Andi M Ichzan

Supervised by
Dr. Ivandini Tribidasari A
Dr. Jarnuzi Gunlazuardi
 Unpredictable weather
Increasing of Osean
surface
Demage of pole
ecosystem
EPA, 2014
 Researcher Electrode Product
Hori et al. 1985 Cadmium, Indium, Tin, Formic acid
and Lead
Kaceco et al, 1998 Silver and Gold CO
Kaneco et al, 2002 Copper, (lithium as Methane
electrolytes)
Le at al, 2011 Copper Methanol
Nakata et al, 2013 Boron Doped Diamond Formaldehyde

Larger yield of product

Wide potential window
High electrochemical stability
High faradic efficiency
 Panglipur, 2016 BDD modified by Acetic acid
copper (23,20%)

Is there any corelation using BDD with electrocatalytic

composite
And the product which consist of two carbon atoms???
Electrocataytic effect same as Copper
Tae et al, 2015 using Ir as composite on Cobalt
electrode coused increasing of efficiency of water
oxidation
Xiao et al 2015 using Ir as composite on Gold
electrode coused widen working area in detection
of mercury
Lack of information about Ir characteristic as
reduction electrode
 Caracterized by CV using
BDD
KNO3 0,1 M and Ir 0,3 mM

BDD Deposit solution (Ir 0,5 mM +

KNO3 0,1 M 1:1) heated 80oC
than cooled

Chronoamperometric
Caracterized by FE-
1,2 V, 10 Min
SEM, XPS, CV
 The Optimum bubbling time
of CO2

Cathode section
bubbling with N2 for 1
hour

Working electrode = BDD, Applying Cyclic

Counter Electrode = Pt Foil voltmetric at potensial
Reference Electrode = 0,5V (-2,0V)
Ag/AgCl

Applying Cyclic Bubling with CO2 at 30, 60,

voltmetric at 90 and 120 minutes
potensial 0,5V (-2,0V) variation time
 Reduction potensial of CO2

Cathode section
bubbling with N2 for 1
hour

Working electrode = BDD, Applying Cyclic

voltmetric at potensial
Ir, & Ir-BDD
0,5V (-2,0V)
Counter Electrode = Pt Foil
Reference Electrode =
Ag/AgCl Bubling with CO2 at
bubling optimum time (60
minutes)
Applying Cyclic
voltmetric at potensial
0,5V (-2,0V)
 Elektroreduction of CO2

Cathode section
bubbling with N2 for 1
hour

Working electrode = BDD, Applying Cyclic

Ir, & Ir-BDD voltmetric at potensial
Counter Electrode = Pt Foil 0,5V (-2,0V)
Reference Electrode =
Ag/AgCl
Bubling with CO2 at
bubling optimum time (60
Applying Cyclic minutes)
UPLC voltmetric at potensial
0,5V (-2,0V) for 1, 2, 3
4, 5, 6, 12, and 24 hours
 A. BDD and BDD-IROx characteriation
BDD Unmodified
Cyclic voltametric characterization

Figure 1.Voltamogram of BDD using KNO3 as the electrolyte on potensial

range -1,0V to 1,5V
 BDD Unmodified
Cyclic voltametric characterization

a b

Figure 2. (a) repeating cyclic (10 Cyclic) voltammetry on Ir 0.3 mM in 0.1

M KNO3 (1: 1). (b) variation of scan rate on Ir 0.3 mM in 0.1 M KNO3 (1: 1).
BDD Modified by Ir
FE- SEM
2500 X Magnification

A B

Figure 3 Characterization of BDD by FESEM

XPS Characterization

25000 C (1s)
BDD
20000
BDD + IrOx

15000
Intensity

O (1s)
10000

5000

IrO2
0

0 200 400 600 800 1000 1200

BE(eV)

Figure 4. XPS characterization of BDD deposited by Iridium

SEM-XPS

Sampel %C %O %Ir %Cl

Name
BDD-Ir 89,31 7,86 2,35 0,47
 Cyclic voltametric Characterization

Figure 5. Voltamogram of BDD and BDD Deposited by Iridium In

KNO3 0,1M
B. Optimum Bubbling time of CO2

60 minutes at -1,54V

Figure 6. voltamogram of variation bubbling time of CO2

 C. Reduction potential of CO2

BDD = -1,54V
BDD + IrOx = -1,40V

Figure 7. Voltamogram of BDD and BDD+ irOx on CO2 reduction

D. Characterization of electroreduction product
1. Formaldehyde
3 mL DNPH + Wait for 2
40oC, hours on the UPLC
1 mL Sampel/ 10 min
Standar dark place

Blank

2,4-Dinitrofenilhidrain

Figure 8. UPLC Cromatogram of formaldehyde blank

 Exces of DNPH
DNPH

2,4-dinitrophenylHidrazone

2,4-dinitrophenylHidrazone
 Calibration Curve HCOH
70

60

50

40

Area
30

y = 10,5467x + 13,8820
20
R = 0,9970
Conc 10
Area
(mg/L)
0
0 1 2 3 4 5 6
0 15,0007
Conc (mg/L)
1 23,5753
2 33,7132
3 45,61371
4 57,49177
5 66,09756
2. Acid Content (Formic and acetic acid)

Acetic acid; 3,8 min

Formic acid; 2,7 min

Conc (mg/L) Area Calibration Curve CH3COOH
0 0,0000 25.0000

Conc (mg/L)
20.0000
10 5,4860
15.0000
20 8,3078 10.0000 y = 0.4229x + 0.3869
5.0000 R = 0.9957
30 13,2551
0.0000
40 17,0118 0 10 20 30 40 50 60
50 21,7003 Area
Calibration Curve HCOOH
Conc (mg/L) Area 40

30
Conc (mg/L)

0 0
20
20 11,2281
10 y = 0.6689x - 0.9709
30 18,14465 R = 0.9941
0
40 26,37733 0 10 20 30 40 50 60
-10
Area
50 33,04739
Preliminary analysis

Acid content BDD Formaldehyde BDD

HCOH
No acid content

Acid content BDD +IrOx Formaldehyde BDD +IrOx

CH3COOH HCOH
Concentration HCOH as the product of
electroreduction of BDD as the Working electrode
area of area of average average
electroreduction area of
sampel + standard area of Conc (mg/L) conc %RPD
time (Hours) sampel (A-B)
standard (A) (B) sampel (mg/L)
65,2596 46,1920 19,0676 0,4917
1 19,1552 0,5000
65,4348 46,1920 19,2428 0,5083 -0,91
64,7980 46,1920 18,6060 0,4479
2 18,5910 0,4465
64,7681 46,1920 18,5761 0,4451 0,16
65,2327 46,1920 19,0407 0,4891
3 19,2535 0,5093
65,6582 46,1920 19,4662 0,5295 -2,21
66,0788 46,1920 19,8868 0,5694
4 19,4725 0,5301
65,2501 46,1920 19,0581 0,4908 4,26
65,1312 46,1920 18,9392 0,4795
5 19,1280 0,4974
65,5087 46,1920 19,3167 0,5153 -1,97
66,2752 46,1920 20,0832 0,5880
6 20,3365 0,6120
66,7817 46,1920 20,5897 0,6360 -2,49
65,9635 46,1920 19,7715 0,5584
12 19,9645 0,5767
66,3495 46,1920 20,1575 0,5950 -1,93
68,2610 46,1920 22,0690 0,7763
24 21,8627 0,7567
67,8483 46,1920 21,6563 0,7371 1,89
Concentration HCOH as the product of electroreduction
of BDD +IrOx as the Working electrode
area of average average
electroreduction area of sampel area of
standard area of Conc (mg/L) conc %RPD
time (Hours) + standard (A) sampel (A-B)
(B) sampel (mg/L)
62,8502 46,1920 16,6582 0,2632
1 16,38495 0,2373
62,3037 46,1920 16,1117 0,2114 3,34
61,1066 46,1920 14,9146 0,0979
2 15,10455 0,1159
61,4865 46,1920 15,2945 0,1339 -2,52
60,246 46,1920 14,054 0,0163
3 14,71155 0,0787
61,5611 46,1920 15,3691 0,1410 -8,94
62,5045 46,1920 16,3125 0,2305
4 16,5449 0,2525
62,9693 46,1920 16,7773 0,2745 -2,81
66,9283 46,1920 20,7363 0,6499
5 20,7001 0,6465
66,8559 46,1920 20,6639 0,6430 0,35
69,6325 46,1920 23,4405 0,9063
6 23,484 0,9104
69,7195 46,1920 23,5275 0,9146 -0,37
69,9723 46,1920 23,7803 0,9385
12 23,78703 0,9392
69,98576 46,1920 23,79376 0,9398 -0,06
73,5561 46,1920 27,3641 1,2783
24 27,39875 1,2816
73,6254 46,1920 27,4334 1,2849 -0,25
 HCOH Concentration as the Electroreduction Product
1.4000

1.2000
Concentration (mg/L)

1.0000

0.8000

BDD
0.6000
BDD + IrOx
0.4000

0.2000

0.0000
1 2 3 4 5 6 12 24
Time of Electroreduction (Hours)
Concentration HC3COOH as the product of electroreduction of
BDD +IrOx as the Working electrode
area of average average
electroreduction time area of area of
sampel + area of Conc (mg/L) conc %RPD
(Hours) standard (B) sampel (A-B)
standard (A) sampel (mg/L)
19,8841 9,1629 10,7212 24,4909
1 10,7315 24,5155
19,9048 9,1629 10,7419 24,5400 -0,19
20,4452 9,1629 11,2823 25,8207
2 11,2810 25,8175
20,4426 9,1629 11,2797 25,8144 0,02
25,6390 9,1629 16,4761 38,1282
3 16,4908 38,1631
25,6685 9,1629 16,5056 38,1981 -0,18
24,9998 9,1629 15,8369 36,6134
4 15,8409 36,6231
25,0079 9,1629 15,8450 36,6327 -0,05
23,1936 9,1629 14,0307 32,3335
5 14,0159 32,2984
23,1640 9,1629 14,0011 32,2632 0,21
25,4128 9,1629 16,2499 37,5922
6 16,1495 37,3543
25,2120 9,1629 16,0491 37,1163 1,24
21,2422 9,1629 12,0793 27,7093
12 12,0895 27,7335
21,2626 9,1629 12,0997 27,7576 -0,17
18,8226 9,1629 9,6597 21,9755
24 9,6400 21,9289
18,7832 9,1629 9,6203 21,8823 0,41
 Concentration of CH3COOH as the electroreduction Product
45.0000

40.0000

35.0000

30.0000
Conc (mg/L)

25.0000

20.0000

15.0000

10.0000

5.0000

0.0000
1 2 3 4 5 6 12 24
time of electroreduction (Hours)
Boron doped diamond modified by Iridium
proved as the great working electrode to
produce acetic acid on CO2
electroreduction where the faradaic
efficiency obtained at 85,93% and
become the major product while
formaldehyde obtained as the minor
product with 1,66% faradaic efficiency
 Characteriation BDD-Ir using raman
Spectroscopy
Concentration of dissolved CO2 on NaCl
(aq) as the medium of eletroreduction
The characterization of electroreduction
Product using Iridium it self as the WE