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NEXT GENERATION GRAVIMETRIC SORPTION ANALYZER XEMIS www.hidenisochema.com
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Page 1: XEMIS - Hiden Isochema

NEXT GENERATION GRAVIMETRIC SORPTION ANALYZER

XEMIS

www.hidenisochema.com

Page 2: XEMIS - Hiden Isochema

MBRMembrane Permeation Analyzer

IGAGravimetric Gas & Vapor Sorption Analyzers

Hiden Isochema is a world leader in the design and manufacture of high accuracy sorption instruments for research, development and production applications in materials science and related fields.

Full details on our complete range of products and services are available on our website.

www.hidenisochema.com

XCSClimate Control

Systems

ABRAutomated Breakthrough

Analyzer

IMIHigh Accuracy Hydrogen Storage Analyzer

XEMISNext Generation Gravimetric Sorption Analyzer

IGASORPDynamic Vapor

Sorption Analyzer

Page 3: XEMIS - Hiden Isochema

The XEMIS is a high accuracy gravimetric sorption analyzer designed for operation with a wide range of gases and vapors at pressures up to 200 bar. Featuring next generation microbalance technology, it allows high resolution measurements on exceptionally small samples.

WIDEST CONTROLLABLE PRESSURE RANGE OF ANY GRAVIMETRIC SORPTION ANALYZERAutomated switching between multiple pressure transducers allows active pressure regulation over 7 orders of magnitude.

UNIQUE EXOSENSING TECHNOLOGY FOR OPERATION WITH AGGRESSIVE SPECIESHiden Isochema’s Exosensing Technology removes sensitive components from the balance chamber and allows safe, reliable operation with flammable, corrosive and toxic gases and vapors.

OPTIMIZED PERFORMANCE FOR SAMPLE SIZES FROM 1 mg TO 5 gOverall baseline stability, combined with symmetric geometry and minimized total buoyancy, offers performance unrivalled in a high pressure sorption analyzer.

ISOTHERM, ISOBAR AND HIGH PRESSURE TGA MEASUREMENTS IN A SINGLE AUTOMATED ANALYZER

Page 4: XEMIS - Hiden Isochema

XEMIS OVERVIEW

ENHANCED FUNCTIONALITY

All-metal construction with high quality VCR fittings ensures reliable operation at high pressures, with quick, easy sample loading.

EXOSENSING TECHNOLOGY

Sensitive components removed from the

microbalance chamber allows operation with

corrosive species.

TWIN THERMOSTATS

COUNTERWEIGHT SIDE SAMPLE SIDE

THERMOSTATED ENCLOSURE

Intrinsic long term stability without the need for rezeroing or recalibrating captures true sorption behavior and records full sorption kinetic data over extended time periods.

NEXT GENERATION DESIGN

Symmetric geometry and precision design engineered microbalance maximizes sensitivity and minimizes buoyancy.

ADVANCED GAS CONTROL SYSTEM

Featuring active pressure regulation.

THE MICROBALANCE

Exodrive Beam Position Control

Counterweight Hangdown

Sample Hangdown

Exosensor Beam Position Detector

Page 5: XEMIS - Hiden Isochema

THE IGA METHOD

TIME

PRESSUREPn

UPT

AKE

En

Pressure/gas composition is changed and actively regulated during sorption at the set point Pn.

Equilibrium points are collected and plotted as an isotherm. The IGA method allows consistent and accurate measurements with faster overall process times.

The weight data is analyzed in real time to determine kinetic parameters and simultaneously predict the equilibrium point, En.

WEI

GH

T

En

PRES

SURE

Pn

TIME

The XEMIS uses Hiden Isochema’s unique IGA (Intelligent Gravimetric Analysis) method for simultaneous, automated determination of sorption kinetics and equilibrium isotherms.

KINETIC ANALYSISThe long term balance stability and isobaric operation of the XEMIS allows analysis of the kinetics of sorption and reaction processes over extended timescales.

The minimal variation in the weight reading for an empty sample holder (the orange trace) provides a highly stable baseline reading above which kinetic processes can be accurately characterized.

Isotherm, isobar and highpressure TGA measurementsin a single automated analyzer Exosensing technology forcompatibility withflammable, corrosive andtoxic gases and vapors Symmetric geometry, with ultralow total system buoyancyfor high accuracy measurementsat high pressures

Measurements at temperaturesfrom 77 K to 500 °C overthe full pressure range

Fast and accurate analysis of equilibriaand kinetics using the IGA method

Full automation and advancedprogrammability including multiplegas inlet switching and automatedspecies decontamination

TIME / HOURS0 10 20 30 40 50 60

983.0

983.2

983.4

983.6

983.8

984.0

984.2

984.4

WEI

GH

T / m

g

24 25 26 27 28 29 30-5

0

5

Δw

/ µg

Page 6: XEMIS - Hiden Isochema

DYNAMIC MIXED GAS MODE

VACUUM VAPOR MODE

XEMIS MODELS

PURE GAS MODE

PURE GAS MODE

DYNAMIC MIXED GAS MODE

XEMIS-001 XEMIS-002 XEMIS-003 XEMIS-100Powerfully combining

the features of the other XEMIS models, the

XEMIS-100 is a flexible mixed gas and vapor

sorption analyzer.

High resolution pure gas and vapor sorption analyzer.

Versatile pure and mixed gas

sorption analyzer.

High resolution pure gas sorption

analyzer.

PURE GAS MODE

VACUUM VAPOR MODE

OPERATING MODES

DYNAMIC VAPOR

OPERATING MODESOPERATING MODES

OPTIONAL

MASS SPECTROMETER

PURE GAS MODE

DYNAMIC VAPOR

OPERATING MODES

OPTIONAL

MASS SPECTROMETER

Page 7: XEMIS - Hiden Isochema

High resolution pure gas sorption analyzer, for precise characterization of sorption equilibria and kinetics.The XEMIS-001 operates with a wide range of gases including flammable, toxic and corrosives species, and features automatic decontamination and shutdown for rapid, safe sample exchange.

Typical application areas:

Carbon capture and storage

Hydrogen and natural gas storage

Gas solubility in ionic liquids

Nanoporous material characterization

Gas sorption on geological materials

XEMIS-001

High resolution gas and vapor sorption analyzer, with anti-condensation protection up to 40 °C.Up to 4 pressure sensors may be selected, offering active pressure control over an unparalleled range.

Typical application areas:

VOC filtration

Thermochemical energy storage

Toxic gas storage and separation

XEMIS-002

T1T2

T3

P1

P2

P3

P4

Pumps

Thermostat

Valve Driver

Gas Handling

Oil-Free Vacuum System

Exhaust

Admit Handling

Temperature Control Interface

Control Computer

V

T1T2

T3

P1

P2

P3

P4

Pumps

Thermostat

Valve Driver

Gas Handling

Oil-Free Vacuum System

Exhaust

Admit Handling

Temperature Control Interface

Control Computer

V

Page 8: XEMIS - Hiden Isochema

Versatile pure and mixed gas sorption analyzer with combined control of pressure, flow and gas composition.An optional vapor generator module allows water or organic solvent vapor to be delivered as part of the gas mixture so more complex investigations can be performed.

Typical application areas:

High pressure catalysis

Flue gas desulfurization

Gas-solid reaction kinetics

XEMIS-003

Advanced gravimetric sorption analyzer for high resolution gas and vapor sorption combined with high pressure TGA.Integration with Hiden Analytical’s range of quadrupole mass spectrometers allows analysis of evolved gas for in-situ TGA-MS and related studies.

Typical application areas:

Energy gas storage

High pressure TGA

Polymer membrane characterization

XEMIS-100

T1T2

T3

P1

P2

P3

P4

Pumps

Thermostat

Valve Driver

Gas Handling

Oil-Free Vacuum System

Exhaust

Admit Handling

Temperature Control Interface

Control Computer

V

Flow Handling

T1T2

T3

P1

P2

P3

P4

Pumps

Thermostat

Valve Driver

Gas Handling

Oil-Free Vacuum System

Exhaust

Admit Handling

Temperature Control Interface

Control Computer

V

Flow Handling

Page 9: XEMIS - Hiden Isochema

EXAMPLE APPLICATION DATA

298 K

348 K

PRESSURE (mbar)

0 200 400 600 800 10000

2

1

4

5

6

7

8

9

3

SO2 A

DSO

RPTI

ON

(mm

ol/g

)

ADSORPTION

DESORPTION

Figure 2: CH4 adsorption by a shale over a range of temperatures.Figure 1: SO2 adsorption by a metal-organic framework (NOTT-300), with kind permission from University of Nottingham, UK.

PRESSURE (bar)

0 20 40 60 80 1000

40

20

80

100

120

140

160

180

60

CH

4 AD

SORP

TIO

N (µ

mol

/g)

298 K

358 K

Figure 4: N2, CO2 and SO2 adsorption isotherms on MFM-300(In) over a range of temperatures and pressures. Reproduced with permission from John Wiley and Sons.

Figure 3: Excess H2 uptake for a 22 mg carbon nanotube, CN4800, using both IGA-003 and XEMIS gravimetric sorption analyzers. Reproduced with permission of The Royal Society of Chemistry.

200 60 80 100 120 140 1600

2

1

4

5

6

7

3

PRESSURE (bar)

EXC

ESS

H2 U

PTAK

E (w

t. %

)

40

IGA DATA

XEMIS DATA UPT

AKE

(mm

ol/g

)

PRESSURE (bar)

SO2

CO2

N2

1E-3 0.01 0.1 1 10 100

02468

1002468

1002468

10273 K283 K288 K293 K298 K

303 K310 K323 K335 K348 K

Figure 6: Dimethylformamide (DMF) adsorption by a metal-organic framework (MOF), with an inset showing a single step kinetic. Data courtesy of Newcastle University, UK.

Figure 5: H2O adsorption on zeolite 13X powder.

20 6 8 10 12 14 262422201816 28-2

2

6

8

10

26

24

22

20

18

16

14

12

28

30

4

PRESSURE (mbar)

H2O

AD

SORP

TIO

N (w

t %)

4

10.0 ˚C Sorption12.5 ˚C Sorption15.0 ˚C Sorption17.5 ˚C Sorption20.0 ˚C Sorption22.5 ˚C Sorption25.0 ˚C Sorption

10 3 4 5 60

5

15

20

10

PRESSURE (mbar)

DM

F AD

SORP

TIO

N (w

t %)

2

ISOTHERMAL SERIES PLOT29.99 °C Sorption 0130 Sequence 020 Scan 01 Dimethylformamide Sorption (y1)

23.2

23

22.8

22.6

22.4

22.2

22

21.8

21.6

21.4

21.2

WEI

GH

T (m

g)

200 700 1200 1700 2200 2700 3200 3700 4200 4700

TIME (mins)

Page 10: XEMIS - Hiden Isochema

XEMIS TECHNICAL SPECIFICATIONS

SUPPORTHiden Isochema offers unrivalled technical support free of charge, for the lifetime of the instrument.Telephone and email access to our team of highly qualified engineers with a guaranteed response within 24 hours.Full 12 month warranty as standard.A range of service contracts available.

CONTACT USIf you have any questions about XEMIS or any of Hiden Isochema products or services, please give us a call, we will be happy to help.Tel: +44 (0) 1925 244 678 Email: [email protected] Web: www.hidenisochema.com

It is Hiden Isochema’s policy to continually improve product performance and therefore specifications are subject to change.

1 Please refer to Hiden Isochema product specialists for detailed compatibility and laboratory safety advice.

PRESSUREDesign pressure 170 bar (standard), or 200 bar (optional)Accuracy ± 0.04 % of rangeTransducer ranges (up to 4) 1, 10, 20, 50, 200 bar

2, 10, 100 mbarBase vacuum at sample < 10-6 mbarTypical setpoint regulation accuracy ± 0.02 % of rangeProgrammable gas inlets Up to 6Dynamic pressure / flow control Optional (XEMIS-003 and XEMIS-100 models) Full scale flow rate 3-1000 ml/min (as defined by order option)

WEIGHTBalance capacity 5 gWeighing range 100 mg / 200 mgResolution 0.1 µg / 0.2 µg Stability ±1 µg short term  (± 5 µg long term)

TEMPERATUREMeasurement range 77 – 773 KTemperature sensors Platinum Resistance Thermometer (Pt100)Measurement accuracy ± 0.1 KTypical setpoint regulation accuracy: Recirculating waterbath ± 0.05 K Furnace options ± 0.1 KLinear ramp TGA option 0.05 – 20 K/min programmableCabinet (balance) temperature stability ± 0.1 KAnti-condensation protection 40 °C (XEMIS-002 and XEMIS-100 models)

MASS SPECTROMETER OPTIONSCoupling method Heated Quartz Inert Capillary (QIC) InletAtomic mass range 1–200 AMU standard (1-300 AMU optional)Detection limit 0.1 to 1 ppm, subject to spectral interference

Better than 20 ppb (Triple Mass Filter option)Detector Dual Faraday/Electron Multiplier

SYSTEM CONSTRUCTIONWetted components All metal Pressure vessel Stainless steel (316L grade) Pressure seals Cajon VCR stainless steel Pressure transducer diaphragms Hastelloy C276 / Inconel 600 Overpressure bursting disc Laser welded stainless steelCorrosive species compatibility Included 1

Vapor species compatibility Included for XEMIS-002 and XEMIS-100 models


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