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1. DEVELOPMENT OF GRAPHENE/TiO2 PASTE ELECTRODE MODIFIED
IONOPHORE CALIX[6]ARENE (GPE/TiO2-CALIX[6]ARENE) FOR DETECTION
OF Pb2+ ION
CHEMISTRY DEPARTMENT
MATHEMATICS AND NATURAL SCIENCES FACULTY
HALU OLEO UNIVERSITY
KENDARI
2019
Presented by:
ALFINA AMELIA AMASI
F1C115021
Supervisor I
Dr. H. Nasriadi Dali, M.Si
Supervisor II
Prof. Dr. Maulidiyah, M.Si.
3. AAS ICP-MS
Some Factors : Availability of equipment,
detection limits, time required, selectivity
and provision of samples.
Voltammetry
Has high sensitivity.
Low detection limit.
Easy use.
Easy sample preparation.
Introduction
(Suliana and Prim, 2014)
5. PROBLEM
STATEMENTS
PURPOSE
BENEFITS
How are the effect of adding Calix[6]arena ionophore as
modifier to the performance GPE/TiO2 ?
How are the performance GPE/TiO2 modified
Calix[6]arene ionophore in determination Pb2+ ion?
To knowing the effect of adding Calix[6]arene ionophore
as modifier to the performance of GPE/TiO2.
To knowing the performance of GPE/TiO2 modified
Calix[6]arene ionophore to determination of Pb2+ ion.
To Provide knowledge about alternative modifier
materials to improve the performance of graphene paste
electrode (GPE).
Add new knowledge about the use of graphene and
compound of calix[6]arene in the research of field,
especially for the determination of Pb2+ ion.
9. RESULT AND
DISCUSSION
Characterizationby EDX Energy Level
C : 0,2 keV; 2,35 keV dan 2,49 keV
O : 0,5 keV
Ti : 0,5 keV; 4,5 keV dan 4,9 keV
No. Unsur % Massa
1. C 94.99
2. O 3.41
3. Ti 1.60
Jumlah 100,00
Table 3. Composition of GPE/TiO2-calix[6]arene material
GPE/TiO2-calix[6]arenematerial
18. RESULT AND
DISCUSSION
Real Sample Test
CyclicVoltamogramrealsampletesof Pb2+measurement
Sampel Nyata
Pb 2+ 1 ppm dalam sampel nyata
Arus(µA)
Potensial (V)
0 -
-
100 -
-
200 -
-
-100 -
-
-200 -
-
-0.5
-
0.5-
-
1
-
0-1
Sampel Ipa (μA) Epa(V)
Real Sample 22.1 0.01
Pb2+ 1,0 ppm in real
sample
53.0 0.04
y = i = 22.1
y = 18.111x + 78.402
x = -3108 ppm
19. CONCLUSION
The optimum modifier composition of electrode with Calix[6]arene ionofor composition
of 0.015 g is indicated by anodic peak current (Ipa) 226 μA and cathodic peak current
(Ipc) -207 μA. Other factors Which affects the pH of the solution and the scan time rate.
The optimum measurement condition of GPE / TiO2-Calix[6]arene in detecting Pb2+
ions is at pH 5 with scan speed of 0.8 V / s
The detection limit obtained from the measurement of GPE/TiO2-Calix[6]arene on Pb2+
ions is 0.04702 ppm and the repeatability of GPE/TiO2-Calix[6]arene performance is
indicated by the value of Horwitz Ratio (HorRat) of 0.98. The stability of the optimum
measurement of GPE/TiO2-Calix[6]arene in analyzing Pb2+ ion is 30 days and there is a
significant influence on Pb2+ ion analysis when added with a disturbing ion as
evidenced by the emergence of a anodic peak current in the addition of Cd2+ and Mn2+
ions. Pb2+ ion levels in real samples are -3.108 ppm
1
2
20. THANK YOU
ALFINA AMELIA AMASI
(F1C1 15 021)
Grateful to be a member of
“Titania Research Group”
Editor's Notes
Bismillah
Salam
Thank you for the opportunity who has given me to present my result of research and title….
By the first,
The field of industry is grawing so rapidly along with the development of the world technology. The rapid growth in the industrial sector, besides providing enormous benefits, can also creat new problems for people’s lives, especially the industrial waste that is produced.
Industrial waste contains various elements harmful to human life. One of them is heavy metals. Heavy metals such as poisoning and certain doses can cause death. One of the metals toxic is Pb
There are some method for analyze ion in the sample, for example method ….. But in ion analysis need consideraction as samo factors … so, is used the voltammetry method, because voltammetry method have many advantages like
Voltammetri is one of the electroanalysis methods. Voltametri method have three electrode….
The performance of the voltametry method is strongly effect by the working electrode material. One of the material use is .. Gpe consist of a mixture.. Other than that, GPE can modified by .. . Besides TiO2, GPE can be modified with kaliks[6]arene To improve electrode performance
Research such as, in 2014 by .. do research …
Will be research by title
As for the purpose of the study who will answer the problem statements is…
This slide is plane of
The purpose of XRD characterization is to find out whether the synthase TiO2 has been formed successfully. Based on the resulting diffractogram the highest intensity of 2 theta 25.20 with the value of the crystal field 101 which is a characteristic of anatase TiO2 in accordance with JCPDS data. This is also supported by research conducted by Thamapat et al., 2008 where the crystal field 101 has the highest intensity compared to other crystal fields. Based on the results of the characterization, it can be seen that anatase TiO2 has been successfully formed and can then be used as a modifier in graphene paste electrode.
Characterization using SEM was carried out to determine the surface morphology of graphene / TiO2 paste and calix[6]arene modified graphene paste electrode. Whereas, the calix modified carbon paste has a smooth and dense surface morphology and even distribution of the calix[6]arene on the surface of the graphene. Based on SEM analysis, it is known that the calix nanoparticles have coated the surface of graphene.
the composition of GPE / TiO2-calix [6] arene, there is an element C of 94.99%. The percentage of element C in the GPE / TiO2-Kaliks[6]arene increas because of the presence of element C on the calix [6] arena.
Based on the measurement results, it was shown that the GPE-TiO2-calix [6] arena voltammogram had a higher peak current compared to GPE / TiO2. the addition of a calyx[6]arene modifier causes a significantly increased surface area indicated by peaks on both the oxidation and reduction curves. The presence of calix is also able to provide a more active place on the surface of the graphene paste electrode. This is oxidation reduction reaction that occurs in solution k3 on voltammetric cells...
The mass variation test of the kaliks[6]arene modifier aims to determine the mass of the best kaliks[6]arene modifier, with variations in the calyx mass covering 0.005; 0.010; and 0.015 grams. The best modifier mass is at the modification mass of 0.015 grams which has anodic peak current higher than the other calyx masses, so that the modiffier mass of 0.015 grams is suitable to be used for subsequent measurements.
Testing the effect of supporting electrolyte pH on the performance of GPE/tio2-kalik[6]arene in Pb2+ ion test solution using citrate buffer with varitions in pH 3,4,5 and 6. The plot result showed that pH 5 produced the highest that the measurement of pb2+ in CV at optimum pH is pH 5
Scan rate testing is done with a variation of 0.02; 0.05; 0,1; and 0.2; V / s. The optimum scan rate is at a scan rate of 0.2 v / s which shows a higher peak current compared to other scan rates. Thus, a scan rate of 0.2 V / s is a scan rate that will be used in the next measurement process.
The area of linearity is a linear curve which shows that the current produced is directly proportional to the concentration of the analyte. Expressed well if the value of linear regression = 0.9 or close to 1. The concentration used is 0.1, 0.3, 0.5, 0.7 and 1 ppm. Based on the voltamogram obtained, the curve of the relationship between concentration and current value was made so that the linearity of the concentration was obtained. Based on the linearity curve obtained a detection limit of 0.04702 ppm.
The measurement repeatability test aims to see the stability of GPE / TiO2-Kaliks in detecting Pb2 + ions carried out in 21 measurements. Advantage is said to be good if the HorRat value is less than 2. The calculation results obtained by the value of HorRat is 0.98, then GPE / TiO2-Kaliks is stated stable in analyzing Pb2+ ions.
The age test of the electrode is a test conducted to determine the stability of the electrode for a long time which is still feasible to use to analyze Pb2 + ions. Measured for 30 days with a once daily measurement period.
Based on the measurement results, on the first day to day 4, the electrodes are still considered feasible because the peak currents produced are still relatively the same. Meanwhile, on day 5 to day 30, there was a significant decrease in flow.
The effect of the addition of other ions in the analysis of pb2 + ions aims to determine the selectivity of GPE / TiO2-calix. The interfering ion test is done by adding each Cd2 + and Mn2 + ion into the analyte.
Based on the measurement results, there is a significant influence on the analysis of PB2 + ions when added to the interference ions. This is evidenced by the emergence of anodic peak currents on testing pb2 + ions on the addition of Cd2 + and Mn2 + ions.
The real sample test aims to determine the ability of GPE / TiO2-calix in analyzing PB2 + in real samples. The real sample used is water in the fields. The measurement results can be seen that in the real sample there is a peak current which indicates the presence of pb2 + ions. Based on anodic data from the real sample, the concentration of pb2 + ions is obtained by entering the anodic value into the equation y = ax + b obtained from the linear curve. The calculation then obtained the concentration of pb2 + ions in a sample of -3.108 ppm
![DEVELOPMENT OF GRAPHENE/TiO2 PASTE ELECTRODE MODIFIED
IONOPHORE CALIX[6]ARENE (GPE/TiO2-CALIX[6]ARENE) FOR DETECTION
OF Pb2+ ION
CHEMISTRY DEPARTMENT
MATHEMATICS AND NATURAL SCIENCES FACULTY
HALU OLEO UNIVERSITY
KENDARI
2019
Presented by:
ALFINA AMELIA AMASI
F1C115021
Supervisor I
Dr. H. Nasriadi Dali, M.Si
Supervisor II
Prof. Dr. Maulidiyah, M.Si.](https://image.slidesharecdn.com/finabismillahuntukhasil-201203102922/85/Fina-bismillah-untuk-hasil-1-320.jpg)
