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IsoSORP® SERIES<br />
GRAVIMETRIC SORPTION ANALYZERS<br />
p Adsorption Isotherms and K<strong>in</strong>etics<br />
by Gas Physisorption and Chemisorption<br />
Mea<strong>su</strong><strong>re</strong>ments w<strong>ith</strong> Ca<strong>ta</strong>lysts, Zeolites,<br />
Activated Carbon, Clay, Sil<strong>ica</strong>, Molecular<br />
Sieves<br />
p Surface A<strong>re</strong>a and Porosity<br />
by Gas Physisorption, Density and Buoyancy<br />
Mea<strong>su</strong><strong>re</strong>ments w<strong>ith</strong> Ca<strong>ta</strong>lysts, Zeolites,<br />
Activated Carbon, Clay, Sil<strong>ica</strong>, Molecular<br />
Sieves<br />
p Absorption and Solubilities<br />
by Gas Solubility Mea<strong>su</strong><strong>re</strong>ments <strong>in</strong><br />
Polymers, Liquids and other Materials<br />
p Gas S<strong>to</strong>rage<br />
Gas S<strong>to</strong>rage Capacity Mea<strong>su</strong><strong>re</strong>ments<br />
w<strong>ith</strong> New and Class<strong>ica</strong>l Materials (Me<strong>ta</strong>l<br />
Organic Frameworks, Me<strong>ta</strong>l Hydrides,<br />
Carbon Nano Tubes, Ionic Liquids)<br />
p Diffusion and Permeation<br />
Mea<strong>su</strong><strong>re</strong>ments of Diffusion Coefficient<br />
of Ad- / Absorption Processes of Gases and<br />
Mixtu<strong>re</strong>s<br />
p Separations<br />
Mea<strong>su</strong><strong>re</strong>ment of the Selectivity of Mixed<br />
Gas Sorption<br />
p Temperatu<strong>re</strong> Programmed Desorption<br />
Determ<strong>in</strong><strong>in</strong>g B<strong>in</strong>d<strong>in</strong>g Energies or Heat<br />
of Adsorption by Desorb<strong>in</strong>g Loaded Sample<br />
Material at Elevated Temperatu<strong>re</strong><br />
p Vapor Permeability and Diffusivity<br />
Mea<strong>su</strong><strong>re</strong>ments of Membranes, Pack<strong>in</strong>g<br />
Materials, Blisters and Foils<br />
p Wett<strong>in</strong>g and Dry<strong>in</strong>g Processes<br />
of Pharmaceut<strong>ica</strong>ls, Construction Materials<br />
and Solid Fuels<br />
p Corrosion Studies<br />
of Alloys for High Temperatu<strong>re</strong> Appl<strong>ica</strong>tions<br />
<strong>in</strong> Power Plants or Gas Turb<strong>in</strong>es<br />
p Filter Material Test<strong>in</strong>g<br />
by Mea<strong>su</strong>r<strong>in</strong>g the Capacity and Selectivity<br />
for Pollu<strong>ta</strong>nts<br />
p Inc<strong>in</strong>eration or Conversion of Toxic<br />
Biolog<strong>ica</strong>l and Chem<strong>ica</strong>l Materials<br />
by High Temperatu<strong>re</strong> and/or High P<strong>re</strong>s<strong>su</strong><strong>re</strong><br />
Vapor<br />
p Ca<strong>ta</strong>lyst<br />
Sulphidation Processes, Cok<strong>in</strong>g and<br />
Lifetime Test<strong>in</strong>g<br />
Magnetic Suspension Balance<br />
The heart of the IsoSORP® <strong>in</strong>struments is the Magnetic Suspension Balance for accurately<br />
weigh<strong>in</strong>g the sample material. Rubotherm’s patented Magnetic Suspension Balance allows<br />
highly accurate weight mea<strong>su</strong><strong>re</strong>ments of samples <strong>in</strong> closed vessels <strong>to</strong> be performed. The<br />
sample is weighed from the outside and the <strong>su</strong>spension force is con<strong>ta</strong>ctlessly transmitted<br />
from the p<strong>re</strong>s<strong>su</strong>rised mea<strong>su</strong>r<strong>in</strong>g cell <strong>to</strong> a microbalance at ambient atmosphe<strong>re</strong>. This means<br />
that mass <strong>ch</strong>anges of a sample <strong>in</strong> a closed <strong>re</strong>ac<strong>to</strong>r can be <strong>re</strong>corded even under ext<strong>re</strong>me<br />
conditions w<strong>ith</strong> the utmost accuracy.<br />
The unique featu<strong>re</strong>s of the Magnetic Suspension Balances a<strong>re</strong>:<br />
p<br />
p<br />
p<br />
p<br />
p<br />
p<br />
Con<strong>ta</strong>ct f<strong>re</strong>e weigh<strong>in</strong>g <strong>in</strong> hermet<strong>ica</strong>lly closed <strong>re</strong>ac<strong>to</strong>rs w<strong>ith</strong> patented<br />
magnetic <strong>su</strong>spension device<br />
Hermetic separation of mea<strong>su</strong><strong>re</strong>ment a<strong>re</strong>a (sample) and weigh<strong>in</strong>g a<strong>re</strong>a (balance) <strong>to</strong><br />
avoid any damage, destruction or <strong>in</strong>terfe<strong>re</strong>nce from the process media (e.g. corrosive<br />
gases, vapors), p<strong>re</strong>s<strong>su</strong><strong>re</strong> or temperatu<strong>re</strong>.<br />
The <strong>re</strong>ac<strong>to</strong>r of the Magnetic Suspension Balance is completely<br />
me<strong>ta</strong>l sealed, even highly agg<strong>re</strong>ssive or corrosive atmosphe<strong>re</strong>s<br />
can be used for mea<strong>su</strong><strong>re</strong>ments <strong>in</strong> a wide p<strong>re</strong>s<strong>su</strong><strong>re</strong> and<br />
temperatu<strong>re</strong> range.<br />
Excellent long term s<strong>ta</strong>bility: The sample can be<br />
au<strong>to</strong>mat<strong>ica</strong>lly disconnected from the balance at<br />
any time <strong>to</strong> <strong>re</strong>-<strong>ta</strong><strong>re</strong> and/or calibrate the balance and<br />
<strong>re</strong>connected and <strong>re</strong>turned <strong>to</strong> the mea<strong>su</strong>r<strong>in</strong>g position <strong>to</strong><br />
cont<strong>in</strong>ue the mea<strong>su</strong><strong>re</strong>ment. High p<strong>re</strong>cision long term<br />
mea<strong>su</strong><strong>re</strong>ments can be performed w<strong>ith</strong>out any basel<strong>in</strong>e<br />
drift or accuracy loss.<br />
Modular construction: The Magnetic Suspension Balance can<br />
be easily adapted <strong>to</strong> new appl<strong>ica</strong>tions.<br />
For thermobalance appl<strong>ica</strong>tions no other <strong>in</strong>strument than<br />
the patented Magnetic Suspension Balance is able <strong>to</strong> work w<strong>ith</strong><br />
high p<strong>re</strong>s<strong>su</strong><strong>re</strong> and high temperatu<strong>re</strong> at the same time and<br />
additionally handle agg<strong>re</strong>ssive media (e.g. H 2 S at high p<strong>re</strong>s<strong>su</strong><strong>re</strong><br />
and/or temperatu<strong>re</strong>) and vapors.<br />
The IsoSORP® <strong>in</strong>struments can be equipped w<strong>ith</strong> diffe<strong>re</strong>nt<br />
versions of the Magnetic Suspension Balance w<strong>ith</strong> the follow<strong>in</strong>g<br />
specif<strong>ica</strong>tions:<br />
Magnetic Suspension Resolution Dynamic Weigh<strong>in</strong>g Range<br />
Balance Type<br />
(Sample Mass)<br />
A 10 0.01 µg 200 mg<br />
A 100 0.1 µg 1 g<br />
E 1 1 µg 10 g<br />
E 10 10 µg 25 g
IsoSORP® SERIES<br />
GRAVIMETRIC SORPTION ANALYZERS<br />
TEMPERATURE CONTROL<br />
O P E R AT I N G P R E S S U R E R A N G E<br />
350 bar<br />
150 bar<br />
IsoSORP® flow<br />
IsoSORP® s<strong>ta</strong>tic<br />
-196°C -150°C -20°C 20°C 50°C 150°C 400°C<br />
Cyro -<br />
Cool<strong>in</strong>g<br />
Cold Gas<br />
Cool<strong>in</strong>g<br />
Liquid<br />
Circula<strong>to</strong>r<br />
Electr<strong>ica</strong>l<br />
Heat<strong>in</strong>g<br />
A ma<strong>in</strong> advan<strong>ta</strong>ge of the Magnetic Suspension Balance is its wide work<strong>in</strong>g temperatu<strong>re</strong><br />
range. The IsoSORP® <strong>in</strong>struments can be operated <strong>in</strong> the sample temperatu<strong>re</strong> range<br />
between -196°C and 400°C. Four devices a<strong>re</strong> applied <strong>to</strong> cover this wide range: cyro-cool<strong>in</strong>g<br />
w<strong>ith</strong> LN 2 or LAr <strong>in</strong> a dewar vessel, cold gas cool<strong>in</strong>g w<strong>ith</strong> N 2 , liquid thermos<strong>ta</strong>tion and<br />
electr<strong>ica</strong>l heat<strong>in</strong>g.<br />
The me<strong>ta</strong>l mea<strong>su</strong>r<strong>in</strong>g cell is always thermos<strong>ta</strong>ted by one of these devices. Depend<strong>in</strong>g on<br />
the temperatu<strong>re</strong> range of the mea<strong>su</strong><strong>re</strong>ment an appropriate device has <strong>to</strong> be located on<br />
the cell. Even dur<strong>in</strong>g a mea<strong>su</strong><strong>re</strong>ment the devices can be <strong>ch</strong>anged w<strong>ith</strong>out caus<strong>in</strong>g any<br />
<strong>ch</strong>ange <strong>in</strong> the mea<strong>su</strong>r<strong>in</strong>g fluid atmosphe<strong>re</strong>. Dur<strong>in</strong>g the ex<strong>ch</strong>ange the Magnetic Suspension<br />
Balance can be set <strong>to</strong> the zero position. After <strong>ch</strong>ang<strong>in</strong>g the thermos<strong>ta</strong>t<strong>in</strong>g device the<br />
mea<strong>su</strong><strong>re</strong>ment can be cont<strong>in</strong>ued w<strong>ith</strong>out basel<strong>in</strong>e drift.<br />
Cyro - Cool<strong>in</strong>g Cold Gas Cool<strong>in</strong>g Liquid Circula<strong>to</strong>r Electr<strong>ica</strong>l Heat<strong>in</strong>g<br />
Temperatu<strong>re</strong> Range<br />
-196°C (LN 2 ) or -150°C … +20°C -20°C … +150°C +50°C … + 400°C<br />
- 186°C (LAr)
IsoSORP® SERIES<br />
GRAVIMETRIC SORPTION ANALYZERS<br />
OPTIONS<br />
Density Mea<strong>su</strong><strong>re</strong>ment<br />
W<strong>ith</strong> the IsoSORP® <strong>in</strong>struments two samples can be weighed simul<strong>ta</strong>neously.<br />
Additionally <strong>to</strong> <strong>re</strong>cord<strong>in</strong>g the mass <strong>ch</strong>ange of the sample material a second – <strong>in</strong>ert –<br />
sample can be weighed. By weigh<strong>in</strong>g a Ti s<strong>in</strong>ker as the second sample the density<br />
of the gas phase <strong>in</strong> the balance is determ<strong>in</strong>ed accord<strong>in</strong>g <strong>to</strong> Ar<strong>ch</strong>imedes’ pr<strong>in</strong>ciple.<br />
Particularly at high p<strong>re</strong>s<strong>su</strong><strong>re</strong>s or <strong>in</strong> gas mixtu<strong>re</strong>s this cannot be calculated<br />
accurately us<strong>in</strong>g equations of s<strong>ta</strong>te.<br />
The density <strong>in</strong>fluences the mea<strong>su</strong><strong>re</strong>d<br />
sample mass, via the buoyancy effect,<br />
and thus should be known accurately.<br />
To Balance<br />
Connection<br />
Zero Po<strong>in</strong>t<br />
Position<br />
Sorption<br />
Mea<strong>su</strong><strong>re</strong>ment<br />
Density<br />
Mea<strong>su</strong><strong>re</strong>ment<br />
Furthermo<strong>re</strong>, density mea<strong>su</strong><strong>re</strong>ment of<br />
b<strong>in</strong>ary mixtu<strong>re</strong>s enables their composition<br />
<strong>to</strong> be calculated w<strong>ith</strong>out the necessity of<br />
further composition analysis (e.g. by gas<br />
<strong>ch</strong>roma<strong>to</strong>graph). The<strong>re</strong>fo<strong>re</strong>, the IsoSORP®<br />
offers two devices <strong>in</strong> one: gravimetric<br />
mea<strong>su</strong><strong>re</strong>ment of mass transfer between a<br />
gaseous fluid phase and the sample and<br />
also the gravimetric mea<strong>su</strong><strong>re</strong>ment of gas<br />
composition.<br />
Electromagnet<br />
Permanent<br />
Magnet<br />
S<strong>in</strong>ker<br />
Example:<br />
Simul<strong>ta</strong>neous<br />
Mea<strong>su</strong><strong>re</strong>ment<br />
of Sorption<br />
and Density<br />
These options a<strong>re</strong> available for<br />
MSB type E1 and E10<br />
Sample<br />
To Balance<br />
Connection<br />
Electromagnet<br />
Permanent<br />
Magnet<br />
Gas Flow <strong>in</strong><br />
Sample Con<strong>ta</strong><strong>in</strong>er<br />
set down <strong>to</strong><br />
sealed Support<br />
Bypass F<strong>re</strong>e Flow<br />
of Gas through Sample<br />
Sample Con<strong>ta</strong><strong>in</strong>er w<strong>ith</strong><br />
“sieve like” bot<strong>to</strong>m<br />
Forced Flow through<br />
Zero Po<strong>in</strong>t Position<br />
Forced Flow Through<br />
A special version of the IsoSORP® was developed <strong>to</strong> <strong>in</strong>vestigate mass transfer processes<br />
<strong>in</strong> a forced flow of gas through bulk material beds. This apparatus is used <strong>to</strong> <strong>in</strong>vestigate<br />
for example <strong>su</strong>percrit<strong>ica</strong>l fluid extraction or <strong>re</strong>actions<br />
Sorption<br />
Mea<strong>su</strong><strong>re</strong>ment<br />
on ca<strong>ta</strong>lysts as close <strong>to</strong> the <strong>re</strong>al process conditions<br />
as possible.<br />
The bulk material con<strong>ta</strong><strong>in</strong>er is placed on a sealed plate<br />
and the gas is forced <strong>to</strong> flow through the material.<br />
The mea<strong>su</strong><strong>re</strong>ment of sample weight <strong>ch</strong>ange due <strong>to</strong><br />
the mass transfer from or <strong>to</strong> the gas phase is carried<br />
out over user configu<strong>re</strong>d time <strong>in</strong>tervals.<br />
The gas flow is s<strong>to</strong>pped for a short time and the<br />
con<strong>ta</strong><strong>in</strong>er is lifted <strong>to</strong> a f<strong>re</strong>ely <strong>su</strong>spended s<strong>ta</strong>te by the<br />
Magnetic Suspension Balance and weighed. By this<br />
procedu<strong>re</strong> dist<strong>in</strong>ct weight da<strong>ta</strong> can be ga<strong>in</strong>ed, ea<strong>ch</strong><br />
after a cer<strong>ta</strong><strong>in</strong> time of gas flow through the sample.<br />
Sample Con<strong>ta</strong><strong>in</strong>er<br />
lifted from Support<br />
for weigh<strong>in</strong>g of<br />
Sample<br />
Gas Flow out
IsoSORP® SERIES<br />
GRAVIMETRIC SORPTION ANALYZERS<br />
BALANCE AND DOSING SYSTEM<br />
A fully au<strong>to</strong>matic IsoSORP® <strong>in</strong>strument is always a comb<strong>in</strong>ation of the<br />
Magnetic Suspension Balance and a gas and/or vapor dos<strong>in</strong>g system.<br />
This pictu<strong>re</strong> is just an example for a s<strong>ta</strong>tic or a flow system. The IsoSORP® <strong>in</strong>struments<br />
a<strong>re</strong> always a comb<strong>in</strong>ation of the Magnetic Suspension Balance (MSB Type E1, shown<br />
on the left side) and a dos<strong>in</strong>g system (Type G-HP flow, shown on the right side).<br />
To <strong>ch</strong>oose the right <strong>in</strong>strument for your appl<strong>ica</strong>tion please select the <strong>re</strong>solution of the<br />
balance and the dos<strong>in</strong>g system <strong>in</strong> the <strong>ta</strong>ble below.<br />
Please <strong>ch</strong>oose a temperatu<strong>re</strong> range under “Temperatu<strong>re</strong> Control” <strong>in</strong> this bro<strong>ch</strong>u<strong>re</strong>.<br />
Magnetic<br />
Suspension<br />
Balance<br />
FlexiDOSE<br />
GAS AND/OR Vapor<br />
DOSING SYSTEM<br />
MSB + DOSING SYSTEM<br />
FlexiDOSE Selection Matrix<br />
Dos<strong>in</strong>g System P<strong>re</strong>s<strong>su</strong><strong>re</strong> Range Media Atmosphe<strong>re</strong> Special featu<strong>re</strong><br />
G-LP STATIC up <strong>to</strong> 1 bar gas s<strong>ta</strong>tic UHV range<br />
G-HP STATIC up <strong>to</strong> 150 bar gas s<strong>ta</strong>tic economic version<br />
G-HPII STATIC up <strong>to</strong> 350 bar gas s<strong>ta</strong>tic me<strong>ta</strong>l block manifold<br />
G&V-HP STATIC up <strong>to</strong> 150 bar gas &vapor s<strong>ta</strong>tic heated<br />
SC-HPII STATIC up <strong>to</strong> 350 bar gas &vapor s<strong>ta</strong>tic <strong>su</strong>percrit<strong>ica</strong>l fluids<br />
S<strong>ta</strong>tic dos<strong>in</strong>g systems a<strong>re</strong> p<strong>re</strong>s<strong>su</strong><strong>re</strong> controllers<br />
<strong>in</strong> whi<strong>ch</strong> all valves a<strong>re</strong> closed (i. e. no gas flow)<br />
once the setpo<strong>in</strong>t p<strong>re</strong>s<strong>su</strong><strong>re</strong> is <strong>re</strong>a<strong>ch</strong>ed.<br />
SC-HPIII STATIC up <strong>to</strong> 700 bar gas &vapor s<strong>ta</strong>tic extended P-range<br />
G-MIX-HP STATIC up <strong>to</strong> 150 bar gas s<strong>ta</strong>tic mixed gas sorption<br />
Dos<strong>in</strong>g System P<strong>re</strong>s<strong>su</strong><strong>re</strong> Range Media Atmosphe<strong>re</strong> Special featu<strong>re</strong><br />
G-LP FLOW up <strong>to</strong> 1 bar gas flow UHV range<br />
G-MP FLOW up <strong>to</strong> 50 bar gas flow economic version<br />
G-HP FLOW up <strong>to</strong> 150 bar gas flow 2-s<strong>ta</strong>ge P-controller<br />
G-HPII FLOW up <strong>to</strong> 350 bar gas flow 2-s<strong>ta</strong>ge P-controller<br />
G&V-LP FLOW up <strong>to</strong> 1 bar gas &vapor flow airbath heated<br />
G&V-MP FLOW up <strong>to</strong> 50 bar gas &vapor flow HPLC-pump dos<strong>in</strong>g<br />
Flow dos<strong>in</strong>g systems a<strong>re</strong> equipped w<strong>ith</strong><br />
a dynam<strong>ica</strong>lly work<strong>in</strong>g upst<strong>re</strong>am p<strong>re</strong>s<strong>su</strong><strong>re</strong><br />
controller at the outlet of the balance<br />
<strong>re</strong>ac<strong>to</strong>r. The p<strong>re</strong>s<strong>su</strong><strong>re</strong> <strong>in</strong> the flow<strong>in</strong>g<br />
atmosphe<strong>re</strong> is controlled by this setup.<br />
G&V-HP FLOW up <strong>to</strong> 150 bar gas &vapor flow HPLC-pump dos<strong>in</strong>g<br />
G-MIX-MP FLOW up <strong>to</strong> 40 bar gas flow/s<strong>ta</strong>tic mixed gas sorption<br />
G-MIX-HP FLOW up <strong>to</strong> 150 bar gas flow/s<strong>ta</strong>tic mixed gas sorption
IsoSORP® SERIES<br />
GRAVIMETRIC SORPTION ANALYZERS<br />
IsoSORP® Appl<strong>ica</strong>tion Examples<br />
Selected experimen<strong>ta</strong>l <strong>re</strong><strong>su</strong>lts mea<strong>su</strong><strong>re</strong>d w<strong>ith</strong> the IsoSORP® series<br />
<strong>in</strong> our cus<strong>to</strong>mers’ labora<strong>to</strong>ries a<strong>re</strong> shown below.<br />
High P<strong>re</strong>s<strong>su</strong><strong>re</strong> Adsorption Isotherm<br />
High p<strong>re</strong>s<strong>su</strong><strong>re</strong> gas adsorption isotherms a<strong>re</strong> mea<strong>su</strong><strong>re</strong>d w<strong>ith</strong> our<br />
IsoSORP® <strong>in</strong>struments.<br />
In the diagram the adsorption isotherm da<strong>ta</strong> up <strong>to</strong> 500 bar of the<br />
th<strong>re</strong>e gases CH 4 , N 2 , Ar on an activated carbon a<strong>re</strong> shown.<br />
K<strong>in</strong>etics<br />
In addition <strong>to</strong> the sorption capacity the <strong>re</strong>action k<strong>in</strong>etics is an impor<strong>ta</strong>nt<br />
<strong>in</strong>formation <strong>to</strong> develop new materials. Due <strong>to</strong> their high accuracy and long<br />
term s<strong>ta</strong>bility the IsoSORP® <strong>in</strong>struments a<strong>re</strong> an ideal <strong>to</strong>ol <strong>to</strong> track dynamic<br />
processes. In the diagram the up<strong>ta</strong>ke curves of H 2 on two diffe<strong>re</strong>nt MOF<br />
materials (me<strong>ta</strong>l organic framework) at 77 K and 298 K a<strong>re</strong> compa<strong>re</strong>d.<br />
From these time dependent up<strong>ta</strong>kes effective diffusion coefficients can<br />
be determ<strong>in</strong>ed, whi<strong>ch</strong> a<strong>re</strong> <strong>ch</strong>aracteristic for the adsorption k<strong>in</strong>etics.<br />
Gas Clean<strong>in</strong>g and Separation<br />
The IsoSORP® <strong>in</strong>struments a<strong>re</strong> well designed <strong>to</strong> mea<strong>su</strong><strong>re</strong> the selectivity of<br />
ad- and absorption of gaseus mixtu<strong>re</strong>s on diffe<strong>re</strong>nt materials.<br />
The diagram shows the <strong>in</strong>dividual adsorption of the components of a gas<br />
mixtu<strong>re</strong> <strong>in</strong> a ionic Liquid BMIM.<br />
Adsorption Isotherms & K<strong>in</strong>etics +++ Surface A<strong>re</strong>a & Porosity +++ Absorption & Solubilities +++ Gas S<strong>to</strong>rage<br />
+++ Diffusion & Permeation +++ Separations +++ Wett<strong>in</strong>g & Dry<strong>in</strong>g Processes +++ Corrosion Studies +++ Filter<br />
Material Test<strong>in</strong>g +++ Ca<strong>ta</strong>lyst TESTING<br />
RUBOTHERM GMBH<br />
Konrad-Zuse-StrASSE 4 · 44801 Bo<strong>ch</strong>um · Germany<br />
Phone: +49 (0)2 34 - 70 99 6 - 0 · Fax: +49 (0)2 34 - 70 99 6 -22<br />
E-Mail: <strong>in</strong>fo@rubotherm.de · www.rubotherm.de<br />
<strong>Te<strong>ch</strong></strong>n<strong>ica</strong>l da<strong>ta</strong> a<strong>re</strong> <strong>su</strong>b<strong>ject</strong> <strong>to</strong> <strong>ch</strong>ange w<strong>ith</strong>out p<strong>rio</strong>r no<strong>tice</strong> <strong>in</strong> l<strong>in</strong>e w<strong>ith</strong> cont<strong>in</strong>uous product improvement. © 2012 RUBOTHERM GMBH | Artwork: DesignBüro S<strong>ch</strong>önfelder