BET surface area measurement of commercial magnesium stearate by krypton adsorption in preference to nitrogen adsorption

2019 ◽  
Vol 568 ◽  
pp. 118522 ◽  
Author(s):  
Darren P. Lapham ◽  
Julie L. Lapham
2019 ◽  
Vol 397 ◽  
pp. 161-168 ◽  
Author(s):  
Naouel Hezil ◽  
Mamoun Fellah ◽  
Ridha Djellabi ◽  
Mohamed Zine Touhami ◽  
Alex Montagne ◽  
...  

The hydrophilic-hydrophobic surface area of alumina powder (Al2O3) oxidized at different temperatures was determined on the base of adsorption of water and butane vapor at 25°C. In the order to study the influence of thermal oxidation upon hydrophilic/hydrophobic character of the surface, samples of Al2O3 were characterized using granulometry, SEM and BET surface area measurement. SEM results showed that the thermal treatment does not affect the morphology of the Alunima. However, the increase of treatment temperature from 250 to 900°C results in changing of the hydrophilic-hydrophobic balance of Al2O3 surface.


1975 ◽  
Vol 15 (02) ◽  
pp. 111-116 ◽  
Author(s):  
E.C. Donaldson ◽  
R.F. Kendall ◽  
B.A. Baker ◽  
F.S. Manning

Abstract The Bartlesville Energy Research Center of the U. S. Bureau of Mines bas developed a method for determining the surface area of geologic materials. A gas chromatograph is used to measure the amount of nitrogen adsorbed on the samples from which the surface areas are computed. The results are compared to surface areas calculated from the Kozeny-Carman equation using Carman's textural factor of 5.0. Excellent agreement is obtained for spherical glass beads and crushed sand. However, the ratio of the surface areas of live homogeneous sandstones obtained by nitrogen adsorption to that determined by the Kozeny-Carman equation ranged from 26 to 43. Hence, gas adsorption should be used for surface area measurements of geologic materials. Introduction The U. S. Bureau of Mines is investigating the adsorption properties of organic compounds on geologic materials at subsurface conditions to determine the migration patterns of waste chemical compounds injected into deep wells. The surface area of the adsorbent is one of the important parameters in the study of adsorption. A search of parameters in the study of adsorption. A search of the literature revealed that very little work on the surface areas of geologic materials has been reported. Brooks and Purcell and Tignor et al. reported surface areas of a few sandstones. They also compared their nitrogen-adsorption surface area measurements to results calculated from the Kozeny-Caman equation and noted a wide discrepancy. These data were insufficient to satisfy the needs of this research problem; therefore, several methods for determining surface area by nitrogen adsorption were studied to selected or devise by modification, a method suited for routine measurement of surface areas. Brooks and Purcell used a static, or pressure-volume, system to measure the surface area pressure-volume, system to measure the surface area of geologic materials. More recently, Nelsen and Eggertsen discussed a continuous-flow apparatus that utilized the principles of gas-liquid chromatography for the surface-area measurement of catalysts. The latter method seemed best suited for routine analysis because it does not require the long periods of evacuation, with attendant experimental error, that are inherent in the static system. A Perkin-Elmer Model 154-D gas-liquid chromatograph was modified to provide the continuous-flow system used in this research. APPARATUS AND PROCEDURE The determination of the surface area of catalysts is explained in detail in the literature. The principles are reiterated here to clarify the modifications of Nelson and Eggertsen's apparatus that were made to simplify and adapt the process to the determination of surface areas of porous geologic materials. The procedure involves measuring the nitrogen physically adsorbed as a monolayer on the surface physically adsorbed as a monolayer on the surface of the rock at the liquefaction temperature of nitrogen. Using the theory developed by Brunauer et al., the adsorbed nitrogen is related to the concentration (or partial pressure) of nitrogen.(1)p 1 (C-1)p---------- = ------- + ---------V(po-p) VmC VmCpo A plot of p/V (po-p) vs p/po yields a straight line having intercept 1/VmC and slope C-I/VmC, from which Vm can be determined. The surface area is then given by(2)VmpgN A N2 10-20A = ------------------s M The only data that must be determined experimentally are the volumes of gas (V), adsorbed on the interstitial surface of the rock at several pressures (p). A schematic diagram of the converted Model 154 chromatograph is shown in Fig. 1. SPEJ P. 111


2017 ◽  
Vol 6 (3) ◽  
pp. 207
Author(s):  
Y.H. Taufiq-Yap ◽  
A. Raslan ◽  
R. Irmawati

<p>Vanadyl pyrophosphate (VO)<sub>2</sub>P<sub>2</sub>O<sub>7</sub> catalysts synthesized via VOPO<sub>4</sub>·2H<sub>2</sub>O were investigated by using BET surface area measurement, X-ray Diffraction (XRD), Scanning Electron Microscope (SEM), and Temperature-Programmed Techniques (TPD and TPRS). H<sub>3</sub>PO<sub>4</sub> and H<sub>4</sub>P<sub>2</sub>O<sub>7</sub> were used as the phosphorus source. Only pyrophosphate phase was observed for both final catalysts after 75 hours of calcination in a reaction flow of <em>n</em>-butane/air mixture (0.75% <em>n</em>-butane/air). However, catalyst derived from H<sub>4</sub>P<sub>2</sub>O<sub>7</sub> based preparation (denoted VPD<sub>pyro</sub>) exhibit better crystallinity and slightly higher BET surface area compared to the H<sub>3</sub>PO<sub>4</sub> based preparation (denoted VPD<sub>ortho</sub>). The nature of the oxidants for both catalysts was investigated by O<sub>2</sub>-TPD. For VPD<sub>pyro</sub>, TPD showed an oxygen peak maximum at 986 K and a shoulder at 1003 K, whereas for VPD<sub>ortho</sub>, the oxygen was desorbed as two peaks maxima at 966 and 994 K. The total amount of oxygen desorbed thermally from VPD<sub>pyro</sub> (3.60×10<sup>20</sup> atom×g<sup>-1</sup>) is higher than that obtained for VPD<sub>ortho</sub> (3.07×10<sup>20</sup> atom×g<sup>-1</sup>). VPD<sub>pyro</sub> displayed a slightly improved activity and selectivity for <em>n</em>-butane oxidation. A proper amount of V<sup>5+</sup> species may have an effect on the enhancement of the catalytic activity.</p>


2015 ◽  
Vol 1113 ◽  
pp. 534-538
Author(s):  
Ku Halim Ku Hamid ◽  
Kamariah Noor Ismail ◽  
Adilah Jamaludin ◽  
Muhammad Aslam Zainudin ◽  
Muhammad Syafiq Md Nasruddin ◽  
...  

The effects of calcinations temperature toward physical properties of ZSM-5 were determined by treatment with different temperature for 24 hour. The main properties of these samples were characterized by means of XRD, FTIR, BET surface area measurement and TGA. The hydrothermal treatments were carried out at various temperature of 200°C-500°C. The content in the natural granite sample were also performed .Throughtout this experiment, from the XRD and FTIR analysis the natural granite samples shows the existing of zeolite component which is SiO2 and aluminium oxide.


2017 ◽  
Vol 895 ◽  
pp. 69-72 ◽  
Author(s):  
Hilman Imadul Umam ◽  
Akfiny Hasdi Aimon ◽  
Ferry Iskandar

The effect of microwave-heating on the morphology and surface area of NaX zeolite was studied. The characteristics of NaX zeolite, which has a porous structure, make NaX zeolite applicable as a catalyst. Generally, the process of NaX zeolite formation with an FAU-type structure, either naturally or synthetically, requires quite a long time. Therefore, in this research the effect of microwave heating on the produced sample was investigated using XRD, SEM, and BET surface area measurement. The heating time parameter was varied to determine the optimal conditions for the synthesis of NaX zeolite. The results indicated that microwave-heating is capable of accelerating the crystallization process and reduce the agglomeration of NaX zeolite, as shown by the XRD and SEM results. Based on the SEM result, the particle size distributions of the samples microwave-heated for 1, 3, and 5 minutes, were 350.5, 262.5, and 243.9 nm respectively. In addition, prolonging the microwave-heating time made the surface area of the samples become larger. The specific surface area of the samples microwave-heated for 1, 3, and 5 minutes, 55.9, 153.5, and 204.1 m2/g respectively.


2006 ◽  
Vol 4 (1) ◽  
pp. 25
Author(s):  
Woraratana Pattarapaprakorn ◽  
Makoto Tono ◽  
Hiro Niyama

A simple module for surface area measurement based on CO2 adsorbtion.at dry-ice methanol temperrature was designed. The designed consists a sample tube, a glass syiringe for pressure measurement, and an anspirator for evacuation. No shopiscate electronic de w used. Dry ice was used Dry ice was coolent in place of liquid nitrogen, which is widely wed in ordinary BET surface area measument. Vacuum tighess w confied acceptable when cooking oil was used a seal liquid at the contact suace of the singe. Error anaIes were done for both vacuum tighness and the prence of riduaI gases due to the use of water-driven aspiration. Adsorbtion measurements of CO2 were conducted using the simple module and a conventional apparatus. Results confirmed that the modue works well within reasonable eximental error, if the weight of sampIe and the initial intake of sample gas are chosen properly. However since the adsorption isotherms of several carbon samples shawed a pleteau at high preure, the BET equation was not applicble. Instead, the Langmuir one-point method would be rocommended for sudface area mesurement.


2009 ◽  
Vol 24 (2) ◽  
pp. 448-451 ◽  
Author(s):  
Boyan Yuan ◽  
Mei Yang ◽  
Hongmin Zhu

Titanium nitride nanopowders were synthesized through a chemical reduction of titanium tetrachloride by sodium in liquid ammonia. The products of the reaction were the mixture of sodium chloride and titanium nitride nanopowders. The mixture was then separated by ammonia extraction. The nanopowders were heated under vacuum up to 1200 °C and were characterized by x-ray diffraction (XRD), transmission electron microscopy (TEM), Brunauer-Emmet-Teller (BET) surface area measurement, and chemical analysis. The results show that the product is nanocrystalline cubic phase TiN with Ti/N atomic ratio performed 1:1, and the surface area is from 20 to 50 m2 ·g−1 depending on the heating temperature. The particle sizes estimated by the TEM analysis correspond well with the results of the surface area measurements. The XRD pattern indicates that the crystal size grows with an increase in heating temperature.


Sign in / Sign up

Export Citation Format

Share Document