www.reecotech.com.vn
H THNG THIT B NGHIN CU XC
TC: CATLAB PCS / MS
H Ni, 04/2014
Trnh by: Trn Minh Hi
www.reecotech.com.vn 2
1. THNG TIN S LC V CNG TY REECO
2. H THNG THIT B CATLAB PCS / MS
3. MT S THIT B NGHIN CU VT LIU HP
PH, XC TC KHC
NI DUNG
Thng tin chung www.reecotech.com.vn 3
Website
Tm kin trn Google
Lnh vc kinh doanh v Phng chm hot ng www.reecotech.com.vn 4
KIN THC KINH NGHIM
NI THT PTN NI THT PTN
D N CHUYN GIAO KH&CN D N CHUYN GIAO KH&CN
THIT B KHOA HC K THUT THIT B KHOA HC K THUT
L i din c quyn, phn phi thit b v h thng KHKT cho cc hng ch to hng
u th gii.
Cc thit b v h thng KHKT c xut x t US, EURO, Israel hoc Nht Bn.
i ng cn b, nhn vin c trnh i hc v trn i hc c o to c bn v
chuyn su, vi s h tr o to t cc
hng sn xut.
To dng mi lin kt hiu qu gia cc nh khoa hc, chuyn gia ci tin, sng to vi
cng ng doanh nghip SX KD.
Sn phm v cc lnh vc KHKT lin quan www.reecotech.com.vn 5
THIT B KHOA HC K THUT THIT B KHOA HC K THUT
Specializing in
Pressure Swing Adsorption Studies
Humidity Generators Gas
Separation Processes
WORLD LEADING
SORPTION
INSTRUMENTS
>1,400,000 instruments installed
around the world!
Thermo
imaging
instruments
for clinical
applications.
KHCH HNG TIU BIU KHCH HNG TIU BIU
1. Trung tm Nghin cu Vt liu Cu trc Nano v Phn t, TP. HCM
2. Trng H Khoa hc T nhin TP. HCM
3. Trng H Cn Th
4. Vin Ti nguyn v Mi trng, TP. HCM
5. Vin Hi dng hc, Nha Trang Khnh Ha
6. Trung tm Quan trc Ti Nguyn v Mi trng tnh k Nng
7. Cng ty Qun l Khai thc Dch v Thy li TP. HCM
8. Trung tm Mi trng v Nng lng TP. HCM
9. Trung tm Quan trc mi trng, Tng cc Mi trng
10. Bnh vin Nguyn Tri Phng
Sn phm v cc lnh vc KHKT lin quan www.reecotech.com.vn 6
An Integrated Microreactor Mass Spectrometer for
Reaction Testing, TPD/R/O and Pulse Chemisorption
Hiden CATLAB SYSTEM Hiden CATLAB SYSTEM
CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 7
CATLAB Schematic
CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 8
Module 1:
- Interchangeable catalyst cartridge
system.
- In-Bed thermocouple.
- Sample mass: typically 25 - 250mg,
2.0g (opt)
- P: ambient
- T: ambient to 1000C, accuracy: +/- 1C
- Ramp rate: 1 to 20C/min
- MFC: 4 streams 3-100ml/min, 8 streams (opt)
- Air thermostat and trace heating to minimise
condensation of liquid feeds / products
Module 2: Hiden QGA Mass Spectrometer
- Multiple Gas and Vapour Analysis : 200
amu mass range, 300 or 510 amu (opt).
- High Sensitivity: detection to 100 ppb.
- < 300 ms response time to changes in gas
concentrations.
- Fast data acquisition: up to 500
measurements per second.
- Low dead volume, heated inlet for fast
response to vapours.
- Soft ionization (APSI-MS soft ionisation mode) for reduced spectral
fragmentation and simplified data interpretation.
- Operate as stand-alone components, could be interfaced with existing lab
equipment such as TGAs (TG-MS) or Gas Chromatographs.
CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 9
The HAL
201 RC type:
gold plated
ion source &
UHV
CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 1
0
FLOW CONTROL
MODULE
Standard CATLAB Layout
CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 11
CATLAB Control Software
Control of Mass Spectrometer, Temperature and Gas Flows in one
software package
Hardware Control Parameters
Control and calibration of
MFCs for different gases Mass Spectrometer Control Furnace Control
CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 12
CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 13
- Stage 1: Configure the temperature profile of the experiment - set
ramp rate, set point and dwell time for each stage
Experimental Setup
Stage 2: Configure gas flows/Pulses for each stage of the experiment
- MFC Assistant to help calculate percentage composition of each
component in gas mixture for the selected flow CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 14
Experimental Setup (cont)
CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 15
MFC Gas Mix Library Editor Gas Mix Calculator
Gas Mixing Control
Experimental Setup (cont)
CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 16
Stage 3: Add measurement stages. Stages are triggered by time or temperature
depending where on the temperature profile the start/stop is placed. Different
MS analysis types can be configured for each stage of the experiment.
Experimental Setup (cont)
CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 17
MID Scan setup for known species. Automatic overlap removal.
Includes library of most common gases. Ion source control for each
species preferential ionisation of some overlapping gases.
Mass Spectrometer Control
CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 18
- Multiple Bar scans can be configured in 3 subscan sections for
optimised sampling of unknowns.
- Ion source control for each subscan
Mass Spectrometer Control
Data plotted with x-axis as time or temperature
MS Data Display
TPR Data
TPR Data
CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 19
3D Bar Graph mode for easy identification of bar mode trends
MS Data Display (cont)
CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 20
Data Analysis
CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 21
- 3D Bar, 2D Bar and MID modes all available in data analysis mode.
- Multiple export/print options.
- Export selectable masses or whole scan to NIST database for identification of
unknowns.
- 2D Bar and MID view linked to enable viewing of Bar scan at any point in the
MID trace and vice versa.
- Peak fitting analysis routines
- Integrated area
- Baseline subtraction
Data Analysis (cont)
CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 22
Pulse Chemisorption
Injection of single gases or multiple reactants
CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 23
Pulse Chemisorption Quantification
Uptake measurements; Dispersion calculation; Metal surface
area; Pulse Adsorption Isotherm
CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 24
Video clip v h thng CATLAB
CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 25
Selected CATLAB Users
Johnson Matthey
Texas A&M University
Hong Kong University
Cambridge University
Bayreuth University
Research complex at Harwell
Sao Paolo University
Bulgarian Academy of Sciences
Universit catholique de Louvain
Kunming University
ETH Zurich
PDVSA (Petroleum of Venezuela)
CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 26
Selected Academic References
Electronic and Geometric Structure of Ce3+ Forming Under Reducing Conditions in Shaped Ceria Nanoparticles Promoted by Platinum . J. Phys. Chem. C, 2014, 118 (4), pp 19741982. O. V. Safonova, A.
Guda, C. Paun, N. Smolentsev, P. M. Abdala, G. Smolentsev, M. Nachtegaal, J. Szlachetko, M. A. Soldatov, A.
V. Soldatov, and J. A. van Bokhoven
The effect of coke deposition on the activity and selectivity of HZSM-5 zeolite during ethylbenzene alkylation reaction in the presence of ethanol. Catal. Sci. Technol., 2014, 4, 1017-1027. Sulaiman S.
Khattaf, C. DAgostino, Muhammad Naseem Akhtar, Nabil Othman Al-Yassir, Nicholas Tan and Lynn F.
Gladden.
Reaction Kinetics of C3H6 Oxidation for Various Reaction Pathways Over Diesel Oxidation Catalysts . Topics in Catalysis, December 2013, Volume 56, Issue 18-20, pp 1916-1921. Harry Oh, Izabela S. Pieta,
Jinyong Luo, William S. Epling
An investigation of the role of surface nitrate species in the oxidation of propene on a Pt-based diesel oxidation catalyst.. Catal. Sci. Technol., 2013, 3, 2349-2356 Sarayute Chansai, Robbie Burch, Christopher
Hardacre, Harry Oh, and William S. Epling.
Molybdenum oxide on Fe2O3 core-shell catalysts; probing the nature of the structural motifs responsible for methanol oxidation catalysts .ACS Catal., 2014, 4 (1), pp 243250, Catherine Brookes , Peter P Wells ,
Giannantonio Cibin , Nikolaos Dimitratos , Wilm Jones , David J Morgan , and Michael Bowker.
Chiral Co(II) metal-organic framework in the heterogeneous catalytic oxidation of alkenes under aerobic and anaerobic conditions. ACS Catal., 2014, 4, pp 10321039 Giulia Tuci, Giuliano Giambastiani, Stephanie
Kwon, Peter Curran Stair, Randall Q. Snurr and Andrea Rossin
CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 27
1. Nghin cu bn ca cc h xc tc Pd/ gi mang -Al2O3 trong qu trnh t chy
xc tc metan c s hin din ca kh gy c SO2
The durability of alumina supported Pd catalysts for the combustion of methane in the
presence of SO2
2. Lin h gia cu trc v tnh nng ca cc xc tc nn tng Cu cu trc xp trong kh
chn lc NOx t kh thi ca cc ng c diesel
Structure-performance relationships of Cu based porous catalysts for selective catalytic
reduction (SCR) of NOx gases from diesel exhausts.
3. nh hng ca tc gia nhit trong kh graphite oxide nhit thp n xp ca
sn phm
The effect of heating rate on porosity production during the low temperature reduction of
graphite oxide.
4. Sng lc xc tc cho vic gim loi H2S ca dng biogas cp liu cho pin nhin liu
mui carbonate nng chy
Screening of catalysts for H2S abatement from biogas to feed molten carbonate fuel cells.
5. Nghin cu c tnh xc tc bng phng php nhit lng hp ph
Calorimetric Adsorption for Catalyst Characterisation
Customer Research Stories
ISSUE : 1120/07
CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 28
1120/01 1120/06 1120/03
Summary
Integrated microreactor and mass spectrometer
Both microreactor and mass spectrometer manufactured by Hiden
Single integrated software package to control MS and microreactor
Ideal for catalyst characterisation and reaction testing
Designed for optimum mass spectrometer performance
CATLAB System for Catalysis Studies & Thermal Analysis www.reecotech.com.vn 29
1/ Thit b kho st Phn tch & Tinh sch kh ca hng L&C, USA
H thng tch hp 03 cng ngh: Hp ph p sut chuyn i (PSA), Hp ph chn khng chuyn i (VSA), v Hp ph nhit chuyn i (TSA).
PSA-300LC
(2cc VMu 20cc)
nh gi kh nng
phn tch, tinh sch
kh ca cc loi vt
liu mi .
PSA-1000
(150cc VMu 3500cc)
Thch hp cho cc d n
R&D, thit lp pilot tinh
sch kh hoc trin khai
sn xut loi vt liu cho
mc ch ny. Thit b kho st Phn tch & Tinh sch kh www.reecotech.com.vn 30
Cc lnh vc s dng TB kho st Phn tch & Tinh sch kh
1.1/ Bt gi v c lp kh CO2
CO2 thot ra c coi l nguyn nhn
ch yu gy bin i kh hu, lm cho
tri t nng ln, m v nguy c th Vit
Nam l mt trong 5 nc hng chu nng
nht. GS.TSKH. H S Thong, PetroTimes.
CO2 thot ra c coi l nguyn nhn
ch yu gy bin i kh hu, lm cho
tri t nng ln, m v nguy c th Vit
Nam l mt trong 5 nc hng chu nng
nht. GS.TSKH. H S Thong, PetroTimes.
Thit b kho st Phn tch & Tinh sch kh www.reecotech.com.vn 31
1.2/ Phn tch cc hydrocarbon nh, k c tinh sch kh TN, biogas,
1.3/ Phn tch khng kh
Nitrogen Generator Portable Oxygen
Concentrator
Thit b kho st Phn tch & Tinh sch kh www.reecotech.com.vn 32
ng dng nghin cu:
- Phn tch, lu gi CO2
bng vt liu MOFs;
- Loi b kh c VOC trong
kh thi, nitrosamines trong
khi thuc l,;
- Tinh sch kh thin nhin,
biogas.
KHCH
HNG
TIU
BIU:
Integrated
software
HR/Vapor Generator
PSA/VSA/TSA System
MS
Thit b kho st Phn tch & Tinh sch kh www.reecotech.com.vn 33
0.00E+00
5.00E-10
1.00E-09
1.50E-09
2.00E-09
2.50E-09
0 500 1000 1500 2000 2500 3000
Ion
Cu
rre
nt,
A
Time, Sec
MS
MS:16 MS:18 MS:44
PSA Data
Thit b kho st Phn tch & Tinh sch kh www.reecotech.com.vn 34
SpaciMS for determination of intra catalyst reactor chemistry www.reecotech.com.vn 35
2. HIDEN SPACI- MS
SPACI-MS (Spatially Resolved Capillary Inlet MS): probing inside of a
monolith, aims at revealing what is happening inside the blackbox.
Measurements:
- Pinpoint and measure diverse pollutants
inside narrow channels of catalyst
monoliths
- Determine transient species distribution in
reactors
- Minimal disruption of reactor flow and
catalyst chemistry
- For sampling from confined space
reactors
- Channelised automotive engine catalysts
- Catalysed Fuel Reformers
- Proton Exchange Membranes
- Fuel Cell Flow Channels
- Exhaust Gas Recirculation (EGR) in
internal combustion engines
Up to 16 capillary sampling probes and
thermocouples
SpaciMS for determination of intra catalyst reactor chemistry www.reecotech.com.vn 36
3. Gas sorption & vapor sorption analysis instruments
WORLD LEADING SORPTION
INSTRUMENTS
The IMI Series offers a multifunctional platform for the
study of physisorption, chemisorption and gas absorption
by materials, from entry level manometric analyzers to
advanced multistream dynamic flow systems.
The IGA Series: The unique IGA method exploits the
relaxation of the sample after pressure or temperature
change to simultaneously determine kinetic parameters
and equilibrium uptake.
The IGAsorp is a fully automated bench top gravimetric
analysis system designed to quickly and accurately
measure the magnitude and kinetics of moisture
sorption by materials.
The XEMIS is a high accuracy sorption microbalance
for precision weighing in extreme environments.
Available as a standalone microbalance or as part of a
fully integrated sorption analyzer, the XEMIS provides
remarkable flexibility, as well as outstanding weighing
stability and accuracy.
Product Applications
Gas sorption analysis
Isotherm determination
Kinetic analysis
Thermodynamic studies
Hydrogen storage
Methane storage
Carbon dioxide sequestration
Gas separation and purification
Supercritical gas adsorption
Shale gas and coal bed methane
Gas solubility in ionic liquids
Chemisorption studies
Chemical reaction studies
Porous coordination frameworks
Activated carbon, carbon molecular sieves and templated carbons
Zeolites and zeotypes
Porous polymers
Gas sorption & vapor sorption analysis instruments www.reecotech.com.vn 37
Thng tin lin h:
ThS. Trn Minh Hi
Cng ty TNHH Khoa hc v K thut REECO
/c: 46/41/37 ng Vn Chui, P. 4, Q. 3, TP. H Ch Minh
T: 0903166704 Email: [email protected]
Website: www.reecotech.com.vn
Thng tin lin h:
ThS. Trn Minh Hi
Cng ty TNHH Khoa hc v K thut REECO
/c: 46/41/37 ng Vn Chui, P. 4, Q. 3, TP. H Ch Minh
T: 0903166704 Email: [email protected]
Website: www.reecotech.com.vn
Cm n Qu v lng nghe!
H thng L vi phn ng kt ni vi My khi ph - Nghin cu xc
nh chc nng, c tnh ca Xc tc d th.
Module 1: L vi phn ng, kim sot
cht ch thng s dng v nhit ;
Module 2: My khi ph t cc.
- H thng cartridge thay mu kho st.
- u d nhit ti v tr mu trong cell o.
- Khi lng mu: 25 - 250mg, 2.0g (opt)
- p sut: p sut mi trng xung quanh
- Nhit : mi trng 1000C, 1C
- Tc gia nhit: t 1 n 20C/pht
- MFC: 4 dng 3-100ml/pht, 8 dng (opt)
Module 1: L VI PHN NG
Sn phm v cc lnh vc KHKT lin quan www.reecotech.com.vn 39
- Phn tch lin tc , nhiu thnh phn kh v
hi cng lc vi gii o: 0 200 amu, n
300 hoc 510 amu (opt).
- nhy cao: 100 ppb.
- Thi gian cho p ng < 300 ms i vi s
thay i nng kh.
- Ly s liu cc nhanh: 500 php o/giy.
- Tch hp chc nng phn tch CO khi c hin din ca N2 v CO2.
- S dng k thut ion ha mm gip gim phn mnh ph v n gin ha s liu.
- Dead-volume rt thp, u thu mu dng ng mao qun thch anh c gia nhit,
gip chng ngng t v cho nhy cao vi trong phn tch hi.
- Vn hnh l mt thit b phn tch c lp, hoc kt hp d dng thnh mt h
thng vi cc thit b khc trong nh Phn tch nhit (TG-MS), sc k, l phn
ng,... My khi ph phn tch nh lng kh www.reecotech.com.vn 40
Model QGA:
H thng L vi phn ng kt ni vi My khi ph www.reecotech.com.vn 41
ng dng ca H thng CATLAB: Nghin cu xc nh chc nng, c tnh ca Xc tc d th.
Xc nh din tch b mt/ bao ph ca kim loi (Phng php:
Hp ph/ Gii hp theo chng trnh nhit - TPD).
Nng lng lin kt ca cc phn t hp ph (TPD).
ng hc phn ng (p chy, oxi ha, metan ha), (TPRx).
Xc nh axit b mt, (NH3 / Pyridine TPD).
Kho st tnh hon nguyn ca xc tc, (TPR).
C ch phn ng, (TPRx).
Xc nh c tnh ca b mt kt ta carbon, (TPO).
Phng php Gii hp theo chng trnh nhit (TPD)
Phng php TPD (Temperature Programmed Desorption) c thc hin thng
qua vic gia nhit tuyn tnh mu xc tc c cho tip xc trc (predose)
vi mt tc cht nht nh, ng thi theo di, xc nh, nh gi cc kh thot ra
trong sut qu trnh gia nhit ny. PP ny cho php:
Xc nh dng, s lng v mnh ca cc tm hot ng xc tc;
ng hc hp ph v C ch gii hp;
Nng lng hot ha hp ph/ gii hp;
Nhit hp ph;
H thng L vi phn ng kt ni vi My khi ph www.reecotech.com.vn 42
Bc phn ng gii hp ph (Order of Desorption)
- Bc 0: tc gii hp khng ph thuc vo
bao ph
- Bc 1: tc gii hp ~ ( bao ph tc thi)1
- Bc 2: tc gii hp ~ ( bao ph tc thi)2 Nhit
2nd order
1st order
0 order
Phng php Kh theo chng trnh nhit (TPR)
Phng php TPR (Temperature Programmed Reduction) kho st phn
ng kh ca H2 vi vt liu xc tc.
S(solid) + 1% H2/He R(solid) + H2O
PP ny cho php:
H thng L vi phn ng kt ni vi My khi ph www.reecotech.com.vn 43
Xc nh cc tiu phn kh c trn b
mt xc tc;
Xc nh s oxi ha biu kin ca xc tc
kim loi gn trn gi mang hoc ion kim loi
trong zeolite v oxit;
Xc nh tng tc gia gi mang v kim
loi;
nh hng hin tng trn y (spillover
phenomena) v s hnh thnh hp kim.
Kho st TPR trn mu CuO
Phng php Oxi ha theo chng trnh nhit (TPO)
Phng php TPO (Temperature Programmed Oxidation) dng
kh Oxi long oxi ha b mt xc tc hoc kt ta carbon.
Phng php c ng dng :
Nghin cu qu trnh oxi ha;
Kim tra mc oxi ha b mt;
Kho st iu kin v nhit thiu kt nhm loi b nhng
tp cht lm nh hng phn ng ca pha hot ng xc tc.
H thng L vi phn ng kt ni vi My khi ph www.reecotech.com.vn 44
Phng php Phn ng theo chng trnh nhit (TPRx)
Phng php TPRx (Temperature Programmed Reaction) c th c thc
hin di hai iu kin:
1. Cho xc tc ng hp ph cc tc cht phn ng trc khi thc hin
chng trnh gia nhit trong kh tr.
H thng L vi phn ng kt ni vi My khi ph www.reecotech.com.vn 45
2. a hn hp tc cht phn ng i qua
xc tc bng dng kh mang song song
vi vic thc hin CT gia nhit.
Cho php:
c tnh cc thng s ng hc;
Ti u ha nhit phn ng;
Nghin cu c ch phn ng;
Nghin cu s gim hot tnh xc tc.
Kho st TPRx phn ng reforming
trn xc tc Ni to sysgas
CH4 + CO2 2H2 + 2CO
K thut kho st hp ph ha hc xung ng xc nh tng lng
hp thu, din tch b mt v phn tn xc tc kim loi (vd: Pd/Al2O3).
H thng L vi phn ng kt ni vi My khi ph www.reecotech.com.vn 46
Sc k kh
(GC)
u do nhit &
dn (TCD)
Khi ph
(QMS)
u im C th phn tch c
nhiu kh gii hp.
nh lng chnh xc
kh phn tch.
Cho tn hiu o lin
tc ca MT thnh
phn phn tch.
Cho tn hiu o lin tc,
xc nh ng thi CC
thnh phn phn tch.
nh lng chnh xc kh
phn tch.
D dng pht hin r kh
v thnh phn khng tinh
khit (gy nhim bn).
Nhc im Khng th thc hin
c cc php o lin
tc.
Khng th xc nh
c mt thnh phn
cha nh danh m m
khng kt hp thm
vi detector.
Ch c th theo di
lin tc mt thnh
phn phn tch c
trong kh mang.
Nc tuyt i
khng c c trong
dng kh phn tch.
Vn chi ph ?!
Bng so snh u v nhc im ca cc loi Detector dng kho st xc
tc bng k thut chng trnh nhit 1
1. A. Trovarelli,6th Italian Chem. Soc. Seminar on Catalysis, 2001, 220
H thng L vi phn ng kt ni vi My khi ph www.reecotech.com.vn 47