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Maximum resolution in minimum time!
Pascal SeriesMercury Intrusion Porosimeters
Reservoir rocks
Ceramic Materials
Building materials
Polymers and resins
Pharmaceuticals
Restoration and conservation
Geology
Mining
Part of Thermo Fisher Scientific
s u r f a c e a n a l y s i s
Pascal SeriesM
ercury Intrusion Porosimeters
Maxim
um resolution in m
inimum
time!
Pascal 140, 240 and 440Maximum resolution in minimum time!
The mercury porosimetry technique is one of the most useful methods to investigate the porous structureof solid samples in a quantitative way. It provides reliable information about pore size/volumedistribution, particle size distribution, bulk (envelope) density and specific surface for most porous solids.
Pressurization by Automatic Speed-up and Continuous Adjustment Logic, or, in short Pascal, is aspecial operating principle developed by Thermo Fisher Scientific and used in the new generation ofautomatic mercury porosimeters described herein.
Pascal self-optimizes analysisparametersMercury porosimetry analysis is based onthe measure of the intrusion of mercury intothe pores of the sample at variouspressures. The pressurization procedure iscritical to the accuracy of the analysisbecause a certain equilibrium time isrequired for the mercury to fill the pore ateach pressure. This depends on the externalpore access diameter and on the shape andcomplexity of the pore network. In principleit is impossible to know which pressure rateis the most suitable for the sample as thepore size range and pore shape in differentsolid samples are unknown. An excessivelyhigh pressurization rate gives wrong resultsbecause the pores are not completely filledat the corresponding pressure, whereas alow pressurization rate wastes valuablelaboratory time. The solution is Pascal.
Pascal does it faster than ever!The pressurization starts “softly” and inabsence of penetration increases quickly tothe maximum predetermined speed. Nine (9)different speed characteristics are availablecovering different application fields andanalytical purposes and making it possible tochoose a balance between the scientificquality of the information and the total runtime. When mercury intrusion is detected bythe mercury level detector, the pressurizationimmediately slows down without stoppingcompletely. The acceleration anddeceleration of the pumping system arebalanced to assure a constant pressure overthe sample during the mercury intrusion intothe pores with the same access size, thusproviding proper equilibrium time.
Pascal fits your sampleThe Pascal method automaticallydetermines the correct pressurization speedaccording to the presence of pores and tothe actual mercury penetration rate therebyeliminating dead times during the analysis.This operation is performed at any pressure.The Pascal method combines all thebenefits in one system:• Optimum information quality at every
speed and at every pressure• Highest resolution• Minimum analysis time
Common featuresand benefits of the Pascal Series
Pascal method of pressurizationDecreases run times by up to 30% withoutsacrificing the reliability of the curves anddoes not require any prior knowledge aboutthe sample characteristics.
Extremely high resolutionPascal units can provide curves with up to2500 data points depending on the selectedspeed and sample nature. At this incrediblyhigh resolution the data points on the curveform a continuous line.
Separately selectable speedranges for intrusion andextrusionNine speed ranges are selectable so thatboth sophisticated researchers, who don’twant to miss anything, and those who are ina hurry, as in the case of quality control, canbe satisfied. Decreased speed ranges can beselected independently of increased speedranges to better define the extrusion curveand minimize instrumental hysteresis effects.
On-board microprocessor andmemory data buffer for stand-alone operationThe on-board microprocessor controls allthe instrument functions and collects theexperimental data storing them in a memorybuffer, therefore a PC is not required to runthe Pascal but only for data elaboration. Onthe other hand the whole analysis can beprogrammed and controlled from a PC,which can be disconnected at any timeduring the analysis freeing it for other tasks.The operator can verify the instrumentstatus and can transfer the experimentaldata to the PC to verify the analysis resultsat any time.
One data station – fourinstruments via multi RS232 linkThe instruments are connected to the PCthrough a standard serial RS232 port. Asingle data station can control up to fourinstruments from a serial port (Pascal140/240/440 and the Sorptomatic forexample). Thus a complete MicrostructureLab can be realized minimizing costs andbench space.
Choice of operation via controlpanel or PCBoth the analysis and the instrument can beprogrammed and controlled in real timeeither from an easy-to-use control panelwith liquid crystal display or from thecomputer screen. Thus the instruments canbe operated even if they are not in the sameroom as the data station, as often occurs inQC labs.
Automatic porosimetercalibrationA special calibration kit is available as anoption to verify the calibration of the system.In addition, a number of certified referencematerials are nowadays available toregularly check the instrument performance.
Pascal porosimeters achieveutmost safety certificationsAll Pascal devices are fully CE certifiedaccording to electromagnetic compatibilityand safety. In addition, the high pressuredevices achieved the full PED (PressureEquipment Directive) certification regularlycontrolled by an external certification body.The utmost certified safety and unmatchedanalytical performance are the best addedvalues of these products.
The Pascal 140 has a dual role:it prepares the sample and the
dilatometer for the analysis andcarries out low pressure
porosimetry measurements
Operations are done automatically thus freeing the operator for other tasks. Thanks to its modular concept, it can be used byitself or together with other Pascal porosimeters, thus modularity of the Pascal system features a “buy what you need” approach.Data from the low pressure intrusion can be combined with data from the other high pressure modules (240 or 440) to get acomplete porosity spectrum of the sample.
Pascal SeriesM
ercury Intrusion Porosimeters
Maxim
um resolution in m
inimum
time!
Automated sample preparation,mercury filling and analysisThe sample preparation process is started bydegassing the sample under vacuum for a certaintime. A special proportional valve makes a “softstart” vacuum, avoiding any risk of powderelutriation. The vacuum is measured by a gaugewhose signal is displayed on the instrument controlpanel. When the minimum vacuum is reached, thesystem proceeds with the mercury filling operationup to the required volume level. Finally, theanalysis begins and the pressure is increased fromvacuum at the rate determined by the Pascalsystem. Depressurization (extrusion) starts whenthe maximum pressure is reached and can proceeddown to atmospheric pressure or vacuum. Forpowder samples, a second run can be made toassure there is no aggregation, thus permitting acorrect particle size distribution measurement.
Data collection and analysisThe experimental data are memorized by theon-board microprocessor and kept in theinternal memory buffer. At any time duringthe analysis the operator can check the statusof the analysis and/or transfer the equilibriumdata to the PC. The low pressure analysis canbe performed also simultaneously with thehigh pressure analyses (by the Pascal240/440) on another sample. The Pascal 140is characterized by its high level ofautomation which simplifies the operator’swork and assures a very high reproducibilityof results.
Pascal 140a fully automated low pressure porosimeterand sample preparation unit
Automatic sample degassingAll samples are pre-treated in the same wayregardless of who is operating the equipmentthus improving analytical reproducibility. Aspecial design proportional valve generates anautomatic soft-start vacuum avoiding any risk ofdragging out light powders from the dilatometer.
Digital vacuum gauge to controlsample degassingThe accurate control and display of vacuumduring sample degassing assures that samplesare properly dried before starting the experiment.
Automatic mercury fillingThe amount of mercury introduced in thedilatometer is measured with the utmostaccuracy assuring reliable and reproduciblemeasurements of bulk and apparent densities.
Double run for powdersde-agglomerationPowders can be properly analyzed in terms ofparticle size distribution avoidingagglomeration effects. The first pressurizationrun breaks all the agglomerates while thesecond run provides a penetration curve relatedonly to the real particle size distribution.
Special kit for ultra-macroporeanalysisA special design dilatometer compensates thehydrostatic pressure over the sample andsignificantly increases the pore diameter or theparticle size detectable by the instrument.
Special vacuum circuit withmercury trapSafety is designed into the Pascal 140. Thevacuum circuit can be completely isolated fromthe ambient and the waste outlet can beconnected to an external exhaust system. Anadditional mercury trap prevents anycontamination of the internal tubing.
Simple, easy to handle andinexpensive dilatometersThe five differentdilatometers modelscan accept and measure samples ofvarious dimensionsand shapes. They areeasy to mount and toclean avoiding anycomplexity that makes the operator’s life difficultand leads to errors.
Dilatometer in vertical positionThe vertical position of the dilatometer preventsany mercury spilling during the filling operationand permits a continuous degassing, thusavoiding the risk of air bubble trapping in thedilatometer.
Many reasons to choosePascal 140
Example of analysis with the Ultramacropore Option installed in the Pascal 140
Pascal SeriesM
ercury Intrusion Porosimeters
Maxim
um resolution in m
inimum
time!
PED conformity assures utmostsafety for high pressure devicesPascal porosimeters assure to customers theutmost certified safety and maximum quality.Pascal 240 and 440 models, reaching 200and 400 MPa respectively, are completelycertified according to the PED (PressureEquipment Directive) certification. PED isintended to guarantee essential safetyrequirements to users, and it is appliedaccording to several parameters related tofluids, volume-pressure rates, materials, etc.In the case of Pascal 240 and 440, it isrelevant to all the hydraulic parts submittedto high pressures, specifically the pressuremultiplier, the high pressure inlet pipe andthe two bodies of the autoclave. Thesecomponents have been certified as a system,and single components are regularly verifiedby an official certification institute. Safety isthe best added value of our products.
Pascal 240The Pascal 240 porosimeter operates up tothe maximum pressure of 200 MPa. Its largeautoclave together with the specialelectrode system makes it an extremelyversatile porosimeter as it can accept allthe dilatometers and is thus able tomeasure a wide range of solid materials:homogeneous, heterogeneous, low and highporosity. The accuracy and reproducibilityare the utmost thanks to the Pascal system.
Pascal 440The Pascal 440 is not only the highestpressure model but it also offers the highestspeed of the series. It reaches its maximumpressure of 400 MPa in the same time asthe Pascal 240 reaches its maximum of 200MPa. It is particularly suited for ceramics,sintered metals, very hard materials and, ingeneral, for all the solids which have a
porosity approaching the micropore region.Thanks to its high pressurization speed, it ishighly recommended in QC labs where shortrun times and productivity are the priorities.
Pascal 240 and Pascal 440Speed and resolution to match any requirement
The Pascal 240 and Pascal 440 high pressure porosimeters take over where the Pascal 140 leaves off tomeasure pores down to the lower mesopore region. They incorporate a new pressurization system,developed to meet the sophisticated analytical requirements of laboratories working with modernmaterials. The pressurization system uses a reversible pump operating continuously, which permits aperfect control in increasing/decreasing the pressurization speed, and a new type of pressure multiplier.The key features of this system are the extremely high maximum speed of pressurization and theimmediate acceleration or deceleration response permitting the optimal application of the Pascal systemduring the analysis. The easy-to-use control panel with liquid crystal display permits the unit to beoperated also without a PC. It lets the operator program the analysis or the calibration and provides auseful guide to operate correctly. It shows the analysis status in real time and indicates incorrectoperations by means of error messages.
Automatic autoclaveopening/closingThe motor driven raising/lowering of theautoclave simplifies the operation andcontributes to the userfriendliness of the unit.
Autoclave oil filling by a pumpingsystemThe pumping system reduces the timenecessary to fill the autoclave before theanalysis begins and assures that air bubblesare removed.
Real blank correction The Pascal 240/440 permit a real “blank”analysis, that is a run without any sample.The blank curve is memorized by the datastation and is then automatically subtractedfrom the normal analyses. This preventserroneous interpretations of the sampleporosity due to the presence of “ghost” poreswhich result when the mercury compressionand temperature effect are not taken intoconsideration.
Control panel with liquid crystaldisplayIt informs the user about the instrumentstatus in real time while the analysis isrunning regardless of whether or not the PC isconnected. It increases safety by continuouslymonitoring the piston position and displayingerror messages if anything goes wrong. Thisinformation can also be shown on the PC’sscreen.
Up to 2500 experimental points inevery runThis means an almost limitless curveresolution. When the low and high pressureanalyses are joined the total number of pointscan be even more!
“Hold pressure” functionThe analysis can be stopped on request bythe operator and the pressure is maintainedconstant at the actual value without timelimits. This permits the study of extremelyslow penetration phenomena.
Pascal 240 accepts all typedilatometersThe Pascal 240 is exceptionally versatile dueto its unusually large autoclave which acceptsthe complete range of dilatometers and thuscan analyze practically any kind of sample.
Only 9 minutes to reach themaximum pressureThe incredibly short time required to reach themaximum pressure makes the Pascal 240 andPascal 440 particularly suited for QCapplications where short analysis times andhigh productivity are most important.
The Pascal 240 and 440offer more than meets the eye
BR10086_E 08/07C
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CalculationsBulk and apparent density, total andincremental pore volume, porosity,incremental specific surface area(four models), average pore size (twomodels), pore size distribution(derivative and histograms), particlesize distribution (Mayer-Stowemodel), pore and particle surfacearea distinction.
Available graphsIntrusion/extrusion, pore sizedistribution (cumulative andderivative), particle size distribution(cumulative and percentage), rawdata plot, overlay of multiple curves.
Data printout and reportingPore volume (raw, normalized,incremental and relative), intrusion/extrusion pressure (corrected), poresize (choice of three measuringunits), surface area (normalized,incremental and relative), pore andparticle percentage fraction in userdefined intervals. Reporting can becustomized by user and printed orsaved in different electronic formats(i.e. Excel, text, etc.)
Many ways to look at the data
