QUANTACHROME QUADRASORB Si

SURFACE AREA & PORE SIZE ANALYZER

TM

© 2008 Quantachrome Corporation 0408 07160 Rev.B

QUADRASORB SI
™

Quantachrome's QUADRASORB SI Surface Area and Pore Size Analyzer is designed to

satisfy busy laboratory needs for high analytical throughput , without sacrificing precision,
flexibility or cost-effectiveness. Up to four simultaneous and independent (SI) analysis
ports remove the limitations of single dewar systems allowing samples to be started as
soon as previous measurements are completed. This measurement flexibility has never
before been available in such a compact and cost-effective package.

QUADRASORB™ SI for standard applications
• Fully automated, multi-sample port analyzer for surface area, pore volume and pore
size measurements. Available with four, three or two sample stations.

• Each of the analysis ports includes separate and independent Dewar (coolant flask),
1000 torr pressure sensor and Po (adsorbate saturated vapor pressure) measurement
station for simultaneous measurements yielding maximum throughput and flexibility.

• Each of the analysis ports includes RTD coolant level sensor to maintain a constant,
small cold-zone for maximum sensitivity. Long life Dewar flasks for measurements
exceeding 30 hours.

• Each analysis port can be independently programmed with different analyses and
measurement conditions and new samples can be started on each port as prior
measurements are completed with little, or no, delay to other samples already
in progress.

• Choose from two measurement techniques: Patented NOVA helium-free method and
classical helium void-volume method. Designed for analyses using many different gases,
including nitrogen, argon, carbon dioxide, krypton, etc.

• Multiple gas dosing methods to optimize analysis time and resolution: 1. MaxiDose ™
automatically adjusts dose size in response to sample demand; 2. Constant Dose Volume
(0.1 - 10 cc per data point); and 3. Delta Volume™ which adds data points in regions
of large uptake so critical pore filling is never missed.

• Low maintenance, vacuum-volumetric system with temperature monitored dosing

manifold. High vacuum/low pressure version available (see below).
®
• Windows -based QuadraWin ™ software provides for instrument control and a
comprehensive range of classical and modern models for reporting surface area and
pore size.

• Wide range of separately supplied sample preparation devices (Degassers) to meet

the need of any laboratory (See page 4).

Krypton/Micropore option for low surface area and

micropore measurements
• All of the functions of the standard model QUADRASORB SI; includes low pressure
(10 torr) sensor and turbo-molecular vacuum pump. Available with optional oil-free
roughing pump.

• Performs krypton gas sorption measurements for very low surface area determination,
eg. pharmaceutical actives, powdered metals, etc. on any or all samples stations.

• Capable of low pressure adsorption data (as low as 4 x 10-5 P/Po) necessary for
more complete characterization of microporous materials, eg. zeolites, activated
carbons, molecular sieves, etc.


 QUADRASORB SI
™

TM
QuadraWin - Software

The Quadrasorb SI analyzer is microprocessor

TM

Transparent blue cover protects

sample stations and Dewars during controlled, and communicates with a Windows® Vista,
analysis operation. Opens vertically 2000 or XP-based PC utilizing Quantachrome’s
for easy access to analysis stations
state-of-the-art, data acquisition and data reduction
software, QuadraWin . A 21CFR Part 11 compliant
TM

Up to four sample stations, software version is available for the pharmaceutical

each with coolant level
sensor and Po cell industry.

State-of-the-art
The QuadraWin software is powerful and user friendly.
Automated, independent
QuadraWin is superior for data reduction, incorporat-
dewar elevators ing the latest DFT (Density Functional Theory)
models. The software guides you through analysis
setup, data reduction, graphs and report printouts.
Communication port for PC During operation one can view the accumulated data,
control via Windows®-based the isotherm and all associated graphs and analyti-
software
cal results up to that point. After a run, reports and
graphs are printed automatically or you can use the
software to determine the best fitting method, to
Lower front panel opens to compare data by overlaying curves or to adjust graph,
provide unrestricted access for
Dewar placement, maintenance size, scaling, titles, plot markers and line colors for best
and clean-up print out.

Analysis Specifications
Transducer Accuracy: 0.11% full scale (1000 torr transducer) each
manifold/sample station

Pressure Resolution: 0.15% reading (10 torr transducer - optional)

manifold

Sensitivity: <1 x 10-7 moles adsorbed/desorbed gas

Multiple graphs show isotherm and related plots
Ultimate Vacuum: 1x10-3 torr achieved by dedicated 2 stage rotary,
direct drive pump
1x10-9 torr achieved by turbo-molecular vacuum Data presentation
pump in QUADRASORB SI - KR/MP A comprehensive range of ­surface area and pore size
methods is available:
Adsorbate: Nitrogen or any other non-corrosive gas
with appropriate coolant • Adsorption and desorption isotherms.
• Multi- and single point BET surface area.
2 • Langmuir surface area.
Surface Area Range: 0.01m /g to no known upper limit (nitrogen)
2
0.0005 m /g to no known upper limit (krypton)KR/MP- • Mesopore size distributions (BJH and DH methods).
model only • t-method by deBoer, Halsey, carbon black (STSA).
• Alpha-s and MP micropore methods.
Pore Volume: Detectable limit less than 0.0001 cc/g • Total pore volume, and average pore size.
• Dubinin-Radushkevich (DR) micropore surface area.
Pore Size Range: 3.5 - 4000Å / 0.35 - 400 nm • Horvath-Kawazoe,(HK) Dubinin-Astakhov(DA) and
Saito-Foley (SF) micropore methods.
Coolant Level: Automatic compensation by RTD coolant level sensor
• Extensive Density Functional Theory (DFT) library
Minimum P/P0 (N2): 1 x 10-3 QUADRASORB SI for unified micro- and mesopore analysis using N2,
4 x 10-5 QUADRASORB SI -KR/MP Ar and CO2.
• Fractal dimension by Frenkel-Halsey-Hill(FHH) or
Neimark-Kiselev (NK) models.
* Pressure transducer and vacuum pump specifications from their respective manufacturers.
QUADRASORB SI
™

Sample Preparation: Degassers

Consistent and reliable surface area results depend upon proper sample preparation procedures. In terms of B.E.T. analysis, the limiting
step in rate of throughput is often sample preparation. The complete degassing of samples can often require several hours, while surface
area measurements may require as little as eight minutes.
Quantachrome manufactures several models of degassers to fulfill your sample preparation needs. These degassers provide a virtually
continuous supply of properly prepared samples for the QUADRASORB SI Surface Area and Pore Size Analyzer.

Autosorb Degasser The FloVac™ Degasser

The gold-standard in sample prepa- The FloVac provides cost effective vacuum
ration for physisorption analyzers. degassing. Complete with single-zone
Individual temperature control and heater (to 400°C), digital temperature
ramp rates for all six stations, plus controller and built-in digital vacuum
optional use of heater timers. Built- gauge. Each sample station has its own
in cold trap for efficient removal adjustable evacuation/backfill rate control.
of condensables at low degassing Flow degassing is also possible and can be
temperatures and for clean vacuum. advantageous in removing large quantities
of moisture prior to vacuum degassing.
Vacuum pump included. Turbo-
Individual cooling stations. Vacuum pump
pumped version available for rapid
not included.
high-vacuum degassing.

MasterPrep™ Degasser  Flow Degasser

Fully featured preparation unit. The popular Flow Degasser has the
Individually heated stations with same heating and cooling features as
programmable heating profiles for R&D, the FloVac but without vacuum
commercial labs and multi-user labora- capability. Ideal for quality control
tories. Dual modes (vacuum or flow) applications, teaching and start-up
for further flexibility and optimization. labs. Each sample station has its own
Temperature control and logging via adjustable flow rate control.
PC software (included). Integral cooling

stations provide additional convenience.
Vacuum pump not included.

Features Flow Degasser FloVac Degasser MasterPrep Autosorb Degasser

Number of sample ports: 6 6 6 6

Separate temperature control All ports at All ports at Yes - with Yes - with independent
for each sample port: same temperature same temperature independent ovens heating mantles

Temperature ramping: No No Yes - up to 20 steps, Yes - with manual

independent for each adjustment, independent
sample port for each sample port

Heating timer: No No Yes Yes

Software ramp control: No No Yes No
Analog ramp control: No No No Yes
Vacuum degas mode: N/A Yes Yes Yes
Vacuum display: N/A Yes Yes Yes
Flow degas mode: Yes Yes Yes No
Maximum temperature: 400°C 400°C 425°C 350°C (450°C with
optional quartz mantles)
Cold trap: N/A No No Yes
Vacuum pump: N/A Sold separately Sold separately Included
(turbo pump optional)
QUADRASORB SI
™

Physical Specifications The Gas Sorption Process

Dimensions: Height: 29.0 inches (73.6 cm) Before performing gas sorption experiments,
Height Open: 44.0 inches (111.6 cm) solid surfaces must be freed from contami-
Width: 25.1 inches (63.7 cm) nants such as water and oils. Surface cleaning
Depth: 21.0 inches (53.3 cm) (degassing) is most often carried out by
Depth Open: 26.2 inches (66.5 cm) placing a sample of the solid in a glass cell
and heating it under vacuum or flowing gas.
Weight: 54.4 kg (120 lbs.) Figure 1 illustrates how a solid particle
containing cracks, orifices and pores of
Electrical: 100 - 240 VAC, 50/60 Hz different sizes and shapes might look after
pretreatment. 1 A section of one greatly
Environmental: 10 - 38°C operating range at enlarged particle of a solid.
90% maximum relative humidity Once clean, the sample is brought to a
constant temperature by means of an
external bath. Then, small amounts of a gas
(the adsorbate) are admitted in steps into
Accessories the evacuated sample chamber. Gas
molecules that stick to the surface of the
solid (adsorbent) are said to be adsorbed
Regulator Assembly and tend to form a thin layer that covers
Proper Quadrasorb functioning is assured the entire adsorbent surface. Based on the 2
when high-quality gas regulators are used. well-known Brunauer, Emmett and Teller The monolayer
Quantachrome supplies complete assemblies (B.E.T.) theory, one can estimate the number of adsorbed
which include two-stage regulators with dual of molecules required to cover the adsor- molecules; typically
gauges, cylinder connector, isolation valve bent surface with a monolayer of adsorbed 15 - 20% saturation.
and 1/8" gas line connector. The regulators molecules, Nm (Figure 2). Multiplying Nm
feature stainless steel, non-venting diaphragms by the cross-sectional area of an adsorbate
and the appropriate CGA fitting for specific molecule yields the sample’s ­surface area.
gases. Different assemblies are available for
nitrogen (and other inerts including helium), Continued addition of gas molecules beyond
hydrogen, carbon monoxide, oxidizing gases monolayer formation leads to the gradual
etc. stacking of multiple layers (multilayers).
The formation occurs in parallel to capillary
Vacuum Pump (standard applications). condensation (Figure 3). The latter process is
approximately described by the Kelvin equa-
All vacuum-volumetric gas sorption analyzers
tion, which relates equilibrium gas pressure
require a good vacuum pump and the Quadrasorb- 3 The multilayer capillary condensation
to the size of capillaries capable of condens-
SI is no exception. The pump shall have the stage approximately 70% ­saturation.
ing gas within them.
capability to pull an ultimate vacuum of 10 millitorr
or below. Quantachrome can supply the correctly As the equilibrium gas pressure
sized pump complete with oil, hoses and fittings. approaches saturation, the pores largely
You are not required to purchase the necessary completely fill with adsorbate (Figure 4).
vacuum pump from Quantachrome, but if you do Knowing the density of the adsorbate, one
the entire system will have been qualified in our can calculate the volume it occupies and,
factory as a set, ensuring consistent performance. consequently, the total pore volume of the
sample. If at this stage one reverses the
Vacuum Pumps (krypton/micropore model). adsorption process by withdrawing known
Low pressure applications require a deeper amounts of gas from the system in steps, 4
vacuum that can only be achieved by a turbo- desorption isotherms are generated. The Total pore volume
molecular pump. The turbo pump is included, resulting ­hysteresis leads to isotherm shapes filling; approximately
and the correct backing pump can be supplied by that can be mechanistically ­related to those 100% ­saturation.
Quantachrome either as a rotary oil pump or as expected from particular pore‑shapes.
an oil-free, dry diaphragm (membrane) pump.
Older calculation methods such as the one Modern pore size models are based on
by Barrett, Joyner and Halenda (B.J.H.) allow Non-local Density Functional Theory
Storage Dewars the computation of pore sizes from equilib- (DFT)- a statistical mechanics approach
For the convenience of having larger quantities rium gas pressures. One can therefore take that allows one to describe the sorption
of liquefied gases on hand, Quantachrome offers experimental curves (isotherms) of adsorbed of gas molecules in nanoporous materials
storage dewars in sizes ranging from 5 liters to gas volumes versus relative ­pressures and at a molecular level. Hence, the application
convert them to cumulative or differential of such microscopic methods produces
30 liters, plus a transfer device and trolley for the
pore size ­distributions. the most accurate surface area and pore
largest size.
size results.
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Our policy of continuous development may cause the information and specifications contained herein to change without notice or liability. © 2008 Quantachrome Corporation 0408 07160 Rev.B