igasorp moisture sorption system specifications ... · pdf fileiga-002 vapour sorption studies...

6
Gravimetric Analysers for the Characterisation of the Sorption Properties of Materials.

Upload: lydung

Post on 22-Mar-2018

222 views

Category:

Documents


3 download

TRANSCRIPT

Specifications

The Sorption Products RangeIGA-001 Gas sorption studies from vacuum to 20 bar.IGA-002 Vapour sorption studies from vacuum incorporating anti-condensation protection. (Technical Data Sheet 137)IGA-003 Dynamic multi-component gas/vapour sorption incorporating gas flow controller. (Technical Data Sheet 138)IGASORP Benchtop system for analysing the moisture sorption properties of materials. (Technical Data Sheet 143)IGA-PTCS Pressure/flow/temperature control system for upgrading existing microbalances. (Technical Data Sheet 139)IGA-DSMS Mass spectrometer interface for gas analysis can be interfaced to all IGA models. (Technical Data Sheet 140)HP-ABR Automated high-pressure breakthrough rigs for characterization of sorbent materials

Additionally, Hiden can supply stand-alone microbalance systems for vacuum or high pressure with data logging/control software.

If you require further, more detailed information on any of the product range, please request the appropriate Technical DataSheet (provided above) and our experienced staff will be happy to provide these details and discuss your specific experimentalapplications.

IGASORP Moisture Sorption SystemThe IGASORP system is specifically designed to study the moisture sorptionproperties of materials. The system uses the same operating principles as in therest of the IGA range. This system is used to model technological applicationswhere moisture behaves as a critical component in either formulation, productionor storage. The fully automated benchtop analyser offers superior performanceand flexibility than traditional methods of moisture analysis while dramaticallyreducing analysis times.

Typical Application Materials➤ Moisture sorption isotherms ➤ Pharmaceutical formulations➤ Hydration/dehydration studies ➤ Excipients, whole tablets➤ Permeation studies ➤ Packaging materials➤ QA/QC of raw/finished materials ➤ Building materials

IGA-PTCS Pressure/Temperature control systemThe IGA-PTCS system adds a pressure/flow and temperature control interface toexisting microbalance systems. The upgraded system has all the functionality ofthe IGA range including the IGAS applications software. Microbalance systemssuch as Cahn and Sartorious can be easily interfaced providing full automation.The IGA-PTCS components consists of:

➤ Pressure control to 20 bar.➤ Temperature control of a wide variety of furnaces to 1000°C.➤ Four stream mass flow control system.➤ IGAS applications software.

IGA-DSMS Mass Spectrometer systemHiden’s range of mass spectrometers can be interfaced to all of the IGA models.The IGA-DSMS combines the gas and gravimetric analysis techniques to providean invaluable tool in materials characterisation. The system can be used to studythermal decomposition and desorption processes.

➤ Broad AMU range with triple mass filter options.➤ Heated capillary transfer.➤ Bypass pumping arrangement for rapid response time.➤ Automated control from IGAS software.➤ Mobile cart for stand-alone operation.

AccessoriesA complete range of accessories and stand-alone modules are offered to supplycomplete turn-key solutions. These include:

➤ Complete range of furnaces from set-point control to high temperature TGapplications.

➤ Liquid nitrogen control systems.➤ Water baths for stable ambient temperature control.➤ Humidifier module for relative humidity control.➤ Vacuum pumping stations.➤ Stand-alone vacuum/pressure microbalance system with data logging

software.

Gravimetric Analysers for theCharacterisation of the SorptionProperties of Materials.

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

TECHNICAL DATA SHEET 146 Printed in England

Manufactured in England by:

HIDEN ISOCHEMA LTD231 EUROPA BOULEVARDWARRINGTON WA5 7TN ENGLAND

Te l: +44 (0) 1925 244 678 Fax: +44 (0) 1925 244 664

E-Mail: [email protected]: www.hidenisochema.com Certificate No. 17958

0

1000

2000

3000

4000

5000

6000

0 5 10 15 20 25Time (Hours)

Wei

ghtc

hang

e(m

icro

gram

mes

)

Moisture sorption on aspirin/blister pack Permeation of moisture through blister packaging in atmosphere of 90% RH at 30°C

0

0.5

1

1.5

2

2.5

0 10 20 30 40 50 10060 70 80 90

%-RH (%)

Con

cent

ratio

n(w

t-%)

Aspirin

Empty blister

The IGASORP system can be used to determine the moisturesorption properties of pharmaceutical materials. The data aboveshows the comparative reactions for an Aspirin tablet and it’sblister packaging material.

The IGASORP system can be used to study the permeationproperties of packaging materials. Such studies proveinvaluable in determining the effectiveness of storage mediaand the shelf-life of hygroscopic materials.

Weight

Balance Capacity*: 5 gramsWeighing Range*: 100mg/200mg/500mgResolution: 0.1 µg for 100mg rangeLong term stability: Nominal +/- 1 µg/weekSample containers: Glass/steel mesh* Larger balance capacities and ranges available

Humidity

Sensor accuracy: +/- 1% (0-90%RH) +/- 2% (90-100%RH)

Sensor response: 15 seconds to 90% of readingControl range: 0%RH (determined by gas supply)

to 95% RHRegulation accuracy: +/- 0.1% RHGas: Typically dry air or nitrogenMax. flow rate: 500 ml/min

Temperature

Bath thermostat:

Measurement range: 5°C to 85°CAccuracy/stability: +/- 0.05°C to +/- 0.1°C across range

Internal heater for rapid drying:

Max. temperature: 350°CMax. heating rate: 10°C/min

More detailed specifications for the complete IGA range can be obtained from the relevant Technical Data Sheet (see below)

Weight

Balance Capacity*: 5 gramsWeighing Range*: Typically 200 mgResolution: 0.2 µgLong term stability: +/- 1 µgSample containers: Glass/quartz/ceramic/steel mesh* Larger balance capacities and ranges available

Pressure

Vessel: Pressurised-UHV SS316/SS304assembly

Design pressure: 20 barsDesign temperature: 500°C at pressure

1000°C with quartz reactor (ambientpressure)

Pressure sensors: Up to three per system ranging from 1 mbar to 20 bar

Control accuracy: +/- 0.025% of transducer span (i.e. 0.25 mbars for 1 bar transducer)

Temperature

Sensors: Type K or platinum resistancethermometers

Range: Liquid nitrogen to 1000°CControl accuracy: +/- 0.05% to +/- 1°C depending on

control equipmentACS: 50°C Anti-condensation protection

(IGA-002)

Flow Control (IGA-003)

Flow rate: 500 ml/min (standard configuration)No. of streams: Up to four

Optional balance purge for corrosivegases

Models IGA-001, IGA-002 and IGA-003 IGASORP

I S O C H E M A

IGA-002 Vapour Sorption SystemThe IGA-002 system is specifically designed to study general vapour sorptionprocesses from vacuum. This model includes all the features of the IGA-001 modelbut additionally incorporates anti-condensation protection rated to 50°C. Anadditional low range pressure sensor is included. The system can be fitted with aUHV pump isolation valve to achieve the best possible vacuum at the sampleposition and a vapour delivery system is incorporated with the pressure controller.The IGA-002 can be used to study water and hydrocarbon vapour sorption onporous materials such as pharmaceuticals, carbons, catalysts, zeolites, clays andpolymers.

➤ The IGA-002 vapour delivery andpressure control system. A broad range ofliquids can be used in the reservoir togenerate the vapour adsorbate.

IGA-003 Multi-component Sorption SystemThe IGA-003 system is designed to study multi-component gas and/or vapour sorption processesfrom vacuum to high pressure. The system incorporates a multiple inlet mass flow control system.An internal gas delivery system injects the gas stream below the sample and extracts aboveenabling a defined gas composition to be established at the sample position. Flow and pressurecontrol are independent allowing different gas compositions to be generated at different pressures.A balance purge can be provided in this system to allow the use of corrosive gases/vapours at thesample position while protecting the integrity of the weighing system. The system can beinterfaced with a humidifier or vapour generator to define vapour compositions in the samplereactor. The IGA-003 system can be used to study multi-component gas/vapour sorption onmaterials such as carbons, zeolites, polymers and catalysts.

➤ The IGA-003 gasinjection/exhaust system. Up tofour gas streams can be mixedprior to injection into the sample

IGA - The Intelligent Gravimetric Analyser

The IGA range from Hiden Isochema provides the ultimate tool for sorption science . . .

The IGA system uses the gravimetric technique to accurately measure the magnitude and dynamics ofgas and vapour sorption on materials. The IGA design integrates precise computer-control andmeasurement of weight change, pressure, temperature, gas flow and composition. The system canautomatically and reproducibly measure sorption isotherms/isobars as well as investigating thermaldesorption in diverse operating conditions. The unique IGA method exploits the relaxation behaviourof the interaction process after pressure/gas composition/temperature changes to simultaneouslyevaluate kinetic parameters and the asymptotic uptake.

An uncompromising attitude to system design coupled with our experience in solving problems insorption science in some of the most prestigious laboratories around the world makes Hiden Isochemathe obvious and only choice for a sorption analyser.

All IGA models incorporate the following features:

➤ Ultra-sensitive microbalance mounted in thermostatted heatsink to provide high resolution andprecise long-term stability.

➤ Pressure vessel incorporating all-metal seals designed to UHV standards to allow measurementsfrom high vacuum to high pressure.

➤ Basic models can be upgraded to extend their range of applications, as your research programdevelops.

➤ State-of-the-art pressure control system capable of accurately controlling the pressure of gasesand vapours across eight decades of pressure measurement.

➤ Versatile temperature controller for ramp and set-point operations in the temperature range fromcryogenic to 1000°C. Internal temperature probe to measure sample temperature.

➤ Full automation and extensive software package for experiment design, system control, dataacquisition/archival, analysis and export.

➤ Unique and innovative approach for the determination of the sorption kinetics and equilibriumisotherms - The IGA method.

➤ Complete range of accessories including vacuum pumping stations, furnaces, humidifier, waterbaths etc. to enable a broad range of experiments to be performed.

The IGA Method

➤ Pressure/gas composition is changed and thenheld constant during sorption at the set point Pn.

➤ Weight data is acquired and analysed in real-time to determine kinetic parameters and predictthe exact point of equilibrium uptake En.

➤ Equilibrium points are collected and plotted asan isotherm. The IGA method provides aconsistent reproducible analysis method point-to-point on the isotherm whilst making theoptimum use of laboratory time.

IGA-001 Gas Sorption SystemThe IGA-001 system is specifically designed as a versatile gravimetricanalysis system. The system can be configured to study general gassorption processes from vacuum to high pressure as well as being usedas a high pressure thermobalance with mass spectrometer interface(IGA-DSMS).

Typical Application Materials

➤ Gas sorption ➤ Zeolites

➤ Sorption kinetic analysis ➤ Carbons

➤ Outgassing behaviour ➤ Metal/intermetallic hydrides

➤ TG studies ➤ High Tc materials/ceramics

➤ In-situ surface area analysis ➤ Polymers

➤ In-situ pore size analysis

INTELLIGENT GRAVIMETRIC ANALYSER

ISOCHEMAISOCHEMA

C

COM

+ -

P

M

T

ISOCHEMAISOCHEMA ANTI-CONDENSATIONSYSTEMANTI-CONDENSATIONSYSTEM

Wall Mounting Bracket

Microprocessor Thermostatted Microbalance Pressure Controller

Vacuum Pump Isolation Valve

Sample (internal temperature probe)

Sample Environment: Furnace Water bath Dewar

Gas/Vapour Delivery: High pressure gases Vapours Gas/Vapour mixtures

Vacuum/Pressure Vessel

Comparison of nitrogen and oxygen adsorption on 5A Zeolite

0

0.5

1

1.5

2

2.5

3

3.5

4

0 1 2 3 4 5 6 7 8 9 10

Pressure (Bars)

Con

cent

ratio

n(w

t-%)

Nitrogen

Oxygen

Kinetics of R-134A sorption on carbon

5200

6200

7200

8200

9200

10200

11200

12200

13200

14200

0 50 100 150 200

Time (Minutes)

Wei

ghtC

hang

e(g

)

m(t)=m•+∆m[1-exp(-kt)] m• = 5205 µg∆m = 8238 µgk = 3.2 x 10-4s-1

Upt

ake

Time

Pressure

Wei

ght

Pre

ssur

e

P

P

E

E

n

n

n

n

The IGA-001 system can be used to determine the gas sorptionproperties of porous materials such as zeolites. The data shows acomparison between the oxygen and nitrogen sorption on a 5Azeolite up to an equilibrium pressure of 10 bars.

The kinetic response shown above (the IGA method) is used todetermine equilibration. Such data can prove useful inunderstanding the non-equilibrium sorption behaviour of materialsin order to determine diffusion and transport parameters ofadsorbates in materials. The example above shows a kineticresponse for the sorption of a freon on activated carbon.

CH4-CO2 Dual component isotherms on carbon at 25°C

0

10000

20000

30000

40000

50000

60000

0 1000 2000 3000 4000 5000 6000 7000 8000

0/100

25/75

50/50

75/25

100/0

Pressure (Millibars)

Wei

ght(

Mic

rogr

ams)

Ratios indicated as CH4/CO2 O

Air/Freon Mixture - adsorption isotherms on activated carbon

0

0 1 2 3 4 5 6 7 8 9

Pressure (Bar)

Am

ount

Ads

orbe

d(g

/g)

40°C55°C70°C85°C100°C125°C150°C

0.05

0.10

0.15

0.20

0.25

The IGA-003 system can be used to determine multi-componentgas sorption isotherms. The data above shows the binary isothermfor carbon dioxide and methane measured on carbon. Eachisotherm was obtained at a constant gas composition. It is similarlypossible to measure a composition scan at constant pressure.

The data shows multi-component isotherms for a freon/air mixtureof 4% on an activated carbon. Such information is required whendesigning filtration systems.

0

0.5

1

1.5

2

2.5

3

3.5

4

4.5

5

0 1 2 3 4 5 6 7

Pressure (Millibars)

Con

cent

ratio

n(w

t-%)

Cyclohexane

Benzene

Mesitylene

Water sorption on polymer paint film Hydrocarbon sorption on ZSM-5

0

2

4

6

8

10

12

14

16

18

0 5 10 15 20 25 30 35

Pressure (Millibars)

Con

cent

ratio

n(w

t-%)

29.5C27.1C24.4C22.8C20.3C

The IGA-002 system can be used to determine the watersorption properties of porous materials such as polymers andzeolites. The data shows isothermal uptake curves measured atclosely separated temperatures between 20°C and 30°C on apolymer paint film.

The IGA-002 system can be used to measure hydrocarbonvapour sorption on porous materials. Such data can be used todetermine sample properties such as pore size from adsorbatemolecular dimensions.

IGA-002 Vapour Sorption SystemThe IGA-002 system is specifically designed to study general vapour sorptionprocesses from vacuum. This model includes all the features of the IGA-001 modelbut additionally incorporates anti-condensation protection rated to 50°C. Anadditional low range pressure sensor is included. The system can be fitted with aUHV pump isolation valve to achieve the best possible vacuum at the sampleposition and a vapour delivery system is incorporated with the pressure controller.The IGA-002 can be used to study water and hydrocarbon vapour sorption onporous materials such as pharmaceuticals, carbons, catalysts, zeolites, clays andpolymers.

➤ The IGA-002 vapour delivery andpressure control system. A broad range ofliquids can be used in the reservoir togenerate the vapour adsorbate.

IGA-003 Multi-component Sorption SystemThe IGA-003 system is designed to study multi-component gas and/or vapour sorption processesfrom vacuum to high pressure. The system incorporates a multiple inlet mass flow control system.An internal gas delivery system injects the gas stream below the sample and extracts aboveenabling a defined gas composition to be established at the sample position. Flow and pressurecontrol are independent allowing different gas compositions to be generated at different pressures.A balance purge can be provided in this system to allow the use of corrosive gases/vapours at thesample position while protecting the integrity of the weighing system. The system can beinterfaced with a humidifier or vapour generator to define vapour compositions in the samplereactor. The IGA-003 system can be used to study multi-component gas/vapour sorption onmaterials such as carbons, zeolites, polymers and catalysts.

➤ The IGA-003 gasinjection/exhaust system. Up tofour gas streams can be mixedprior to injection into the sample

IGA - The Intelligent Gravimetric Analyser

The IGA range from Hiden Isochema provides the ultimate tool for sorption science . . .

The IGA system uses the gravimetric technique to accurately measure the magnitude and dynamics ofgas and vapour sorption on materials. The IGA design integrates precise computer-control andmeasurement of weight change, pressure, temperature, gas flow and composition. The system canautomatically and reproducibly measure sorption isotherms/isobars as well as investigating thermaldesorption in diverse operating conditions. The unique IGA method exploits the relaxation behaviourof the interaction process after pressure/gas composition/temperature changes to simultaneouslyevaluate kinetic parameters and the asymptotic uptake.

An uncompromising attitude to system design coupled with our experience in solving problems insorption science in some of the most prestigious laboratories around the world makes Hiden Isochemathe obvious and only choice for a sorption analyser.

All IGA models incorporate the following features:

➤ Ultra-sensitive microbalance mounted in thermostatted heatsink to provide high resolution andprecise long-term stability.

➤ Pressure vessel incorporating all-metal seals designed to UHV standards to allow measurementsfrom high vacuum to high pressure.

➤ Basic models can be upgraded to extend their range of applications, as your research programdevelops.

➤ State-of-the-art pressure control system capable of accurately controlling the pressure of gasesand vapours across eight decades of pressure measurement.

➤ Versatile temperature controller for ramp and set-point operations in the temperature range fromcryogenic to 1000°C. Internal temperature probe to measure sample temperature.

➤ Full automation and extensive software package for experiment design, system control, dataacquisition/archival, analysis and export.

➤ Unique and innovative approach for the determination of the sorption kinetics and equilibriumisotherms - The IGA method.

➤ Complete range of accessories including vacuum pumping stations, furnaces, humidifier, waterbaths etc. to enable a broad range of experiments to be performed.

The IGA Method

➤ Pressure/gas composition is changed and thenheld constant during sorption at the set point Pn.

➤ Weight data is acquired and analysed in real-time to determine kinetic parameters and predictthe exact point of equilibrium uptake En.

➤ Equilibrium points are collected and plotted asan isotherm. The IGA method provides aconsistent reproducible analysis method point-to-point on the isotherm whilst making theoptimum use of laboratory time.

IGA-001 Gas Sorption SystemThe IGA-001 system is specifically designed as a versatile gravimetricanalysis system. The system can be configured to study general gassorption processes from vacuum to high pressure as well as being usedas a high pressure thermobalance with mass spectrometer interface(IGA-DSMS).

Typical Application Materials

➤ Gas sorption ➤ Zeolites

➤ Sorption kinetic analysis ➤ Carbons

➤ Outgassing behaviour ➤ Metal/intermetallic hydrides

➤ TG studies ➤ High Tc materials/ceramics

➤ In-situ surface area analysis ➤ Polymers

➤ In-situ pore size analysis

INTELLIGENT GRAVIMETRIC ANALYSER

ISOCHEMAISOCHEMA

C

COM

+ -

P

M

T

ISOCHEMAISOCHEMA ANTI-CONDENSATIONSYSTEMANTI-CONDENSATIONSYSTEM

Wall Mounting Bracket

Microprocessor Thermostatted Microbalance Pressure Controller

Vacuum Pump Isolation Valve

Sample (internal temperature probe)

Sample Environment: Furnace Water bath Dewar

Gas/Vapour Delivery: High pressure gases Vapours Gas/Vapour mixtures

Vacuum/Pressure Vessel

Comparison of nitrogen and oxygen adsorption on 5A Zeolite

0

0.5

1

1.5

2

2.5

3

3.5

4

0 1 2 3 4 5 6 7 8 9 10

Pressure (Bars)

Con

cent

ratio

n(w

t-%)

Nitrogen

Oxygen

Kinetics of R-134A sorption on carbon

5200

6200

7200

8200

9200

10200

11200

12200

13200

14200

0 50 100 150 200

Time (Minutes)

Wei

ghtC

hang

e(g

)

m(t)=m•+∆m[1-exp(-kt)] m• = 5205 µg∆m = 8238 µgk = 3.2 x 10-4s-1

Upt

ake

Time

Pressure

Wei

ght

Pre

ssur

e

P

P

E

E

n

n

n

n

The IGA-001 system can be used to determine the gas sorptionproperties of porous materials such as zeolites. The data shows acomparison between the oxygen and nitrogen sorption on a 5Azeolite up to an equilibrium pressure of 10 bars.

The kinetic response shown above (the IGA method) is used todetermine equilibration. Such data can prove useful inunderstanding the non-equilibrium sorption behaviour of materialsin order to determine diffusion and transport parameters ofadsorbates in materials. The example above shows a kineticresponse for the sorption of a freon on activated carbon.

CH4-CO2 Dual component isotherms on carbon at 25°C

0

10000

20000

30000

40000

50000

60000

0 1000 2000 3000 4000 5000 6000 7000 8000

0/100

25/75

50/50

75/25

100/0

Pressure (Millibars)

Wei

ght(

Mic

rogr

ams)

Ratios indicated as CH4/CO2 O

Air/Freon Mixture - adsorption isotherms on activated carbon

0

0 1 2 3 4 5 6 7 8 9

Pressure (Bar)

Am

ount

Ads

orbe

d(g

/g)

40°C55°C70°C85°C100°C125°C150°C

0.05

0.10

0.15

0.20

0.25

The IGA-003 system can be used to determine multi-componentgas sorption isotherms. The data above shows the binary isothermfor carbon dioxide and methane measured on carbon. Eachisotherm was obtained at a constant gas composition. It is similarlypossible to measure a composition scan at constant pressure.

The data shows multi-component isotherms for a freon/air mixtureof 4% on an activated carbon. Such information is required whendesigning filtration systems.

0

0.5

1

1.5

2

2.5

3

3.5

4

4.5

5

0 1 2 3 4 5 6 7

Pressure (Millibars)

Con

cent

ratio

n(w

t-%)

Cyclohexane

Benzene

Mesitylene

Water sorption on polymer paint film Hydrocarbon sorption on ZSM-5

0

2

4

6

8

10

12

14

16

18

0 5 10 15 20 25 30 35

Pressure (Millibars)

Con

cent

ratio

n(w

t-%)

29.5C27.1C24.4C22.8C20.3C

The IGA-002 system can be used to determine the watersorption properties of porous materials such as polymers andzeolites. The data shows isothermal uptake curves measured atclosely separated temperatures between 20°C and 30°C on apolymer paint film.

The IGA-002 system can be used to measure hydrocarbonvapour sorption on porous materials. Such data can be used todetermine sample properties such as pore size from adsorbatemolecular dimensions.

IGA-002 Vapour Sorption SystemThe IGA-002 system is specifically designed to study general vapour sorptionprocesses from vacuum. This model includes all the features of the IGA-001 modelbut additionally incorporates anti-condensation protection rated to 50°C. Anadditional low range pressure sensor is included. The system can be fitted with aUHV pump isolation valve to achieve the best possible vacuum at the sampleposition and a vapour delivery system is incorporated with the pressure controller.The IGA-002 can be used to study water and hydrocarbon vapour sorption onporous materials such as pharmaceuticals, carbons, catalysts, zeolites, clays andpolymers.

➤ The IGA-002 vapour delivery andpressure control system. A broad range ofliquids can be used in the reservoir togenerate the vapour adsorbate.

IGA-003 Multi-component Sorption SystemThe IGA-003 system is designed to study multi-component gas and/or vapour sorption processesfrom vacuum to high pressure. The system incorporates a multiple inlet mass flow control system.An internal gas delivery system injects the gas stream below the sample and extracts aboveenabling a defined gas composition to be established at the sample position. Flow and pressurecontrol are independent allowing different gas compositions to be generated at different pressures.A balance purge can be provided in this system to allow the use of corrosive gases/vapours at thesample position while protecting the integrity of the weighing system. The system can beinterfaced with a humidifier or vapour generator to define vapour compositions in the samplereactor. The IGA-003 system can be used to study multi-component gas/vapour sorption onmaterials such as carbons, zeolites, polymers and catalysts.

➤ The IGA-003 gasinjection/exhaust system. Up tofour gas streams can be mixedprior to injection into the sample

IGA - The Intelligent Gravimetric Analyser

The IGA range from Hiden Isochema provides the ultimate tool for sorption science . . .

The IGA system uses the gravimetric technique to accurately measure the magnitude and dynamics ofgas and vapour sorption on materials. The IGA design integrates precise computer-control andmeasurement of weight change, pressure, temperature, gas flow and composition. The system canautomatically and reproducibly measure sorption isotherms/isobars as well as investigating thermaldesorption in diverse operating conditions. The unique IGA method exploits the relaxation behaviourof the interaction process after pressure/gas composition/temperature changes to simultaneouslyevaluate kinetic parameters and the asymptotic uptake.

An uncompromising attitude to system design coupled with our experience in solving problems insorption science in some of the most prestigious laboratories around the world makes Hiden Isochemathe obvious and only choice for a sorption analyser.

All IGA models incorporate the following features:

➤ Ultra-sensitive microbalance mounted in thermostatted heatsink to provide high resolution andprecise long-term stability.

➤ Pressure vessel incorporating all-metal seals designed to UHV standards to allow measurementsfrom high vacuum to high pressure.

➤ Basic models can be upgraded to extend their range of applications, as your research programdevelops.

➤ State-of-the-art pressure control system capable of accurately controlling the pressure of gasesand vapours across eight decades of pressure measurement.

➤ Versatile temperature controller for ramp and set-point operations in the temperature range fromcryogenic to 1000°C. Internal temperature probe to measure sample temperature.

➤ Full automation and extensive software package for experiment design, system control, dataacquisition/archival, analysis and export.

➤ Unique and innovative approach for the determination of the sorption kinetics and equilibriumisotherms - The IGA method.

➤ Complete range of accessories including vacuum pumping stations, furnaces, humidifier, waterbaths etc. to enable a broad range of experiments to be performed.

The IGA Method

➤ Pressure/gas composition is changed and thenheld constant during sorption at the set point Pn.

➤ Weight data is acquired and analysed in real-time to determine kinetic parameters and predictthe exact point of equilibrium uptake En.

➤ Equilibrium points are collected and plotted asan isotherm. The IGA method provides aconsistent reproducible analysis method point-to-point on the isotherm whilst making theoptimum use of laboratory time.

IGA-001 Gas Sorption SystemThe IGA-001 system is specifically designed as a versatile gravimetricanalysis system. The system can be configured to study general gassorption processes from vacuum to high pressure as well as being usedas a high pressure thermobalance with mass spectrometer interface(IGA-DSMS).

Typical Application Materials

➤ Gas sorption ➤ Zeolites

➤ Sorption kinetic analysis ➤ Carbons

➤ Outgassing behaviour ➤ Metal/intermetallic hydrides

➤ TG studies ➤ High Tc materials/ceramics

➤ In-situ surface area analysis ➤ Polymers

➤ In-situ pore size analysis

INTELLIGENT GRAVIMETRIC ANALYSER

ISOCHEMAISOCHEMA

C

COM

+ -

P

M

T

ISOCHEMAISOCHEMA ANTI-CONDENSATIONSYSTEMANTI-CONDENSATIONSYSTEM

Wall Mounting Bracket

Microprocessor Thermostatted Microbalance Pressure Controller

Vacuum Pump Isolation Valve

Sample (internal temperature probe)

Sample Environment: Furnace Water bath Dewar

Gas/Vapour Delivery: High pressure gases Vapours Gas/Vapour mixtures

Vacuum/Pressure Vessel

Comparison of nitrogen and oxygen adsorption on 5A Zeolite

0

0.5

1

1.5

2

2.5

3

3.5

4

0 1 2 3 4 5 6 7 8 9 10

Pressure (Bars)

Con

cent

ratio

n(w

t-%)

Nitrogen

Oxygen

Kinetics of R-134A sorption on carbon

5200

6200

7200

8200

9200

10200

11200

12200

13200

14200

0 50 100 150 200

Time (Minutes)

Wei

ghtC

hang

e(g

)

m(t)=m•+∆m[1-exp(-kt)] m• = 5205 µg∆m = 8238 µgk = 3.2 x 10-4s-1

Upt

ake

Time

Pressure

Wei

ght

Pre

ssur

e

P

P

E

E

n

n

n

n

The IGA-001 system can be used to determine the gas sorptionproperties of porous materials such as zeolites. The data shows acomparison between the oxygen and nitrogen sorption on a 5Azeolite up to an equilibrium pressure of 10 bars.

The kinetic response shown above (the IGA method) is used todetermine equilibration. Such data can prove useful inunderstanding the non-equilibrium sorption behaviour of materialsin order to determine diffusion and transport parameters ofadsorbates in materials. The example above shows a kineticresponse for the sorption of a freon on activated carbon.

CH4-CO2 Dual component isotherms on carbon at 25°C

0

10000

20000

30000

40000

50000

60000

0 1000 2000 3000 4000 5000 6000 7000 8000

0/100

25/75

50/50

75/25

100/0

Pressure (Millibars)

Wei

ght(

Mic

rogr

ams)

Ratios indicated as CH4/CO2 O

Air/Freon Mixture - adsorption isotherms on activated carbon

0

0 1 2 3 4 5 6 7 8 9

Pressure (Bar)

Am

ount

Ads

orbe

d(g

/g)

40°C55°C70°C85°C100°C125°C150°C

0.05

0.10

0.15

0.20

0.25

The IGA-003 system can be used to determine multi-componentgas sorption isotherms. The data above shows the binary isothermfor carbon dioxide and methane measured on carbon. Eachisotherm was obtained at a constant gas composition. It is similarlypossible to measure a composition scan at constant pressure.

The data shows multi-component isotherms for a freon/air mixtureof 4% on an activated carbon. Such information is required whendesigning filtration systems.

0

0.5

1

1.5

2

2.5

3

3.5

4

4.5

5

0 1 2 3 4 5 6 7

Pressure (Millibars)

Con

cent

ratio

n(w

t-%)

Cyclohexane

Benzene

Mesitylene

Water sorption on polymer paint film Hydrocarbon sorption on ZSM-5

0

2

4

6

8

10

12

14

16

18

0 5 10 15 20 25 30 35

Pressure (Millibars)

Con

cent

ratio

n(w

t-%)

29.5C27.1C24.4C22.8C20.3C

The IGA-002 system can be used to determine the watersorption properties of porous materials such as polymers andzeolites. The data shows isothermal uptake curves measured atclosely separated temperatures between 20°C and 30°C on apolymer paint film.

The IGA-002 system can be used to measure hydrocarbonvapour sorption on porous materials. Such data can be used todetermine sample properties such as pore size from adsorbatemolecular dimensions.

Specifications

The Sorption Products RangeIGA-001 Gas sorption studies from vacuum to 20 bar.IGA-002 Vapour sorption studies from vacuum incorporating anti-condensation protection. (Technical Data Sheet 137)IGA-003 Dynamic multi-component gas/vapour sorption incorporating gas flow controller. (Technical Data Sheet 138)IGASORP Benchtop system for analysing the moisture sorption properties of materials. (Technical Data Sheet 143)IGA-PTCS Pressure/flow/temperature control system for upgrading existing microbalances. (Technical Data Sheet 139)IGA-DSMS Mass spectrometer interface for gas analysis can be interfaced to all IGA models. (Technical Data Sheet 140)HP-ABR Automated high-pressure breakthrough rigs for characterization of sorbent materials

Additionally, Hiden can supply stand-alone microbalance systems for vacuum or high pressure with data logging/control software.

If you require further, more detailed information on any of the product range, please request the appropriate Technical DataSheet (provided above) and our experienced staff will be happy to provide these details and discuss your specific experimentalapplications.

IGASORP Moisture Sorption SystemThe IGASORP system is specifically designed to study the moisture sorptionproperties of materials. The system uses the same operating principles as in therest of the IGA range. This system is used to model technological applicationswhere moisture behaves as a critical component in either formulation, productionor storage. The fully automated benchtop analyser offers superior performanceand flexibility than traditional methods of moisture analysis while dramaticallyreducing analysis times.

Typical Application Materials➤ Moisture sorption isotherms ➤ Pharmaceutical formulations➤ Hydration/dehydration studies ➤ Excipients, whole tablets➤ Permeation studies ➤ Packaging materials➤ QA/QC of raw/finished materials ➤ Building materials

IGA-PTCS Pressure/Temperature control systemThe IGA-PTCS system adds a pressure/flow and temperature control interface toexisting microbalance systems. The upgraded system has all the functionality ofthe IGA range including the IGAS applications software. Microbalance systemssuch as Cahn and Sartorious can be easily interfaced providing full automation.The IGA-PTCS components consists of:

➤ Pressure control to 20 bar.➤ Temperature control of a wide variety of furnaces to 1000°C.➤ Four stream mass flow control system.➤ IGAS applications software.

IGA-DSMS Mass Spectrometer systemHiden’s range of mass spectrometers can be interfaced to all of the IGA models.The IGA-DSMS combines the gas and gravimetric analysis techniques to providean invaluable tool in materials characterisation. The system can be used to studythermal decomposition and desorption processes.

➤ Broad AMU range with triple mass filter options.➤ Heated capillary transfer.➤ Bypass pumping arrangement for rapid response time.➤ Automated control from IGAS software.➤ Mobile cart for stand-alone operation.

AccessoriesA complete range of accessories and stand-alone modules are offered to supplycomplete turn-key solutions. These include:

➤ Complete range of furnaces from set-point control to high temperature TGapplications.

➤ Liquid nitrogen control systems.➤ Water baths for stable ambient temperature control.➤ Humidifier module for relative humidity control.➤ Vacuum pumping stations.➤ Stand-alone vacuum/pressure microbalance system with data logging

software.

Gravimetric Analysers for theCharacterisation of the SorptionProperties of Materials.

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

TECHNICAL DATA SHEET 146 Printed in England

Manufactured in England by:

HIDEN ISOCHEMA LTD231 EUROPA BOULEVARDWARRINGTON WA5 7TN ENGLAND

Te l: +44 (0) 1925 244 678 Fax: +44 (0) 1925 244 664

E-Mail: [email protected]: www.hidenisochema.com Certificate No. 17958

0

1000

2000

3000

4000

5000

6000

0 5 10 15 20 25Time (Hours)

Wei

ghtc

hang

e(m

icro

gram

mes

)

Moisture sorption on aspirin/blister pack Permeation of moisture through blister packaging in atmosphere of 90% RH at 30°C

0

0.5

1

1.5

2

2.5

0 10 20 30 40 50 10060 70 80 90

%-RH (%)

Con

cent

ratio

n(w

t-%)

Aspirin

Empty blister

The IGASORP system can be used to determine the moisturesorption properties of pharmaceutical materials. The data aboveshows the comparative reactions for an Aspirin tablet and it’sblister packaging material.

The IGASORP system can be used to study the permeationproperties of packaging materials. Such studies proveinvaluable in determining the effectiveness of storage mediaand the shelf-life of hygroscopic materials.

Weight

Balance Capacity*: 5 gramsWeighing Range*: 100mg/200mg/500mgResolution: 0.1 µg for 100mg rangeLong term stability: Nominal +/- 1 µg/weekSample containers: Glass/steel mesh* Larger balance capacities and ranges available

Humidity

Sensor accuracy: +/- 1% (0-90%RH) +/- 2% (90-100%RH)

Sensor response: 15 seconds to 90% of readingControl range: 0%RH (determined by gas supply)

to 95% RHRegulation accuracy: +/- 0.1% RHGas: Typically dry air or nitrogenMax. flow rate: 500 ml/min

Temperature

Bath thermostat:

Measurement range: 5°C to 85°CAccuracy/stability: +/- 0.05°C to +/- 0.1°C across range

Internal heater for rapid drying:

Max. temperature: 350°CMax. heating rate: 10°C/min

More detailed specifications for the complete IGA range can be obtained from the relevant Technical Data Sheet (see below)

Weight

Balance Capacity*: 5 gramsWeighing Range*: Typically 200 mgResolution: 0.2 µgLong term stability: +/- 1 µgSample containers: Glass/quartz/ceramic/steel mesh* Larger balance capacities and ranges available

Pressure

Vessel: Pressurised-UHV SS316/SS304assembly

Design pressure: 20 barsDesign temperature: 500°C at pressure

1000°C with quartz reactor (ambientpressure)

Pressure sensors: Up to three per system ranging from 1 mbar to 20 bar

Control accuracy: +/- 0.025% of transducer span (i.e. 0.25 mbars for 1 bar transducer)

Temperature

Sensors: Type K or platinum resistancethermometers

Range: Liquid nitrogen to 1000°CControl accuracy: +/- 0.05% to +/- 1°C depending on

control equipmentACS: 50°C Anti-condensation protection

(IGA-002)

Flow Control (IGA-003)

Flow rate: 500 ml/min (standard configuration)No. of streams: Up to four

Optional balance purge for corrosivegases

Models IGA-001, IGA-002 and IGA-003 IGASORP

I S O C H E M A

Specifications

The Sorption Products RangeIGA-001 Gas sorption studies from vacuum to 20 bar.IGA-002 Vapour sorption studies from vacuum incorporating anti-condensation protection. (Technical Data Sheet 137)IGA-003 Dynamic multi-component gas/vapour sorption incorporating gas flow controller. (Technical Data Sheet 138)IGASORP Benchtop system for analysing the moisture sorption properties of materials. (Technical Data Sheet 143)IGA-PTCS Pressure/flow/temperature control system for upgrading existing microbalances. (Technical Data Sheet 139)IGA-DSMS Mass spectrometer interface for gas analysis can be interfaced to all IGA models. (Technical Data Sheet 140)HP-ABR Automated high-pressure breakthrough rigs for characterization of sorbent materials

Additionally, Hiden can supply stand-alone microbalance systems for vacuum or high pressure with data logging/control software.

If you require further, more detailed information on any of the product range, please request the appropriate Technical DataSheet (provided above) and our experienced staff will be happy to provide these details and discuss your specific experimentalapplications.

IGASORP Moisture Sorption SystemThe IGASORP system is specifically designed to study the moisture sorptionproperties of materials. The system uses the same operating principles as in therest of the IGA range. This system is used to model technological applicationswhere moisture behaves as a critical component in either formulation, productionor storage. The fully automated benchtop analyser offers superior performanceand flexibility than traditional methods of moisture analysis while dramaticallyreducing analysis times.

Typical Application Materials➤ Moisture sorption isotherms ➤ Pharmaceutical formulations➤ Hydration/dehydration studies ➤ Excipients, whole tablets➤ Permeation studies ➤ Packaging materials➤ QA/QC of raw/finished materials ➤ Building materials

IGA-PTCS Pressure/Temperature control systemThe IGA-PTCS system adds a pressure/flow and temperature control interface toexisting microbalance systems. The upgraded system has all the functionality ofthe IGA range including the IGAS applications software. Microbalance systemssuch as Cahn and Sartorious can be easily interfaced providing full automation.The IGA-PTCS components consists of:

➤ Pressure control to 20 bar.➤ Temperature control of a wide variety of furnaces to 1000°C.➤ Four stream mass flow control system.➤ IGAS applications software.

IGA-DSMS Mass Spectrometer systemHiden’s range of mass spectrometers can be interfaced to all of the IGA models.The IGA-DSMS combines the gas and gravimetric analysis techniques to providean invaluable tool in materials characterisation. The system can be used to studythermal decomposition and desorption processes.

➤ Broad AMU range with triple mass filter options.➤ Heated capillary transfer.➤ Bypass pumping arrangement for rapid response time.➤ Automated control from IGAS software.➤ Mobile cart for stand-alone operation.

AccessoriesA complete range of accessories and stand-alone modules are offered to supplycomplete turn-key solutions. These include:

➤ Complete range of furnaces from set-point control to high temperature TGapplications.

➤ Liquid nitrogen control systems.➤ Water baths for stable ambient temperature control.➤ Humidifier module for relative humidity control.➤ Vacuum pumping stations.➤ Stand-alone vacuum/pressure microbalance system with data logging

software.

Gravimetric Analysers for theCharacterisation of the SorptionProperties of Materials.

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

TECHNICAL DATA SHEET 146 Printed in England

Manufactured in England by:

HIDEN ISOCHEMA LTD231 EUROPA BOULEVARDWARRINGTON WA5 7TN ENGLAND

Te l: +44 (0) 1925 244 678 Fax: +44 (0) 1925 244 664

E-Mail: [email protected]: www.hidenisochema.com Certificate No. 17958

0

1000

2000

3000

4000

5000

6000

0 5 10 15 20 25Time (Hours)

Wei

ghtc

hang

e(m

icro

gram

mes

)

Moisture sorption on aspirin/blister pack Permeation of moisture through blister packaging in atmosphere of 90% RH at 30°C

0

0.5

1

1.5

2

2.5

0 10 20 30 40 50 10060 70 80 90

%-RH (%)

Con

cent

ratio

n(w

t-%)

Aspirin

Empty blister

The IGASORP system can be used to determine the moisturesorption properties of pharmaceutical materials. The data aboveshows the comparative reactions for an Aspirin tablet and it’sblister packaging material.

The IGASORP system can be used to study the permeationproperties of packaging materials. Such studies proveinvaluable in determining the effectiveness of storage mediaand the shelf-life of hygroscopic materials.

Weight

Balance Capacity*: 5 gramsWeighing Range*: 100mg/200mg/500mgResolution: 0.1 µg for 100mg rangeLong term stability: Nominal +/- 1 µg/weekSample containers: Glass/steel mesh* Larger balance capacities and ranges available

Humidity

Sensor accuracy: +/- 1% (0-90%RH) +/- 2% (90-100%RH)

Sensor response: 15 seconds to 90% of readingControl range: 0%RH (determined by gas supply)

to 95% RHRegulation accuracy: +/- 0.1% RHGas: Typically dry air or nitrogenMax. flow rate: 500 ml/min

Temperature

Bath thermostat:

Measurement range: 5°C to 85°CAccuracy/stability: +/- 0.05°C to +/- 0.1°C across range

Internal heater for rapid drying:

Max. temperature: 350°CMax. heating rate: 10°C/min

More detailed specifications for the complete IGA range can be obtained from the relevant Technical Data Sheet (see below)

Weight

Balance Capacity*: 5 gramsWeighing Range*: Typically 200 mgResolution: 0.2 µgLong term stability: +/- 1 µgSample containers: Glass/quartz/ceramic/steel mesh* Larger balance capacities and ranges available

Pressure

Vessel: Pressurised-UHV SS316/SS304assembly

Design pressure: 20 barsDesign temperature: 500°C at pressure

1000°C with quartz reactor (ambientpressure)

Pressure sensors: Up to three per system ranging from 1 mbar to 20 bar

Control accuracy: +/- 0.025% of transducer span (i.e. 0.25 mbars for 1 bar transducer)

Temperature

Sensors: Type K or platinum resistancethermometers

Range: Liquid nitrogen to 1000°CControl accuracy: +/- 0.05% to +/- 1°C depending on

control equipmentACS: 50°C Anti-condensation protection

(IGA-002)

Flow Control (IGA-003)

Flow rate: 500 ml/min (standard configuration)No. of streams: Up to four

Optional balance purge for corrosivegases

Models IGA-001, IGA-002 and IGA-003 IGASORP

I S O C H E M A