A Low-Cost, Rapid Method for Determining Carbon Black Surface Area

1983 ◽  
Vol 56 (2) ◽  
pp. 440-449 ◽  
Author(s):  
Jerry B. Pausch ◽  
Caroline A. McKalen
Keyword(s):  
Carbon Black ◽  
Surface Area ◽  
Low Cost ◽  
Control Procedure ◽  
Simple Method ◽  
Surface Areas ◽  
Measuring Surface ◽  
Headspace Gas ◽  
Black Surface ◽  
Area Data

Abstract For practical use of this method as a quality control procedure for carbon black, a combination of 4 mm3 and 6 mm octane doses appears to be the best compromise for a sample size of 0.1 g. These conditions cover well, a surface area range of 10–140 m2/g and surface areas up to 180 m2/g can be estimated. Larger doses of octane will extend the linear range on the high side, but the slope of the calibration curve is reduced significantly. A smaller slope yields lower precision. The regular testing of standards appears necessary to achieve optimum accuracy of surface area. At the present time, the method is calibrated against nitrogen surface area data, so the advantage of octane more closely simulating the rubber molecule is lost. We need to obtain adsorption isotherms that are better defined throughout the linear adsorption coefficient range for a number of carbon blacks, and thus become self-calibrated against octane. A more versatile dosing technique is preferred to enable these experiments to be run. An alternate approach is to correlate the headspace results with data obtained by other techniques such as CTAB. The advantages of automated headspace gas chromatography for measuring surface area have been outlined before . It is a rapid and simple method, which also exhibits relatively low labor involvement. The number of samples capable of being analyzed per day is significantly higher than by any other technique.

Identification of Carbon Black by Surface-Area Measurements

1943 ◽  
Vol 16 (3) ◽  
pp. 687-691
Author(s):  
F. H. Amon ◽  
W. R. Smith ◽  
F. S. Thornhill
Keyword(s):  
Carbon Black ◽  
Surface Area ◽  
Point Of View ◽  
Curing Temperature ◽  
Single Type ◽  
Surface Areas ◽  
Vulcanized Rubber ◽  
Chemical Combination ◽  
Black Surface ◽  
Rubber Stock

Abstract In general then, we may conclude that carbon black can be recovered from rubber stocks with unchanged surface-area. The nitric acid technique is the most effective method of effecting the separation. The digestion temperature must be controlled to between 60° and 70° C, for a total of not more than 3 to, 4 hours. This method of identifying the carbon black in an unknown rubber stock is directly applicable only in the presence of a single type of carbon black. If blends of blacks are employed in the material under investigation, some secondary identification is also required. The nonimpingement-type blacks, for example, are readily identified by microscopic observation. From the known surface-areas of these materials and the total per cent carbon present in the stock, a fairly positive identification of the blend can be made. The fact that carbon black can be recovered quantitatively and with unchanged surface-area from vulcanized rubber stocks appears to lend impetus to a physical concept of carbon black reinforcement. This point of view implies that any chemical combination between the ingredients of the rubber stock and the carbon black would be evidenced by some alteration in the surface of the latter. A few experiments were performed in an attempt to establish to what extent this concept was valid. One hundred grams of Grade-6 carbon black were intimately mixed with 6.6 grams of sulfur. This is about the ratio in which they are present in a standard rubber batch. Samples of this mixture were subjected to the standard curing temperature of 134° C for 30, 60, and 90 minutes. The free sulfur was then extracted for 40 hours with acetone ,and the combined sulfur on the carbon was determined. Values of 0.16, 0.21, and 0.4 per cent combined sulfur were obtained. The original sample of Grade-6 carbon black had a surface-area of 108 square meters per gram. The extracted sample of black containing 0.4 per cent of combined sulfur had a surface-area of 109 square meters per gram. These values are identical within experimental error. While unaltered surface-area need not necessarily be interpreted as evidence of complete lack of surface reactions, it is the authors' opinion that the extent of chemical combination at the carbon black surface is very small. This interpretation is in accord with the views expressed in a previous publication3, where it was suggested that the chief role of carbon black in rubber reinforcement may rest on its ability to orient the chains of rubber molecules and thus alter the extent and type of rubber-sulfur bonds normally formed in non-reinforced rubber stocks.

scholarly journals Tuning the hierarchical pore structure of graphene oxide through dual thermal activation for high-performance supercapacitor

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Jeongpil Kim ◽  
Jeong-Hyun Eum ◽  
Junhyeok Kang ◽  
Ohchan Kwon ◽  
Hansung Kim ◽  
...  
Keyword(s):  
Graphene Oxide ◽  
Pore Structure ◽  
Specific Capacitance ◽  
Surface Area ◽  
Thermal Annealing ◽  
High Performance ◽  
Annealing Process ◽  
Supercapacitor Electrode ◽  
Simple Method ◽  
Surface Areas

AbstractHerein, we introduce a simple method to prepare hierarchical graphene with a tunable pore structure by activating graphene oxide (GO) with a two-step thermal annealing process. First, GO was treated at 600 °C by rapid thermal annealing in air, followed by subsequent thermal annealing in N2. The prepared graphene powder comprised abundant slit nanopores and micropores, showing a large specific surface area of 653.2 m2/g with a microporous surface area of 367.2 m2/g under optimized conditions. The pore structure was easily tunable by controlling the oxidation degree of GO and by the second annealing process. When the graphene powder was used as the supercapacitor electrode, a specific capacitance of 372.1 F/g was achieved at 0.5 A/g in 1 M H2SO4 electrolyte, which is a significantly enhanced value compared to that obtained using activated carbon and commercial reduced GO. The performance of the supercapacitor was highly stable, showing 103.8% retention of specific capacitance after 10,000 cycles at 10 A/g. The influence of pore structure on the supercapacitor performance was systematically investigated by varying the ratio of micro- and external surface areas of graphene.

Accessibility of the Carbon Black Particle Surface to Elastomers

1970 ◽  
Vol 43 (2) ◽  
pp. 464-469 ◽  
Author(s):  
P. Aboytes ◽  
A. Voet
Keyword(s):  
Carbon Black ◽  
Particle Surface ◽  
Carbon Black Particle ◽  
Carbon Chain ◽  
Chain Structure ◽  
Inert Atmosphere ◽  
Chemical Surface ◽  
Molecular Weights ◽  
Surface Areas ◽  
Black Surface

Abstract Experimental carbon blacks were prepared with the generally encountered slit-shaped pores of discrete dimensions of 9,12.5, and 16 A˚ width in greatly differing size distribution. Equilibrium adsorption in the saturation range was determined in n-hexane for butadiene—styrene elastomers of the SBR type of average molecular weights of 1500; 2000; 15,000; and 300,000. In attempting to correlate the saturation adsorption values with carbon black surface areas, it was found that a simple linear relation in the range investigated could only be obtained by assuming that pores of 9 A˚ width were inaccessible to SBR of 1500 and 2000 MW; that pores of 9 and 12.5 A˚ width were inaccessible to SBR of 15,000 MW; and that all pores smaller than 20 A˚ width were inaccessible to SBR of 300,000 MW. The data indicated that there are no differences between high, regular and low structure blacks in saturation elastomer adsorption under conditions of equivalent dispersion. Equally, upon breaking the persistent carbon chain structure by dry ball milling in an inert atmosphere and equalizing the chemical surface properties by removal of surface oxides, no difference in elastomer adsorption from solution was observed. It must be concluded that commonly used high molecular elastomers do not have any access to smaller carbon black pores. Since access to the surface is a prerequisite for reinforcement, it is obvious that the surface in the pores of carbon black generally does not participate in reinforcing elastomers. The elastomer adsorbed per unit external black surface area appears to be independent of the carbon chain structure, indicating that the so called surface activity of the carbon black is independent of the chain length.

Carbon Black Surface Areas by the Harkins and Jura Absolute Method

1967 ◽  
Vol 40 (5) ◽  
pp. 1305-1310 ◽  
Author(s):  
G. Kraus ◽  
K. W. Rollmann
Keyword(s):  
Particle Size ◽  
Carbon Black ◽  
Surface Area ◽  
Nitrogen Adsorption ◽  
Absolute Method ◽  
Carbon Blacks ◽  
Surface Areas ◽  
Particle Size Determination ◽  
Light Reflectance ◽  
Adsorption Surface

Abstract The Harkins and Jura (HJ) absolute method of surface area determination (Harkins and Jura, J. Am. Chem. Soc. 66, 919, 1944) has been applied to a large number of carbon blacks. Surface area is calculated from the heat of immersion of the solid powder covered by a preadsorbed multilayer of the immersion liquid. For non-porous carbon blacks good agreement with nitrogen adsorption surface areas is obtained, but with porous blacks the HJ method gives smaller values since micropores are filled and bridged over by the pre-adsorbed film. Thus the HJ areas are more nearly representative of particle size and may be used to calibrate indirect methods of particle size determination. An example of this is shown using light reflectance values on dry carbon black and possible complications due to particle size distribution in the use of the reflectance test are discussed.

A Comparison of Methods for Determining Surface Areas of Carbon Black

1973 ◽  
Vol 46 (1) ◽  
pp. 192-203 ◽  
Author(s):  
R. A. Klyne ◽  
B. D. Simpson ◽  
M. L. Studebaker
Keyword(s):  
Carbon Black ◽  
Specific Surface ◽  
Surface Area ◽  
Specific Surface Area ◽  
Surface Areas ◽  
Furnace Black ◽  
Area Increase ◽  
Experimental Errors ◽  
Specific Surface Areas ◽  
Surface Area Increase

Abstract 1. The various tint tests correlate with each other—it does not make much difference which of the three procedures is used. The discrimination between similar blacks is comparable. Specific surface areas obtained by the three methods are comparable and differences appear to be due to experimental errors. (Compare Figures 5–7). 2. Surface areas larger than some 90 to 100 m2/g cannot be reliably determined from tint strength measurements alone. 3. Structure exerts a pronounced effect on tint strength of furnace blacks, especially above 90 to 100 m2/g. Porosity and/or composition are apparently also variables which affect tinting strength. 4. Densichron reflectance on the dry carbon black can be used to estimate specific surface areas up to about 140 m2/g; but, since theabsoluteerrorincreases as the specific surface area increases, this method loses some of its reliability at values above about 110 m2/g. The relative error in reflectance determinations does not vary greatly over the furnace-black range. Densichron reflectance is influenced by composition, evidently due to composition-related differences in optical properties of the carbons. 5. In CTAB adsorption measurements, titration errors and handling errors tend to be rather constant for blacks of different surface area. Hence, CTAB permits better discrimination among blacks of small particle size. 6. The errors in Densichron reflectance surface area increase with specific surface area. Hence, the deviations between CTAB and reflectance surface area which are due to experimental error increase with the surface area of the sample.

Large Surface Area of HMDS Plasma Polymerized Thin Film Used for Production of Miniaturized Structures

2010 ◽  
Vol 636-637 ◽  
pp. 1065-1072 ◽  
Author(s):  
Lilian Marques Silva ◽  
Roberto R. Lima ◽  
E.R. Fachini ◽  
E.W. Simões ◽  
E. Pecoraro ◽  
...  
Keyword(s):  
Thin Film ◽  
Thin Films ◽  
Surface Area ◽  
Preliminary Analysis ◽  
Low Cost ◽  
Large Surface Area ◽  
Polar Organic Compounds ◽  
Organic Mixtures ◽  
Surface Areas ◽  
Good Agreement

The aim of this work was the production of a large surface area of hexamethyldisilazane (HMDS) plasma-deposited thin films and their applicability in a miniaturized structure useful for preliminary analysis of organic mixtures. The HMDS plasma films were produced with different surface areas and morphologies, and all films adsorbed polar and non-polar organic compounds. A low cost miniaturized structure was manufactured in glass using a Milling cutter and covered with HMDS plasma films. Good agreement was observed between simulation and experimental results on those microstructures. The observed different performance between pure and mixtures of organic compound samples suggests that the proposed system is a simple setup that could be useful for rough analysis of a fuel.

scholarly journals A Case Study of Waste Scrap Tyre-Derived Carbon Black Tested for Nitrogen, Carbon Dioxide, and Cyclohexane Adsorption

Molecules ◽  
2020 ◽  
Vol 25 (19) ◽  
pp. 4445 ◽  
Author(s):  
Zuzana Jankovská ◽  
Marek Večeř ◽  
Ivan Koutník ◽  
Lenka Matějová
Keyword(s):  
Activated Carbon ◽  
Carbon Black ◽  
Specific Surface ◽  
Surface Area ◽  
Sorption Capacity ◽  
Specific Surface Area ◽  
Textural Properties ◽  
Pyrolytic Carbon ◽  
Surface Areas ◽  
Wide Range

Waste scrap tyres were thermally decomposed at the temperature of 600 °C and heating rate of 10 °C·min−1. Decomposition was followed by the TG analysis. The resulting pyrolytic carbon black was chemically activated by a KOH solution at 800 °C. Activated and non-activated carbon black were investigated using high pressure thermogravimetry, where adsorption isotherms of N2, CO2, and cyclohexane were determined. Isotherms were determined over a wide range of pressure, 0.03–4.5 MPa for N2 and 0.03–2 MPa for CO2. In non-activated carbon black, for the same pressure and temperature, a five times greater gas uptake of CO2 than N2 was determined. Contrary to non-activated carbon black, activated carbon black showed improved textural properties with a well-developed irregular mesoporous-macroporous structure with a significant amount of micropores. The sorption capacity of pyrolytic carbon black was also increased by activation. The uptake of CO2 was three times and for cyclohexane ten times higher in activated carbon black than in the non-activated one. Specific surface areas evaluated from linearized forms of Langmuir isotherm and the BET isotherm revealed that for both methods, the values are comparable for non-activated carbon black measured by CO2 and for activated carbon black measured by cyclohexane. It was found out that the N2 sorption capacity of carbon black depends only on its specific surface area size, contrary to CO2 sorption capacity, which is affected by both the size of specific surface area and the nature of carbon black.

TEM measurement of surface area of automotive catalysts

1994 ◽  
Vol 52 ◽  
pp. 776-777
Author(s):  
M. H. Yao ◽  
D. R. Liu ◽  
R. J. Baird ◽  
R. K. Usmen ◽  
R. W. McCabe
Keyword(s):  
Electron Microscopy ◽  
Surface Area ◽  
Average Particle Size ◽  
Weighted Average ◽  
Average Particle ◽  
Automotive Catalysts ◽  
Surface Areas ◽  
Measuring Surface ◽  
Major Factors ◽  
Average Size

The specific surface area of supported noble metal particles in an automotive catalyst is defined as the exposed surface area per unit mass of these particles. It is of great importance to know this parameter, since this is one of the major factors that determine the effectiveness of the catalyst. Commonly used methods for characterizing catalysts, such as X-ray diffraction and TEM, do not directly provide a measure of surface area, but, instead, provide a measure of the “average size” of supported particles. Moreover, the “average sizes” obtained from different experimental techniques are often not comparable. Furthermore, many previous electron microscopy catalyst studies measured only simple average particle size, and no detailed procedure for measuring area-weighted average size or surface area appear to have been reported.In the current study, a procedure for measuring surface area of supported particles by transmission electron microscopy(TEM) was developed, and applied to measure surface areas of various production three-way automotive catalysts.

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