SlideShare a Scribd company logo
1 of 7
Download to read offline
IOSR Journal of Applied Chemistry (IOSR-JAC)
e-ISSN: 2278-5736.Volume 10, Issue 4 Ver. I (April. 2017), PP 67-73
www.iosrjournals.org
DOI: 10.9790/5736-1004016773 www.iosrjournals.org 67 |Page
Synthesis and Characterization of Different Molecular Weights
Polyacrylamide
Raid Saleh Shatat1*
, S. Kalimulla Niazi1
,Azlan Ariffin2
1
Riyadh Colleges of Dentistry and Pharmacy, 84891 Riyadh 11681, Kingdom of Saudi Arabia. Tel: 920000842.
Fax: 920000843
2
School of Material and Mineral Resources, UniversitiSains Malaysia, KampusKejuruteraan, 14300
NibongTebal, SeberangPerai Selatan, Penang, Malaysia
*corresponding Author
Abstract: Polyacrylamides of varying molecular weights (very low, low, medium, high and very high) were
synthesized using free radical polymerization and characterized by Infra Red (IR) spectroscopy, viscosity
measurements, glass transition temperature (Tg) measurement and thermal gravimetric analysis (TGA).
Thioglycolic acid and hydrogen peroxide were used as initiators to synthesis very low and low molecular weight
polyacrylamides respectively. Molecular weights (medium, high and very high) polyacrylamides were
synthesized using potassium persulfate and N,N,N',N'- tetramethylethylenediaminesystem as initiators. The
synthesis of medium, high and very high molecular weight polyacrylamides were achieved by increasing the
concentration of acrylamide monomer. Fourier Transform Infrared Spectroscopy (FTIR) of polyacrylamides
showed strong absorption at wave number 1655 cm-1
due to the presence of primary amide band. The results
also showed that the increase in the intrinsic viscosity and glass transition temperature were proportional to the
increase in molecular weight of polyacrylamide. On the other hand it can be seen an increase in molecular
weight caused a decrease of weight loss %.
Keywords:polyacrylamide, molecular weight, free radical polymerization, characterization.
I. Introduction
Natural polyelectrolytes (e.g. starch, gelatin, tannins, etc.) and inorganic electrolytes (e.g. aluminum
sulphate, ferric sulphate, ferric chloride, etc.) have been traditionally as agents in water and wastewater
treatment for the removal of colloidal suspended solids. The operations of these agents involve particle
agglomeration by coagulation and flocculation processes (1). The uses of synthetic organic polyelectrolytes in
water and wastewater treatment have been introduced in late 1950. Synthetic polyelectrolytes have been used
extensively as coagulation aids or to replace inorganic electrolytes coagulants completely (2). The use of
synthetic polyelectrolytes as flocculant is increasing rapidly. Polyelectrolytes increase floc strength allowing
bigger and stronger flocs to be formed. The increased floc strength can improve settling characteristics.
Synthetic organic polyelectrolytes are known to be more efficient than the inorganic electrolytes agents in the
removal of suspended colloidal particles (3). The effectiveness of synthetic organic polyelectrolytes as
flocculants increases with increasing molecular size, the limit of which is only dictated by problems in
solubility. Polyelectrolytes having molar masses greater than 10 million g/mol do not dissolve readily but tend
to form gel lumps known as "fish eyes". Polymers of lower molar mass are highly soluble in water due to the
hydration of functional groups along the molecule. Polyacrylamide shows high solubility in water, while it is
insoluble in most other common organic liquids such as methanol, ethanol and acetone. However, despite this
highly hydrophilic character, the main technical application of polyacrylamide is for flocculation of aqueous
suspension and related purposes. Polyacrylamides can be classified to three categories: non-ionic, anionic and
cationic polyacrylamides (4). Polyacrylamides were used extensively as a flocculant in the clarification of water
in industrial and municipal processes (5). Cationic polyelectrolytes are a class of polyelectrolytes that derive
their unique properties from the density and distribution of positive charges along a macromolecular backbone
as well as molecular weight. Cationic functional groups can strongly interact with suspended, negatively
charged particles or oil droplets and are useful for many applications including wastewater treatment and
papermaking. There is a greater variety of molecular structures in the cationic family than any of the other
polyelectrolytes. The present study involves the synthesis and characterization of different molecular weight
polyacrylamides using free radical polymerization.
Synthesis and characterization of different molecular weights polyacrylamide
DOI: 10.9790/5736-1004016773 www.iosrjournals.org 68 |Page
II. Materials and methods
Chemicals
Acrylamide (Fluka, 99%), potassium persulfate (98%), and N,N,Nâ€Č,Nâ€Č- tetramethylethylenediamine (TMEDA)
(98%)were purchased from Fluka, Germany as laboratory grade .Thioglycolic acid, hydrogen peroxide, acetone,
ethanol and methanol were purchased from Merck, Germany as laboratory grade.
Equipment and instrumentation
The polymerization reaction was carried out in a Memmert water bath (thermostatically controlled,
heating capacity up to 100ÂșC). A 1 litre five-necked Pyrex glass reactor was suitably placed into the Memmert
water bath. The reactor was equipped with a mechanical stirrer, condenser equipped with water collector,
thermometer and nitrogen gas (Oxygen Free Nitrogen) inlet tube.
Recrystallization of chemicals
Acrylamide (AM) was dissolved in acetone at 56ÂșC (boiling point of acetone) to form a saturated
solution, the solution was then filtered to remove insoluble particles and allowed to cool so that the dissolved
substance is crystallized, the solid crystals were separated from acetone by filtration under suction using a
BĂŒchner funnel, washed with cold acetone and then dried in vacuum for 24 h at 60 ÂșC. This method was
repeated twice. Potassium persulfate was recrystallized twice from distilled water at 100ÂșC (boiling point of
distilled water) using the same procedure described above. The rest of the chemicals were used without further
purification.
Synthesis of different molecular weight polyacrylamides
Acrylamide monomer is crystalline. It is relatively stable and is soluble in water and many organic
solvents (acetone, ethanol, methanol, etc.). Acrylamide polymerizes easily by conventional free radical methods.
Solutions of acrylamide in water polymerize at 40 ÂșC under the influence of nearly all free radical sources
including persulfates, peroxides, azo compounds and redox couples. The synthesis of different molecular weight
polyacrylamides is strongly influenced by temperature, solvent, type of initiator, concentration of the initiator
and concentration of the monomer.
Synthesis of very low molecular weight polyacrylamide
Under nitrogen atmosphere, a mixture of acrylamide monomer (10gm), thioglycolic acid (0.20gm) and
tetrahydrofuran (THF) (20ml) were placed in 500 ml five-necked Pyrex glass reactor equipped with a reflux
condenser and a mechanical stirrer placed in a constant temperature bath at 40ÂșC.The polymerization was
performed for 2 h under stirring. The polyacrylamide was isolated and re-precipitated by pouring its solution
into acetone. It was then dried under vacuum at 60ÂșC for 24 h.
Synthesis of low molecular weight polyacrylamide
The acrylamide monomer was polymerized in distilled water, using hydrogen peroxide as the initiator.
Nitrogen gas was bubbled inside a five-necked Pyrex glass reactor containing the acrylamide monomer (20 gm),
distilled water (200 ml) as a solvent and hydrogen peroxide (0.5 ml) as initiator. The reactor was placed in a
constant temperature bath 90ÂșC for 3 h under stirring. The polyacrylamide was isolated and re-precipitated by
pouring its solution into acetone. It was then dried under vacuum at 60ÂșC for 24 h.
Synthesis of medium, high and very high molecular weight polyacrylamide
High purity of the monomer and initiators and the absence of oxygen are essential in the
polymerization process. High concentration of monomers, low concentration of initiators are required to
synthesized medium, high and very high molecular weight polyacrylamides. Different molecular weight
(medium, high and very high) polyacrylamides were synthesized using the potassium persulfate and N,N,N’,N’-
tetramethylethylenediamine (TMEDA) system as initiator. Increasing the concentration of acrylamide monomer
will increase the molecular weight of the resulting polyacrylamide. Thus, under nitrogen atmosphere 15, 30 and
50 gm of acrylamide monomer were polymerized in (500ml) distilled water as a solvent and the (0.135gm)
potassium persulfate/(180ÎŒl) TEMDA system as initiator to produce medium, high and very high molecular
weight polyacrylamides respectively.
The mixture were placed in 500 ml five-necked Pyrex glass reactor equipped with a reflux condenser
and mechanical stirrer placed in a constant temperature bath at 40ÂșC. The polymerization was performed for 2 h
under stirring. The polyacrylamide was isolated and re-precipitated by pouring its solution into acetone. It was
then dried under vacuum at 60ÂșC for 24 h.
Synthesis and characterization of different molecular weights polyacrylamide
DOI: 10.9790/5736-1004016773 www.iosrjournals.org 69 |Page
Characterization of synthesized polyacrylamide
The polymer characterization is almost as important as polymer preparation. Without characterization, polymer
synthesis becomes additional exercise.
Fourier Transform Infrared (FTIR) Spectra analysis
Fourier transform infrared spectroscopy (FTIR) is a very important step in polymer characterization. FTIR is
used very extensively for the characterization of polymer materials in polymer chemistry (6). FTIR technique is
normally used in the investigation of polymer structure and analysis of their functional groups.
Nicolet FTIR machine, Model: Avator 360 FTIR spectrometer, manufactured by Nicolet analytical instrument
USA Inc., USA was used in this study. Analysis was conducted by identification of acrylamide monomer and
synthesized products (polyacrylamide).
Potassium bromide (KBr) pellet was prepared by using a sampling device. Approximately 5-10 mg of
the sample powder and 90-95 mg of KBr was blended, triturated and mixed well with agate mortar and pestle
for 5 min. The mixture was transferred to the IR sampling device and then compacted using an IR hydraulic
press for 60 seconds. KBr pellet was placed into FTIR window and then scanned by taking blank spectrum.
After completion of the spectrum of the blank, KBr pellet was taken off from the window and KBr pellet thinly
coated with test sample was placed again in the FTIR window to measure the spectrum of the sample. On
average, 10 scans were used for the synthesized sample.
Glass transition temperature (Tg) measurement
Glass transition temperature (Tg) is an important characteristic property of a polymeric material
because its fabrication and/or applications depend on it. It is a feature of polymeric materials that they may be
entirely amorphous, partly amorphous and partly crystalline. The glass transition temperature (Tg)of all
synthesized polyacrylamides were measured using Perkin-Elmer, Differential Scanning Calorimetry (DSC)
thermal analyzer. It is equipped with a DSC cell programmed at a heating rate of 10 ÂșC/min., measuring
temperature range was 25 ÂșC to 250 ÂșC.Samples were prepared for DSC measurement by weighting between 5.0
mg to 10.0 mg of dry polymer into an aluminum pan. The pan was then sealed with an aluminum cap. Similarly,
an empty aluminum pan was used as reference.
Viscosity average molecular weight of polyacrylamide
The viscosity average molecular weight of polyacrylamides was carried out by determining the
intrinsic viscosities of the polyacrylamides using Ubbelohede viscometer, no. 4809 ASTM at 25 ± 0.1ÂșC. The
polyacrylamide solutions were prepared in distilled water. The intrinsic viscosity calculations were made for
polyacrylamide after filtration through 250-micron sieve to remove any undissolved ‘gel’ lumps.
Dilute solution viscosity method was used to determine the viscosity average molecular weight of the
polyacrylamide samples by determining their intrinsic viscosities. Test sample was prepared by dissolving 0.5g
of polyacrylamide in 100 ml distilled water at room temperature using magnetic stirrer. The resultant solution
was filtered through 250-micron sieve to remove any undissolved ‘gel’ lumps. A series of polyacrylamide
working solution with concentrations ranging between 5 X 10-3
and 1 X 10-3
g/ml were prepared by appropriate
dilution of the test sample with distilled water.
Approximate amounts of the solution were transferred into Ubbelhode viscometer and the viscometer
placed inside a water bath set at 25 ± 0.1ÂșC and allowed to equilibrate. The efflux time (i.e. the time taken for
the liquid inside the viscometer to pass from the upper meniscus to the lower meniscus was determined). An
average of the three readings (which did not differ by more than 3 seconds) was taken for each sample.
Thermal gravimetric analysis (TGA)
Samples were prepared for TGA measurements by weighting between 5.0 to 10.0 gm of dry polyacrylamide into
aluminum pan. The pan was then sealed with aluminum cap.
Thermal gravimetric analysis (TGA) of different molecular weight polyacrylamides were carried out in the
temperature range of 30-600 ÂșC at a heating rate of 10 ÂșC/min under nitrogen using Perkin-Elmer.
III. Results and Discussion
The molecular weight of polyacrylamide can be varied by several techniques, including monomer
concentration, initiator concentration and initiator type and polymerization temperature. The monomer
concentration can be increased to 50% or more for high molecular weight polyacrylamide since the viscous
polymer molecular weight is the internal phase. High purity of the monomer and initiators and the absence of
oxygen are essential in the polymerization process.
The polymerization reaction at different temperaturesof acrylamide monomer with different initiators
i.e. thioglycolicacid (40ÂșC), hydrogen peroxide (90ÂșC), and potassium persulfate/ N,N,N’,N’-
tetramethylethylenediamine (TMEDA) (40ÂșC), gave the targeted very low, low, medium, high and very high
Synthesis and characterization of different molecular weights polyacrylamide
DOI: 10.9790/5736-1004016773 www.iosrjournals.org 70 |Page
molecular weight polyacrylamide products (shown in Table 1). The synthesis of high and very high molecular
weight polyacrylamide was achieved by increasing the concentration of acrylamide monomer using potassium
persulfate/TMEDA as initiatorat moderate temperature.
The synthesis route of the preparation of polyacrylamide is shown in table 1. The choice of initiators and
monomer concentrations were also studied.
Table 1: Type of initiator used and resultant molecular weight polyacrylamide
Type of initiator used Resultant molecular weight polyacrylamide
Thioglycolicacid Very low
Hydrogen peroxide Low
Potassium persulfate/ (TMEDA) Medium, high and very high
The structure of different molecular weight polyacrylamides was determined through the study of FTIR spectra.
Glass transition temperature (Tg), viscosity average molecular weight and thermal gravimetric analysis of
polyacrylamide were also carried out.
Synthesis of very low molecular weight polyacrylamide
Very low molecular weight polyacrylamide was synthesized by free radical polymerization using
thioglycolic acid as initiator at moderate temperature (40ÂșC).The ratio of thioglycolic acid to acrylamide
monomer was about 0.02 (g/g) and polyacrylamide with molecular weight of about 20,000 g/mole was
produced. The use of thioglycolic acid as a chain transfer agent has been shown to be a very effective method
for the production of very low molecular weight polyacrylamide (7).
Thioglycolic acid is used as a chain transfer agent where it is desirable to decrease the molecular
weight in radical polymerization. Thioglycolic acid enters the propagation scheme by giving up a proton to the
growing radical chain, terminating it, but possibly initiating a new chain.
The thioglycolic acid was found to be an acceptable initiator for the production of a very low molecular
weight polyacrylamide at moderate temperature and maximum yield was obtained without any unwanted side
products. The product was a white coloured liquid with very low viscosity.
Acetone was used to isolate and re-precipitate the polyacrylamide product from its liquid solution and dried
under vacuum at 60ÂșC for 24 h to produce a yield of 70-75% of very low molecular weight polyacrylamide.
Synthesis of low molecular weight polyacrylamide
Low molecular weight polyacrylamide was synthesized using hydrogen peroxide as initiator and the
reaction was carried out at high temperature (90ÂșC) to give polyacrylamide free of contaminates detected by
FTIR spectroscopy. The product was a low viscosity white colour liquid. The polyacrylamide product was
precipitated from its liquid solution using acetone and then dried under vacuum at 60ÂșC for 24 h to produce a
yield of 70-75% of low molecular weight polyacrylamide.
The molecular weight was found to be 170 X 103
g/mol using viscosity measurements, which is considered to be
low.
Synthesis of medium, high and very high molecular weight polyacrylamide
Potassium persulfate/TMEDA system as initiator was used for the synthesis of medium, high and very
high molecular weight polyacrylamides. TMEDA exerts a high promoting effect on the free radical
polymerization initiated by potassium persulfate. The rate of polymerization increases by about three times in
the presence of TMEDA. Potassium persulfate/TMEDA system can reduce the reaction time and react at
moderate temperature (40ÂșC).
Potassium persulfate/ TMEDA system was found to be an acceptable redox initiator for the production
of medium, high and very high molecular weight polyacrylamides at moderate temperature and a maximum
yield of 90-95% was obtained without any unwanted side products. The product was a high viscosity white
colour liquid. Polyacrylamide was precipitated from the solution using acetone and then dried under vacuum at
60ÂșC for 24 h. Figure 1 shows the effect of monomer concentration on molecular weight of polyacrylamide. As
shown, the concentration of acrylamide monomer strongly affects the molecular weight of polyacrylamide. An
increase in acrylamide monomer concentration caused an increase in molecular weights of polyacrylamide.
The fact that high concentration of monomer will initiate many sites, resulting in longer
polyacrylamide chains, on the other hand shorter polyacrylamide chains at lower concentration of monomer.
This is reflected in their corresponding intrinsic viscosity values.
Intrinsic viscosity of a polymer is a measure of its hydrodynamic volume in solution, which in turn
depends upon its molecular weight, nature of the solvent and the temperature of the medium (8). For polymers
of low molecular weight, the hydrodynamic volume will be low and thus it has low intrinsic viscosity value.
Synthesis and characterization of different molecular weights polyacrylamide
DOI: 10.9790/5736-1004016773 www.iosrjournals.org 71 |Page
Further, in the case of high molecular weight polymers the hydrodynamic volume will be high and therefore
higher will be its intrinsic viscosity. This has been observed in practice (Figure 1).
Figure 1: Influence of monomer concentration on molecular weight of polyacrylamide
IV. Characterization
Fourier Transform Infrared (FTIR) spectra analysis
Fourier Transform Infrared Spectroscopy (FTIR) of polyacrylamide showed strong absorption at wave
number 1655 cm-1
due to the presence of a primary amide band which is used to distinguish true polyacrylamide
from the alternative polymerization product poly(ÎČ-alanine) which has instead a secondary amide band at 1555
cm-1
(4). The band for (N—H) stretching vibration appears at 3448 cm-1
of the NH2 group. Further, the absence
of (C==C) band which usually appears at 1610 cm-1
proved that the acrylamide monomer has been completely
converted to polyacrylamide and no residue of monomer is present in the polymer (9) studied the FTIR spectra
of polyacrylamide, their finding is in a good agreement with our results.
Glass transition temperature (Tg) measurement
The glass transition is a physical change from the glassy to the liquid state which occurs in amorphous
solids when they are heated. This point is characterised by the glass transition temperature determined by
Differential Scanning Calorimetry (DSC). The glass transition temperature, Tg, of very low, low, medium, high
and very high molecular weight polyacrylamide appeared at 100.944, 109.077, 120.811, 148.727 and 154.461°C
respectively.
This shows that up to these relatively high temperatures the polyacrylamide was in the glassy state and
thus relatively resistant to the ingress (way in) or egress (way out) of small molecule penetrate, and it is
necessary to use higher temperatures to put the polymer in the rubbery state where adsorbed solvent molecules
are sufficiently mobile to be desorbed.Molecular weight influences Tg significantly. At lower molecular weights
where the excess of free volume associated with chain ends is significant. As molecular weight increases the
concentration of chain ends decreases until its contribution to the free volume becomes negligible.
Louie and Hartwig observed an increase in glass transition temperature with increase the molecular weight of
polymer. The results of this work are in a good agreement with their work (10).
Synthesis and characterization of different molecular weights polyacrylamide
DOI: 10.9790/5736-1004016773 www.iosrjournals.org 72 |Page
Determination of approximate molecular weight
Viscometry and application of Mark-Houwink equation is one of the simplest and most rapid methods
used for determining the molecular weights of polymers.Molecular weight of the polyacrylamide samples can be
estimated from the intrinsic viscosity values. Mark–Houwink equation is generally employed for the estimation
of molecular weight of linear polymers.
The molecular weights of polyacrylamide samples were determined by determining their intrinsic
viscosities using Ubbelohede viscometer. The polyacrylamide samples were filtered with 250-micron sieve after
dissolution in distilled to prevent particulate impurities from entering the capillary of the viscometer and affect
the flow rate of the solution through it.
The determination of viscosity average molecular weight from the measurement of intrinsic viscosity
require working in a dilute solution using a suitable solvent. Therefore, in this study, the concentration of
polyacrylamide solutions ranging from 1x10-3
to 5x10-3
g/ml were prepared by appropriate dilution of the test
sample with distilled water. By increasing the concentration of polyacrylamide, the intermolecular interactions
increased leading to the formation of intermolecular complexes, resulting in the enhancement of densities.
Therefore, relatively higher values in the efflux time at higher concentration of polyacrylamide solution were
predictable.
The values of relative, specific, reduced and inherent viscosities of the various concentrations of the
very low, low, medium, high and very high polyacrylamides were determined.
It was found that by increasing the polyacrylamide concentrations from 1x10-3
to 5x10-3
g/ml the efflux time
increased. As a result, the relative viscosity increased with an increase in the polyacrylamide concentration.
Other viscosities namely specific and reduced viscosities also increased with an increase in the polyacrylamide
concentration. On the other hand, the inherent viscosity was inversely proportional to the increase in
polyacrylamide concentration.
The intrinsic viscosity [η], which is defined as the intercept on the abscissa at zero concentration, was
determined by plotting the reduced viscosity of the solution of different concentrations of polyacrylamide
solutions. Intrinsic viscosity of the very low, low, medium, high and very high polyacrylamides samples were
obtained.The results of intrinsic viscosity and viscosity average molecular weight are tabulated in table 2. It can
be seen that the increase in the intrinsic viscosity was proportional to the increase in molecular weight of
polyacrylamide.
Table 2: Intrinsic viscosity and viscosity average molecular weight of different polyacrylamides
Polyacrylamide Intrinsic viscosity (g/dl) Viscosity average molecular weight (g/mole)
Very low 13 19,040
Low 76 173,089
Medium 186 508,563
High 456 1,625,402
Very high 1535 Over 5 million
Thermal gravimetric analysis (TGA)
TGA is used primarily for determining thermal stability of polymers. TGA method is based on
continuous measurement of weight on a sensitive balance as sample temperature is increased in an inert
atmosphere. Data are recorded as a thermogram of weight versus temperature. Initially weight loss may arise
from evaporation of residual moisture or solvent, but at higher temperatures it results from polymer
decomposition (11). The thermal stability of the different molecular weight polyacrylamides has been studied
by TGA from 50ÂșC up to approximately 600ÂșC. The very high molecular weight polyacrylamide displayed the
highest stability in the series, indicating the importance of the molecular weight for thermal stability. On the
other hand, very low molecular weight polyacrylamide displayed the lowest stability.
The increase in molecular weight caused a decrease of weight loss %. The residue at 600ÂșC being
11.67%, 14.68%, 17.83%, 19.45%, and 22.55% for the cases of very low, low, medium, high and very high
molecular weight polyacrylamides respectively. The activation energy values for various stages of
decomposition were calculated from thermal gravimetric analysis (TGA). The TGA of polyacrylamide was
three-staged, as observed before by Ismail et al. (12). First, the loss of water which is nonstoichiometric
occurred. This is followed by the subsequent loss of ammonia and other gaseous products from the
polyacrylonitrile structure formed during the decomposition of polyacrylamide and partly from the remaining
polyacrylamide in the course of heating to 600 ÂșC.
For polyacrylamide moisture release takes place at a slow rate over the temperature zone of 40-200ÂșC
accounting for successive release of absorbed moisture and bound (H-bounded) water. A relatively high mass
loss zone then follows till about 400ÂșC which correspond to cyclization of polyacrylamide and associated
liberation of NH3. A much sharper mass loss zone appears over the temperature zone of 400-500ÂșC accounting
Synthesis and characterization of different molecular weights polyacrylamide
DOI: 10.9790/5736-1004016773 www.iosrjournals.org 73 |Page
for large-scale thermal degradation with the liberation of H2, CO and NH3, leaving a residue of about 22% at
600ÂșC (9).
References
[1]. Gill, R. I. S. (1985). The flocculation of kaolinite suspensions using cationic polyacrylamide. Ph.D, thesis, The University of
Reading, Reading, Berkshire. England.
[2]. Culp, R.L. (1977). Direct filtration. J. Amer. Water Works Assoc., 69 (7), 378.
[3]. Gill, R. I. S. and Herrington, T. M. (1988). Floc size studies on kaolin suspensions flocculated with cationic polyacrylamides,
Colloid and surfaces, 32, 331-344.
[4]. Molyneux, P. (1982). Water-soluble synthetic polymers: properties and behavior. Volume I. Florida: CRC Press.
[5]. Ives, K.J. (1978). The Scientific Basis of Flocculation, NATO ASI series, Sijthoff and Noordhoof, Alphen aan den Rijin, (Ed.).
[6]. Thompson, H. W. and Torkington, P. (1945). Trans. Farad. Soc., 41, 246.
[7]. Öz, N and Akar, A. (2000). Low molecular weight polyacrylic acid with pendant aminomethylenephosphonic acid groups. J. App.
Poly. Sci., 78, 870-874.
[8]. Nayak, B. R. and Singh, R. P. (2001). Synthesis and characterization of grafted hydroxypropyl guar gum by ceric ion induced
initiation. Eur. Poly. J., 37(8), 1655-1666
[9]. Ghosh, P. Chakrabarti, A. and Siddhanta S. K. (1999). Studies on stable aqueous polyaniline prepared with the use of
polyacrylamide as the water soluble support polymer. Euro. Poly. J., 35(5), 803-813.
[10]. Louie, J. and Hartwig, J.F. (1997). Discrete high molecular weight triarylaminedendrimers prepared by palladium-catalyzed
amination. J. Am. Chem. Sco., 119, 11659-11696.
[11]. Stevens, M. P. (1990). Polymer Chemistry an Introduction (2nd
ed.) 171-172.
[12]. Ismail, M. Vangani, V. Rakshit, A. K. (1997). Terpolymerization of acrylamide, acrylic acid, and acrylonitrile: synthesis and
properties. J. App. Poly. Sci.,69, 217-228.

More Related Content

What's hot

Extraction of glycosides
Extraction of glycosidesExtraction of glycosides
Extraction of glycosidesZainab&Sons
 
Drug stability
Drug stability Drug stability
Drug stability jaatinpubg
 
Extration of tannins
Extration of tanninsExtration of tannins
Extration of tanninsZainab&Sons
 
Process chemistry
Process chemistryProcess chemistry
Process chemistryDivya V
 
Preliminary phytochemical and diuretic potential of methanolic extract of azi...
Preliminary phytochemical and diuretic potential of methanolic extract of azi...Preliminary phytochemical and diuretic potential of methanolic extract of azi...
Preliminary phytochemical and diuretic potential of methanolic extract of azi...srirampharma
 
Coumarins
CoumarinsCoumarins
CoumarinsRahul B S
 
TANNINS&FLAVENOID AND GLYCOISIDE
TANNINS&FLAVENOID AND GLYCOISIDETANNINS&FLAVENOID AND GLYCOISIDE
TANNINS&FLAVENOID AND GLYCOISIDEMINANI Theobald
 
Phytochemistry of plant drugs
Phytochemistry of plant drugsPhytochemistry of plant drugs
Phytochemistry of plant drugsAl Riyad Hasan
 
phytochemical assay of phenolic compounds
phytochemical assay of phenolic compounds phytochemical assay of phenolic compounds
phytochemical assay of phenolic compounds gaurav gautam
 
Extraction, Estimation and Thin Layer Chromatography of Tannins: A Review
Extraction, Estimation and Thin Layer Chromatography of Tannins: A ReviewExtraction, Estimation and Thin Layer Chromatography of Tannins: A Review
Extraction, Estimation and Thin Layer Chromatography of Tannins: A ReviewDr. Amit Gangwal Jain (MPharm., PhD.)
 

What's hot (19)

Extraction of glycosides
Extraction of glycosidesExtraction of glycosides
Extraction of glycosides
 
Drug stability
Drug stability Drug stability
Drug stability
 
Extration of tannins
Extration of tanninsExtration of tannins
Extration of tannins
 
Alkaloids
AlkaloidsAlkaloids
Alkaloids
 
Antioxidants and preservatives
Antioxidants and preservativesAntioxidants and preservatives
Antioxidants and preservatives
 
Process chemistry
Process chemistryProcess chemistry
Process chemistry
 
Preliminary phytochemical and diuretic potential of methanolic extract of azi...
Preliminary phytochemical and diuretic potential of methanolic extract of azi...Preliminary phytochemical and diuretic potential of methanolic extract of azi...
Preliminary phytochemical and diuretic potential of methanolic extract of azi...
 
Coumarins
CoumarinsCoumarins
Coumarins
 
Terpenoids
Terpenoids Terpenoids
Terpenoids
 
TANNINS&FLAVENOID AND GLYCOISIDE
TANNINS&FLAVENOID AND GLYCOISIDETANNINS&FLAVENOID AND GLYCOISIDE
TANNINS&FLAVENOID AND GLYCOISIDE
 
Glycosides Note
Glycosides Note Glycosides Note
Glycosides Note
 
Phytochemistry of plant drugs
Phytochemistry of plant drugsPhytochemistry of plant drugs
Phytochemistry of plant drugs
 
phytochemical assay of phenolic compounds
phytochemical assay of phenolic compounds phytochemical assay of phenolic compounds
phytochemical assay of phenolic compounds
 
Rutin
RutinRutin
Rutin
 
Luucky
LuuckyLuucky
Luucky
 
Alkaloids,
Alkaloids, Alkaloids,
Alkaloids,
 
Extraction, Estimation and Thin Layer Chromatography of Tannins: A Review
Extraction, Estimation and Thin Layer Chromatography of Tannins: A ReviewExtraction, Estimation and Thin Layer Chromatography of Tannins: A Review
Extraction, Estimation and Thin Layer Chromatography of Tannins: A Review
 
Glycosides introduction
Glycosides introductionGlycosides introduction
Glycosides introduction
 
Alkaloids (full)
Alkaloids (full)Alkaloids (full)
Alkaloids (full)
 

Similar to Synthesis and Characterization of Polyacrylamide by Molecular Weight

0 immobilization of laccase
0 immobilization of laccase0 immobilization of laccase
0 immobilization of laccaseRajesh Dahiya
 
Biocompatibility of Polymethylmethacrylate resins
Biocompatibility of Polymethylmethacrylate resinsBiocompatibility of Polymethylmethacrylate resins
Biocompatibility of Polymethylmethacrylate resinsHashmat Gul
 
Studies on some economic and effective Ion exchange Resin used as catalyst in...
Studies on some economic and effective Ion exchange Resin used as catalyst in...Studies on some economic and effective Ion exchange Resin used as catalyst in...
Studies on some economic and effective Ion exchange Resin used as catalyst in...IOSR Journals
 
shao2003.pdf
shao2003.pdfshao2003.pdf
shao2003.pdfmarakiwmame
 
SYNTHESIS OF DRUG CARRIER POLYACRYLIC
SYNTHESIS OF DRUG CARRIER POLYACRYLICSYNTHESIS OF DRUG CARRIER POLYACRYLIC
SYNTHESIS OF DRUG CARRIER POLYACRYLICTaghreed Al-Noor
 
Synthesis and Characterization of cyclohexylidene containing novel cardo pol...
	Synthesis and Characterization of cyclohexylidene containing novel cardo pol...	Synthesis and Characterization of cyclohexylidene containing novel cardo pol...
Synthesis and Characterization of cyclohexylidene containing novel cardo pol...inventionjournals
 
Synthesis, Characterization and Performance Evaluation of Poly Octadecyl Meth...
Synthesis, Characterization and Performance Evaluation of Poly Octadecyl Meth...Synthesis, Characterization and Performance Evaluation of Poly Octadecyl Meth...
Synthesis, Characterization and Performance Evaluation of Poly Octadecyl Meth...IOSRJAC
 
Ind. Eng. Chem. Res. 2009, 48, 4866–4871_Synthesis of Ultrahigh Molecular Wei...
Ind. Eng. Chem. Res. 2009, 48, 4866–4871_Synthesis of Ultrahigh Molecular Wei...Ind. Eng. Chem. Res. 2009, 48, 4866–4871_Synthesis of Ultrahigh Molecular Wei...
Ind. Eng. Chem. Res. 2009, 48, 4866–4871_Synthesis of Ultrahigh Molecular Wei...Shashi Kant
 
depolymerization-of-high-molecular-weight-into-a-predicted-low-molecular-weig...
depolymerization-of-high-molecular-weight-into-a-predicted-low-molecular-weig...depolymerization-of-high-molecular-weight-into-a-predicted-low-molecular-weig...
depolymerization-of-high-molecular-weight-into-a-predicted-low-molecular-weig...trunghieuchinh
 
multicomponent reaction mediated by PEG-400
multicomponent reaction mediated by PEG-400multicomponent reaction mediated by PEG-400
multicomponent reaction mediated by PEG-400Anilkumar Shoibam
 
Synthesis and Characterization of PMMA Nano-composites
Synthesis and Characterization of PMMA Nano-composites Synthesis and Characterization of PMMA Nano-composites
Synthesis and Characterization of PMMA Nano-composites Kanchan Ramteke
 
10.1016@j.carbpol.2011.04.046.pdf
10.1016@j.carbpol.2011.04.046.pdf10.1016@j.carbpol.2011.04.046.pdf
10.1016@j.carbpol.2011.04.046.pdfyassine471731
 
Melamine epichlorohydrin prepolymers syntheses and characterization
Melamine epichlorohydrin prepolymers syntheses and characterizationMelamine epichlorohydrin prepolymers syntheses and characterization
Melamine epichlorohydrin prepolymers syntheses and characterizationArif Yavuz Akartepe
 
Semple et al 2016 J Poly Sci_Part_A__Polymer_Chemistry
Semple et al 2016 J Poly Sci_Part_A__Polymer_ChemistrySemple et al 2016 J Poly Sci_Part_A__Polymer_Chemistry
Semple et al 2016 J Poly Sci_Part_A__Polymer_ChemistryJ. Edward Semple
 
Isolation of polysacchide presentation
Isolation of polysacchide presentationIsolation of polysacchide presentation
Isolation of polysacchide presentationmd salik
 

Similar to Synthesis and Characterization of Polyacrylamide by Molecular Weight (20)

Gatot trimulyadi
Gatot trimulyadiGatot trimulyadi
Gatot trimulyadi
 
0 immobilization of laccase
0 immobilization of laccase0 immobilization of laccase
0 immobilization of laccase
 
Biocompatibility of Polymethylmethacrylate resins
Biocompatibility of Polymethylmethacrylate resinsBiocompatibility of Polymethylmethacrylate resins
Biocompatibility of Polymethylmethacrylate resins
 
Studies on some economic and effective Ion exchange Resin used as catalyst in...
Studies on some economic and effective Ion exchange Resin used as catalyst in...Studies on some economic and effective Ion exchange Resin used as catalyst in...
Studies on some economic and effective Ion exchange Resin used as catalyst in...
 
shao2003.pdf
shao2003.pdfshao2003.pdf
shao2003.pdf
 
SYNTHESIS OF DRUG CARRIER POLYACRYLIC
SYNTHESIS OF DRUG CARRIER POLYACRYLICSYNTHESIS OF DRUG CARRIER POLYACRYLIC
SYNTHESIS OF DRUG CARRIER POLYACRYLIC
 
Synthesis and Characterization of cyclohexylidene containing novel cardo pol...
	Synthesis and Characterization of cyclohexylidene containing novel cardo pol...	Synthesis and Characterization of cyclohexylidene containing novel cardo pol...
Synthesis and Characterization of cyclohexylidene containing novel cardo pol...
 
Synthesis, Characterization and Performance Evaluation of Poly Octadecyl Meth...
Synthesis, Characterization and Performance Evaluation of Poly Octadecyl Meth...Synthesis, Characterization and Performance Evaluation of Poly Octadecyl Meth...
Synthesis, Characterization and Performance Evaluation of Poly Octadecyl Meth...
 
Bech2007
Bech2007Bech2007
Bech2007
 
Ind. Eng. Chem. Res. 2009, 48, 4866–4871_Synthesis of Ultrahigh Molecular Wei...
Ind. Eng. Chem. Res. 2009, 48, 4866–4871_Synthesis of Ultrahigh Molecular Wei...Ind. Eng. Chem. Res. 2009, 48, 4866–4871_Synthesis of Ultrahigh Molecular Wei...
Ind. Eng. Chem. Res. 2009, 48, 4866–4871_Synthesis of Ultrahigh Molecular Wei...
 
depolymerization-of-high-molecular-weight-into-a-predicted-low-molecular-weig...
depolymerization-of-high-molecular-weight-into-a-predicted-low-molecular-weig...depolymerization-of-high-molecular-weight-into-a-predicted-low-molecular-weig...
depolymerization-of-high-molecular-weight-into-a-predicted-low-molecular-weig...
 
multicomponent reaction mediated by PEG-400
multicomponent reaction mediated by PEG-400multicomponent reaction mediated by PEG-400
multicomponent reaction mediated by PEG-400
 
Zhengguolin
ZhengguolinZhengguolin
Zhengguolin
 
Synthesis and Characterization of PMMA Nano-composites
Synthesis and Characterization of PMMA Nano-composites Synthesis and Characterization of PMMA Nano-composites
Synthesis and Characterization of PMMA Nano-composites
 
10.1016@j.carbpol.2011.04.046.pdf
10.1016@j.carbpol.2011.04.046.pdf10.1016@j.carbpol.2011.04.046.pdf
10.1016@j.carbpol.2011.04.046.pdf
 
Melamine epichlorohydrin prepolymers syntheses and characterization
Melamine epichlorohydrin prepolymers syntheses and characterizationMelamine epichlorohydrin prepolymers syntheses and characterization
Melamine epichlorohydrin prepolymers syntheses and characterization
 
Formulationassessment
FormulationassessmentFormulationassessment
Formulationassessment
 
Semple et al 2016 J Poly Sci_Part_A__Polymer_Chemistry
Semple et al 2016 J Poly Sci_Part_A__Polymer_ChemistrySemple et al 2016 J Poly Sci_Part_A__Polymer_Chemistry
Semple et al 2016 J Poly Sci_Part_A__Polymer_Chemistry
 
P44088390
P44088390P44088390
P44088390
 
Isolation of polysacchide presentation
Isolation of polysacchide presentationIsolation of polysacchide presentation
Isolation of polysacchide presentation
 

More from IOSRJAC

Isolation of Natural Dyes from Hibiscus Rosa Sinensis and Marigold Flower and...
Isolation of Natural Dyes from Hibiscus Rosa Sinensis and Marigold Flower and...Isolation of Natural Dyes from Hibiscus Rosa Sinensis and Marigold Flower and...
Isolation of Natural Dyes from Hibiscus Rosa Sinensis and Marigold Flower and...IOSRJAC
 
Effect of Chemical Treatment on the Morphology and Mechanical Properties of P...
Effect of Chemical Treatment on the Morphology and Mechanical Properties of P...Effect of Chemical Treatment on the Morphology and Mechanical Properties of P...
Effect of Chemical Treatment on the Morphology and Mechanical Properties of P...IOSRJAC
 
One Pot Hydrothermal Synthesis Characterizations Of Silver Nanoparticles On R...
One Pot Hydrothermal Synthesis Characterizations Of Silver Nanoparticles On R...One Pot Hydrothermal Synthesis Characterizations Of Silver Nanoparticles On R...
One Pot Hydrothermal Synthesis Characterizations Of Silver Nanoparticles On R...IOSRJAC
 
Kinetics and Thermodynamic Studies of Adsorption of Methylene Blue from Aqueo...
Kinetics and Thermodynamic Studies of Adsorption of Methylene Blue from Aqueo...Kinetics and Thermodynamic Studies of Adsorption of Methylene Blue from Aqueo...
Kinetics and Thermodynamic Studies of Adsorption of Methylene Blue from Aqueo...IOSRJAC
 
Characterization of Physicochemical Water Quality Parameters of River Gudar (...
Characterization of Physicochemical Water Quality Parameters of River Gudar (...Characterization of Physicochemical Water Quality Parameters of River Gudar (...
Characterization of Physicochemical Water Quality Parameters of River Gudar (...IOSRJAC
 
Synthesis, Identification and Surface Active Properties of Some Nonionic Surf...
Synthesis, Identification and Surface Active Properties of Some Nonionic Surf...Synthesis, Identification and Surface Active Properties of Some Nonionic Surf...
Synthesis, Identification and Surface Active Properties of Some Nonionic Surf...IOSRJAC
 
Geochemical Features of Oil on Biomarkers
Geochemical Features of Oil on BiomarkersGeochemical Features of Oil on Biomarkers
Geochemical Features of Oil on BiomarkersIOSRJAC
 
Simple Synthesis of Some Novel Polyfunctionally Derivatives of 2H-Coumarin-2-...
Simple Synthesis of Some Novel Polyfunctionally Derivatives of 2H-Coumarin-2-...Simple Synthesis of Some Novel Polyfunctionally Derivatives of 2H-Coumarin-2-...
Simple Synthesis of Some Novel Polyfunctionally Derivatives of 2H-Coumarin-2-...IOSRJAC
 
Facial and Simple Synthesis of Some New (Pyrazole and Triazole) Coumarin Deri...
Facial and Simple Synthesis of Some New (Pyrazole and Triazole) Coumarin Deri...Facial and Simple Synthesis of Some New (Pyrazole and Triazole) Coumarin Deri...
Facial and Simple Synthesis of Some New (Pyrazole and Triazole) Coumarin Deri...IOSRJAC
 
Air Transport and Tourism in Indonesia
Air Transport and Tourism in IndonesiaAir Transport and Tourism in Indonesia
Air Transport and Tourism in IndonesiaIOSRJAC
 
Studies on Anti-Inflammation Activity of Phenols Using Newly Introduced Balab...
Studies on Anti-Inflammation Activity of Phenols Using Newly Introduced Balab...Studies on Anti-Inflammation Activity of Phenols Using Newly Introduced Balab...
Studies on Anti-Inflammation Activity of Phenols Using Newly Introduced Balab...IOSRJAC
 
Kinetic Modeling of Vitamin C (Ascorbic Acid) Degradation in Blanched Commonl...
Kinetic Modeling of Vitamin C (Ascorbic Acid) Degradation in Blanched Commonl...Kinetic Modeling of Vitamin C (Ascorbic Acid) Degradation in Blanched Commonl...
Kinetic Modeling of Vitamin C (Ascorbic Acid) Degradation in Blanched Commonl...IOSRJAC
 
Simple and Eco-friendly Synthesis of Glycosides bearing triazolo[3,4-b][1,3,4...
Simple and Eco-friendly Synthesis of Glycosides bearing triazolo[3,4-b][1,3,4...Simple and Eco-friendly Synthesis of Glycosides bearing triazolo[3,4-b][1,3,4...
Simple and Eco-friendly Synthesis of Glycosides bearing triazolo[3,4-b][1,3,4...IOSRJAC
 
Synthesis, Anticonvulsant Activity and Cytotoxicity of Novel Valproic Acid De...
Synthesis, Anticonvulsant Activity and Cytotoxicity of Novel Valproic Acid De...Synthesis, Anticonvulsant Activity and Cytotoxicity of Novel Valproic Acid De...
Synthesis, Anticonvulsant Activity and Cytotoxicity of Novel Valproic Acid De...IOSRJAC
 
Influence of Tetra Alkyl Ammonium Cation and Temperature on Molecular Interac...
Influence of Tetra Alkyl Ammonium Cation and Temperature on Molecular Interac...Influence of Tetra Alkyl Ammonium Cation and Temperature on Molecular Interac...
Influence of Tetra Alkyl Ammonium Cation and Temperature on Molecular Interac...IOSRJAC
 
Adsorptive Removal of Methylene Blue Using Groundnut Shell Activated Carbon C...
Adsorptive Removal of Methylene Blue Using Groundnut Shell Activated Carbon C...Adsorptive Removal of Methylene Blue Using Groundnut Shell Activated Carbon C...
Adsorptive Removal of Methylene Blue Using Groundnut Shell Activated Carbon C...IOSRJAC
 
Synthesis and Studies of Some New Dioxouranium (VI) Complexes with Azoester L...
Synthesis and Studies of Some New Dioxouranium (VI) Complexes with Azoester L...Synthesis and Studies of Some New Dioxouranium (VI) Complexes with Azoester L...
Synthesis and Studies of Some New Dioxouranium (VI) Complexes with Azoester L...IOSRJAC
 
Profiling of Zn2+ Ion Sorption in Modeled Aqueous Solutions by different Part...
Profiling of Zn2+ Ion Sorption in Modeled Aqueous Solutions by different Part...Profiling of Zn2+ Ion Sorption in Modeled Aqueous Solutions by different Part...
Profiling of Zn2+ Ion Sorption in Modeled Aqueous Solutions by different Part...IOSRJAC
 
Antimicrobial activities of Six Types of Wheat Bran
Antimicrobial activities of Six Types of Wheat BranAntimicrobial activities of Six Types of Wheat Bran
Antimicrobial activities of Six Types of Wheat BranIOSRJAC
 
Corn Silk as Corrosion Inhibitor for Mild Steel in 0.1M HCl Medium
Corn Silk as Corrosion Inhibitor for Mild Steel in 0.1M HCl MediumCorn Silk as Corrosion Inhibitor for Mild Steel in 0.1M HCl Medium
Corn Silk as Corrosion Inhibitor for Mild Steel in 0.1M HCl MediumIOSRJAC
 

More from IOSRJAC (20)

Isolation of Natural Dyes from Hibiscus Rosa Sinensis and Marigold Flower and...
Isolation of Natural Dyes from Hibiscus Rosa Sinensis and Marigold Flower and...Isolation of Natural Dyes from Hibiscus Rosa Sinensis and Marigold Flower and...
Isolation of Natural Dyes from Hibiscus Rosa Sinensis and Marigold Flower and...
 
Effect of Chemical Treatment on the Morphology and Mechanical Properties of P...
Effect of Chemical Treatment on the Morphology and Mechanical Properties of P...Effect of Chemical Treatment on the Morphology and Mechanical Properties of P...
Effect of Chemical Treatment on the Morphology and Mechanical Properties of P...
 
One Pot Hydrothermal Synthesis Characterizations Of Silver Nanoparticles On R...
One Pot Hydrothermal Synthesis Characterizations Of Silver Nanoparticles On R...One Pot Hydrothermal Synthesis Characterizations Of Silver Nanoparticles On R...
One Pot Hydrothermal Synthesis Characterizations Of Silver Nanoparticles On R...
 
Kinetics and Thermodynamic Studies of Adsorption of Methylene Blue from Aqueo...
Kinetics and Thermodynamic Studies of Adsorption of Methylene Blue from Aqueo...Kinetics and Thermodynamic Studies of Adsorption of Methylene Blue from Aqueo...
Kinetics and Thermodynamic Studies of Adsorption of Methylene Blue from Aqueo...
 
Characterization of Physicochemical Water Quality Parameters of River Gudar (...
Characterization of Physicochemical Water Quality Parameters of River Gudar (...Characterization of Physicochemical Water Quality Parameters of River Gudar (...
Characterization of Physicochemical Water Quality Parameters of River Gudar (...
 
Synthesis, Identification and Surface Active Properties of Some Nonionic Surf...
Synthesis, Identification and Surface Active Properties of Some Nonionic Surf...Synthesis, Identification and Surface Active Properties of Some Nonionic Surf...
Synthesis, Identification and Surface Active Properties of Some Nonionic Surf...
 
Geochemical Features of Oil on Biomarkers
Geochemical Features of Oil on BiomarkersGeochemical Features of Oil on Biomarkers
Geochemical Features of Oil on Biomarkers
 
Simple Synthesis of Some Novel Polyfunctionally Derivatives of 2H-Coumarin-2-...
Simple Synthesis of Some Novel Polyfunctionally Derivatives of 2H-Coumarin-2-...Simple Synthesis of Some Novel Polyfunctionally Derivatives of 2H-Coumarin-2-...
Simple Synthesis of Some Novel Polyfunctionally Derivatives of 2H-Coumarin-2-...
 
Facial and Simple Synthesis of Some New (Pyrazole and Triazole) Coumarin Deri...
Facial and Simple Synthesis of Some New (Pyrazole and Triazole) Coumarin Deri...Facial and Simple Synthesis of Some New (Pyrazole and Triazole) Coumarin Deri...
Facial and Simple Synthesis of Some New (Pyrazole and Triazole) Coumarin Deri...
 
Air Transport and Tourism in Indonesia
Air Transport and Tourism in IndonesiaAir Transport and Tourism in Indonesia
Air Transport and Tourism in Indonesia
 
Studies on Anti-Inflammation Activity of Phenols Using Newly Introduced Balab...
Studies on Anti-Inflammation Activity of Phenols Using Newly Introduced Balab...Studies on Anti-Inflammation Activity of Phenols Using Newly Introduced Balab...
Studies on Anti-Inflammation Activity of Phenols Using Newly Introduced Balab...
 
Kinetic Modeling of Vitamin C (Ascorbic Acid) Degradation in Blanched Commonl...
Kinetic Modeling of Vitamin C (Ascorbic Acid) Degradation in Blanched Commonl...Kinetic Modeling of Vitamin C (Ascorbic Acid) Degradation in Blanched Commonl...
Kinetic Modeling of Vitamin C (Ascorbic Acid) Degradation in Blanched Commonl...
 
Simple and Eco-friendly Synthesis of Glycosides bearing triazolo[3,4-b][1,3,4...
Simple and Eco-friendly Synthesis of Glycosides bearing triazolo[3,4-b][1,3,4...Simple and Eco-friendly Synthesis of Glycosides bearing triazolo[3,4-b][1,3,4...
Simple and Eco-friendly Synthesis of Glycosides bearing triazolo[3,4-b][1,3,4...
 
Synthesis, Anticonvulsant Activity and Cytotoxicity of Novel Valproic Acid De...
Synthesis, Anticonvulsant Activity and Cytotoxicity of Novel Valproic Acid De...Synthesis, Anticonvulsant Activity and Cytotoxicity of Novel Valproic Acid De...
Synthesis, Anticonvulsant Activity and Cytotoxicity of Novel Valproic Acid De...
 
Influence of Tetra Alkyl Ammonium Cation and Temperature on Molecular Interac...
Influence of Tetra Alkyl Ammonium Cation and Temperature on Molecular Interac...Influence of Tetra Alkyl Ammonium Cation and Temperature on Molecular Interac...
Influence of Tetra Alkyl Ammonium Cation and Temperature on Molecular Interac...
 
Adsorptive Removal of Methylene Blue Using Groundnut Shell Activated Carbon C...
Adsorptive Removal of Methylene Blue Using Groundnut Shell Activated Carbon C...Adsorptive Removal of Methylene Blue Using Groundnut Shell Activated Carbon C...
Adsorptive Removal of Methylene Blue Using Groundnut Shell Activated Carbon C...
 
Synthesis and Studies of Some New Dioxouranium (VI) Complexes with Azoester L...
Synthesis and Studies of Some New Dioxouranium (VI) Complexes with Azoester L...Synthesis and Studies of Some New Dioxouranium (VI) Complexes with Azoester L...
Synthesis and Studies of Some New Dioxouranium (VI) Complexes with Azoester L...
 
Profiling of Zn2+ Ion Sorption in Modeled Aqueous Solutions by different Part...
Profiling of Zn2+ Ion Sorption in Modeled Aqueous Solutions by different Part...Profiling of Zn2+ Ion Sorption in Modeled Aqueous Solutions by different Part...
Profiling of Zn2+ Ion Sorption in Modeled Aqueous Solutions by different Part...
 
Antimicrobial activities of Six Types of Wheat Bran
Antimicrobial activities of Six Types of Wheat BranAntimicrobial activities of Six Types of Wheat Bran
Antimicrobial activities of Six Types of Wheat Bran
 
Corn Silk as Corrosion Inhibitor for Mild Steel in 0.1M HCl Medium
Corn Silk as Corrosion Inhibitor for Mild Steel in 0.1M HCl MediumCorn Silk as Corrosion Inhibitor for Mild Steel in 0.1M HCl Medium
Corn Silk as Corrosion Inhibitor for Mild Steel in 0.1M HCl Medium
 

Recently uploaded

(ANVI) Koregaon Park Call Girls Just Call 7001035870 [ Cash on Delivery ] Pun...
(ANVI) Koregaon Park Call Girls Just Call 7001035870 [ Cash on Delivery ] Pun...(ANVI) Koregaon Park Call Girls Just Call 7001035870 [ Cash on Delivery ] Pun...
(ANVI) Koregaon Park Call Girls Just Call 7001035870 [ Cash on Delivery ] Pun...ranjana rawat
 
Gfe Mayur Vihar Call Girls Service WhatsApp -> 9999965857 Available 24x7 ^ De...
Gfe Mayur Vihar Call Girls Service WhatsApp -> 9999965857 Available 24x7 ^ De...Gfe Mayur Vihar Call Girls Service WhatsApp -> 9999965857 Available 24x7 ^ De...
Gfe Mayur Vihar Call Girls Service WhatsApp -> 9999965857 Available 24x7 ^ De...srsj9000
 
APPLICATIONS-AC/DC DRIVES-OPERATING CHARACTERISTICS
APPLICATIONS-AC/DC DRIVES-OPERATING CHARACTERISTICSAPPLICATIONS-AC/DC DRIVES-OPERATING CHARACTERISTICS
APPLICATIONS-AC/DC DRIVES-OPERATING CHARACTERISTICSKurinjimalarL3
 
Structural Analysis and Design of Foundations: A Comprehensive Handbook for S...
Structural Analysis and Design of Foundations: A Comprehensive Handbook for S...Structural Analysis and Design of Foundations: A Comprehensive Handbook for S...
Structural Analysis and Design of Foundations: A Comprehensive Handbook for S...Dr.Costas Sachpazis
 
Call Girls in Nagpur Suman Call 7001035870 Meet With Nagpur Escorts
Call Girls in Nagpur Suman Call 7001035870 Meet With Nagpur EscortsCall Girls in Nagpur Suman Call 7001035870 Meet With Nagpur Escorts
Call Girls in Nagpur Suman Call 7001035870 Meet With Nagpur EscortsCall Girls in Nagpur High Profile
 
SPICE PARK APR2024 ( 6,793 SPICE Models )
SPICE PARK APR2024 ( 6,793 SPICE Models )SPICE PARK APR2024 ( 6,793 SPICE Models )
SPICE PARK APR2024 ( 6,793 SPICE Models )Tsuyoshi Horigome
 
The Most Attractive Pune Call Girls Budhwar Peth 8250192130 Will You Miss Thi...
The Most Attractive Pune Call Girls Budhwar Peth 8250192130 Will You Miss Thi...The Most Attractive Pune Call Girls Budhwar Peth 8250192130 Will You Miss Thi...
The Most Attractive Pune Call Girls Budhwar Peth 8250192130 Will You Miss Thi...ranjana rawat
 
Model Call Girl in Narela Delhi reach out to us at 🔝8264348440🔝
Model Call Girl in Narela Delhi reach out to us at 🔝8264348440🔝Model Call Girl in Narela Delhi reach out to us at 🔝8264348440🔝
Model Call Girl in Narela Delhi reach out to us at 🔝8264348440🔝soniya singh
 
(SHREYA) Chakan Call Girls Just Call 7001035870 [ Cash on Delivery ] Pune Esc...
(SHREYA) Chakan Call Girls Just Call 7001035870 [ Cash on Delivery ] Pune Esc...(SHREYA) Chakan Call Girls Just Call 7001035870 [ Cash on Delivery ] Pune Esc...
(SHREYA) Chakan Call Girls Just Call 7001035870 [ Cash on Delivery ] Pune Esc...ranjana rawat
 
Introduction to IEEE STANDARDS and its different types.pptx
Introduction to IEEE STANDARDS and its different types.pptxIntroduction to IEEE STANDARDS and its different types.pptx
Introduction to IEEE STANDARDS and its different types.pptxupamatechverse
 
High Profile Call Girls Nagpur Isha Call 7001035870 Meet With Nagpur Escorts
High Profile Call Girls Nagpur Isha Call 7001035870 Meet With Nagpur EscortsHigh Profile Call Girls Nagpur Isha Call 7001035870 Meet With Nagpur Escorts
High Profile Call Girls Nagpur Isha Call 7001035870 Meet With Nagpur Escortsranjana rawat
 
Introduction to Multiple Access Protocol.pptx
Introduction to Multiple Access Protocol.pptxIntroduction to Multiple Access Protocol.pptx
Introduction to Multiple Access Protocol.pptxupamatechverse
 
Porous Ceramics seminar and technical writing
Porous Ceramics seminar and technical writingPorous Ceramics seminar and technical writing
Porous Ceramics seminar and technical writingrakeshbaidya232001
 
Processing & Properties of Floor and Wall Tiles.pptx
Processing & Properties of Floor and Wall Tiles.pptxProcessing & Properties of Floor and Wall Tiles.pptx
Processing & Properties of Floor and Wall Tiles.pptxpranjaldaimarysona
 
Extrusion Processes and Their Limitations
Extrusion Processes and Their LimitationsExtrusion Processes and Their Limitations
Extrusion Processes and Their Limitations120cr0395
 
VIP Call Girls Service Kondapur Hyderabad Call +91-8250192130
VIP Call Girls Service Kondapur Hyderabad Call +91-8250192130VIP Call Girls Service Kondapur Hyderabad Call +91-8250192130
VIP Call Girls Service Kondapur Hyderabad Call +91-8250192130Suhani Kapoor
 
(PRIYA) Rajgurunagar Call Girls Just Call 7001035870 [ Cash on Delivery ] Pun...
(PRIYA) Rajgurunagar Call Girls Just Call 7001035870 [ Cash on Delivery ] Pun...(PRIYA) Rajgurunagar Call Girls Just Call 7001035870 [ Cash on Delivery ] Pun...
(PRIYA) Rajgurunagar Call Girls Just Call 7001035870 [ Cash on Delivery ] Pun...ranjana rawat
 
Architect Hassan Khalil Portfolio for 2024
Architect Hassan Khalil Portfolio for 2024Architect Hassan Khalil Portfolio for 2024
Architect Hassan Khalil Portfolio for 2024hassan khalil
 

Recently uploaded (20)

(ANVI) Koregaon Park Call Girls Just Call 7001035870 [ Cash on Delivery ] Pun...
(ANVI) Koregaon Park Call Girls Just Call 7001035870 [ Cash on Delivery ] Pun...(ANVI) Koregaon Park Call Girls Just Call 7001035870 [ Cash on Delivery ] Pun...
(ANVI) Koregaon Park Call Girls Just Call 7001035870 [ Cash on Delivery ] Pun...
 
Gfe Mayur Vihar Call Girls Service WhatsApp -> 9999965857 Available 24x7 ^ De...
Gfe Mayur Vihar Call Girls Service WhatsApp -> 9999965857 Available 24x7 ^ De...Gfe Mayur Vihar Call Girls Service WhatsApp -> 9999965857 Available 24x7 ^ De...
Gfe Mayur Vihar Call Girls Service WhatsApp -> 9999965857 Available 24x7 ^ De...
 
APPLICATIONS-AC/DC DRIVES-OPERATING CHARACTERISTICS
APPLICATIONS-AC/DC DRIVES-OPERATING CHARACTERISTICSAPPLICATIONS-AC/DC DRIVES-OPERATING CHARACTERISTICS
APPLICATIONS-AC/DC DRIVES-OPERATING CHARACTERISTICS
 
Structural Analysis and Design of Foundations: A Comprehensive Handbook for S...
Structural Analysis and Design of Foundations: A Comprehensive Handbook for S...Structural Analysis and Design of Foundations: A Comprehensive Handbook for S...
Structural Analysis and Design of Foundations: A Comprehensive Handbook for S...
 
Call Girls in Nagpur Suman Call 7001035870 Meet With Nagpur Escorts
Call Girls in Nagpur Suman Call 7001035870 Meet With Nagpur EscortsCall Girls in Nagpur Suman Call 7001035870 Meet With Nagpur Escorts
Call Girls in Nagpur Suman Call 7001035870 Meet With Nagpur Escorts
 
SPICE PARK APR2024 ( 6,793 SPICE Models )
SPICE PARK APR2024 ( 6,793 SPICE Models )SPICE PARK APR2024 ( 6,793 SPICE Models )
SPICE PARK APR2024 ( 6,793 SPICE Models )
 
The Most Attractive Pune Call Girls Budhwar Peth 8250192130 Will You Miss Thi...
The Most Attractive Pune Call Girls Budhwar Peth 8250192130 Will You Miss Thi...The Most Attractive Pune Call Girls Budhwar Peth 8250192130 Will You Miss Thi...
The Most Attractive Pune Call Girls Budhwar Peth 8250192130 Will You Miss Thi...
 
Model Call Girl in Narela Delhi reach out to us at 🔝8264348440🔝
Model Call Girl in Narela Delhi reach out to us at 🔝8264348440🔝Model Call Girl in Narela Delhi reach out to us at 🔝8264348440🔝
Model Call Girl in Narela Delhi reach out to us at 🔝8264348440🔝
 
(SHREYA) Chakan Call Girls Just Call 7001035870 [ Cash on Delivery ] Pune Esc...
(SHREYA) Chakan Call Girls Just Call 7001035870 [ Cash on Delivery ] Pune Esc...(SHREYA) Chakan Call Girls Just Call 7001035870 [ Cash on Delivery ] Pune Esc...
(SHREYA) Chakan Call Girls Just Call 7001035870 [ Cash on Delivery ] Pune Esc...
 
Introduction to IEEE STANDARDS and its different types.pptx
Introduction to IEEE STANDARDS and its different types.pptxIntroduction to IEEE STANDARDS and its different types.pptx
Introduction to IEEE STANDARDS and its different types.pptx
 
★ CALL US 9953330565 ( HOT Young Call Girls In Badarpur delhi NCR
★ CALL US 9953330565 ( HOT Young Call Girls In Badarpur delhi NCR★ CALL US 9953330565 ( HOT Young Call Girls In Badarpur delhi NCR
★ CALL US 9953330565 ( HOT Young Call Girls In Badarpur delhi NCR
 
High Profile Call Girls Nagpur Isha Call 7001035870 Meet With Nagpur Escorts
High Profile Call Girls Nagpur Isha Call 7001035870 Meet With Nagpur EscortsHigh Profile Call Girls Nagpur Isha Call 7001035870 Meet With Nagpur Escorts
High Profile Call Girls Nagpur Isha Call 7001035870 Meet With Nagpur Escorts
 
Introduction to Multiple Access Protocol.pptx
Introduction to Multiple Access Protocol.pptxIntroduction to Multiple Access Protocol.pptx
Introduction to Multiple Access Protocol.pptx
 
Porous Ceramics seminar and technical writing
Porous Ceramics seminar and technical writingPorous Ceramics seminar and technical writing
Porous Ceramics seminar and technical writing
 
Roadmap to Membership of RICS - Pathways and Routes
Roadmap to Membership of RICS - Pathways and RoutesRoadmap to Membership of RICS - Pathways and Routes
Roadmap to Membership of RICS - Pathways and Routes
 
Processing & Properties of Floor and Wall Tiles.pptx
Processing & Properties of Floor and Wall Tiles.pptxProcessing & Properties of Floor and Wall Tiles.pptx
Processing & Properties of Floor and Wall Tiles.pptx
 
Extrusion Processes and Their Limitations
Extrusion Processes and Their LimitationsExtrusion Processes and Their Limitations
Extrusion Processes and Their Limitations
 
VIP Call Girls Service Kondapur Hyderabad Call +91-8250192130
VIP Call Girls Service Kondapur Hyderabad Call +91-8250192130VIP Call Girls Service Kondapur Hyderabad Call +91-8250192130
VIP Call Girls Service Kondapur Hyderabad Call +91-8250192130
 
(PRIYA) Rajgurunagar Call Girls Just Call 7001035870 [ Cash on Delivery ] Pun...
(PRIYA) Rajgurunagar Call Girls Just Call 7001035870 [ Cash on Delivery ] Pun...(PRIYA) Rajgurunagar Call Girls Just Call 7001035870 [ Cash on Delivery ] Pun...
(PRIYA) Rajgurunagar Call Girls Just Call 7001035870 [ Cash on Delivery ] Pun...
 
Architect Hassan Khalil Portfolio for 2024
Architect Hassan Khalil Portfolio for 2024Architect Hassan Khalil Portfolio for 2024
Architect Hassan Khalil Portfolio for 2024
 

Synthesis and Characterization of Polyacrylamide by Molecular Weight

  • 1. IOSR Journal of Applied Chemistry (IOSR-JAC) e-ISSN: 2278-5736.Volume 10, Issue 4 Ver. I (April. 2017), PP 67-73 www.iosrjournals.org DOI: 10.9790/5736-1004016773 www.iosrjournals.org 67 |Page Synthesis and Characterization of Different Molecular Weights Polyacrylamide Raid Saleh Shatat1* , S. Kalimulla Niazi1 ,Azlan Ariffin2 1 Riyadh Colleges of Dentistry and Pharmacy, 84891 Riyadh 11681, Kingdom of Saudi Arabia. Tel: 920000842. Fax: 920000843 2 School of Material and Mineral Resources, UniversitiSains Malaysia, KampusKejuruteraan, 14300 NibongTebal, SeberangPerai Selatan, Penang, Malaysia *corresponding Author Abstract: Polyacrylamides of varying molecular weights (very low, low, medium, high and very high) were synthesized using free radical polymerization and characterized by Infra Red (IR) spectroscopy, viscosity measurements, glass transition temperature (Tg) measurement and thermal gravimetric analysis (TGA). Thioglycolic acid and hydrogen peroxide were used as initiators to synthesis very low and low molecular weight polyacrylamides respectively. Molecular weights (medium, high and very high) polyacrylamides were synthesized using potassium persulfate and N,N,N',N'- tetramethylethylenediaminesystem as initiators. The synthesis of medium, high and very high molecular weight polyacrylamides were achieved by increasing the concentration of acrylamide monomer. Fourier Transform Infrared Spectroscopy (FTIR) of polyacrylamides showed strong absorption at wave number 1655 cm-1 due to the presence of primary amide band. The results also showed that the increase in the intrinsic viscosity and glass transition temperature were proportional to the increase in molecular weight of polyacrylamide. On the other hand it can be seen an increase in molecular weight caused a decrease of weight loss %. Keywords:polyacrylamide, molecular weight, free radical polymerization, characterization. I. Introduction Natural polyelectrolytes (e.g. starch, gelatin, tannins, etc.) and inorganic electrolytes (e.g. aluminum sulphate, ferric sulphate, ferric chloride, etc.) have been traditionally as agents in water and wastewater treatment for the removal of colloidal suspended solids. The operations of these agents involve particle agglomeration by coagulation and flocculation processes (1). The uses of synthetic organic polyelectrolytes in water and wastewater treatment have been introduced in late 1950. Synthetic polyelectrolytes have been used extensively as coagulation aids or to replace inorganic electrolytes coagulants completely (2). The use of synthetic polyelectrolytes as flocculant is increasing rapidly. Polyelectrolytes increase floc strength allowing bigger and stronger flocs to be formed. The increased floc strength can improve settling characteristics. Synthetic organic polyelectrolytes are known to be more efficient than the inorganic electrolytes agents in the removal of suspended colloidal particles (3). The effectiveness of synthetic organic polyelectrolytes as flocculants increases with increasing molecular size, the limit of which is only dictated by problems in solubility. Polyelectrolytes having molar masses greater than 10 million g/mol do not dissolve readily but tend to form gel lumps known as "fish eyes". Polymers of lower molar mass are highly soluble in water due to the hydration of functional groups along the molecule. Polyacrylamide shows high solubility in water, while it is insoluble in most other common organic liquids such as methanol, ethanol and acetone. However, despite this highly hydrophilic character, the main technical application of polyacrylamide is for flocculation of aqueous suspension and related purposes. Polyacrylamides can be classified to three categories: non-ionic, anionic and cationic polyacrylamides (4). Polyacrylamides were used extensively as a flocculant in the clarification of water in industrial and municipal processes (5). Cationic polyelectrolytes are a class of polyelectrolytes that derive their unique properties from the density and distribution of positive charges along a macromolecular backbone as well as molecular weight. Cationic functional groups can strongly interact with suspended, negatively charged particles or oil droplets and are useful for many applications including wastewater treatment and papermaking. There is a greater variety of molecular structures in the cationic family than any of the other polyelectrolytes. The present study involves the synthesis and characterization of different molecular weight polyacrylamides using free radical polymerization.
  • 2. Synthesis and characterization of different molecular weights polyacrylamide DOI: 10.9790/5736-1004016773 www.iosrjournals.org 68 |Page II. Materials and methods Chemicals Acrylamide (Fluka, 99%), potassium persulfate (98%), and N,N,Nâ€Č,Nâ€Č- tetramethylethylenediamine (TMEDA) (98%)were purchased from Fluka, Germany as laboratory grade .Thioglycolic acid, hydrogen peroxide, acetone, ethanol and methanol were purchased from Merck, Germany as laboratory grade. Equipment and instrumentation The polymerization reaction was carried out in a Memmert water bath (thermostatically controlled, heating capacity up to 100ÂșC). A 1 litre five-necked Pyrex glass reactor was suitably placed into the Memmert water bath. The reactor was equipped with a mechanical stirrer, condenser equipped with water collector, thermometer and nitrogen gas (Oxygen Free Nitrogen) inlet tube. Recrystallization of chemicals Acrylamide (AM) was dissolved in acetone at 56ÂșC (boiling point of acetone) to form a saturated solution, the solution was then filtered to remove insoluble particles and allowed to cool so that the dissolved substance is crystallized, the solid crystals were separated from acetone by filtration under suction using a BĂŒchner funnel, washed with cold acetone and then dried in vacuum for 24 h at 60 ÂșC. This method was repeated twice. Potassium persulfate was recrystallized twice from distilled water at 100ÂșC (boiling point of distilled water) using the same procedure described above. The rest of the chemicals were used without further purification. Synthesis of different molecular weight polyacrylamides Acrylamide monomer is crystalline. It is relatively stable and is soluble in water and many organic solvents (acetone, ethanol, methanol, etc.). Acrylamide polymerizes easily by conventional free radical methods. Solutions of acrylamide in water polymerize at 40 ÂșC under the influence of nearly all free radical sources including persulfates, peroxides, azo compounds and redox couples. The synthesis of different molecular weight polyacrylamides is strongly influenced by temperature, solvent, type of initiator, concentration of the initiator and concentration of the monomer. Synthesis of very low molecular weight polyacrylamide Under nitrogen atmosphere, a mixture of acrylamide monomer (10gm), thioglycolic acid (0.20gm) and tetrahydrofuran (THF) (20ml) were placed in 500 ml five-necked Pyrex glass reactor equipped with a reflux condenser and a mechanical stirrer placed in a constant temperature bath at 40ÂșC.The polymerization was performed for 2 h under stirring. The polyacrylamide was isolated and re-precipitated by pouring its solution into acetone. It was then dried under vacuum at 60ÂșC for 24 h. Synthesis of low molecular weight polyacrylamide The acrylamide monomer was polymerized in distilled water, using hydrogen peroxide as the initiator. Nitrogen gas was bubbled inside a five-necked Pyrex glass reactor containing the acrylamide monomer (20 gm), distilled water (200 ml) as a solvent and hydrogen peroxide (0.5 ml) as initiator. The reactor was placed in a constant temperature bath 90ÂșC for 3 h under stirring. The polyacrylamide was isolated and re-precipitated by pouring its solution into acetone. It was then dried under vacuum at 60ÂșC for 24 h. Synthesis of medium, high and very high molecular weight polyacrylamide High purity of the monomer and initiators and the absence of oxygen are essential in the polymerization process. High concentration of monomers, low concentration of initiators are required to synthesized medium, high and very high molecular weight polyacrylamides. Different molecular weight (medium, high and very high) polyacrylamides were synthesized using the potassium persulfate and N,N,N’,N’- tetramethylethylenediamine (TMEDA) system as initiator. Increasing the concentration of acrylamide monomer will increase the molecular weight of the resulting polyacrylamide. Thus, under nitrogen atmosphere 15, 30 and 50 gm of acrylamide monomer were polymerized in (500ml) distilled water as a solvent and the (0.135gm) potassium persulfate/(180ÎŒl) TEMDA system as initiator to produce medium, high and very high molecular weight polyacrylamides respectively. The mixture were placed in 500 ml five-necked Pyrex glass reactor equipped with a reflux condenser and mechanical stirrer placed in a constant temperature bath at 40ÂșC. The polymerization was performed for 2 h under stirring. The polyacrylamide was isolated and re-precipitated by pouring its solution into acetone. It was then dried under vacuum at 60ÂșC for 24 h.
  • 3. Synthesis and characterization of different molecular weights polyacrylamide DOI: 10.9790/5736-1004016773 www.iosrjournals.org 69 |Page Characterization of synthesized polyacrylamide The polymer characterization is almost as important as polymer preparation. Without characterization, polymer synthesis becomes additional exercise. Fourier Transform Infrared (FTIR) Spectra analysis Fourier transform infrared spectroscopy (FTIR) is a very important step in polymer characterization. FTIR is used very extensively for the characterization of polymer materials in polymer chemistry (6). FTIR technique is normally used in the investigation of polymer structure and analysis of their functional groups. Nicolet FTIR machine, Model: Avator 360 FTIR spectrometer, manufactured by Nicolet analytical instrument USA Inc., USA was used in this study. Analysis was conducted by identification of acrylamide monomer and synthesized products (polyacrylamide). Potassium bromide (KBr) pellet was prepared by using a sampling device. Approximately 5-10 mg of the sample powder and 90-95 mg of KBr was blended, triturated and mixed well with agate mortar and pestle for 5 min. The mixture was transferred to the IR sampling device and then compacted using an IR hydraulic press for 60 seconds. KBr pellet was placed into FTIR window and then scanned by taking blank spectrum. After completion of the spectrum of the blank, KBr pellet was taken off from the window and KBr pellet thinly coated with test sample was placed again in the FTIR window to measure the spectrum of the sample. On average, 10 scans were used for the synthesized sample. Glass transition temperature (Tg) measurement Glass transition temperature (Tg) is an important characteristic property of a polymeric material because its fabrication and/or applications depend on it. It is a feature of polymeric materials that they may be entirely amorphous, partly amorphous and partly crystalline. The glass transition temperature (Tg)of all synthesized polyacrylamides were measured using Perkin-Elmer, Differential Scanning Calorimetry (DSC) thermal analyzer. It is equipped with a DSC cell programmed at a heating rate of 10 ÂșC/min., measuring temperature range was 25 ÂșC to 250 ÂșC.Samples were prepared for DSC measurement by weighting between 5.0 mg to 10.0 mg of dry polymer into an aluminum pan. The pan was then sealed with an aluminum cap. Similarly, an empty aluminum pan was used as reference. Viscosity average molecular weight of polyacrylamide The viscosity average molecular weight of polyacrylamides was carried out by determining the intrinsic viscosities of the polyacrylamides using Ubbelohede viscometer, no. 4809 ASTM at 25 ± 0.1ÂșC. The polyacrylamide solutions were prepared in distilled water. The intrinsic viscosity calculations were made for polyacrylamide after filtration through 250-micron sieve to remove any undissolved ‘gel’ lumps. Dilute solution viscosity method was used to determine the viscosity average molecular weight of the polyacrylamide samples by determining their intrinsic viscosities. Test sample was prepared by dissolving 0.5g of polyacrylamide in 100 ml distilled water at room temperature using magnetic stirrer. The resultant solution was filtered through 250-micron sieve to remove any undissolved ‘gel’ lumps. A series of polyacrylamide working solution with concentrations ranging between 5 X 10-3 and 1 X 10-3 g/ml were prepared by appropriate dilution of the test sample with distilled water. Approximate amounts of the solution were transferred into Ubbelhode viscometer and the viscometer placed inside a water bath set at 25 ± 0.1ÂșC and allowed to equilibrate. The efflux time (i.e. the time taken for the liquid inside the viscometer to pass from the upper meniscus to the lower meniscus was determined). An average of the three readings (which did not differ by more than 3 seconds) was taken for each sample. Thermal gravimetric analysis (TGA) Samples were prepared for TGA measurements by weighting between 5.0 to 10.0 gm of dry polyacrylamide into aluminum pan. The pan was then sealed with aluminum cap. Thermal gravimetric analysis (TGA) of different molecular weight polyacrylamides were carried out in the temperature range of 30-600 ÂșC at a heating rate of 10 ÂșC/min under nitrogen using Perkin-Elmer. III. Results and Discussion The molecular weight of polyacrylamide can be varied by several techniques, including monomer concentration, initiator concentration and initiator type and polymerization temperature. The monomer concentration can be increased to 50% or more for high molecular weight polyacrylamide since the viscous polymer molecular weight is the internal phase. High purity of the monomer and initiators and the absence of oxygen are essential in the polymerization process. The polymerization reaction at different temperaturesof acrylamide monomer with different initiators i.e. thioglycolicacid (40ÂșC), hydrogen peroxide (90ÂșC), and potassium persulfate/ N,N,N’,N’- tetramethylethylenediamine (TMEDA) (40ÂșC), gave the targeted very low, low, medium, high and very high
  • 4. Synthesis and characterization of different molecular weights polyacrylamide DOI: 10.9790/5736-1004016773 www.iosrjournals.org 70 |Page molecular weight polyacrylamide products (shown in Table 1). The synthesis of high and very high molecular weight polyacrylamide was achieved by increasing the concentration of acrylamide monomer using potassium persulfate/TMEDA as initiatorat moderate temperature. The synthesis route of the preparation of polyacrylamide is shown in table 1. The choice of initiators and monomer concentrations were also studied. Table 1: Type of initiator used and resultant molecular weight polyacrylamide Type of initiator used Resultant molecular weight polyacrylamide Thioglycolicacid Very low Hydrogen peroxide Low Potassium persulfate/ (TMEDA) Medium, high and very high The structure of different molecular weight polyacrylamides was determined through the study of FTIR spectra. Glass transition temperature (Tg), viscosity average molecular weight and thermal gravimetric analysis of polyacrylamide were also carried out. Synthesis of very low molecular weight polyacrylamide Very low molecular weight polyacrylamide was synthesized by free radical polymerization using thioglycolic acid as initiator at moderate temperature (40ÂșC).The ratio of thioglycolic acid to acrylamide monomer was about 0.02 (g/g) and polyacrylamide with molecular weight of about 20,000 g/mole was produced. The use of thioglycolic acid as a chain transfer agent has been shown to be a very effective method for the production of very low molecular weight polyacrylamide (7). Thioglycolic acid is used as a chain transfer agent where it is desirable to decrease the molecular weight in radical polymerization. Thioglycolic acid enters the propagation scheme by giving up a proton to the growing radical chain, terminating it, but possibly initiating a new chain. The thioglycolic acid was found to be an acceptable initiator for the production of a very low molecular weight polyacrylamide at moderate temperature and maximum yield was obtained without any unwanted side products. The product was a white coloured liquid with very low viscosity. Acetone was used to isolate and re-precipitate the polyacrylamide product from its liquid solution and dried under vacuum at 60ÂșC for 24 h to produce a yield of 70-75% of very low molecular weight polyacrylamide. Synthesis of low molecular weight polyacrylamide Low molecular weight polyacrylamide was synthesized using hydrogen peroxide as initiator and the reaction was carried out at high temperature (90ÂșC) to give polyacrylamide free of contaminates detected by FTIR spectroscopy. The product was a low viscosity white colour liquid. The polyacrylamide product was precipitated from its liquid solution using acetone and then dried under vacuum at 60ÂșC for 24 h to produce a yield of 70-75% of low molecular weight polyacrylamide. The molecular weight was found to be 170 X 103 g/mol using viscosity measurements, which is considered to be low. Synthesis of medium, high and very high molecular weight polyacrylamide Potassium persulfate/TMEDA system as initiator was used for the synthesis of medium, high and very high molecular weight polyacrylamides. TMEDA exerts a high promoting effect on the free radical polymerization initiated by potassium persulfate. The rate of polymerization increases by about three times in the presence of TMEDA. Potassium persulfate/TMEDA system can reduce the reaction time and react at moderate temperature (40ÂșC). Potassium persulfate/ TMEDA system was found to be an acceptable redox initiator for the production of medium, high and very high molecular weight polyacrylamides at moderate temperature and a maximum yield of 90-95% was obtained without any unwanted side products. The product was a high viscosity white colour liquid. Polyacrylamide was precipitated from the solution using acetone and then dried under vacuum at 60ÂșC for 24 h. Figure 1 shows the effect of monomer concentration on molecular weight of polyacrylamide. As shown, the concentration of acrylamide monomer strongly affects the molecular weight of polyacrylamide. An increase in acrylamide monomer concentration caused an increase in molecular weights of polyacrylamide. The fact that high concentration of monomer will initiate many sites, resulting in longer polyacrylamide chains, on the other hand shorter polyacrylamide chains at lower concentration of monomer. This is reflected in their corresponding intrinsic viscosity values. Intrinsic viscosity of a polymer is a measure of its hydrodynamic volume in solution, which in turn depends upon its molecular weight, nature of the solvent and the temperature of the medium (8). For polymers of low molecular weight, the hydrodynamic volume will be low and thus it has low intrinsic viscosity value.
  • 5. Synthesis and characterization of different molecular weights polyacrylamide DOI: 10.9790/5736-1004016773 www.iosrjournals.org 71 |Page Further, in the case of high molecular weight polymers the hydrodynamic volume will be high and therefore higher will be its intrinsic viscosity. This has been observed in practice (Figure 1). Figure 1: Influence of monomer concentration on molecular weight of polyacrylamide IV. Characterization Fourier Transform Infrared (FTIR) spectra analysis Fourier Transform Infrared Spectroscopy (FTIR) of polyacrylamide showed strong absorption at wave number 1655 cm-1 due to the presence of a primary amide band which is used to distinguish true polyacrylamide from the alternative polymerization product poly(ÎČ-alanine) which has instead a secondary amide band at 1555 cm-1 (4). The band for (N—H) stretching vibration appears at 3448 cm-1 of the NH2 group. Further, the absence of (C==C) band which usually appears at 1610 cm-1 proved that the acrylamide monomer has been completely converted to polyacrylamide and no residue of monomer is present in the polymer (9) studied the FTIR spectra of polyacrylamide, their finding is in a good agreement with our results. Glass transition temperature (Tg) measurement The glass transition is a physical change from the glassy to the liquid state which occurs in amorphous solids when they are heated. This point is characterised by the glass transition temperature determined by Differential Scanning Calorimetry (DSC). The glass transition temperature, Tg, of very low, low, medium, high and very high molecular weight polyacrylamide appeared at 100.944, 109.077, 120.811, 148.727 and 154.461°C respectively. This shows that up to these relatively high temperatures the polyacrylamide was in the glassy state and thus relatively resistant to the ingress (way in) or egress (way out) of small molecule penetrate, and it is necessary to use higher temperatures to put the polymer in the rubbery state where adsorbed solvent molecules are sufficiently mobile to be desorbed.Molecular weight influences Tg significantly. At lower molecular weights where the excess of free volume associated with chain ends is significant. As molecular weight increases the concentration of chain ends decreases until its contribution to the free volume becomes negligible. Louie and Hartwig observed an increase in glass transition temperature with increase the molecular weight of polymer. The results of this work are in a good agreement with their work (10).
  • 6. Synthesis and characterization of different molecular weights polyacrylamide DOI: 10.9790/5736-1004016773 www.iosrjournals.org 72 |Page Determination of approximate molecular weight Viscometry and application of Mark-Houwink equation is one of the simplest and most rapid methods used for determining the molecular weights of polymers.Molecular weight of the polyacrylamide samples can be estimated from the intrinsic viscosity values. Mark–Houwink equation is generally employed for the estimation of molecular weight of linear polymers. The molecular weights of polyacrylamide samples were determined by determining their intrinsic viscosities using Ubbelohede viscometer. The polyacrylamide samples were filtered with 250-micron sieve after dissolution in distilled to prevent particulate impurities from entering the capillary of the viscometer and affect the flow rate of the solution through it. The determination of viscosity average molecular weight from the measurement of intrinsic viscosity require working in a dilute solution using a suitable solvent. Therefore, in this study, the concentration of polyacrylamide solutions ranging from 1x10-3 to 5x10-3 g/ml were prepared by appropriate dilution of the test sample with distilled water. By increasing the concentration of polyacrylamide, the intermolecular interactions increased leading to the formation of intermolecular complexes, resulting in the enhancement of densities. Therefore, relatively higher values in the efflux time at higher concentration of polyacrylamide solution were predictable. The values of relative, specific, reduced and inherent viscosities of the various concentrations of the very low, low, medium, high and very high polyacrylamides were determined. It was found that by increasing the polyacrylamide concentrations from 1x10-3 to 5x10-3 g/ml the efflux time increased. As a result, the relative viscosity increased with an increase in the polyacrylamide concentration. Other viscosities namely specific and reduced viscosities also increased with an increase in the polyacrylamide concentration. On the other hand, the inherent viscosity was inversely proportional to the increase in polyacrylamide concentration. The intrinsic viscosity [η], which is defined as the intercept on the abscissa at zero concentration, was determined by plotting the reduced viscosity of the solution of different concentrations of polyacrylamide solutions. Intrinsic viscosity of the very low, low, medium, high and very high polyacrylamides samples were obtained.The results of intrinsic viscosity and viscosity average molecular weight are tabulated in table 2. It can be seen that the increase in the intrinsic viscosity was proportional to the increase in molecular weight of polyacrylamide. Table 2: Intrinsic viscosity and viscosity average molecular weight of different polyacrylamides Polyacrylamide Intrinsic viscosity (g/dl) Viscosity average molecular weight (g/mole) Very low 13 19,040 Low 76 173,089 Medium 186 508,563 High 456 1,625,402 Very high 1535 Over 5 million Thermal gravimetric analysis (TGA) TGA is used primarily for determining thermal stability of polymers. TGA method is based on continuous measurement of weight on a sensitive balance as sample temperature is increased in an inert atmosphere. Data are recorded as a thermogram of weight versus temperature. Initially weight loss may arise from evaporation of residual moisture or solvent, but at higher temperatures it results from polymer decomposition (11). The thermal stability of the different molecular weight polyacrylamides has been studied by TGA from 50ÂșC up to approximately 600ÂșC. The very high molecular weight polyacrylamide displayed the highest stability in the series, indicating the importance of the molecular weight for thermal stability. On the other hand, very low molecular weight polyacrylamide displayed the lowest stability. The increase in molecular weight caused a decrease of weight loss %. The residue at 600ÂșC being 11.67%, 14.68%, 17.83%, 19.45%, and 22.55% for the cases of very low, low, medium, high and very high molecular weight polyacrylamides respectively. The activation energy values for various stages of decomposition were calculated from thermal gravimetric analysis (TGA). The TGA of polyacrylamide was three-staged, as observed before by Ismail et al. (12). First, the loss of water which is nonstoichiometric occurred. This is followed by the subsequent loss of ammonia and other gaseous products from the polyacrylonitrile structure formed during the decomposition of polyacrylamide and partly from the remaining polyacrylamide in the course of heating to 600 ÂșC. For polyacrylamide moisture release takes place at a slow rate over the temperature zone of 40-200ÂșC accounting for successive release of absorbed moisture and bound (H-bounded) water. A relatively high mass loss zone then follows till about 400ÂșC which correspond to cyclization of polyacrylamide and associated liberation of NH3. A much sharper mass loss zone appears over the temperature zone of 400-500ÂșC accounting
  • 7. Synthesis and characterization of different molecular weights polyacrylamide DOI: 10.9790/5736-1004016773 www.iosrjournals.org 73 |Page for large-scale thermal degradation with the liberation of H2, CO and NH3, leaving a residue of about 22% at 600ÂșC (9). References [1]. Gill, R. I. S. (1985). The flocculation of kaolinite suspensions using cationic polyacrylamide. Ph.D, thesis, The University of Reading, Reading, Berkshire. England. [2]. Culp, R.L. (1977). Direct filtration. J. Amer. Water Works Assoc., 69 (7), 378. [3]. Gill, R. I. S. and Herrington, T. M. (1988). Floc size studies on kaolin suspensions flocculated with cationic polyacrylamides, Colloid and surfaces, 32, 331-344. [4]. Molyneux, P. (1982). Water-soluble synthetic polymers: properties and behavior. Volume I. Florida: CRC Press. [5]. Ives, K.J. (1978). The Scientific Basis of Flocculation, NATO ASI series, Sijthoff and Noordhoof, Alphen aan den Rijin, (Ed.). [6]. Thompson, H. W. and Torkington, P. (1945). Trans. Farad. Soc., 41, 246. [7]. Öz, N and Akar, A. (2000). Low molecular weight polyacrylic acid with pendant aminomethylenephosphonic acid groups. J. App. Poly. Sci., 78, 870-874. [8]. Nayak, B. R. and Singh, R. P. (2001). Synthesis and characterization of grafted hydroxypropyl guar gum by ceric ion induced initiation. Eur. Poly. J., 37(8), 1655-1666 [9]. Ghosh, P. Chakrabarti, A. and Siddhanta S. K. (1999). Studies on stable aqueous polyaniline prepared with the use of polyacrylamide as the water soluble support polymer. Euro. Poly. J., 35(5), 803-813. [10]. Louie, J. and Hartwig, J.F. (1997). Discrete high molecular weight triarylaminedendrimers prepared by palladium-catalyzed amination. J. Am. Chem. Sco., 119, 11659-11696. [11]. Stevens, M. P. (1990). Polymer Chemistry an Introduction (2nd ed.) 171-172. [12]. Ismail, M. Vangani, V. Rakshit, A. K. (1997). Terpolymerization of acrylamide, acrylic acid, and acrylonitrile: synthesis and properties. J. App. Poly. Sci.,69, 217-228.