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Samples are placed in glass cells to be degassed and analyzed by the BET machine. Glass rods are placed within the cell to minimize the dead space in the cell. Sample cells typically come in sizes of 6, 9 and 12 mm and come in different shapes. 6 mm cells are usually used for fine powders, 9 mm cells for larger particles and small pellets and 12 mm are used for large pieces that cannot be further reduced. The cells are placed into heating mantles and connected to the outgas port of the machine.

After the sample is degassed, the cell is moved to the analysis port ( [link] ). Dewars of liquid nitrogen are used to cool the sample and maintain it at a constant temperature. A low temperature must be maintained so that the interaction between the gas molecules and the surface of the sample will be strong enough for measurable amounts of adsorption to occur. The adsorbate, nitrogen gas in this case, is injected into the sample cell with a calibrated piston. The dead volume in the sample cell must be calibrated before and after each measurement. To do that, helium gas is used for a blank run, because helium does not adsorb onto the sample.

Schematic representation of the BET instrument. The degasser is not shown.

Shortcomings of bet

The BET technique has some disadvantages when compared to NMR, which can also be used to measure the surface area of nanoparticles. BET measurements can only be used to determine the surface area of dry powders. This technique requires a lot of time for the adsorption of gas molecules to occur. A lot of manual preparation is required.

The surface area determination of metal-organic frameworks

The BET technique was used to determine the surface areas of metal-organic frameworks (MOFs), which are crystalline compounds of metal ions coordinated to organic molecules. Possible applications of MOFs, which are porous, include gas purification and catalysis. An isoreticular MOF (IRMOF) with the chemical formula Zn 4 O(pyrene-1,2-dicarboxylate) 3 ( [link] ) was used as an example to see if BET could accurately determine the surface area of microporous materials. The predicted surface area was calculated directly from the geometry of the crystals and agreed with the data obtained from the BET isotherms. Data was collected at a constant temperature of 77 K and a type II isotherm ( [link] ) was obtained.

The structure of catenated IRMOF-13. Orange and yellow represent non-catenated pore volumes. Green represents catenated pore volume.
The BET isotherms of the zeolites and metal-organic frameworks. IRMOF-13 is symbolized by the black triangle and red line. Adapted from Y.S. Bae, R.Q. Snurr, and O. Yazaydin, Langmuir , 2010, 26 , 5478.

The isotherm data obtained from partial pressure range of 0.05 to 0.3 is plugged into the BET equation, [link] , to obtain the BET plot ( [link] ).

BET plot of IRMOF-13 using points collected at the pressure range 0.05 to 0.3. The equation of the best-fit line and R 2 value are shown. Adapted from Y.S. Bae, R.Q. Snurr, and O. Yazaydin, Langmuir , 2010, 26 , 5479.

Using [link] , the monolayer capacity is determined to be 391.2 cm 3 /g.

Now that X m is known, then [link] can be used to determine that the surface area is 1702.3 m 2 /g.

Bibliography

  • B. H. Davis, J. Phys. Chem. , 1986, 90 , 4702.
  • K. S. Sing, Langmuir , 1987, 3 , 2.
  • Brunauer-Emmett-Teller (BET) Surface Area Analysis and Barrett-Joyner-Halenda (BJH) Pore Size and Volume Analysis , Testing and Analysis Techniques. CERAM.
  • S. Brunauer, L. S. Deming, W. E. Deming, and E. Teller, J. Am. Chem. Soc. , 1940, 62 , 1723.
  • S. Brunauer, P. H. Emmett, and E. Teller, J. Am. Chem. Soc. , 1938, 60 , 309.
  • Y. S. Bae, R. Q. Snurr, and O. Yazaydin, Langmuir , 2010, 26 , 5475.

Questions & Answers

What fields keep nano created devices from performing or assimulating ? Magnetic fields ? Are do they assimilate ?
Stoney Reply
why we need to study biomolecules, molecular biology in nanotechnology?
Adin Reply
?
Kyle
yes I'm doing my masters in nanotechnology, we are being studying all these domains as well..
Adin
why?
Adin
what school?
Kyle
biomolecules are e building blocks of every organics and inorganic materials.
Joe
anyone know any internet site where one can find nanotechnology papers?
Damian Reply
research.net
kanaga
sciencedirect big data base
Ernesto
Introduction about quantum dots in nanotechnology
Praveena Reply
what does nano mean?
Anassong Reply
nano basically means 10^(-9). nanometer is a unit to measure length.
Bharti
do you think it's worthwhile in the long term to study the effects and possibilities of nanotechnology on viral treatment?
Damian Reply
absolutely yes
Daniel
how to know photocatalytic properties of tio2 nanoparticles...what to do now
Akash Reply
it is a goid question and i want to know the answer as well
Maciej
characteristics of micro business
Abigail
for teaching engĺish at school how nano technology help us
Anassong
Do somebody tell me a best nano engineering book for beginners?
s. Reply
there is no specific books for beginners but there is book called principle of nanotechnology
NANO
what is fullerene does it is used to make bukky balls
Devang Reply
are you nano engineer ?
s.
fullerene is a bucky ball aka Carbon 60 molecule. It was name by the architect Fuller. He design the geodesic dome. it resembles a soccer ball.
Tarell
what is the actual application of fullerenes nowadays?
Damian
That is a great question Damian. best way to answer that question is to Google it. there are hundreds of applications for buck minister fullerenes, from medical to aerospace. you can also find plenty of research papers that will give you great detail on the potential applications of fullerenes.
Tarell
what is the Synthesis, properties,and applications of carbon nano chemistry
Abhijith Reply
Mostly, they use nano carbon for electronics and for materials to be strengthened.
Virgil
is Bucky paper clear?
CYNTHIA
carbon nanotubes has various application in fuel cells membrane, current research on cancer drug,and in electronics MEMS and NEMS etc
NANO
so some one know about replacing silicon atom with phosphorous in semiconductors device?
s. Reply
Yeah, it is a pain to say the least. You basically have to heat the substarte up to around 1000 degrees celcius then pass phosphene gas over top of it, which is explosive and toxic by the way, under very low pressure.
Harper
Do you know which machine is used to that process?
s.
how to fabricate graphene ink ?
SUYASH Reply
for screen printed electrodes ?
SUYASH
What is lattice structure?
s. Reply
of graphene you mean?
Ebrahim
or in general
Ebrahim
in general
s.
Graphene has a hexagonal structure
tahir
On having this app for quite a bit time, Haven't realised there's a chat room in it.
Cied
what is biological synthesis of nanoparticles
Sanket Reply
what's the easiest and fastest way to the synthesize AgNP?
Damian Reply
China
Cied

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Source:  OpenStax, Nanomaterials and nanotechnology. OpenStax CNX. May 07, 2014 Download for free at http://legacy.cnx.org/content/col10700/1.13
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