the PVOH there is 1 head-to-head link in every 5 monomer

configuration around successive carbon atoms are independent

units. This large value signifies that the formation of head -to-

and unrelated, thus the two parts of PVOH chain are more

than a few carbon atoms apart are unrelated in terms of head linkages was more favored during the polymerization

process.

direction in space. Thus PVOH chain tends to adapt a tight,

ball-like form in solution.

between the molecular weight and the intrinsic viscosity for

PVOH in aqueous solution at 25C as shown in the equation

below (Eq 6): The obtained results were not guaranteed to be fully

[ ] (Eq 6) accurate due to inevitable instrumental and experimental

errors encountered during the experiment. Instrumental errors

The was calculated to be 7.037104 and 420.4 g mol-1 for include the use of uncalibrated apparatus such as the

volumetric flasks, pipettes, and burets, which contributes to

the uncleaved and cleaved PVOH, respectively. This value is

the uncertainty in calculating for the concentrations of

an average of molecular weights of molecules since PVOH is

solutions especially since concentration of solutions plays a

a polydisperse polymer; it is due to the dependence of

vital role in calculating for the viscosities. Another factor is

viscosity on both size and mass thus it produces is own

the non-uniformity of the temperature of water bath since it

affects the viscosity of the solutions. Experimental error due to 2. Uncleaved Solutions

the limitations of the experimenter includes inaccurate a. 1 st uncleaved solution

measurement of time at the appearance of the blue color in the c = 0.8192 g (100 mL)-1

reaction mixtures, which affected the calculation of the rate of = 0.9980 g cm-3

reaction.

Table B1. Data for the 1st uncleaved PVOH solution

(1/c)(ln

time (s) (cP) sp (ln /n 0 ) sp / c /n 0 )

V. CONCLUSION

39.95 1.160 0.2978 0.2607 0.3635 0.3182

Using Flory and Leutner method M v was calculated 40.32 1.171 0.3098 0.2699 0.3782 0.3294

to be 3.723104 and 222.4 g mol-1 for the uncleaved and 38.71 1.124 0.2575 0.2291 0.3143 0.2797

cleaved PVOH, respectively. This was obtained by calculating

the intrinsic viscosity for both uncleaved and cleaved solution 39.30 1.141 0.2767 0.2442 0.3377 0.2982

by plotting specific viscosity as a function of concentration. 38.70 1.124 0.2572 0.2289 0.3139 0.2794

The intrinsic viscosity of the uncleaved and cleaved PVOH

39.40 1.144 0.2798 0.3415 0.3010

was 0.9434 and 0.0195 100mL g -1 , respectively. The

obtained values for the cleaved PVOH proved the dependence

of viscosity to molar mass. The fraction of reverse linkages

b. 2 nd uncleaved solution

was calculated to be 0.1966; the inverse of this value, 5.086,

means that there is 1 reverse link in every 5 monomer units. c = 0.4096 g (100 mL)-1

= 0.9980 g cm-3

REFERENCES

(ln (1/c)(ln

time (s) (cP) sp /n 0 ) sp / c /n 0 )

(1) Viscosity of Polymer Solutions. Retrieved September 29,

39.15 1.137 0.2718 0.2404 0.6635 0.5870

2017 from

https://www.eng.yale.edu/polymers/docs/classes/polyphys/lect 39.59 1.149 0.2861 0.2516 0.6984 0.6143

ure_notes/5/handout5_wsu2.html 38.62 1.121 0.2546 0.2268 0.6215 0.5537

(2) Intrinsic Vsicsity: Chain Linkage in Polyvinyl Alcohol. 38.25 1.110 0.2426 0.2172 0.5922 0.5302

Retrieved September 29, 2017 from 38.81 1.127 0.2607 0.2317 0.6366 0.5657

http://www.chem.mun.ca/courseinfo/c3303/labs/exp_a.pdf

38.88 1.129 0.2631 0.6424 0.5702

[] = 0.9434

M v = 7.034104 g mol-1

APPENDICES M n = 3.723104 g mol-1

A. COLLECTED DATA

3. Cleaved Solutions

1. Viscometer a. 1 st cleaved solution

0 = 0.8937 cP c = 0.8192 g (100 mL)-1

= 0.9970 g cm-3 = 1.0978 g cm-3

B = 0.02909

Table B1. Data for the 1st cleaved solution.

Table A1. Data for calibration of viscometer. (1/c)(ln

time (s) (cP) sp (ln /n 0 ) sp / c /n 0 )

time (s) B

35.33 1.128 0.2625 0.2331 0.3204 0.2845

30.97 0.02894

37.37 1.193 0.3354 0.2892 0.4094 0.3530

31.08 0.02884

36.34 1.161 0.2986 0.2613 0.3644 0.3189

30.41 0.02948

36.99 1.181 0.3218 0.2790 0.3928 0.3406

30.82 0.02909

35.52 1.134 0.2693 0.2384 0.3287 0.2911

36.31 1.160 0.2975 0.3631 0.3176

b. 2 nd cleaved solution 5) Mn

c = 0.8192 g (100 mL)-1

= 0.9980 g cm-3

Table B2. Data for the 2nd cleaved solution.

(ln (1/c)(ln

time (s) (cP) sp /n 0 ) sp / c /n 0 )

6) Reverse linkages fraction,

34.45 1.0001 0.1191 0.1125 0.2908 0.2747

( )

33.23 0.9647 0.0795 0.0765 0.1940 0.1867

34.05 0.9885 0.1061 0.1009 0.2591 0.2462 ( )

32.80 0.9522 0.0655 0.0635 0.1599 0.1549

32.80 0.9522 0.0655 0.0635 0.1599 0.1549

32.56 0.9453 0.0577 0.0561 0.1409 0.1370

32.48 0.9430 0.0551 0.0536 0.1346 0.1310

33.20 0.9637 0.0784 0.1913 0.1836

[] = 0.0195

M v = 420.4 g mol-1

M n = 222.4 g mol-1

B. SAMPLE CALCULATIONS

1) Viscometer constant, B

2) Viscosity of solutions,

3) Specific viscosity, sp

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