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A simplified circuit diagram of a thermal conductivity detector.

This detector is part of a typical commercial instrument such as a Micromeritics AutoChem 2920 ( [link] ). This instrument is an automated analyzer with the ability to perform chemical adsorption and temperature-programmed reactions on a catalyst, catalyst support, or other materials.

A photograph of a Micromeritics AutoChem 2920.

Temperature programmed reduction (tpr)

TPR will determine the number of reducible species on a catalyst and will tell at what temperature each of these species was reduced. For example palladium is ordinarily found as Pd(0) or Pd(II), i.e., oxidation states 0 and +2. Pd(II) can be reduced at very low temperatures (5 - 10 °C) to Pd(0) following [link] .

PdO+H 2 Pd(0)+H 2 O MathType@MTEF@5@5@+=faaagCart1ev2aaaKnaaaaWenf2ys9wBH5garuavP1wzZbqedmvETj2BSbqefm0B1jxALjharqqtubsr4rNCHbGeaGqiVu0Je9sqqrpepC0xbbL8FesqqrFfpeea0xe9Lq=Jc9vqaqpepm0xbba9pwe9Q8fs0=yqaqpepae9pg0FirpepeKkFr0xfr=xfr=xb9Gqpi0dc9adbaqaaeGaciGaaiaabeqaamaabaabaaGcbaGaaeiuaiaabsgacaqGpbGaae4kaiaabIeadaWgaaWcbaGaaeOmaaqabaGccqGHsgIRcaqGqbGaaeizaiaabIcacaqGWaGaaeykaiaabUcacaqGibWaaSbaaSqaaiaabkdaaeqaaOGaae4taaaa@3BF0@

A 128.9 mg 1wt% Pd/Al 2 O 3 samples is used for the experiment, [link] . Since we want to study the oxidation state of the commercial catalyst, no pre-treatment needs to be executed to the sample. A 10% hydrogen-argon mixture is used as analysis and reference gas. Argon has a low thermal conductivity and hydrogen has a much higher thermal conductivity. All gases will flow at 50 cm 3 /min. The TPR experiment will start at an initial temperature of 200 K, temperature ramp 10 K/min, and final temperature of 400 K. The H 2 /Ar mixture is flowed through the sample, and past the detector in the analysis port. While in the reference port the mixture doesn’t become in contact with the sample. When the analysis gas starts flowing over the sample, a baseline reading is established by the detector. The baseline is established at the initial temperature to ensure there is no reduction. While this gas is flowing, the temperature of the sample is increased linearly with time and the consumption of hydrogen is recorded. Hydrogen atoms react with oxygen atoms to form H 2 O.

A sample of Pd/Al 2 O 3 in a typical sample holder.

Water molecules are removed from the gas stream using a cold trap. As a result, the amount of hydrogen in the argon/hydrogen gas mixture decreases and the thermal conductivity of the mixture also decrease. The change is compared to the reference gas and yields to a hydrogen uptake volume. [link] is a typical TPR profile for PdO.

tpr
A typical TPR profile of PdO. Adapted from R. Zhang, J. A. Schwarz, A. Datye, and J. P. Baltrus, J. Catal. , 1992, 138 , 55.

Pulse chemisorption

Once the catalyst (1 wt% Pd/Al 2 O 3 ) has been completely reduced, the user will be able to determine how much palladium is active. A pulse chemisorption experiment will determine active surface area, percentage of metal dispersion and particle size. Pulses of hydrogen will be introduced to the sample tube in order to interact with the sample. In each pulse hydrogen will undergo a dissociative adsorption on to palladium active sites until all palladium atoms have reacted. After all active sites have reacted, the hydrogen pulses emerge unchanged from the sample tube. The amount of hydrogen chemisorbed is calculated as the total amount of hydrogen injected minus the total amount eluted from the system.

Questions & Answers

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I start with an easy one. carbon nanotubes woven into a long filament like a string
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what is the function of carbon nanotubes?
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what is nanomaterials​ and their applications of sensors.
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what is nano technology
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what is system testing?
AMJAD
preparation of nanomaterial
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Yes, Nanotechnology has a very fast field of applications and their is always something new to do with it...
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In this morden time nanotechnology used in many field . 1-Electronics-manufacturad IC ,RAM,MRAM,solar panel etc 2-Helth and Medical-Nanomedicine,Drug Dilivery for cancer treatment etc 3- Atomobile -MEMS, Coating on car etc. and may other field for details you can check at Google
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anybody can imagine what will be happen after 100 years from now in nano tech world
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after 100 year this will be not nanotechnology maybe this technology name will be change . maybe aftet 100 year . we work on electron lable practically about its properties and behaviour by the different instruments
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Prasenjit Reply
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the Beer law works very well for dilute solutions but fails for very high concentrations. why?
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Source:  OpenStax, Physical methods in chemistry and nano science. OpenStax CNX. May 05, 2015 Download for free at http://legacy.cnx.org/content/col10699/1.21
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