SD0100030

PHYSICO-CHEMICAL SfUDY
ON GUAR GUM

A thesis submitted for the M. Sc. Degree in Chemistr

>trv

NAHLA MUBARAK MAHMOUD

Department of Chemistry
Faculty of Science
University of Khartoum

May 2000'

3 2 / 37
 CONTENTS
Dedication ' :. , ,..'....... I
Acknowledgement ..; II
English Abstract '.'. „,..,.... .. lit
Arabic Abstract V
List of Tables VII
List of Figures , ; VIII

CHAPTER ONE
INTRODUCTION
1.1.0 Gums ;
1.1.1. Definition ............ ;
1.1.2. Seed Gums '; i
1.1.3. Exudate Gums '. L
;
1.1.4. Preparative Fractionation ->
1.2.0. Guar Gum ; n
1.2.1. Historical Background : ->
1.2.2. Guar Plant... 3
1.2.2.1. Description ^
1.2.2.2. Classification of Cyamopsis tetragonoloba(L)
Taubert , 3
1.2.2.3. Guar Seed j.
1.2.3. Extraction and Purification of Guar Gum 4
1.2.4. Structure , 7
2 5. Physico-chemical Properties of Guar Gum g
' 1.2.5.1 Viscosity . g
1.2.5.2. Viscosity-Molecular weight Relationship JJ
.1.2.5.3. Specific Rotaion p
1.2.5.4 Trace Elements...; p
.2.6. Molecular Weight 13
.2.7. Applications of guar gum p
1.2.7.1. Food Industry 14
1.2.7.1.1. Dressings and sauces ; , ]^
1.2.7.1.2 Beverages 15
1.2.7.1.3. Processed Cheese Products p
1.2.7.1.4. Baked Goods ,5
1.2.7.1.5. Pastry Icings •
1.2.7.1.6. Meat Binder
1.2.7.1.7. Canned Meat Products and Pet
Foods
 1.2.7. 2. Non-food Industry .....; ...... 17
1.2.7.2.1. Paper Industry 17
1.2.7.2.2. Mining Industry 17
1.2.7.2.3. Oil-Well Drilling 18
1.2.7.2.4. Explosives 18
1.2.7.2.5. Tobacco 18
1.2.7.2.6. Cosmetics and Pharmaceuticals 18
1.2.7.2.7. Ceramics, Asphalt and Coal 18
1.2.7.3. Applications of Guar Gum Derivatives 19

TWO
EXPERIMENTAL
2.1.0. Source oF Materials 1(,
2.1".lv. Guar Gum Fractionation ^Q
2.2.0. Physico-chemical Properties of Guar Gum ....:... ^,
;
2.2.1. Infra-red Spectra Z^
2.2.2. Moisture Content Z\;
2.2.3. Ash Content ^
2.2.4. Nitrogen (Protein) Content ^
2.2.5. Determination of pH .,
2.2..6. Determination of Viscosity ' ' ~
2.2.7. Determination of Specific Rotation
23
2.2.8. Determination of Elements in Guar Gum

CHAPTER THREE
RESULTS AND DISCUSSION
3.1.0. Fractionation of guar gum
25
3.2.0. Physico-chemical Properties of guar gum .....'
3.2.!. Infra - red Spectra •., ^
3.2.2. Moisture content Z,n
3.2..3. Ash Content ~^'
3.2.4. Nitrogen ( Pi\-iein) Content ^~
3.2.5. Del erm niation of pH -,o
3.2.o. Intrinsic A i-scosiiy on
3.2.7-. Molecular Weight Zo
3.2 ;S. Specific Hotation ; -,q
v2N. Metal C>-:.ieiu ~

47
 Dedication

To- my
 Acknowledgement

I would like to express my deep sense of gratitude and sincere

ippreciation to my supervisor Professor Ali Mohamed KJieir for his
:ontinuous encouragement, guidance and help throughout this work.
I also wish to express my gratitude to all-members of the Chemistry
Department, Faculty of Science, University of Khartoum,,for allowing me to
ise their facilities and for their moral support.
Special gratitude is extended to the staff of the Botany Department,
•"acuity of Science, U. of K., for allowing me to use their laboratories and
lbrary. ;
Best regards are due to the Food Analysis Department,Research and
ndustrial Consultancy Centre, for providing laboratory facilities.
M>\ deepest thanks are offered to my family members for their
n\ aluable assistance, endless support and encouragement.
Thanks are extended to my friends and colleagues for their moral
uppori. . , • ' ,

I am also very grateful to Miss Hameida Elameen and Abd Elhadi

Uxlalla for computer facilities.
All praise is due to ALLAH who helped me and gave me health and
>atience to complete this revsearch.
 DISCLAIMER

Portions of this document may be

illegible in electronic image products.
Images are produced from the best
available original document
 Abstract

Giiar plant is an annual summer plant and it can resists diseases, pests
and drought. Guar gum is used in a lot of industries.
The present study deals with some physical properties of two
commercial grade samples of guar gum Cyamopsis tetraaonoloba which were
produced in 1996 and 1997 seasons (Sjand Svrespectively). Our analytical
data are compared with those of previous :workers in this area and
international quality.
 Nitrogen content determination,showed that the gum samples had a
value of 0.678% and 0.732% and water-insoluble fraction had a value of
0.118%. The values decreased in the water-soluble fractions giving 0.049%,
0.053% and 0.056%.
Water-soluble component and its fractions record the following
results:
pH measurements showed that the water-soluble component had pH
6.70 and 6.84 while its fractions had pH 5.90 and 7.00
Viscosity measurements showed that water-soluble fractions had
intrinsic viscosity of 6.4 and 6:8 dL. g' . The fractions derived from water-
soluble fraction had intrinsic viscosity of 6.6, 7and 7.5 dL.g"1.
Using Mark-Howink equation, the calculated average molecular
weights for the water-soluble components were 7.01 x lO3 and 7.62xlO5 g
mol"1 andifor its fractions were 7.31 x 105. . 7.93 x 105 and 8.73xlO5 g mo!"1.
The specific rotation for the whole water-soluble component was
•i-58G and +59°, while that for the fraction samples increased and gave the
values of+64°,+66° and+65°.
X-ray fluorescence (XRF) method indicated that the gum samples
and fractions contained traces of following elements: K, Ca, Mn. Fe, Cr, Zn,
Pb. Cu, As, Ni, Se, Rb, Sr. Zr. Y, Nb.

iv
 LIST OF TABLES

1. Composition of the components of guar seed 9

2. Some physical data for samples of guar gum and its fractions- 32
3. Nitrogen and protein contents in samples of guar gum and its
fractions 33
4. pH for samples of guar gum and its fractions 33
5. The flow time, ts. for water-soluble fractions of guar gum and its
tractions at 25°C ., •'. ". ' 34

6. The reduced viscosity, (r]sp/ C%), for Fsi, Fsv Fi, F2 and F3
fractions of giiar gum at 25°C , 35
7. Intrinsic viscosity and molecular weight for fractions of guar giim

35
8. The optical rotation, a°. for water-soluble fractions of guar gum
and its fractions F ! ; F ; and F3 at 25°C . 35
9. Comparison of specific Rotations, [a]^, of water-soluble

fractions FSJ and Fs^ of guar gum and its fractions at 25°C 36
'10 Dejennination of elements contained in samples and fractions
of guar gum in % and ppm 37

(vu)
 LIST OF FIGURES

1. Guar plant before pods formation 5

.:. Mature guar plant 5

3. Guar pods and -seeds 6

-1. Transverse section (brought guar seed. 6

;:>. Proposed structure' for guar gum 9

o. The infra-red spectrum of guar gum sample (S> ) 38

'.'. 1 lie infra-red spectrum of water- insoluble fraction (I) of

•guar gum -. .' 39

•A. 'ihe infra-red spectrum of fraction one (F| )of guar gum 40
l
>. 1 he infra-red spectrum of fraction two (F 2 )of guar gum 4i

io. 1 he infra-red spectrum of fraction three (F 3 )of guar gum. 42

I 1. Reduced viscosity . (]] / 0%) , versus concentration (C%)

j"or water- soluble fractions FSi and F o of guar gum at 25°C. 43

1 ..:. Reduced visco-m;- . t \\^J i'%) , versusconeentration (C%)

tor 1-; .Fj and F; fractions of guar gum a!;25°C. 44

i 1 Optical rotation u , \ ersus concentration (C°"o) for vvater-

M)luble iVaciioii-, oiOuar gtim F S! and' Fs: at 25°C -^

i-1. Optical rotatio!!-'. </". versus chncentration-(C°-o) for F l 5 F2

' * - • •

i ••. i n )
CHAPTER ONE
INTRODUCTION
 . INTRODUCTION

1.1.0. Gums:
1.1. 1. Definition:
Water-soluble, gums are polysaccharidic materials which are more
or less soluble in water to form a viscous solution, a gelatinous paste, or a
jelly (depending on the concentration employed) and which are insoluble in
most organic solvents. Using of 'water-soluble'gums, may be
distinguished-from, similar-appearing tree exudates, the resins, which are
insoluble in water but soluble in organic solvents .

1.1.2. Seed Gums:

• (4)

Seeds were also an ancient source of gums. It is generally accepted

that the galactomannan (polysaccharide gum), is a reserve polysaccharide.
which is utilized in germination. The vast majority of galactomannan
polysaccharides extracted from higher plants have originated in the
Leguminoseae family. The galactomannans from the seeds ofguarand
carob (locust bean) have found widespread use , as industrial
( 5 ) , • • ' . . . <

hydrocolloids.

1.1.3. Exudate Gums:

Plants that produce commercial gums are usuallly shrubs or low
growing trees from which the gums exude as vermiform or tear shapes.
Among exudate gums.'true gum arabic is a dried gummy exudation obtained
from trees belonging to various species of the genus Acacia.

(1)
: . ;L JL-4- Preparative Fractoir^tipn:
; The techniques for fractionating the polydisperse polymer are^divided
into preparative and analytical methods/'* Preparative method ."is based on
the fact that the solubility of macromolecules is a function of molecular
weight. The partial precipitation is a result of the decrease in solvent power
as controlled by temperature or by varying the ratio of solvent to non-
; solvent in a binary mixture. Precipitation is carried out by addition of
ethanol or acetone to an aqueous solution of the polysaccharide.
Differential solubility by , collecting. the different fractions of gum
according to their solubility in distilled water (fraction A), salt (fraction B)'
and the residual insoluble gel (fraction C). (8)
Fractionation is, perhaps, more successful if derivatives are used. (9)
(10)
Guar gum was acetylated. Then guaran triacetate was fractionated.
Gums can also be fractionated by careful precipitation with neSr saturated
sodium sulphate solutions } ] ^
Polysaccharides in general can also be fractionated by precipitation
with a specific complexihg agent. (9) Addition of small amounts of Fehling
solution to aqueous solutions of guar gum causes the precipitation of a
polysaccharide-copper complex.(12)

1.2.0. Guar Gum:

Guar flour is the ground endosperm of guar seeds. Its industrial value
rests upon the gum (78-82% of the endosperm) which is a natural, water
dispersable, hydrocolloid. The hydrocolloid commercially known as guar
gum is chemically a galactomannan - and designated guaran.
1.2.1. Historical Background:
The early history of old-world legume guar is unknown. However,
established records and circumstantial evidence indicate man cultivated
 guar In Indo-Pakistan subcontinent for numerous generations, until
recently guar lias remained as a milfer crop. Guar plant (leaves,; Pods, and
seeds) is; used for cattle feed saiid; human eorisumption. It is also used in
medicinal purpose.(13)
In the United States, guar, was first investigated as a source of gum in
, 1945. The consumption of guar gum has grown rapidly; since its
commercial introduction in 1953.(14)
Recently, Sudan has introduced guar as a cash crop to supply the only
guaran producing company which is established in Singa town in 1996.
However, guar plant is found as a local crop in the areas, of Red1 Sea
mountains and Arashekol mountains at White Nile State/ 15)

1.2.2.Guar Plant:
Guar plant is a drought-tolerent summer legume.

1.2.2.1. Description :
Guar is an annual bushy branching plant. The length ofguar plant
can reach 3m. Plants vaiy from 1-leader branch type to heavily branched
one (Fig. 1). It has small pink ,to white flowers and alternated trifoliolate
leaves (Fig.2)., It has well -developed lateral root system, with large light
colored nodules. Pod length is 12 cm and carries 5-12 seeds (Fig.3). Pods
emerge from just above the ground to the top of the plant in dense clusters.
Plant maturity occurs in 125-135 days to 160-175 days.(16)

1.2.2.2. Classification of Cvamopsis tetragonoloba

(L)Taubert Wtf.wo).
Common Names . : Guar .Cluster bean, Siambean, Calcutta lucerne
Synonym : Cvamopsis psoralioides DC.

13)
 'Kinsdom = • • :. Plantae
Phylum " Angiq spermae
Sub Phylum : 'Diodtyledones
Division " Lignosae
Group Rosaceae , (Rosales), (Rutales)
Grade Dialypetalae
Order Leguminales
Family Leguminosae
Sub Family : Papilionoideae
Genus •; ' -.: • ? Cyamopsis

1.2.2.3. Guar Seed:

The guar seed is dicotyledonous, having a diameter of
approximately 1/8 in ( 8mm) (Fig.3:).(14) '
In his pioneering work Anderson screened seeds of 163 species of
legumes for sources of endosperm gums. He reported that guar seed
(lj)
contains about 50% endosperm and yielded approximately 42% gum.
According to A. M. Goldstein, E. N. Alter and J. K. Seaman(l4) (Table 1)
the major components of guar seed are the seed coat (14-17%), endosperm
(35-42%), and germ (43-4.7%) (Fig.4). The germ contains most of the
protein in the seed while the endosperm contains the galactomanhan gum.
Menon et.al. found that gum content of a whole seed, endosperm
content, and percentage of gum in endosperm varied between 1.9.1 -
34.1%, 3 8 . 0 - 49.9% and 47-68%, respectively, in 86 guar seleenons
grown in India in 1968. (b)

1.2.3. Extraction and Purification of Guar Gum :

The extraction on a commercial scale of galactomannan gum from

guar seed usually invoh'es a preliminary removal of the tough seed - coat
Ui

>5 ?^^&'b?f-j&^&j'*7i.±£m

Fig. 1 : Gnar FJant before pods formation Fig.2 Mature Guar plant
 Fig. 3 : Guar pods (A) and seeds (B)

Fig. 4 : Transverse section through guar seed

(6)
 by some form of milling on; grinding^ The digferehee in hardness of the
various seed components is utilized, anS a<purification fs accomplished by
multi stage grinding and sifting.
There are" many types of grinders such as attrition mills that can be
employed because of the difference in hardness of the endosperm and
germ.
After the endosperm is separated from the hull- and germ, it is ground
to a fine pairticilesi^earid marketed as guafgum.(14)
Purification of the the crude galactomannan is achieved either by
repeated precipitations with ethanol, or by precipitation of the copper or
barium complex/regeneration of the galactomannan, and, finally,
reprecipitation with ethanol. Fehling solution is the reagent commonly
used, although cupric acetate and barium hydroxide have also been
employed. (5)
1.2.4, Structure :
Methylation, fragmentation, and periodate oxidation show that guar
gum (guaran) consists of linear chains of (!-» 4) p-D-mannopyranosyl
units with a - D - galactopyranosyl units 'attached by (l-> 6) linkages.
Enzymic hydrolysis of guaran gives mannobiose (4-0-(3-D-

mannopyranosyl-D-mannose), mannotriose, and 6-0-a-D-

galactopyranosly-D-mannopyranose , confirming earlier methylation
results and showing that B-D-(l-» 4) linkages are present in the mannan
and that side chain D-galactose units are attached by a : D - ( l - > 6 )
linkages ( F i g , 5) ;.(14)
Galactomannan polysaccharide of guar gum contains 34.5% D-
galactose anhydride and 63.4% D-mannose anhydride. (il)
No ketos'es or uronic aci^s have been detected in the polysaccharidic
material (guaran)'.(21>22'23)

(7)
 1.2,5, Physido-chemihal Propgifles^of

Guar gum is a non ionic neutral polysaccharide galactomannan.

There are no standards for grade identification of guar gum. However, the
available grades can be differentiated on the basis of purity and viscosity.
Food-grade guar gum is stiDStantialy pure endosperm. It usually has
a small residue'of hull and germ owing to imperfect purification. A typical
analysis of the impurities in food-grade guar gum gives crude fiber 2.5 %;
moisture, 10 -15%; protein , 5-6% ; ash, 0.5- 0.8% .A comparison of this
analysis; with that of pure endosperm components (Table 1) shows the
effectiveness of the separation as done by the usual commercial processing
techniques. Technical - grade guar gum is usually a less purified gum.
Most guar gums marketed to the food industry produce viscosities
of 3000-5000: cps in a 1% solution . Viscosity is not only influenced by
purity but also by processing techniques.

1.2;5.1. Viscosity:
Guar gum forms viscous, colloidal dispersions (solutions) when
hydrated in cold water/14 ' .
Temperature influences the rate of hydration and development of
maximum viscosity. Guar solutions prepared at higher temperatures reach
maximum viscosity much faster than those at lower temperatures.
However, the advantage of using heat to achieve faster hydration ,of the
gum'is partly offset by the possible degradative effect of prolonged heat in
certain processing conditions . The maximum viscosities of guar gum
dispersions are achieved at temperatures of about 25-40 C. (lj)
In dilute'solutions, the viscosity of guar gum increases linearly with
concentration up to about 0.5%. Thereafter, guar gum solutions behave as

(8)
 Fig. 5 : Structure proposed for guar gym

rr

Table 1: Composition of the Components of Guar Seed

•••' ' S e e d p a r t K1 Protein Ether > Ash Moisture, Grude Type of ,

(N X 6.25) % Extract, % % % Fiber, % Carbohydrate
Hull (14-17%) 5 0.3 4 10 36.0 D-Glucose
Endospem 5 0.6 0,6 10 1,5 Galactomanan
(35-42%) 55.3 5.2 4.6 10 18.0 D-Glucose
Genn(43-47%)

(9)
 non -'Newtonian solutions-mainly as a result of#he complex surface
• ' * • • • • • • ' ; • ' • - . " i ' < * * *

attractions at higher concentration: '

Guar gum is stable over a wide pH range. The nonionic nature>:of the
molecule is responsible for the almost constant viscosity of solutions in the
pH range 1-10.5 .# However, previously hydrated guar gum is compatible
with high alkalinity; and modified guar gums that develop high viscosity in
concentrated, caustic solutions have recently become available. The
optimum rate of hydration for guar gum occurs between pH 7.5 and 9.
Despite the rate differences, maximum viscosities are the same in both
(14)

acidic and alkaline media.

Guar gum is nonionic. Therefore compatibility with salts is exhibited
over a wide range of electrolyte concentration. High concentrations cf
multivalent salts affect hydration and produce gels.
Guar gum is compatible with many materials, including pearl starches and
with most other gums such as gum arabic . It acts synergistically to increase
viscosity when, combined with.some other gums or with starches.
In the presence of sugar, guaran competes with the sugar for the available
water, and high percentages of sugar have a marked delaying action on the
hydration of the gum . In addition, the viscosity of guaran-sugar solutions
decreases gradually in direct proportion to the sugar concentration . Sugar is
effective in protecting guaran solutions against hydrolysis and loss of
viscoity when solutions are heated or autoclaved. The presence of 5-10° b
(13.25.26)

sugar in the liquid gives improved viscosity.

Guar gum solutions require a hydration time of about 2 hrs to reach
maximum viscosity. The gradual decrease in viscosity which occurs after
24 hrs is usually accompanied by a drop in pH. Two factors responsible
for this viscosity decrease are fermentation -and enzymatic hydrolysis.

.0)
However*, bacteriosfatic and bacteriocidal preservatives: in siffficient
(14}
concentrations j5rovi<ieprelection for guar,gum solutions.
1.2.5.2. Viscosity-Moleeular Weight Relationships:
The viscosity of dilute polymer solutions-is measured in simple glass
capillary viscorheters,through which the time required for a fixed volume
of liquid tp flow is measured'.There are two common varieties of.capillary
viscometer : Ostwald-Fenske, and Ubbelohde. If the solution and solvent
have the same density, and neglecting possible effects of shear rate, the
flow times of these liquids are proportional to their viscosities. Some
common viscosity functions derived from these data are listed below:-
Relative viscosity rjr = T]soi, / r)soiv. = tsoi./tsoiv. (1)
Specific viscosity risp. = rj r - 1 (2)
Reduced viscosity rjred. = r)sp/C (3);
Inlierent viscosity rjinh. = (Ln r|r)/C (4)
Intrinsic viscosity [r\]• = ( rjsp./C }c = o = [( Ln r|r) /C] c = o (5)
The intrinsic viscosity [r\] is the quantity usually correlated with
molecular weight: *

[r\] = K ' M v a (6)

Mark-Houwink equation. M v is the viscosity - average molecular

weight. The constants K' and a must be determinded for each experimental
system by measuring the intrinsic viscosity of polymer samples whose

molecular weight is known as the result of other measurements. Since M v

is not usually available, and because Mv is more nearly equal to ivlw than

to other average molecular weights, it is common to use values of M w to

calibrate the viscosity method, and to rewrite equation (6):

[il ] - K/' IVUa (7)(27)

(11)
 Molecular theories of the' viscosity of dilute and more concentrated
solutions of random-coil .polymers have been applied to five molecular
•weight fractions of giiar galactomannan. The staudinger constants k and a,
were calculated. Values deduced were K - 3.8 x TO and a -0.723. l2M

1.2.5.3. Specific Rotation:

i The .optical -activity of-organic molecules is related to their structure
and is a characteristic property of the substance . (29j
Although polarized light has many uses , to the physical chemist one of
its principal functions .is in polarimetry, the measurement of the angle of
rotation, that is, the angle through Which the plane of polarization of the
light is rotated by passage of the beam through an optically active material
•This rotation or change in the plane of vibration of the plane-polarized light
depends upon the wave length of the light, the-nature of the material, its
density or concentration, and the length of the light path.{M)}
Vibrational Raman optical activity spectra of carbohydrates in aqueous
solution associated with the glycosidic linkage in the saccharides were
measured between 700-1500 cm. ( i l )
Guar gum gives 'dextrorotatory optical rotations in solution. It has a
specific optical rotation of ~53'21'and+54.5(21"-2' in I N sodium hydroxide
solution. •

1.2.5.4. Trace Elements:

The basis of quantitative X-ray fluorescence spectrometry(XRF) is:
to follow the identification of a certain element ( t h e matrix) • with a
measurement of the intensity qf one of its characteristic lines, then to use
this intensitv to estimate the concentration.of that element. (j3)

(12)
I.2.6.- Molecular Weight:
Galactomannans,' like many other natural polysaccharides, tend to be
polydisperse and,- consequently, can not be accurately described by a single
molecular weight. Instead, average molecular weights are obtained, the
values of which are dependent on the techniques used.
Anumber of problems arise in connection with the measurement of
molecular weights of galactomannans. Firstly, it is very difficult to obtain
true solutions of many of the gums, especially of locust-bean gum and guar
gum. Consequently , the solutions must be filtered or centrifiiged to
remove undissolved or partially hydrated gum. This immediately raises the
problem of fractionation of the sample, as the result may not mean very
much if a large portion of the sample is removed before analysis. Secondly,
the values depend upon the rigorous evaluation of the molecular shape. For
example, Deb, And Mukheriee used a dissymmetry method and assumed
for molecules of guar gum a spherical shape, which is highly unlikely; the
molecular weight derived was 1, 720,000, a value that seems unreasonably
large but may, however, be due to aggregation.
A third problem, pertaining to chemical methods, arises because of
the very high molecular weights of some galactomannans .Agum having a
molecular weight of 250,000 has only one reducing end - group for every
fifteen hundred or so sugar residues; thus, in methods involving end-group
analysis, avery high level of accuracy is required; in addition, highly
purified samples are essential. Periodate-oxidation methods can be
complicated by over-oxidation. ^
By the application of membrane osmometry to a commercial sample of
guar gum, a number-average molecular weight of Mn = 240,000 for both
the gum and its peracetate was obtained. Light -scattering and viscosity
measurements gave a weight-average molecular weight of M,v = 950.000.
The large difference between Mn and Mw indicated the presence of species
having a broad spectrum of molecular weight in p ommercial guar £um.(5)
Using a modified version of the Launer and Tomimatsu assay Mn of guaran
was found to be 250,000 while Mwis 1,900,000 determined with a Spinco
ultracentrifuge.(34)
1.2.7.0. Applications of Guar Gum:
1.2.7.1. Food Industry:
1.2.7.1.1. Dressings and Sauces:
Advantages of using of guar gum in salad dressings are: its cold
- water dispersibility, its compatibility with highly acidic emulsions, and
its , comparatively low cost on asviscosity basis. It functions as an femulsion
stabilizer by increasing the viscosity of the aqueous phase, thereby
decreasing the separation rate of the water and oil phases.
Guar is useful as a thickener in pickle and relish sauces when rapid
cooling is used. It provides good body, a clean appearance, and it can be
prepared in solution. The addition of guar gum to barbecue sauces and
similar meat sauces is effective in stabilization. The gum reduces the
tendeny of the .sauces to separate and improves the: shelf life of the final
products.

1.2.7.1.2. Beverages:
Guar is often used as a thickening or viscosity control agent in
beverages. Sugarless dietetic beverages require incorporation of a gum to
improve body and mouth feel. Guar gum is useful because of its resistance
to breakdown under the low pH conditions. In addition, since guar is
soluble in cold water, it is easy to use in most beverage processing plants.lt
is economical to use and practical because of its high viscosity, fast
hydralion rate, and extremely bland flavor.

(14)
 ^•Bi|fi|| of 'guar gum and carrageenan* are used • in certain cocoa
products as effective stabilizing and suspending agents.

1.2.7.1.3^ ^Processed Cheese Products:

The use of guar gum in cold-pack cheese products eliminates
syneresis or weeping and improves texure and flavor.In soft cheeses, the
use of gifergum increases the yield of curd solids and produces curds,of a
soft, compact, tender texture with a separated lipid whey. Guar gum also
adds to pasteurized processed cheese as a stabilizer.
Guar gum has a broad application in frozen foods because of the
stability of its aqueous dispersions or solutions. This hydration ability and
water-binding property also makes the gum useful as an ice cream
stabilizer and especially useful in high-temperature, short-time processes.

1.2.7.1.4. Baked Goods:

Stabilizers are often added to packaged cake mixes and guar gum
offers several functional advantages in single-step mixing procedures:
reduced batter mixing time, reduced crumbling in the finished cake, easier
application of frostings and icings, and greater moisture retention during
prolonged shelf life. Guar gum is also suitable for use in frozen cakes.
The addition of guar, solutions to doughs while kneading give
increased yields and produce a dough of greater resiliency and a drier, less
flabby appearance. Baked products have a better, softer texture as well as a
longer shelf life. In cake and biscuit doughs, the addition of guar gum
yields softer and more moist products that are more readily removed from
their pans and easily sliced without crumbling.
When guar gum is added to batters of doughnuts, spoon bread, etc.,
it imparts desirable binding and film-forming properties that retard the
penetration of fats and oils.

(15)
 - Addition of guar gum to starch-gluten loaves of bread produced an
i V', '. •'• • i ' ' . " - ' ' . . ' • '•,' ' \' ' ' • '' '•• •
, . - I ^ . - ' - . i \-.-j»..-ii i t j •:••.** ••• , ' . , • ' • ; • ' ; • : <

effective" increase in baked loaf volume. In frozen pie-fillings, guaf gum-

starch corhbiriatiohs are effective in preventing dehydration, shrinking, andi
cracking of the filling. ;
1.2.7.1.5. P^itry Icings:
Acomrhon ^problem in packaged iced bakery goods is the
accumulation of moisture within the transparent wrapping. The moisture
causes !the icing to adhere to the wrapping and results in an unpleasant
appearance. Addition of guar gum to icings eliminates this problem by
absorbing the free water.
1.2.7.1.6. Meat Binder:
The strong water-holding properties of guar gum in both hot and
cold water make it effective as a binder and lubricant in the manufacture of
sausage products and related stuffed meat products.

1.2.7.1.7. Canned Meat Products and Pet foods:

In the processing of canned meat products, the addition of guar
gum offers reduction of the bumping tendency during the cooking of the
meat products; increase in the ease of pumping of the cooked product;
reduction of splashing and spilling of contents while filling cans, thus
making control of fill weights easier and keeping the cans cleaner for
labeling; viscosity control of the liquid phase during processing and
cooling; and greater resistance to sterilization temperatures.
Advantages in the finished product include prevention of fat
migration during storage, control of free water separation in the can during
storage and reduction of the tendency for void development in the can. (lj)

(16)
1.2.7.2. Nori- Food Industry:
r.2.7.2.1. Paper Industry:
, Guar gum is used as a size for paper and textiles.f3:>) The major
use of galaqtomannan in paper making is in the wet end of the process. The
gum is addecl to the pulp suspension just before the sheet is formed.
Galactomannans replace or supplement the natural hemicelluloses
in paper bonding. Advantages gained by addition of galactomannans to
pulp include improved sheet formation with a more regular distribution of
pulp fibers (less Fiber bundles); increased mullen bursting strength;
increased fold strength ; increased tensile strength; increased pick; easier
pulp hydration; improved finish; decreased porosity; increased flat crush of
corrugating medium; increased machine speed with maintenance of test
results; increased retention of fines. (b)

l.2.7;2.2i Mining Industry:

Guar gum is used in froth flotation of potash as an auxiliary
reagent, depressing the gangue minerals, which might be clay, talc or
shale. Guar gum is also used as a floceulant or settling agent to concentrate
ores or tailings in the mining industry.
Guar gum is approved by the U.S. Public Health Service for use in
potable water treatment as a coagulant aid in conjunction with such
coagulants as alum (potassium aluminum sulfate), iron (III) sulfate, and
lime (calcium oxide). In industrial waters, guar gum flocculates clays,
carbonates, hydroxides and silica when used alone or in conjunction with
inorganic coagulants.

1,2.7.2.3. Oil - Well Drilling:

Water -Soluble polymers Have found a broad range of application
in the production of petroleum. They serve one or more functions, such .as

(17)
water-loss control, viscosity control, flpcculation, suspension, turbulent
friction reduction or mobility control.(13)

1.2.7.2.4. Explosives:
In the production of water-resistant ammonium nitrate stick
explosive, guar gum is used as a binding agent.(36) It is also used as a
thickner and gelling agent for slurry explosives.(14)

1.2.7.2.5. Tobacco:
Guar g u m is used as a binder in making reconstituted t o b a c c c o . ( j / )

1.2.7.2 .6. Cosmetics and Pharmaceuticals

Guar gum is used to thicken various cosmetics and
pharmaeeutieals.(38) It is also used as a binder and disintegrator for
compressed tablets.(39) Coarse granulations 6f guar gum are ordinarily used
for this purpose. Guar gum in larger doses is being investigated as a bulk
laxative.(14)

1.2.7.2 .7. Ceramics, Asphalt and Coal:

Guar gum is used as a thickening agent in asphalt emulsions and
ceramics.(40) It is also used as dispersant to stabilize aqueous powder of
coal slurries.

1.2.7.3. Applications of Guar Gum Derivatives:

There are some of the more important, industrial derivatives thereof
include the carboxymethyl'ether, oxidized guar gum, andhydroxyalkyl
ethers.

(18)
 Regular guar, for 'example, is rapidly adsorbed onto hydrated
mineral surfaces by hydrogen bonding to cause- flocculation. E5y the
introduction of hydroxyalkyl side chains, adsorption rates are modified. In
this way, a slightly reduced flocculation rafe to almost no flocculation can
be achieved for a wide range of mining applications.
Similarly, guar interacts with hydrated cellulosic surfaces to affect the
formation and strength of a sheet ^during paper production. By
hydroxyalkylation of guar, adsorption rates onto hydrated cellulose
surfaces are altered for certain useful paper making applications.
One of the novel improvements attainable through hydroxyalkylation of
guar is solubility in water- miscible solvents such as glycols and alcohol.
Solvent miscibility enables hydroxyalkyl guar derivatives to be used as
thickeners for certain slurry explosives .
Hydroxyalkyl-guar is . suited to textile thickening and; sizing
(141

operations. ' •

Carboxymethylated guar gum is used in food industry. It was

evaluated as a thikener in printing of cotton textiles with reactive dyes. (4j 5

(19)
CHAPTERTWO
EXPERIMENTAL
 2. EXPERIMENTAL
>

2.1.0. Source of Materials:

Guar gum ;'is milled endosperm from the1 seed of Cyamopsis
tetragonoloba plant. Production of 1996 and 1997 were kindly supplied by
Sudanese Guar Company Ltd. Singa. The two commercial samples were
named'Si and ;S2 respectively .The water-soluble component of each
commercial samples were extracted and named Fsi and Fs2 .
The present study deals with structure, general composition and
properties of guar gum , particularly water-soluble component.

2.1.1. Guar Gum Fractionation(44'21):

One litre of 0.3% aqueous suspension of guar flour (S2) was
prepared. Guar flour was readily separated into water - soluble and water -
insoluble components. The water-insoluble component was separated from
soluble component by centrifuge. It was washed repeatedly with fresh
portions of acetone. After the final washing, the brownish white
precipitate was dried over calcium chloride in a vacuum desiccator. It was
then ground, stored in stoppered tube and named (I),
The water- soluble component of guar gum (Fs 2 ) was poured into a 3-
necked 3 litres round-bottom flask connected with a mechanical stirrer and
separator/ funnel. Acetone (95% w/v) was added drop by drop from a
separator/ funnel to the stirred solution. When a suitable quantity of fine
white filaments of gum was formed, the additon of acetone was stopped.
This phase was obtained by adding 100ml acetone. The solution was
allowed to stand overnight. Then the precipitate was separated by
centrifuge, washed repreatedly with fresh portions of acetone and dried in a
desiccator. It was then gound.and stored in stoppered. tube. This was
considered as fraction one (F[).

(20)
 This operation was repeated with fraction two (F2) and fraction three
(F3) respectively by successive addition of 30 rfil acetone portions.

2.2.0 Physico - Chemical Properties of Guar Gum :

2.2.1 Infra - Red Spectra^ :
Infra. - red spectra of S2 sample (1997 product), I (water - insoluble
fraction) V\t F?! and F3(water-soluble fractions) were recorded in the region
600 - 4000 cm"1 using Perkin - Elmer 1330 IR spectrophotometer.

2.2.2 Moisture Content*2!:

l.Og Sample (Si,S2,1, Fi,F2 and F3) was heated in a porcelain
crucible in an oven at 105°C for 6 hrs. It was then cooled in a desiccator
and weighed, The procedure was repeated until a constant weight was
obtained . The percentages of the moisture, contents were calculated as
follows:
Moisture % = (Wi-W 2 ) x 100

Where:
Wj = oiginal weight of t.he sample
: W2 = : weight of the sample after drying

2.2.3. Ash Content (2) :

. l.Og of sample (S),S2, I jFj,F2 and F3) was weighed to the nearest
0.00lg in a dry porcelain crucible . The crucible was ignited in a muffle
furnace at 550°C for 6 hrs, until free from carbon . It was then cooled in a
desiccator and weighed
The procedure was repeated to a constant weight of a carbon free ash.
The percentages of the total ash of dry samples were obtained by the
following equation:

(21)
 Ash% . = • ' Weight of residue . x 100
Weight of sample.

2.2.4 Nitrogen (Protein) Content (45,46).

Nitrogen content was determined by a semi-micro-Kjeldahl method.

0.2g of each sample (SI,S2>I,F1,F2 and F3) was digested in a small digestion
flask using 0,8g: of catalyst mixture (96% anhydrous sodium sulphate, 4%
cupric sulphate) .2ml of concentrated sulphuric acid were added to the flask
and the contents were digested for 3 lirs till clear liquid was obtained.

The digest was cooled, diluted and then transferred to the distillation
unit using minimum volume of distilled water. It was then made alkaline
with 20 ml of 40% aqueous sodium hydroxide solution. The ammonia was
distilled into 1.0ml of 25 boric acid solution for half an hour. 3drops of
bromocresol green- methyl red mixed indicator were added. The apparatus
was steamed out for 5 minutes and then distillate was titrated with 0.0IN
HC1. •

The nitrogen and crude protein percentages were calculated according

to the following equations: •
•. Nitrogen % - V x NA x 0.014x100

• ) . - . ' W

Where: ' . ' ; - : • ;

V = the volume of titrant.

NJV , T= normality of the acid.
L
, W - weight of the sample
Protein % = Nitroeen % x 6.25 '

•(22)
 2.2.5. Determination of pH:
pH of the solutions of whole guar gums ;0.25%.to 0.05% were
determined using Kent Eil 7020 pH meter at 35°C .
pH of the solutions of fraction gums F ] , F2 and F3 were also
determined by the same method.

2.2.6. Determination of Viscosity(47'48):

0.25% aqueous solution: was prepared from each water-soluble
component (Fsj and Fs2) of guar, gum and eachfractions (Fl5F2 and F3).
The rates of flow recorded for successive dilutions (0.25% to 0.05%) using
the Ubbelohde viscometer in-a constant temperature water bath at 25°C .
The viscosities of these solutions were determined .

2.2.7. Determination of Specific Rotation (49'50):

•••"••• 'The specific rotations of, 0.25% to 0.05% for Fsi, Fs2 (whole water-
soluble component) Fj, F2 and F3 (fractions), aqueous solutions were
determined using Perkin -Elmer polarimeter.
The polarimeter tube, 100mm in length, was filled with the solution.
It was then placed in the- polarimeter and kept at 25°C in at use of water
bath.
The specific rotations were determined according to the following
relation: ;
[aft,= 100 a
LC
Where : •. \

[o.}'{) = specific rotation for a given wavelength

(589nm) at a given temperature (25°C).
a .= observed angle of rotation

(23)
 L = length of light path in decimeters ; .
C •=• • concentration of solute, g solute/lOOml solution..

2.2.8. Determination of Elements in Guar Gum(51):

In common with other methods of physico-chemical analysis, the
analysis of low concentrations by X-ray fluorescencce spectrometry can be
defined in terms of the ability to detect and measure a very weak response
superimposed upon a back ground of almost equivalent strength . ( J J }
In this study, X-ray fluorescencpe (XRF) was used to determine the
contents of some of metals (atomic number > 18) present in guar gum.
The XRF spectrophotometer used was C d - 1 0 9 XRF system : Cd -
109 annular X-ray excitation source, Pop Top Si (Li) detector Model SLP
06175-P, Canberra Bin Power Supply, High, Voltage Power Supply,
Spectroscopy Amplifier, Series 35 Plus Multichannel Analyzer (MCA) .
Before analysis, gum samples (Si and S2),water- insoluble component
(I) and water- sojuble fraetions( Fi,F2 and F3 )were prepared in,pellet form,
using a pressing machine. Each time a pellet was placed centrally on top of
the Cd -109 source to be irradiated. The counting was started by processing
and displaying, of amplified signal on MCA which is connected directly
with a computer where the X-ray spectrum is analysed. .

(24)
 CHAPTER THREE
RESULTS AND DISCUSSION
 3. RESULTS AND DISCUSSION

Guar'igurn has^ emerged as a -new industrial crop. It can be.expected that

!
the demand for guar gum will continue to increase.
i Guar gum production in Sudan is a very recent development only started
in 1996. Its application in non - food industries was unknown in the
country.Though, it has been used' in food-industry recently.
•Guar gum is, indeed , a versatile product. The physico - chemical
properties of guar :gum are important in their industrial applications.
• Marketed; • ;guar gum !
: is the endosperm flour. It is separated and
.ground by the usual mechanical processing technique that does not produce
completely pure, endosperm. Therefore, the gum is not perfectly pure but
contains small amounts of hull and germ. Contents such as protein,, ash. and
moisture are considered as guar gum impurities. Since the whole seed is
edible, this contamination dilutes slightly the amount of gum quality. 'but
does not harm its suitability as a food additive.

3.1. Fractlonatoin of Guar Gum:

E. Heyne and R.L. Whistljsr, separated water- soluble component of
guar gum into 17 fractions. Analysis of the fractions indicated that tractions
(3) to (12) were identical in composition (galactomannan polysacchande);
they represent the main portion that precipitates in 2,5 - 40% ethanol.
Fractionation of guaran acetate into 7 parts showed that they have identical
optical rotation. (2l)
P.'A. Hui and H. Neukom fractionated guar gum to (a) cold-uater
soluble, (b) hot -water soluble and (c) hot-water insoluble fractions. They
found a wide spread of sugar compositions and variation in molecular
vveight of separated fractions.(:i2;

(25)
 The present study,, fractionation by addition of acetone to water-soluble
component- (at room temperature) of (commercial grade sample (S.,) of guar,
gum has been carried out and some of physico-chetnical parameters have',
been determined. Results are compared between whole and gum fractions
and among gum fractions themselves.
Table (2) shows some physical data for the two comrnercial products of
guar gum (S S,). the water-insoluble fraction (at room temperature) and the
three fractions that separated from water-soluble fraction. Table (2) also
explains the, percentages of their yields.

3.2.0. Physico-chemical Properties of Guar Gum:

Guar gum used was yellowish white flour. It was dissolved in water
forming aqueous suspension. , Discarding of water-insoluble fraction
resulted in clear water-soluble fraction. Guar gum solutions behave as non-
Newtonian solution up to the concentration about 0.5% .

3.2.1. Infra-red Spectra:

Figures (6) (7) (8) (9) (10) show the characteristic functional groups
of a commercial .sample of giiar giim (S ),. water -insoluble fraction, (I) and
f - . . • • •• ; -

water - soluble fractions (F} ,F7 and F3). The frinctional groups of the five
samples concide with the structure of galactomannan polysaccharide t--1--4-01
(1- 4-p-D-mannopyranosyl units,with a- D- gaiactopyranosyl units).
Although water - insoluble fraction contains high percentages of fibre
and protein, it contains also amount of galactomannan polysaccharide.

(26)
3.2,2. Moisture Content: /•
Table (2) shows that the moisture content p;.2, 7,8%) for the whole
gum Sj and S2 respectively. They are in close agreement with the value
reported by Thomas et al.(5%)(56) , but they are lower than the range of;
moisture content reported,by Whistler ( 8-12%)(13\ ; The water-soluble
fractions have moisture contents (5.2% ,5.3% ,7.5%) higher than that of
water-insoluble fraction (4.7%) due to their higher content of
gaiactomannan polysaccaride(gum).Among the fractions F 3 has the highest
content of moisture.

3.2.3.Ash Content:
Table (2) shows the ash content for the two commercial samples S K
and S2 (1.14, 0.81% respectively). The ash content of S2 is in the ranged
reported by Whistler (l3) (0.5 -1.0% ) and Sj content is in close agreement
with the range. :
The values of ash content for the water-soluble fractions are (0.66%,
0.60%, 0.50%) lower than that of the whole samples . Water-insoluble
fraction has ash value of 0.88% higher than values of water- soluble
fractions. This may be due to the'presence of hull and germ constituents!
that can mix during separation processing.

3.2,4. Nitrogen (Protein) Content:

From Table (3) the values of protein content for the two commercial
guar gum samples are 4.24% , 4.58% nearly somewhat in agreement with
5% ihe value which reported for pure endosperm in Table(l)° 4) . They are
also within the range (4% -5%) reported by Stein, Mall and Co. (D7) for
protein content in commercial guar gum.
Water-soluble fractions contain only traces of protein (0.31% ,0.33%
and 0.35%). F3 has the highest content of nitrogen. Water-insoluble

(27)
 fraction contains slightly greater percent of protein ;(0.74%) than water-
• . . ; . { • • • » • . - , ; : • •• i * - " ; •

;
" "• • • ; • } • " . - . . ' . • < • ' • . ' - ':- - '• '

soluble fractions because it was contaminated with hMl and germ.

3.2.5. Determination of pH :
Guar gum is neutral'gum. It has no uronic acids.Neutral gums such as
guar gum usually form solutions which are not dependent on pH .
Table (4) shows that the pH values of whole gum (6.7, 6.84) and of
fractions Fi,F 2 and F3 7.0, 5.9, 5.9 respectively.

3.2.6. Initrinsic Viscosity :

Viscosity is a commercial value of the gum. The higher the viscosity
of the: gum, the higher its .commercial value. Gums are industrially
demanded according to their viscosities.
In our study , Table 7 shows that the intrinsic viscosities are 6.4, 6.8
dl.g"1 for the whole water - soluble fractions and 6.6, 7.0, 7.5 dl.g"1 for
its fractions. F 3 represents the highest value. In general there is little
variation in the intrinsic viscosity values of the whole samples- (Fsj and
FS2) and fractions (F| ,F2 and F3).
Gums having a high content of D-galactose have viscosities higher
than those of gums with lower D-galactose content/^ Therefore, the
variation in the intrinsic viscosity values of the fractions ensures spread of
sugar compositions in guar gum.

3.2.7. Molecular-Weight:
The variation in the molecular weight values reported in literature for
guar gum is due to the difference in sample preparation, purification of
samples and the techniques used.

(28)
 Table (7) shows that the molecular weights of the two water-soluble
component of the commercial samples (7.01 x 103, 7.62 x 10 "'* g mol"').
The values are close to 9.5 x 105 which resulted by using light -scattering
and viscosity measurements.(3) Although in the latter, the value of
molecular weight was calculated from viscosity data by using constants
derived by Koleske and Kurath differ from the ones we used.
The values of average molecular weights in our study are lower than
2.2 x 106 (58 > and 1.9 x 106 (5}
but they are within the range (500,000
- l,000,000)(59) reported in the literature.
Again Table (7) shows that molecular weight of the three fractions
(F, ; F 2 and F3) are 7.31 x 105, 7.93 xlO5 and 8.73x105 . F3 has the highest
value of molecular weight. Although there is variation in molecular
weights of samples and fractions , but it is not far.
From results of Hui and Neukom(:i2): galactomannans which make up
guar gum differed in the ratio of galactose to mannose, cold water-soluble
fraction 1:1.3 while hot water - soluble fraction 1:1.7 water-insoluble ratio
i:7 and original sample 1:2. That reflect a wide spread of sugar
compositions in guar gum and ensures polydispersity in molecular weight
observed in our results.

3.2.8. Specific Rotation :

Table (9) gives the values of specific optical rotation for Fsi and Fs2
H-580.- 59°). It also shows the specific optical rotations of fractions (+64°,
-66°, -r 65°). F2 represents the highest value and the values of the three
fractions are higher than those of the whole sample. All of them are lower
than, the value of +77° reported by P.A. Hui and H.Neukom.(:>2)

(29)
 3.2.9. Metal Content:
The metals Ca, K, Na, Mg, Fe , Zn ,Cu and Mn play an important role
in physiological effects and nutrition.
The presence of metals in addition to carbohydrate and protein has
made guar glim of high potential for the use in food industry and
Pharmaceuticals.
Table (10) shows the element content (atomic number >18) in
percentages and ppm.
Arsenic, lead, zinc and copper contents is very important in determining
the level of toxicity. They must not exceed certain level. Minimum
standards for good quality guar gum powder have been defined in the
United States and by European Union Specification as follows: As:
maximum 3ppm, Pb: max. lOppm, Zn and Cu: maximum 50ppm. In our
study, commercial samples and fractions (Table 10) contain As, Pb, Zn and
Cu within the standard limits.

3.3. Conclusion:
Guar gum is a natural high molecular - weight hydrocolloidal
polysaccharide. It is composed of galactan and man nan units combined
through glycosidic linkages, which may be described chemically as
galactomannan. Dissolved in cold or hot water, guar gum forms a slime of
high viscosity.
We have succeeded in obtaining optically different compounds of
varying molecular masses by fractional precipitation of guar gum using
acetone after separation of water-insoluble components by centrifugation.
This fractionation of gum confirmed the polydispersity in molecular weight.
The differences between water-insoluble fraction and water-soluble
iVaciions in contents of metals, protein, moisture and ash .In addition to

(30)
above differences , the water-soluble fractions differ from each other in
;
their molecular masses(viscosity) and specific rotations..
In comparison with other gums like locust bean >gum,(52) gum
tragacanth(61) and gum arabic(62), giiar gum is amuch more homogeneous
polysaccharide because of little variation in molecular weight values
(viscosity) between water-soluble fractions in addition to a small amount
of water-insoluble fraction in the whole sample.

(31)
 Table 2: Some physical data for samples
: ! ofzuargiim and its fractions

Sample Fractionation Moisture % Ash %

Yield %
Si • • —

5.2 , 1.14
s2 _ _ _

. 7.8 0.81

;
' :*I ; / 24.0 , .; 4.7 i 0.88
F, 34.0 5.2 0.66
F2 18.2 5.3 0.60
; F 3 ., 23.5 .7.5 0.50

*I, F(, F2 and F3 obtained from S2

(32)
Table 3 : Nitrogen and protein contents in sampies
ofguar gum and its fractions:

Sample N. % Protein % ;
s, 0.678 4.24
0.732 4.58
I 0,118 0,74
F, 0.049 0.31
F2 0.053 0.33
F3 0.056 0.35

Table 4; pH for samples of gnar

gum and its fractions:

Sample PH .
S,(FSl) 6.70
S2(Fs3) • 6.84
F, 7,00
' F2 5.90
. F3 ' .5.90

(33)
Table 5: The flow time, u, for Fsj and Fs? water - soluble fractions ofsuar sum
audits fractions Fu F?.andF\ at 25°C

c% Fs, ,.-,- Fs2 F, F2 F3

g/ 100cm3 ts sec. tssec „ . ts s e c . ts sec. ts sec.
0.25 70.00 •-- 74.30 71.75 73.20 74.50

0.20 5L80 . .60.00 . 53.00 54.10 78.50

0.15 36.70 38.60" 37.60 38.30 39.10

0.10 25.00 ;; 26.00 25.50 26.00 26.50

0.05 16.50 16.90 16.70 16.95 17.20

Table 6 : The reduced viscosity, n*/C%it, for Fsu Fsjt.
Fu F7 and Fi fractions of'euar sum at 25°C:

c% FSl • .Fs 2 • :
•! F.i. ; F2
g/100cm3 T1sp/G% T] S p/C% Tlsp/C% Tlsp/C%

0.250 20.80 22.30 21.40 21.90 22.35

0.200 17.90 21.50 • 18.45 • 18.95 19.40
0.150 15.00 16.10 15.50 15.95 16.40 '
0.100 12.10 13.00 12.60 13.00 13.50 :
0.050 09.20 09.90 09.60 10.00 10.50

Table 7: Intrinsic viscosity and molecular

weight for fractions of guar sum

Sample hldl.g 1 Mw g mol"1 :

,F S l ; 6.4 , 7.01xl0 5 , ;

Fs 2 . : ' : 6.8 ; 7 . 6 2 x 1 0 ' •;. |

;'
Fi 6.6 7.31X103 !

F2 7.0 7.93x10'
F3 • :
= 7.5 : 8.73xlO5 i

(35)
Table8: the optical rotation, a°, for waters soluble
• • • • : < - . . . * , • • • . . •

• • • - . • - - t-'>_* ||.j • • • ••

fractions of guar gum'Fsu Fs?and its fractions

FhF7 andFi at 23°C:

; C%, •
a°
g/100cm3 ..', FSj; Fs2- F2 F3 ;
, ,0.250 0.145 0.1470 0.160 0.165 o.i652 ;
0.200 0.116 0.1180 0 . 1 2 8 '•{ 0.132 ; G.i3oo
0.150 0.088 0.0890 0.096 0.099 0.0975
oaoo 0.058 0.0590 0.064 0.066 0.0650 |
0.050 0.029 0.0295 0.032 0.033 0.0325

a
jD > of water-soluble fractions
and Fs^ ofguargum and its fractions (25°C)

Sample HD
Fs, +58°
Fs2 +59°
F, +64°
F2 +66°
F3 • +65°

(36)
 l^table JO: Determination of elements contained in samples
and fractions of suar sum in % andppm
* . • ( • ; • : .

it'-' ; •
s:, r s2 I •F, | F 2 ; • :;• ;F3-;- :•';

f% 0r3l9 0.358 0,2858 0386 0.272 0.280 ' j

0,267. 0.129 0.104 0.115 0.113 0.103 :
•tin.

fpn; ppm ; 33,900,; 41,700 39.900 31.900 38.200 39:800 :;

•FQ ppm 63,900, 65.500 62.000 56.600 62.500 63:900

^, *" pp m 51.500 57.500 72.900 61.900 43.800 31.100

^ ^ - ppm 11.600 14.500 7.750 11.200 10.400 7.390 ;

I f "'•ppm L460| 1,340. 1,210 1.610 1.680 1.090:

^ u 9.960 9.180 11.900 7.570 5.470 4.540 1
;'t.|P PPm
;]P S ppm 1.010 0.786 0.967 0.600 0.511 0.3-58

I S P P ^ : 7.750 8.590 ; 13.100 , 4.190 11.800. ,5.820

jRb ppm 6.670 I 8.720 4.080 L320 1.190 1.230

•v PPm
6.180 6.160 7.720 1.180 1.050 O.S4'2

^PPm
1.020 1.110 1.360 •, 0.911 0.757 ;
i
Y 1.320 1.640 1,320 r 0.982 0.797
: PP m
i
: ^bppm 0.755 0.731 0.500 0.456 0.310
'
! 5® ppm
2.610 1.780
I, :

(37)
illliti
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(41).
3600 2000 '\500 600
WAVENUMBE8CCMJL

Fi&^tO..;.: Theinfrajredspectriim of fraction three (F3) of guar gum

Si™iifliii»iirmt^iOTMimMSmM^""™Mfl1iWn)itH??'" ltl ^ ! ^ nrrnt-iiin n i
Fig. (11): Reduced viscosity (TjSp/C%) versus concentration (C%) for
water-soluble fractions Fsi and FS2 of guar gum at 25°C.

25 -1

20 -

15 •

10-

0
0 0.05 0.1 0.15 0,2 0.25 0.3
C%(g/ 100 ml)

(43)
Fig. (12) : Reduced viscosity (T|sp/C%) versus concentration (C%) for
Fi, F2 and F3 fractions of guar gum: at 25°C.

25 -

20 -

15 -

1.0-

0
0.05 0.1 0.15 0.2 0.25
C%(g/100ml)

(44)
Fig. (13) : Optical Rot^ti^; ctofyersusrcb water1-
.1f . ;\
soluble fractions of guar gum Fsi and Fyi at 25°C.

0.15 -I

0.14 -

0.13 -

0.12 -

0.11 -

0.1 -

0.09 -

0.08 -
•Fsl
Fs2
0.07 -

0.06 -

0.05 -

0.04 -

0.03 -

0.02 -

0.01 -

0*
0 0.05 0.1. 0.15 0.2 0.25
C%(g/100ml)

(45);
 Fig. (14): Optical Rotation, a°, versus concentration (C%) for Fi, F2;
and F3 fractions of guar gum at 25°C.

0.19 -
0.18 -
0.17 -
0.16 -
0.15 -
0.14 -
0.13 -
0.12 -
a
0.11 -
0.1-
0.09 -
0.08 -
0.07 -
0.06 -
0.05 -
0.04 -
0.03 -
•0.02 -
0.01 -
OH

0.05 0.1 0.15 0.2 , 0.25

C% (g/ 100 ml)

(46)
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