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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

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