Document
I10IP018EN-B_ChemBet_Pulsar_Brochure-compressé
Contenu du document
Crystallite Size
Dispersion
Metal Area
Pulse Titration
TPR / TPO / TPD
ChemBET Pulsar -TPR/ TPD
ChemBET Pulsar
Automatic Chemisorption Analyzer
TPR/TPD
2
Instrument Features
The ChemBET Pulsar TPR/TPD represents the very best in catalyst characterization using
automated flow methods of analysis.
Fully automated analysis sequences are programmed using the TPRWin software.
Titrations for metal area and dispersion determination use an automatic loop injector
and automatic gas switching. Furnace temperature ramping provides for temperature
programmed methods and sample preparation, both including rapid furnace cooling
using forced air for higher throughput. The Pulsar uses a proven TCD detector both
oxidation AND ammonia resistant, with stable current control for baseline stability and
reproducible signals. Plumbed in stainless-steel for maximum chemical compatibility,
the Pulsar is ideal for use with a wide range of gases. High-temperature quartz sample
cells are standard, as is the in-cell thermocouple providing accurate sample temperature
measurements.
An optional quadrapole mass spectrometer is available allowing for species
c@7?erentiation during temperature programmed analyses.
Automation
Interchangeable Injection Loop
Calibration
Automatic Titration Valve
Bypass Valves Cell Sample
Temperature Monitoring
Vapor Trap
"%?BCold Trap@??P
1100 oC Furnace,
Software Controlled
Automatic Switching
between Multiple Gas
Inputs
Forced Air Cooling Valve Status Display
Display Cover
Rapid titration & extreme sensitivity.
TPA overlays for easy comparison.
ChemBET Pulsar
Automatic Chemisorption Analyzer
TPR/TPD
3
Specifications
Automatic Injection Loop
Automatic Gas Switching between 4 ports
Automatic Forced Air Cooling of Furnace Calibration Port
Quartz Glassware
Self-sealing Sample Cell Holders
Stainless-Steel Plumbing
V ariable Gas Flow Rate Control
Sample Cell Bypass
I n-Line Cold Trap with Bypass
Supplementary Outgas/
Preparation Station
M ass Spec Connection Port
High Temperature (350 oC) Heating Mantle
High Temperature (1100oC) Furnace
Cell Sample Thermocouple
Capability (Automatic)
Pulse Titration (metal area)
Temperature programmed Reduction (TPR)
Temperature programmed Desorption (TPD@??P
Temperature programmed Oxidation (TPO@??P
Temperature programmed Surface Reaction (TPSR)
Gas Compatibility:
Input Pressure (gauge): Gas Lines: Voltage:
Frequency: Power:
Mantle, Max Temp: Mantle Power:
Furnace, Max Temp: Furnace Power: H
2, O 2, CO, CO 2, N 2O, SO 2,
NH
3, N 2, Ar, Kr, He
70-140 kPa (10-20 psig)
5 x 1.5m 1/8” s.s. (supplied)
100 - 240 VAC
50/60 Hz
70 VA
350
oC
125 W
1100
oC
575 W
Software Control
Programming of the following actions
creates a customized multi-step
@5?u#macro`y? which automatically controls
the analysis:
Gas switching
Manifold purge
Start/stop signal acquisition
Temperature ramping (by rate)
Temperature ramping (by time)
Multiple heating/cooling profiles
Cooling fan on/off
Pulse injection
The following data are presented on
screen in real time and automatically
stored:
TCD signal
Sample temperature
Time
Utilities
1
2
1
2
Thermal Conductivity Detector:
TCD Filaments:
Furnace Cooling: Gas Input Ports:
Loop Volumes Supplied: Dual-Filament
Diffusion Type
Oxidation and Ammonia
Resistant
Forced air
(PC Controlled)
5
50, 100, 250 µL
(others available)
Hardware
Features
ChemBET Pulsar
Automatic Chemisorption Analyzer
TPR/TPD
4
Carbons, Fuel Cells, etc.
Industrial Catalysts(eg. Hydrocracking, Hydrodesulfurization,
Hydrodenitrogenation
and Fischer-Tropsch@??P
Supported Metals
"%?B Reforming, Partial
Oxidation, Hydrogenation,
Automotive Exhaust, etc.@??P
TPR: Temperature
Programmed Reduction
Many heterogeneous catalysts are used
as the zero-valence metal, but start life
as the oxide. An important factor in
catalyst design and use is the ease of
reduction of the metal oxide and TPR is
a direct measure of that. A reducing gas
mixture, say 2%-5% H
2 in N 2, flowing over
the oxide will cause reduction at some
point as the temperature is raised using
a linear heating ramp. The signal caused
by consumption of hydrogen represents
the rate of reaction and goes through
a maximum at a temperature that is
characteristic of both the oxide and the
heating rate.
Repeating the same analysis on a fresh
sample at a different heating rate is the
means by which activation energy for the
process can be evaluated. Low loadings
of metal oxides, especially surface oxides,
generate little water and a successful
analysis can be done without trapping it.
Larger amounts of moisture generated
by the reduction of bulk oxides can be
trapped prior to reaching the detector to
leave a clean signal based solely on the
change in hydrogen concentration.
TPO: Temperature
Programmed Oxidation
Carbons and carbides are amenable to
evaluation by careful oxidation while
being heated. A stream of diluted
oxygen (e.g. 2-10% O
2 in He) directed
over the sample during a linear heating
ramp generates a signal due to the loss
of O
2 from the gas stream. The products
of oxidation, CO and CO
2 , need not be
trapped. The specially chosen filaments
used in the Pulsar"tas TCD detector are
resistant to oxidation and operate
normally in the suggested gas mixtures.
Different forms of carbon such as
amorphous, nanotube, filament
and graphitic, oxidize at different
temperatures due to varying availability
of reactive carbon-carbon bonds. In
this way, fullerenes, soots, cokes on
catalysts, etc can be quickly characterized
and differentiated. Oxidation catalysts,
e.g. those incorporating chromium,
cobalt, copper and manganese, and
redox supports like ceria can also be
characterized by TPO.
TPD: Temperature
Programmed Desorption
Species previously adsorbed can be
desorbed into a stream of pure carrier
gas to generate a characteristic finger-
print. The most common application
is ammonia TPD, by which one can
evaluate relative acid site strength of,
for example, zeolites. Basic sites can
similarly be evaluated by TPD of carbon
dioxide.
Some materials may be characterized
by decomposition, or dissociation, of
the bulk solid, not merely by desorption
from the surface. Such examples
include carbonates resulting from CO
2
removal studies, hydrides used as
potential hydrogen storage materials,
etc.
Pulse Titration:
Quantitative Analysis
This technique is used to determine the
following data:
(i) strong chemisorption uptake,
(ii) active metal area, (iii) metal
dispersion, (iv) average nanocluster
(crystallite) size.
After suitable in-situ preparation,
which may be combined with TPR/TPO,
the sample is automatically titrated
with small, known volumes (pulses)
of reactive gas. The detector senses
the excess gas which does not react
with the sample. The total volume of
gas which does react with the sample is
automatically determined by simple back
calculation using TPRWin software.
B.E.T. Surface Area:
Physisorption
The Pulsar can determine total (B.E.T.)
surface area with remarkable sensitivity.
By flowing various mixtures of nitrogen
and helium over the sample cooled
with liquid nitrogen, the surface area
can be determined from 0.1 square
meters upwards. Using mixtures
of krypton and helium the limit of
detection is extended down to 0.01
square meters. A single point B.E.T.
result can be obtained in under ten
minutes. TPRWin software records the
signals automatically, computes the
B.E.T. @5?u#C`y? constant, y-intercept, slope
and correlation coefficient of the least-
squares best-fit.
Measurement Capabilities &
Applications
Zeolites
(eg. FCC, Isomerization)
Corporate Headquarters-USA
Quantachrome Instruments
a brand of Anton-Paar
1900 Corporate Drive
Boynton Beach, FL 33426
© 2019 Quantachrome Corporation I10IP018EN-B Trademarks and registered trade mark are the
property of their respective owners.Serving Porous
Materials and Powder
Characterization Needs
Since 1968
ChemBET Pulsar
Automatic Chemisorption Analyzer
TPR/TPD
Entreprise(s) concernée(s) :
Produit(s) concerné(s) :
Date d'upload du document :
mardi 12 janvier 2021