Professional Documents
Culture Documents
Bhasa Inggris Kimia
Bhasa Inggris Kimia
ABSTRACT
Total organic carbon content (Kot) is one important parameter for water quality criteria.
In this study the method of determination of Kot in the water, where organic substances in the
sample oxidized for Catalysis and carbon dioxide determined konduktometri oxidation results.
Oxidizing Unit used a glass column reactor inside the walls of TiO2 film coated and UV light
"black light" as the source of the photo. Performance test system developed shows that the range
of 10 to 100 ppm of TOC (total organic content) have good linearity and the results are not
significantly different compared with the TOC meter Kot commercial or similar but uses a
system of shaped photocatalyst suspension (ANATOC). By using a thin layer of catalyst that
mobilized the reactor problems can be avoided and the savings of the use of catalysts, because
they do not need to inject the suspension of catalyst each time such an analysis on the suspension
system.
1. INTRODUCTION
Kot is one important parameter as the criterion of water for different designation, such as
drinking water, water needs and / or industrial waste. Generally agreed that the value of Kot used
as general indicators of water contamination by volatile organic substances and nonvolatile1, 2.
In this context, it is necessary that the method is simple, fast and inexpensive way to determine
Kot in water at various designation (ranging from industrial wastewater with a high-Kot to the
ultra pure water with very low content of Kot) without losing sensitivitanya. In general, Kot
determination involves two main stages, ie the conversion of organic matter into CO 2 and H2O
and CO2 yielded quantitative determination. Conversion oganik substances into CO 2, and H2O
can be done in several ways, namely chemical oxidation, 3.4 therma combustion, l5, 6 pyrolysis,
7 fotodekomposisi, 8.9 and fotokatalik.10 Oxidation by chemical oxidation is limited to nonorganic substances volatile, thermal combustion requires great energy to achieve high
temperatures in the combustion chamber, the pyrolysis can only accommodate small sample size
and sensitivity is difficult to increase when dealing with samples with very low Kot,
photooxidation require high-energy UV light (UV-C) to obtain complete oxidation.
Photocatalytic oxidation mode chosen in this study has the advantage of being able to work at
room temperature, using a source of low-energy photons (UV-A). Energy photons with <410
nm is required to activate the TiO 2 catalyst to produce strong oxidizing species that will
memineralisasi organic substances produce CO2. The system was developed to handle samples
with small volume, and can accommodate both volatile compounds and non-volatile.
Carbon dioxide is produced, in general, can be measured by nondispersive infrared (NDIR)
absorption spectrometry, thermal conductivity 11.12, 13 or determined by titration volumetri14,
15 gravimetry, 16 and various methods of ion chromatography 0.17 to 22 after its CO 2 absorbed
into the acid or alkaline solution. NDIR, thermal conductivity, and ion chromatography analysis
tools require a fairly expensive. Titimetri and gravimetric can not provide adequate sensitivity
when dealing with samples were very low Kot. In this study the determination of the CO 2 is done
by konduktometri23 a simple and inexpensive yet sensitive enough, after the CO 2 was collected
directly into the mineral-free pure water.
2. Experiment
2.1. Immobilization of TiO2 thin film on the inner wall of the glass column.
Coating TiO2 by sol-gel method using 0.5 M precursor titanium (IV) bis acetyl
diisopropoksi asetonat (TAA, Aldrich) in ethanol and propanol ekivolum. Inner walls of the
column that has been cleaned with mineral acids, demineralized water and organic solvent and
then dried. Into a glass column (pyrex and / or quartz) which has net inserted precursor solution
and let stand a few moments. Precursor solution was then removed and the walls of the column is
dried gradually from room temperature up to 1200 C. Into the column and then added water and /
or pure oxygen while heated to a temperature reaches 400 o C and held until the black layer and /
or gray all turned white and transparent. Coating was repeated up to five times.
2.2. Characterization of TiO2 thin film on the inner walls of the column.
The presence of a thin film on the inner wall of the column was characterized using UVVis spectrometry (according gapnya energy), SEM-Scanning Electron Microscope-(profile / thin
film surface topography and thickness), and XRD-X-ray Difractometer (identity existence of
rutile crystal form and / or anatase). Examination of UV-Vis spectrum is done by cutting some of
the column and split it into two pieces, then place them on the street light in watertight
compartments and the use of comparison samples of air and / or columns that are not covered.
SEM examination performed with specimens that are similar to those used in the examination of
UV-Vis. While the examination conducted on the powder XRD exfoliated from the TiO2 film.
2.3. Performance testing reactor
2.3.1. Reactor configuration
Reactor configuration consists of two coils column inner wall of glass that is coated TiO2
connected in series. Each reactor coil wrapped around the black light and UV lamp each power 8
watts. Bersistem loop reactor using sirkulator periltastik pump and reservoir buffer capability as
a gas separator. Carbon dioxide is separated from the gas liquid separator dilairkan into the
reservoir also functions as a cell which is controlled by a digital conductivity conductometer.
2.3.2. Performance testing reactor
Before use dikonditioning reactor system with 20 ml of mineral water and run the system
until the signal konduktometri stable. Then injected into the reactor as much as 5 ml sample
solution containing certain Kot (for standard / calibration curve) and / or samples to be
determined KOTnya content. This study used two types of chemical compounds, namely glucose
and / or acid bensoat, as a reference / comparator Kot content with concentrations ranging from 0
to 60 ppm. Previously conducted preliminary experiments to determine the time required to
complete oxidized organic substances used in the concentration area.
solution indicates the amount of carbon dioxide gas is formed. Conductivity value will no longer
remain after the formation of carbon dioxide (all organic matter has been oxidized). The time
needed to complete oxidation depends on the amount of organic substances in the reactor, to
contain up to 60 ppm Kot it took less than 15 minutes (Figure 7). Test of linear relationship
between Kot with value (kf2 - ki2) is done by using the value of kf after konduktifitasnya
constant (> 15 minutes). It appears that in the concentration range between 5 to 60 ppm obtained
a fairly good degree of linear (Figure 8).
In this way some artificial samples containing the same concentration of organic substances
measured KOTnya value and results compared with measurement of the same sample but using
methods / instrumentation ANATOC (commercial instrument measuring the TOC or Kot-based
photocatalytic oxidation with TiO2 suspension and measurement konduktometri). The results
shown in Table 1 below:
Table 1. The measurement results of sample with Instrumentation developed and ANATOC
[record made Kot theoretical value is 17.001 ppm]
No. Sample results of measurement (ppm)
The proposed instrumentation ANATOC
1 17,979 17,370
2 17,023 15,030
3 16,550 15,328
4 16,550 15,228
average 17.026 15.989
Difference measurement range 0.673 1.083
From the table it can be seen that the results of measurements with the technique and
instrumentation that was developed has a smaller range of measurements and a smaller
difference to the theoretical value. A difference may indicate that the oxidation process in
measurement by oxidation ANATOC rudimentary guide operations over the given time line
procedure is very short. Although still to be done further tests regarding the working area of
concentration range (linearity), precision and accuracy, the influence of types of organic
substances and the sample matrix, but it can be said that in principle the proposed system has the
potential to be developed as TOC or Kot meter memenruhi simple criteria (injek sample and see
the results), without input inexpensive catalyst / chemicals each time analysis (Nearly
chemicalless) and therefore environmentally friendly.
4. Conclusion
From this research can be concluded that the glass column reactor with TiO2-coated
surface of the inner wall can function as an oxidising unit at Kot meter instrumentation. Kot
meter instrumentation developed, where the value of konduktan Kot derivatized carbon dioxide
reservoir cells results photocatalytic oxidation reactor perfect, able to provide adequate
measurement results as similar systems are already available commercially, but using the catalyst
suspension.
5. Acknowledgements
Osaka Gas Foundation International Cultural Exchange (OGFICE) of part suportnya in
the development of glass-walled reactor column in the active photocatalyst.
6. References
1. Miller, A.Z. J., Mantoura, R.F.S.; Preston, M.R. March Chem, 1993, 41, 215.
2. Benner, R., Hedges, J.I. March Chem. 1993, 41, 161.
3. Miller, AEJ, Mantoura, RFS; Suzuki, Y.; Preston MR Mar. Chem., 1993, 41, 223.
4. Van Hall, C.E.; Barth, D.; Stenger, V.A. Anal. Chem. 1995, 37, 769.
5. Montgomery, H.A.C.; Thom, N.S. Analyst 1962, 87, 689.
6. Sharp, J.H. Mar. Chem. 1973, 1, 211.
7. Test Methods for Total Organic Carbon in Water, American Society for Testing Materials,
Philadelphia, PA, 1985, ASTM D2579-85.
8. Edwards RT, McKelvie, ID; Ferret, PC, Hart, BT; Bapat, JB, Koshy, K. Anal. Chem. Acta
1992, 26, 287.
9. Van Steenderen, R.A.; Liu, J.S. Anal. Chem. 1981, 52, 2157.
10. Matthews W.R. in Photocatalytic Purification and Treatment ofv Water and Waste Water, ed.
Ollies DF, Elsevier Science Publishers BV, USA, 1993, p. 121-137.
11. Huber, S.A.; Frimmel, F.H. Anal. Chem. 1991, 63, 2122.
12. Van Hall, C.E.; Safranko, J., Stenger, V.A. Anal. Chem. 1963, 35, 315.
13. Kieselbach, R. Anal. Chem. 1954, 26, 1312.
14. Seligson, D., Seligson, H. Anal. Chem. 1951, 23, 315.
15. Maxon, W.D.; Johnson, M.J. Anal. Chem. 1955, 27, 1784.
16. Pickhardt, W.P.; Oember, A.N; Mitchell, J. Anal. Chem, 1955, 27, 1784.
17. Tanaka, K., Fritz, J.S. Anal. Chem. 1987, 59, 708.
18. Kreling, J.R.; DeZwaan, J. Anal. Chem. 1986, 58, 3028.
19. Okada, T.; Kuwamoto, T. Anal. Chem. 1985, 57, 829.
20. Brandt, G., Kettrup, A. Fresenius Z. Anal. Chem. 1985, 320, 485.
21. Cochrange, R.A.; Hillman, D.E. J. Chromatogr. 1982, 241, 392.
22. Fung, Y.S.; Wu, Z., Dao, K.L. Anal. Chem. 1996, 68, 2186.
23. ANATOC operational guide line for determination of the TOC base on photocatalytic
oxidation employing titanium dioxide suspension, Sydney, Australia, 1997.
Tools
The tools used consist of: steam distrilasi equipment, vacuum distillation equipment terfraksi,
penampak spot UV, GC-SM analysis equipment (Hewlett packard 5890 series II-MSD 5970
series) evaporators, vacuum liquid chromatography column and reflux equipment.
Preliminary Analysis
Preliminary analysis of patchouli oil includes physical properties and chemistry as
numbers ester, solubility in 90% ethanol, density, putaaran optics and refractive index, and initial
levels of patchouli alcohol in patchouli oil by using GC-BC. Purification oil with steam
distillation method 100 ml of patchouli oil incorporated into the distillation flask and add water
as much as 3500 mL. Then didistilsi steam for 13 hours to obtain distillate mixture of patchouli
oil and water. Patchouli oil is separated from the water and added to anhydrous Na2SO4 and
filtered. After the oil separately, and then testing the properties of chemical and physical-level
analysis of patchouli alcohol in patchouli oil after purification by using a GC-BC. Increased
levels of patchouli alcohol by the method distrilasi terfraksi at low Patchouli oil 50 mL (the
result of purification by steam distillation) is inserted into the vacuum distillation flask.
Furthermore terfraksi distilled patchouli oil at low pressure and separated into different fractions
based on differences in boiling point. Each distillate was analyzed by GC-BC so that the content
of patchouli alcohol can be known. Peni ngkatan patchouli alcohol content by extraction
5 g of patchouli oil (the result of vacuum distillation terfraksi) was dissolved in ether, then
extracted with 2 x 100 mL 1 M NaOH solution Then the resulting two-layer solution is not
intermingled organic layer and water layer. In the organic layer, was added anhydrous Na2SO4,
and filtered so that the resulting filtrate and sediment. Then the filtrate was concentrated,
weighed heavy residue and analyzed the components that are neutral with KG-BC. While in the
water layer, add concentrated HCl and diekstrksi by 2 x 100 mL ether. In the organic layer is
added anhydrous Na2SO4 and then filtered to produce filtrate and precipitate.
Increased levels of patchouli alcohol by vacuum liquid chromatography
40 g of silica gel GF 245 in a beaker glass, inserted into the vacuum column until the height
reached 5 cm. Then eluted with n-hexane until homogeneous. A total of 5 g of patchouli oil
prepared with 10 g of silica gel 60 g nach Stahl until dry. Then the sample is inserted into the
column and eluted with 150 mL n-hexane, collected into 3 fractions. Then eluted again with 150
mL of ether, 150 mL of chloroform, 150 mL of ethyl acetate and also collected into 3 fractions.
Selanjtunya each fraction checked by thin layer chromatography to determine the pattern of the
stain, with the eluent n-hexane: ethyl acetate: chloroform (80:15:5). Then analyzed by GC-BC so
patchouli alcohol content can be known.
Derivatisasi
patchouli
oil
by
way
of
methylation
0.1 g minyka patchouli (the vacuum liquid chromatography) is inserted into a saponification
flask. Then add 5 mL of ethanol and 1.5 mL of 0.25 m KOH solution alkoholis Enter a boiling
stone, then a 10-minute direfluks solution. After boiling, the upper fraction kondesor added 0.5
mL BF3 / methanol then direfluks again for 5 minutes, then cooled and inserted from the top
kondesor 5 mL n-hexane. Subsequently added 1 mL saturated NaCl. Then shaken until
equilibrium, n-hexane fraction was separated and analyzed to determine changes in organoleptic
odor of patchouli oil.
Figure 3. Chromatogram of essential oil after purification by steam destrilasi analyzed using GCBC.
Increased levels of patchouli alcohol by distillation metodde terfraksi on tekana renddah
In this terfraksi distrilasi process pressure was 75 mmHg and reached a maximum of 2 fraction
produced both of which were analyzed by GC-BC. The first fraction results distrilasi terfraksi
vacuum out as distillate at a temperature of 46-80 C and the second fraction out at a temperature
of 85-120 C. Detailed results can be seen in table 2.
Table 2. Results fractions of vacuum distrilasi terfraksi patchouli oil
Figure 4. Chromatogram of essential oil extracted with 1 M NaOH (acid fraction) were analyzed
by GC-BC
Results of analysis using GC-BC shows, these two fractions contain patchouliu alcohol,
as if no separation occurs. In the chromatogram fractions I, patchouli alcohol appears at tr 32.27
min with levels of 38.55%. In the chromatogram fraction II, patchouli alcohol appears at tr 32.63
min with levels of 49.9%. Separation of the less well is because the lack of pressure exerted on
the process of distillation. According to previous research, patchouli alcohol can be separated
from other compounds if the low pressure distillation terfraksi given pressure 3-2 mmHg.
Tugas individu
DISUSUN OLEH
RINA DWISMAR
60500109019
JURUSAN KIMIA
FAKULTAS SAINS DAN TEKNOLOGI
UNIVERSITAS ISLAM NEGERI ALAUDDIN
MAKASSAR
2010