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1. INTRODUCTION
2. EXPERIMENTAL
2.2. Characterization
The modified bentonites were characterized by XRD, BET surface area and FTIR. XRD
studies were conducted using a Phillips PW 3442 diffractometer with a CuKct radiation
(1.54060/~) for crystalline phase detection between 4 and 80~ (20) and the obtained patterns
were compared with JCPDS data files. Physisorption measurements were performed with a
Beckman Coulter SA 3100 instrument; BET surface areas were determined by nitrogen
adsorption at-196~ with an Ar/N2 ratio of 70/30. The presence of functional groups and
evaluation of the solids purity were achieved by FTIR; spectra were recorded in a Perkin-
Elmer 283 spectrometer in a range of 4000-400 cm -~. Samples were mixed with KBr and
pressed into a disc.
XRD spectrum of bentonite without sodium carbonate showed the phases corresponding to
bentonite, but other phases as kaolin/montmorillonite, quartz and muscovite were also
identified. Table 1 shows the composition of original bentonite. This clay presents a high
content in silicon, which can be associated to quartz. The higher CaO content in comparison
to alkalis content (Na20, K20) refers to this clay as a calcium bentonite. These types of
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bentonites are not very expansible in relation to sodium betonites. On the other hand, the
lower Fe203 content is associated to the white color found in our bentonite
Table 1
Chemical analysis of original bentonite
Fig. 1 shows XRD spectra of original and modified bentonite using 3.0 M sodium
carbonate concentration. Some phases, such as Na2CO3.10H20 y NazCa(CO3)2.5H20 were
very hard to determine them. If amorphous salts of sodium carbonate or very small crystals of
these salts are generated on the surface of the modified bentonites during the hydrothermal
process, they cannot diffract and are not able to be detected by XRD.
I Na2c03.10H20, NaZCa(CO3)2.SI-I20
|
| . . . . , . . . . i . . . . , . . . . , . . . . , . . . . i . . . . , . . . . , . . . . i . . . . . . . . . , . . . . , . . . . , . . . . | - 9
5 10 15 20 25 30 35 40 45 50 55 60 65 70 75
2theta
Fig. 1. XRD of modified bentonite using 3.0 M Na2CO3 solution.
Fig. 2 shows FTIR spectra of original and modified bentonite. The band at 1460 cm -I
represents carbonate anions placed on the surface of bentonite. This band disappears when the
clay is washed with abundant distillated water which indicates that the sodium carbonate is
present on the surface of the modified clay. As we mentioned above, calcium bentonite does
not expand its sheets and they cannot occlude carbonate species.
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washed _A ........
lk t
. . . .
Fig. 2. FTIR of modified bentonite with 3.0 M sodium carbonate and washed with distillate water in
1"10 relation solid: water.
Table 2 shows the surface areas of original and modified bentonite. As can seen, the
surface area of the original bentonite is lower in comparison with other values reported for
bentonites. These results can be associated to the presence of quartz (or other more dense
phases) in the composition of the treated materials which decrease the porosity of bentonite.
Furthermore, another possible cause is related to original composition of bentonite (calcium
bentonite) which, as w e mentioned above, they are less expansible than sodium bentonites.
When the bentonite is modified with sodium carbonate, the surface area decreases due to the
accumulation of this salt on the surface of solid. This decrease is higher when the sodium
carbonate is more concentrated
Table 2
Surface area of the original and modified bentonite using different concentrations of sodium
carbonate.
Fig. 3 shows the pH of the solutions as a function of bentonite mass for 3.0M bentonite.
In general, the behavior of:all assayed modified bentonites was very similar, including the
original clay used as reference: the theoretical and experimental pH increased as the weight of
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the studied solids. However, the experimental pH values were higher than those of the
theoretical ones. The observed difference could be due to the way in which both pH values
were determined. The experimental pH values were obtained using a glass electrode which is
only sensitive to the amount of free protons in the synthetic gastric juice; while, the
theoretical pH values were determined using the expression pH=-log[H +] which is applied to
results of the acid-base titrations. During the neutralization procedure with NaOH, other ions
or species such as magnesium, calcium and pepsin enzyme along with free proton ions can
interact with the O H groups making the calculated pH lower than the experimental one.
Rivera et al. [3, 5] reported similar results. These authors suggest using experimental pH as a
more effective way to determine the neutralization capacity of zeolites.
7
6
5
4
I--o--TI
~ E
3
. Q..cl--
.---- [] -0 ''~''O''a "
I
O , , , , , , , , , , |
therapeutic properties on the control of the acidity, these doses reduce the enzymatic activity
of the pepsin.
Although, the sodium carbonate was determined outside of the bentonite sheets, these
modified bentonites can be used for dispersing the carbonate salt which achieved due to a
high contact between the antacid (sodium carbonate) and the free protons of the reaction
medium.
7 -- 2 . 0 M
- - ~ 1.5 M
r
3
2J 9 i - . ~ - - . . . . - .
To determine the interaction of the synthesized solids with pepsin, variable quantities of
modified clays, depending on its antacid activity (pH between 3 and 4), were mixed with the
synthetic gastric juice. Fig. 5 shows the UV-visible spectrum of solutions from 3M bentonite
before and after interaction with the synthetic gastric juice.
2.5
2.0
8 1.5
0.5
0
195 200 2'50 3"00 350 400 450 5"00 5"50 6"00 650 760 750 800
Wavelenght (rim)
Fig. 5. Pepsine UV-Visible spectra recorded after and before the contact with modified bentonite (3M)
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The UV-visible spectrum of original acid solution with pepsin, without interaction with
any solid, shows a maximum at 272 nm and a minimum at 250 nm. After interaction with 3M
bentonite, a small decrease in the maximum absorbance of the pepsin was observed. This
small decrease is probably due to adsorption of the enzyme onto the surface of the bentonite.
These results show that there was not a chemical reaction between the enzyme and the solid.
The interactions pepsin-solid were also determined by FT-IR spectroscopy. Fig. 5
shows the spectra of the solids after the contact with the synthetic gastric juice. Just before the
FT-IR spectrum was recorded, the solids were washed three times with abundant distillated
water. Under such experimental conditions, we cannot observe any band corresponding to
pepsin. These results show that the interaction bentonite-pepsin is weak, and it can be
eliminated by water.
3.0
2.0~
o~~4~_.~
bentonite
3500 3000 2500 2000 1500 1000 500
Wavelen~t (cm- 1)
Fig. 6. FTIR spectra of modified bentonites contacted with gastric synthetic juice and after washed
with abundant distillate water
4. C O N C L U S I O N S
The hydrothermal treating of calcium bentonites using sodium carbonate was not effective to
incorporate this salt inside of the framework. Sodium bentonite must be assayed for a possible
occlusion of the sodium carbonate into the structure of clay. Finally, it was possible to use
these bentonites as support of effective antacids as sodium carbonate. They could be used in
combination with other properties of clays as anti flatulent. Those medical properties of the
clays, in combination with an antacid effect, make this material a good multipurpose medical
drug.
ACKNOWLEDGEMENT
Authors are grateful to FONACIT F-2001000774 and CDCH-UC for financial support.. We
also acknowledge the insightful comments of Prof. Oscar Valbuena and Prof. G. Pinto
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REFERENCES