Experimental Section
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Experimental Section
3.1
Equipment
Table 3-1: Applied equipment for measurements, including name of model and providing company
(Analytical) Method /
Model
Company
Electron Beam Modification
ELSA
Institut für Oberflächenmodifizierung
CNS Elemental Analysis
Vario IL
Elementaranalyse Systeme Hanau
Gas Chromatography
HP 6890 Series GC Systems
Hewlett Packard
ICP-OES
Optima 8000
Perkin Elmer
Light Source
Hg medium pressure lamp
Heraeus
Purpose
Maldi-MS
Daltonics
Bruker
N2-Sorption
Asap 2010
Micromeritics Instruments
LM10
NanoSight
Thermal Analysis
STA 409
Netzsch
TEM
Jem 2100
Jeol
TPR
Ami 100
Altamira Instruments
UV/Vis
Lambda 650 s
Perkin Elmer
XRD
XRD-7
Zeiss
Nanoparticle Tracking Analysis
K. Striegler, Modified Graphitic Carbon Nitrides for Photocatalytic Hydrogen Evolution from Water, BestMasters, DOI 10.1007/978-3-658-09740-0_3, © Springer Fachmedien Wiesbaden 2015
20
3.2
3 Experimental Section
Chemicals
Table 3-2: Overview of used chemicals, their formula, molecular weight and commercial producer
Compound
Formula
MW / g mol-1
Company
4,6-Diamino-2-mercaptopyrimidine
C4H6N4S
142.2
Sigma-Aldrich
C4H5N3OS
161.2
Sigma-Aldrich
4-Dimethylaminopyridine
C7H10N2
122.7
Fluka
Acetonitril (for HPLC)
C2H3N
041.1
VWR
Ammonia (25 %)
NH3
017.0
Merck
Barbituric acid
C4H4N2O3
128.1
Bernd Kraft
Cobalt (II) acetate tetrahydrate
Co(OAc)2 ·4H2O
249.1
Merck
Cobalt (II) chloride hexahydrate
CoCl2 ·6H2O
237.9
Merck
Cyanuric acid
C3H3N3O3
129.1
Sigma-Aldrich
C2H4N4
084.1
Sigma-Aldrich
879.9
Abcr
4-Amino-6-hydroxy-2mercaptopyrimidine
Dicyandiamide Erythrosine B
C20H6I4Na2O 5
Ethanol (absolute, 99.9 %)
C2H6O
046.1
VWR
Ethylacetate (99 %)
C4H8O2
088.1
Sigma-Aldrich
Ethylene glycol (99 %)
C2H6O2
062.1
Sigma-Aldrich
Hexane (chemically pure)
C6H14
086.2
Merck
Hexachloroplatinic acid hexahydrate
H2[PtCl6] ·6H2O
517.9
Private
Hydrochloric acid (37 %)
HCl
036.5
Merck
Melamine
C3H6N6
126.1
Alfa Aesar
Methanol (chemically pure)
CH4O
032.0
Merck
Nitric acid (65 %)
HNO3
063.0
Merck
N,N'-Diisopropylcarbodiimide
C7H14N2
126.2
Sigma-Aldrich
Polyvinylpyrrolidone
(C6H9NO)x
̴ 10 000
Sigma-Aldrich
Potassium chromate
KCr2O4
194.2
Sigma-Aldrich
Pyrrole
C4H5N
067.1
Sigma-Aldrich
Rhodium chloride trihydrate
RhCl3·3H2O
209.3
Sigma-Aldrich
Sodium chloride
NaCl
058.4
Merck
Triethanolamine
C6H15NO3
149.2
VWR
Trithiocyanuric acid
C3H3N3S3
177.3
Abcr
Thiobarbituric acid
C4H4N2O2S
144.2
Sigma Aldrich
3.3 Syntheses
3.3
21
Syntheses
3.3.1 Synthesis of g-C3N4 15 g of melamine were suspended in 75 ml water, the water was evaporated and the sample calcined for 4 h at 550 °C under nitrogen atmosphere. The heating rate was 2.3 °C min-1 and the sample was allowed to cool down to room temperature under nitrogen atmosphere in the oven. The obtained product was pestled and characterized. 3.3.2 Synthesis of Copolymerized g-C3N4 15 g melamine or dicyandiamide as precursor and a defined amount of comonomers
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