SYNTHESIS OF CELLULOSE-
1
N,N'-METHYLENE BISACRYLAMIDE-ACRYLATE ACID
2
COPOLYMER WITH SIMULTANEOUS METHOD,
3
CHARACTERIZATION AND APPLICATIONS
4 5
Meri Suhartini1*, Jadigia Ginting2, Sudirman,3
6
1 National Nuclear Energy Agency, Jl. Lebak Bulus Raya No.49, Jakarta, Indonesia 7
2PSTBM BATAN, BATAN PUSPIPTEK, Serpong, Tangerang Selatan 15314 8
9 10
A R T I C L E I N F O A B S T R A C T 11 12
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Cellulose modification was carried out using N, N'- methylenebisacrylamide (MBA) as crosslinking agent and Acrylate Acid (AA) as grafting agent. Gamma rays from Cobalt-60 was used as the initiator by simultaneously irradiation method. The aim of study to improve the physical and chemical properties of cellulose as lead metal ion adsorbent. The results showed that the maximum grafting (353%) wa s achieved at 40 kGy. The thermal analysis and ion exchange capacity measurement showed that the copolymer has a better thermal stability and ion exchange than pure cellulose. The applications of copolymer on Pb2+ ion adsorption indicated that the best adsorption found as 99.8% of 3 ppm Pb ion sorbent at pH ± 7.
© 2010 Atom Indonesia. All rights reserved
13
INTRODUCTION∗
14 15
Cellulose is the most abundant polymeric
16
material on earth and possesses several valuable
17
physicochemical properties suchas a fine cross-
18
section, good biocompatibility, high durability and
19
thermal stability, and good mechanical properties.
20
Cellulose is a reactive chemical due to the presence
21
of three hydroxyl groups ineach glucose residue,
22
which are mainly responsible for the reactions of
23
cellulose. [1] Cellulose contained in rice straw can
24
be modified to obtain chemical or physical
25
properties of the cellulose characteristics for suitable
26
use. Modified cellulose is also practical as a raw
27
material in the manufacture of membranes for
28
various separation techniques such as osmosis,
29
dialysis, microfiltration, ultrafiltration,
30
nanofiltration, reverse osmosis, pervaporation and
31
electrodialysis [1]. Modification of cellulose lately
32
utilize grafting techniques form (copolymer) that
33
commonly called graft copolymerization. Graft
34
copolymerization can be implemented in various
35
ways such as chemistry, photochemistry, enzymatic,
36
induction or induction plasma radiation [2].
37
∗Corresponding author.
E-mail address: [email protected]
38
Cellulose is highly crystalline and generally
39
insoluble, due to the intramolecular hydrogen bond
40
networks extending from the O(30)-H hydroxyl to
41
the O(5) ring oxygen of the next unit across the
42
glycosidic linkage and from the O(2)-H hydroxyl to
43
the O(60) hydroxyl of the next residue. Nowadays
44
the main uses of cellulose are for papers or
45
cardboards, membranes, tissues, explosives, textiles
46
and construction materials. An extensive scope of
47
applications of cellulose is limited for insoluble in
48
common solvents and by the lack of properties
49
inherent to synthetic polymers. Significant efforts
50
have been paid to the chemical modification of
51
cellulose [11] to improve resistance to heat or
52
abrasion [33,35], mechanical strength [36,37],water
53
or oil repellency [38e40], or antibacterial activity
54
[41]. One convenient route introducing new
55
chemical and physical properties to cellulose is the
56
graft modification. Three approaches are generally
57
used for synthesis graft copolymers (Scheme 2).
58
“Grafting onto” involves the reaction between
59
functional groups on two different polymers.
60
“Grafting from” involves a polymers with functional
61
groups (macro-initiator). that initiates the
62
polymerization of vinyl monomers. “Grafting
63
through” involves (co)polymerization of
64
macromonomer(s). [42]
65
In this study, isolated (cellulose) from rice straw as
66
polymers, and monomers as compiler (copolymer
67
formation) by copolymerization technique.
68
Copolymerization technique induced gamma
69
radiation simultaneously is N,N'-
70
methylenebisacrylamide (MBA) and acrylic acid
71
(AA). MBA as a crosslinking agent can lead to
72
increase molecular weight and degree of
73
polymerization. It can be predicted that MBA
74
prevent degradation in the reaction of radical
75
formation caused by radiation [3]. On the other
76
hand, AA as a grafting agent have carboxyl groups
77
that play a role in supporting the ion exchange
78
ability as an adsorbent metal cations. Rahmawati in
79
research has managed to modify the cellulose as
80
fiber ion exchanger with grafted acrylic acid
81
(monomer) on cellulose using the technique of pre-
82
irradiation graft copolymerization has a Cu2+ ion
83
adsorption capacity of 14.6 mg/g was determined by
84
AAS, and 3.54 meq/g is determined by titration [4].
85
Modification of cellulose is frequently called
86
biopolymer engineering.
87
In this study, biopolymer engineering of rice
88
straw cellulose is made by graft copolymerization of
89
acrylic acid (AA) and crosslinking N-N'-
90
methylenebisacrylamide (MBA) with gamma ray
91
irradiation.
92 93
EXPERIMENTAL METHOD
94 95
Materials
96
Rice straw obtained from the Agricultural
97
Land in Cigombong-Bogor, N-N'-
98
methylenebisacrylamide pa., Acrylate Acid pa.,
99
NaOH, H2O2, HCl, Copper Nitrate.
100 101
Procedure
102 103
Cellulose insulation from rice straw [4]
104 105
Copolymerization
106
Each cellulose approximately 0.2 grams was
107
put into 16 polyethylene plastic bags, then 1.0 mL
108
of N-N'-methylenebisacrylamide pa 1% (w / v) is
109
added to each bag. Into 8 each bag was added 0.75
110
mL of 99% acrylic acid (Copolymer A). 8 more into
111
each bag was added 0.75 mL of acrylic acid 19.8%
112
(Copolymer B). Bags were closed by a plastic seal
113
and then irradiated with gamma rays (60Co source)
114
at a dose of 10, 20, 30 and 40 kGy and dose rate of 5
115
kGy/hour. Copolymer Cellulose-MBA-AA that
116
produced is washed with distilled water to remove
117
residual monomers and then dried in an oven at
118
700C until the weight remains. The success is
119
determined by the percentage of grafting
120
copolymerization (Grafting, %G). The cellulose
121
before (W0) and after grafting (W1) calculated by the
122
following formula to get %G [5].
123 124 125 126 127
Characterization of Copolymer 128 129
Analysis of functional groups of the copolymer
130
using FTIR
131
Copolymers of cellulose-MBA-AA are
132
measured transmission of infrared light absorption
133
in the area of wave number 4000 cm-1 to 400 cm-1.
134 135
Thermal analysis by differential scanning
136
calorimetry (DSC)
137
The thermal properties of the copolymer is
138
analyzed at the temperature range of 60-600 0C and
139
a speed of 10 0C/min [6].
140 141
Determining the degree of development (swelling
142
capacity,% S) in water
143
0.05 grams (W1) copolymer put in a plastic
144
cup container. Then added 50 ml of water with a
145
temperature of 60 0C and allowed to stand for 24
146
hours. Then the copolymer is filtered with 120 mesh
147
stainless steel strainer, drained for 30 minutes and
148
weighed (W2) [6].
149 150
151 152
153 154
Ion exchange capacity
155
25 mg copolymers which have the best
156
percentage of grafting (%G) put into the erlenmeyer.
157
Then added 25.0 mL NaOH 0.1 N and stirred with a
158
magnetic stirrer for 15 minutes and filtered. Then
159
pipette 5.0 mL and the filtrate was added 2-3 drops
160
of phenolphthalein indicator (pp). Furthermore, the
161
filtrate is titrated with a HCl 0.05 N solution until
162
the color changes into pink [7].
163 164
165
(3)
166 167
Application
168
Cellulose-MBA-AA (copolymer A) is used
169
as an adsorbent of heavy metal ions. The metal used
170
in this study is Pb with a concentration of 3 ppm, 5
171
ppm, and 10 ppm were calculated adsorption
172
capacity, the effect of pH, adsorption isotherms of
173
Langmuir and Freundlich, as well as the analysis of
174
Eq. ...
Eq. ..
the surface of cellulose-MBA-AA before and after
175
used as an adsorbent by SEM-EDAX.
176 177 178
RESULTS AND DISCUSSION
179 180
Copolymerization Cellulose-MBA-AA
181
Determining the percentage of copolymer
182
grafting by gravimetric. This measurement is
183
intended to look at the success of graft
184
copolymerization or how many AA monomers are
185
grafted on cellulose with increasing doses of
186
irradiation. Graph the percentage of grafting (%
187
grafting) with the irradiation dose in the copolymer
188
are presented in Fig 1.
189 190
0 100 200 300 400
0 20 40 60
% Grafting
Irradiation dose(kGy)
Copoly mer A
191 192
Fig 1. Effect of irradiation dose to the percentage of grafting 193
(%G) in of cellulose-MBA-AA (Copolymer) 194
195 196
Figure 1 shows that copolymer A and B
197
have the same linearity pattern where increasing
198
doses of irradiation (10-40 kGy) will raise the
199
percentage of grafting copolymer (%G). The
200
percentage of grafting to the copolymer A (at the
201
lowest dose of 137.61%, and 353.82% at the highest
202
dose) was higher when compared with the sample
203
copolymer B (at the lowest dose amounted to
204
47.79% and 70.21% at the highest dose ). Effect of
205
irradiation dose to the percentage of grafting for
206
some variation of the concentration of acrylic acid
207
follows largely the logarithmic equation, increasing
208
of dose irradiation will increases the percentage of
209
grafting copolymer to achieve optimum of grafting
210
limit. Increased percentage of grafting copolymer A
211
and B obtained is different because amount of
212
radicals formed, radical position, availability and
213
diffusion of monomer and gel formation. Results
214
percentage of the best grafting occurred in
215
irradiation dose of 40 kGy. In addition, percentage
216
of grafting for acrylic acid with high concentration
217
(copolymer A) has bigger yield than low
218
concentration (copolymer B).
219 220 221
Characteristics of cellulose-MBA-AA
222
Characterization is necessary to know the
223
characteristics of cellulose-MBA-AA that has
224
formed a good group function, thermal analysis, ion
225
exchange capacity and other physical and chemical
226
properties [8].
227 228
Thermal analysis
229
Thermal analysis aims to determine the
230
thermal stability of cellulose which has been
231
modified. Thermal properties of the modified
232
cellulose (copolymer) better than pure cellulose
233
which is observed in the temperature range of 20-
234
600 0C. At the temperature 300-600 0C generally
235
cellulose can be degraded by heat optimally.
236
Samples for thermal analysis are copolymer
237
cellulose-MBA-AA of the highest percentage of
238
grafting (copolymer A and copolymer B ) then
239
compared with pure cellulose. The results of the
240
DSC thermogram of cellulose-MBA-AA is
241
presented in Fig 2.
242 243
244 245
Fig. 2. DSC thermogram of the isolated rice straw cellulose and 246
cellulose copolymer-MBA-AA 247
248
Figure 2 shows that pure cellulose and
249
copolymers B have calorimetry pattern nearly same,
250
there is a low exothermic peak at point (340 0C)
251 before the peak in the highest exothermic (≥ 50
252
mW). The exothermic peak point on pure cellulose
253
at 462.5 0C is lower than copolymer B sample (530
254
0C). In the other words, the energy required to heat a
255
sample of copolymer B more than the pure
256
cellulose. This is caused by the formation of graft
257
copolymer which increases the molecular weight
258
and degree of polymerization of copolymer B thus
259
requiring higher energy to degrade copolymer B.
260
This is consistent with the theory of bond energy
261
where the greater molecular weight of a substance,
262
the greater the energy needed to break the bonds
263
between the substance. In addition, samples of
264
Copolymer A decreased DSC at every interval and
265
has a single point temperature endothermic peak at a
266
temperature of 550 0C of resulting molecular weight
267
and degree of polymerization higher than copolymer
268
B. Thus we can say that the copolymers of
269
cellulose-MBA-AA has stability properties thermal
270
better than pure cellulose that can be seen from a
271
higher temperature needed to degrade these
272
compounds.
273 274
Analysis of functional groups of cellulose-MBA-
275
AA
276
Analysis of the functional groups carried
277
out to observe the changement of functional groups.
278
After the copolymerization process analysis of
279
functional groups in this study conducted on a
280
sample of cellulose-MBA-AA with the highest
281
percentage of grafting of acrylic acid with high
282
concentrations of (A) and copolymer with low
283
concentrations of acrylic acid (B). The FTIR
284
spectrum copolymer cellulose-MBA-AA with a
285
high concentration of acrylic acid (Copolymer A)
286
and low (Copolymer B) compared with the FTIR
287
spectrum of cellulose isolated from rice straw (pure
288
cellulose) is presented in Figure 3. The formation of
289
the copolymer is characterized by the emergence of
290
the peak (peak) that there are no the spectra of rice
291
straw cellulose insulation results. In general shift
292
wave number can also describe the occuring
293
crosslinking.
294
MBA is a ketone compound and acrylic acid
295
is a carboxylic acid compound. Carboxylic acid and
296
ketones groups will appear peak of C=O in the
297
range of wave number 1820-1660 cm-1 [9]. FTIR
298
spectra cellulose-MBA-AA indicates the occurrence
299
of crosslinking N,N'-methylenebisacrylamide
300
(MBA) and grafting from acrylic acid because it
301
appears that there are no peaks in the FTIR spectra
302
pure cellulose. Copolymer A has the peak of the
303
weak of the functional groups of C=O at wave 1818
304
cm-1, and 1666 cm-1 for copolymer B. The
305
emergence of the peak of the functional group C=O
306
at wave number 1818 cm-1 which is accompanied by
307
functional groups -OH peak at wave number 3040
308
cm-1 in order to interpret the carboxylic acid
309
compound in the copolymer or in other words there
310
has been a graft of acrylic acid on cellulose , while
311
the typical peak of the monomer N, N'-
312
methylenebisacrylamide (MBA) is characterized by
313
functional groups -NH peak at wave number 3793
314
cm-1 of the acrylic acid copolymer with a high
315
concentration of (A); 3709 cm-1 of the copolymer
316
with a low concentration of acrylic acid (B) that
317
shows there has been crosslinking N,N'-
318
methylenebisacrylamide on cellulose.
319 320
Table 1. Functional groups and wave number of the isolated rice 321
straw (pure cellulose) and cellulose-MBA-AA in the FTIR 322
spectra 323
Functional Wave Number (cm-1)
groups cellulose from isolated rice straw
Copolymer A (Cellulosa- MBA-AA with
high concentration
AA)
Copolymer B (Cellulosa- MBA-AA with
low concentration
AA) -OH
C-O C1-O-C4
-CH alifatic -CH aromatic C=C -NH
3307 1008 900 2892 3613 - - -
3040 1361 924 2794 3694 1583 3793 1818
3024 1340 912 2799 3532 1582 3709 1666
324 325 326
327 328 329
Fig 3. FTIR spectra 330
(a.Pure cellulose, b.Copolymers B, c.Copolymers A) 331
332 333
The degree of swelling (swelling capacity,% S) in
334
water
335
The degree of swelling in each of the
336
samples presented in Fig.4.
337 338 339 340 341 342 343 344
345 346 347
Fig 4. Effect of irradiation dose to degree of swelling (%S) on 348
cellulose MBA-AA 349
350
On testing the degree of swelling of the pure
351
cellulose obtained results swelling percentage (%S)
352
amounted to 544.49% when compared with
353
copolymer cellulose-MBA-AA to be impaired
354
significantly. %S in water resulting for copolymers
355
A at a dose of 10, 20, 30 and 40 kGy, respectively
356
was 213.08%, 187.04%, 146.97% and 144.15%,
357
while copolymer B respectively was 331.17%,
358
301.95%, 266.01% and 259.05%.
359
The decline in %S of a dose of 10 kGy to 40
360
kGy indicates that there is a reduction of the
361
hydroxyl groups of cellulose chains indicate the
362
number of monomer or substituted in –OH group.
363
The more substituted monomers will increase the
364
ability to adsorb heavy metals. The copolymer with
365
the lowest %S can be used as adsorbent. %S in the
366
lowest water on acrylic acid copolymer with a high
367
concentration of (A) and low (B) occurs at a dose of
368
40 kGy with a value of 144.15% and 259.05%.
369
Figure 4 shows that the greater the dose of
370
irradiation would decrease percentage of copolymer
371
swelling in water. It can happen because the
372
radiation can increase the density of the bonds
373
between the molecules in copolymers formed,
374
causing water adsorption decreases. In addition, the
375
copolymers with high concentration (acrylic acid)
376
has a relatively small percentage of the swelling
377
compared to the concentration of acrylic acid is low,
378
then speculated growing number of monomer will
379
reduce %S in the water.
380 381
Ion exchange capacity
382
Ion exchange capacity testing aims to
383
determine the ability of the copolymer for
384
adsorption of the metal ion. The working principle
385
of ion exchange capacity is to neutralize residual
386
NaOH (from mixing with cellulose MBA-AA) with
387
HCl until it reaches a point equivalent. The value of
388
ion exchange capacity of the irradiation dose is
389
presented in Fig.5.
390
391 392 393
Fig5. Effect of the irradiation dose to ion exchange capacity on 394
cellulose-MBA-AA 395
396
Figure 5 shows that each of the samples
397
increased ion exchange capacity with increasing
398
doses of irradiation. Best ion exchange capacity
399
values occurred at a dose of 40 kGy which the value
400
of ion exchange capacity for copolymer B is 22.73
401
meq/g and copolymer A is18.3 meq/g higher than
402
the pure cellulose (14,46 meq/g). This is caused by
403
the high degree of polymerization of the copolymer
404
B which add groups -OH, -COOH, -NH (derived
405
from AA and MBA monomers polymerized) in
406
cellulose. These groups can perform ion exchange in
407
excess NaOH solution such as Na+ into -ONa, and -
408
COONa so that there will be a decrease in the
409
concentration of NaOH solution [10].
410 411
Application
412 413
Effect of Pb Concentration to adsorption
414
One of the factors that may affect the ability
415
of the adsorbent in the adsorption of the metal ion is
416
concentration [11]. Pb has various concentration of
417
3 ppm, 5 ppm, and 10 ppm were subsequently
418
adsorbed by the cellulose and cellulose-MBA-AA.
419
The percentage of adsorption of pure cellulose and
420
cellulose-MBA-AA shown in Fig. 6.
421 422
423 424
Fig.6. Effect of Pb concentration to adsorption 425
426
Figure 6 indicate that the cellulose-MBA-
427
AA can adsorb better than pure cellulose. At a
428
concentration of 3 ppm and 5 ppm, the percentage
429
tends to be stable adsorption on the cellulose-MBA-
430
AA of 99.8% and of 98% pure cellulose. The
431
percentage of adsorption cellulose-MBA-AA is
432
higher due to the monomer AA and MBA
433
(copolymer) adding active groups on the cellulose-
434
MBA-AA as COOH, -C=O, -OH and -NH that can
435
adsorb metal ions (ion exchange) whereas cellulose
436
contains only hydroxyl group (OH). However, at
437
concentrations of 10 ppm a decline in the percentage
438
of adsorption on the cellulose-MBA-AA was 1.83
439
whereas in pure cellulose an increase of 0.43. This
440
is due to the bond between Pb with active group -
441
COOH, -C=O, more powerful than the -OH so that
442
events are slower desorption that cause the
443
percentage of adsorption decreases.
444 445
Effect of Pb concentration on the adsorption
446
capacity
447
In addition the percentage of adsorption, the
448
adsorption capacity also needs to be calculated to
449
determine the amount of metal ions which can be
450
adsorption [12]. The results of measurements
451
adsorption capacity for cellulose and cellulose-
452
MBA-AA shown in Fig.7
453 454
455 456
Fig 7. Effect of Pb concentration on the adsorption capacity (Q) 457
458
Fig. 7 shows that the value of the adsorption
459
capacity increases by increasing concentrations of
460
Pb. In addition, pure cellulose and cellulose-MBA-
461
AA has a value of adsorption capacity that is not
462
extremely different at 46.21 mg /g for cellulose-
463
MBA-AA and 42.42 mg / g for pure cellulose at a
464
concentration of 10 ppm.
465 466
Effect of pH on the percentage of adsorption
467
Another thing to consider in the use of
468
cellulose-MBA-AA as an adsorbent is the effect of
469
pH on the adsorption of Pb (pH variation used was 5
470
(acid) 7 (neutral), and 9 (alkaline)). As for the effect
471
of pH on the adsorption of Pb presented in Fig. 8.
472 473
474 475
Fig. 8. Effect of pH to the Pb adsorption 476
477
The fig.8 indicate that the optimum
478
adsorption of Pb is 90.28% at neutral (pH ± 7).
479
Alkaline (pH=9), the percentage of adsorption
480
deflate (58.40%). This is due to the pH neutral,
481
coordinated bond between the metal and the
482
adsorbent occurs through nitrogen or sulfur atom. In
483
this condition causes the atoms nirogen start
484
deprotonated thus negatively charged, which will
485
result in the interaction of metal ions and adsorbent
486
stronger so that the amount of metal ions are
487
adsorbed more [13]. On the other hand, acidic (pH
488
1-5), the active sites of the adsorbent is nitrogen in
489
organic ligand in a state of partial protonated so
490
positively charged that causes repulsion between the
491
adsorbent surface with the metal ions thereby
492
reducing the metal ion adsorption capacity whereas
493
at alkaline pH conditions (8-14) the number of -OH
494
ions more than the protons (H+ ions) in solution
495
[13]. The number of -OH ions in solution in
496
reactions between Pb (positively charged) with -OH
497
ions are characterized by formation of deposits that
498
could potentially cover the surface and pores of the
499
cellulose-MBA-AA.
500 501
Adsorption isotherms
502
The type of adsorption isotherm can be used
503
to study the mechanism of adsorption. This study
504
used two types of isotherm models. the adsorption
505
isotherm and adsorption equilibrium can be shown
506
on the Pb ions in a solution by using adsorbents
507
(cellulose-MBA-AA)
508
Adsorption equilibrium on phase solid-
509
liquid are generally adopted two types of adsorption
510
isotherms are Frendlich and Langmuir.
511
Determination of equilibrium models depends on
512
the determinant coefficient (R2). From the
513
adsorption isotherm can be determined adsorption
514
mechanism that occurs between the adsorbate
515
molecules to the surface of the adsorbent. The
516
mechanism may occur Freundlich or Langmuir.In
517
determining the type of the isotherm is used
518
adsorbent copolymer cellulose-MBA-AA and at pH
519
7 with time of agitation for 60 minutes.
520
Copolymer’s adsorption isotherms of cellulose-
521
MBA-AA for Langmuir and Freundlich isotherm
522
shown in Fig. 9
523 524 525 526 527 528 529 530 531 532 533 534 535 536 537 538 539 540 541 542 543 544 545 546 547
Fig 9. (a) Langmuir isotherm and (b) Freundlich isotherms on 548
Cellulose-MBA-AA 549
550
Figure 9 shows that the Langmuir isotherm
551
types have a high linearity is 1, while the Freundlich
552
isotherm has linearity is 0.9. The linearity of the
553
results of the adsorption of Pb tends to be dominant
554
following the Langmuir isotherm. Langmuir
555
isotherm is a chemical adsorption occurs because
556
the chemical bond between the adsorbate with
557
adsorbent surface. Due to the chemical bonding that
558
occurs quite strong then when the adsorbent surface
559
is already covered adsorbate, adsorbate adsorbed
560
only on one layer, if exercised an increase in
561
temperature and concentration. Langmuir obtained
562
by assuming that the adsorption occurs in a
563
homogeneous surface of the adsorbent. The
564
weakness point of this reaction Langmuir isotherm
565
is the smaller regeneration of the adsorbent because
566
chemical bonding that occurs is so strong that the
567
metal ions that have been adsorbed by the adsorbent
568
is difficult to be released back, and other reagents
569
needed to remove it.
570 571 572
Surface Analysis cellulose-MBA-AA
573 574
Surface analysis before adsorbing Pb by SEM
575
Surface analysis with SEM was conducted
576
to determine the morphology of the adsorbent’s
577
surface of the pure cellulose and cellulose -MBA-
578
AA. Analysis is based on the adsorbent surface
579
characteristic X-rays generated from the transition
580
between the electrons of a particular energy levels
581
within an atom. Analysis of the surface of cellulose
582
and cellulose-MBA-AA using a scanning electron
583
microscope with a magnification of 4,000 times.
584
Before analyzed, pure cellulose and cellulose-MBA-
585
AA are coated by particles of platinum (Pt) to aid
586
the conductivity of the analyte. The comparison of
587
the results of the analysis of the surface of pure
588
cellulose and cellulose-MBA-AA shown in Fig. 10.
589
590
Fig. 10. SEM micrographs with 4000x magnification on the 591
adsorbent of (a) pure cellulose and (b) cellulose- 592
MBA-AA 593
594
Figure 10 shows that in pure cellulose still
595
looks fibers (fibrils) covered with particles of Pt
596
which are characteristic of pure cellulose while the
597
cellulose-MBA-AA has a porous and have a
598
compiler structure is different due to the occurrence
599
of MBA and AA [14].
600 601
Surface analysis after adsorbing Pb by EDAX
602
In this research, SEM is equipped with
603
EDAX (Energy Dispersive X-Ray Analysis) that
604
can be used to determine the elemental composition
605
of a sample. When a sample was photographed by
606
SEM and then forwarded to the EDAX. EDAX able
607
to determine each element in the sample. EDAX can
608
ensure that the copolymer can adsorb metal ions
609
adsorbed namely Pb with a concentration of 10 ppm
610
at pH=7 are shown in the following fig.11.
611 612 613 614 615
616 617
Fig.11. Spectrum of cellulose-MBA-AA in Adsorbing Pb 618
619
Figure 11 indicates that metal ions that
620
dominate on the cellulose-MBA-AA is Pb. This
621
indicates that there has been a Pb metal ion
622
adsorption by cellulose-AA-MBA with a
623
concentration shown in Table 2.
624 625 626
Table 2. Composition of cellulose-MBA-AA After Adsorbing 627
Pb 628
629
Unsur Wt (%)
Carbon 43.83
Oxygen` 52.40
Sodium 1.4
Magnesium 0.01
Silicon 0.01
Phosfor 0.3
Chlor 0.17
Zinc 0.5
Pb 1.24
Total 100
630 631
Table 2 shows that the Pb is adsorbed by
632
cellulose-MBA-AA amounted to 1.24% (Wt%)
633
indicating that there has been a process of
634
adsorption. However, some other metals such as Zn
635
0.5%, 1.4% sodium and magnesium 0.01% is
636
probably coming from the content of the straw
637
which they are contained (bonded) when pure
638
cellulose isolated.
639 640 641
CONCLUSION
642 643
It has been successfully synthesized the
644
cellulose by copolymerization using 40 kGy
645
irradiation dose in the present of MBA and AA. The
646
grafting degree is 353 %.
647
The application of the cellulose on Pb 2+ ion
648
adsorption indicated that the adsorption reached
649
99,8 % of 3 ppm Pb2+ at pH around 7.
650 651 652 653 654
655
ACKNOWLEDGMENT
656 657
The authors would like to thank to Mr.
658
Supandi From CIRA-BATAN for irradiating the
659
samples in this work.
660 661 662
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663 664 665
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