Determination of Total Moisture in Carbon Blacks

1930 ◽  
Vol 3 (2) ◽  
pp. 340-341
Author(s):  
G. M. Carson

Abstract IN THE course of an extended research on various grades of carbon black, determinations of total moisture were made by an adaptation of an old method. The method used was similar to one described by Allen and Jacobs (1) for measuring water in tar. The chief difference in the present method is that small amounts of moisture in carbon blacks must be weighed, whereas the larger amounts in tar could be measured. The difficulties in weighing the evolved moisture are described in the ensuing method of determination. Five grams of carbon black were placed in a 500-cc. round-bottom flask with 25 to 35 cc. of dry xylene and 200 cc. of dry mineral oil. A short air condenser led to the bottom of a 25-cc. distilling flask, which in turn was connected to two or more calcium chloride tubes. The flask containing the sample was heated to 150-175° C. in an oil bath, a stream of dry nitrogen being passed through the apparatus. The water and xylene were distilled into the small distilling flask and thence, by warming in a water bath, into the calcium chloride tubes, the current of nitrogen being continued. It required but a few minutes to remove the water from the xylene, indicated by the disappearance of cloudiness, and the calcium chloride tubes were then connected directly to the nitrogen line and the gas was passed through until the tubes reached constant weight. ylene is not adsorbed by calcium chloride and nitrogen does not remove water from it at room temperature during the time required for the experiment. The increase in weight of the calcium chloride tubes is the amount of water in the sample of carbon black. The amount of water thus determined is considerably higher than the 105° C. oven loss in 5 hours, and indicates that most of the moisture is of the “bound” or “capillary” type.

1986 ◽  
Vol 59 (3) ◽  
pp. 497-511 ◽  
Author(s):  
E. M. Dannenberg

Abstract It has been seen from the above survey that a few of the treadwear predictor correlations have the required accuracy to provide a satisfactory alternative to road testing of tires for the wear performance of carbon blacks, depending on requirements and circumstances. Correlations based on laboratory rubber testing of rubber mixes and tread compounds are to be preferred over those based solely on carbon black colloidal and morphological measurements. In the author's opinion, Cotten and Dannenberg's correlation of treadwear index with Angle Abrasion measurements of 30 phr compounds and heated bound rubber, and Westlinning and Wolff's correlation with rebound resilience, and the Monsanto Rheometer determination of αF are satisfactory in most instances for the prediction of the treadwear index behavior of carbon blacks.


Author(s):  
Evgeny N. Egorov ◽  
Nikolay I. Kol'tsov ◽  
Nikolay F. Ushmarin

The article investigated the influence of various technological additives (zincolet BB 222, lubstab-01 and MA-L22) on the technological properties of the rubber mixture, physical, mechanical and operational characteristics of rubber based on nitrile butadiene caoutchouc BNKS-40AMN. Basic rubber mixture studied included caoutchouc, BC-FF percadox, zinc monomethacrylate, maleide F, triallyl isocyanurate, acetonanil N, MGF-9 and THM-3 oligoester acrylates, carbon black P 514 and other ingredients. The rubber mixture was prepared on laboratory rolls LB 320 160/160 in two stages. At the first stage, BNKS-40AMN caoutchouc was mixed with ingredients and processing aids. As technological additives, zincolet BB 222, lubstab-01 and MA-L22 were used. In the second mixing step, BC-FF percadox and vulcanization coagents were introduced. For the obtained variants of the rubber mixture the vulcanization characteristics were studied on an MDR 3000 Basic rheometer at a temperature of 170 °C. The rubber mixture prepared was vulcanized in a P-V-100-3RT-2-PCD type vulcanizing press at 150 °C for 40 min. Determination of elastic-strength and operational properties of rubber were carried out according to the standards existing for the rubber industry. The oil resistance of the vulcanizates was evaluated by changing their elastic strength after exposure to standard liquid SZHR-1 at a temperature of 125 °C, as well as by changing the mass of the samples after exposure to a mixture of isooctane with toluene at room temperature. It was found that the introduction of technological additives in the rubber compound improves the distribution of carbon black P 514 and powdered ingredients (zinc monomethacrylate, maleide F, triallyl isocyanurate, acetonanil H) in the caoutchouc matrix. Increased elastic strength indicators and their smallest changes after exposure to aggressive hydrocarbon media is characterized a rubber containing technological additive MA-L22. A comparison of technological, elastic-strength properties and resistance to aggressive media for rubbers containing butadiene-nitrile caoutchoucs BNKS-18AMN, BNKS-28AMN and BNKS-40AMN with optimal technological additives for them was done. It has been established that rubber containing BNKS-40AMN and technological additive MA-L22 is characterized by improved vulcanization properties, increased elastic strength indicators and their smallest changes after exposure to aggressive hydrocarbon media.


1982 ◽  
Vol 55 (2) ◽  
pp. 382-390 ◽  
Author(s):  
E. L. Charsley ◽  
J. G. Dunn

Abstract (1) The experimental variables which are found to affect significantly the measured T15 value for compounded carbon blacks are: (a) the maximum temperature achieved during the pyrolysis step and (b) the flow rate of air and the heating rate used during the oxidation step. (2) There is a definite correlation between the T15 value and the surface area of a carbon black, both in its free form and when compounded in a rubber. The T15 value is dependent on the cure method of the rubber and has also recently been reported to depend on the manufacturing source of the carbon black. This technique, therefore, cannot be recommended as suitable for the identification of a carbon black type in an unknown formulation. It can be used, however, as a routine quality control check on batch rubbers. (3) Thermogravimetry can be used as a rapid and accurate method for the determination of the carbon black content of rubbers, at levels as far apart as 0.1% and 30%.


2011 ◽  
Vol 19 (2) ◽  
Author(s):  
M. Maliński ◽  
Ł. Chrobak ◽  
J. Zakrzewski ◽  
K. Strzałkowski

AbstractThis paper presents step by step the procedure of determination of the quantum efficiency of luminescence of Mn2+ ions in the Zn1−x−yBexMnySe crystals. The method is based on the photoacoustic spectroscopy approach. In the paper, the experimental spectra of absorbance, transmission, absorption and photoacoustic spectra of the samples are presented and analyzed from the point of view of the possibility of determination of the quantum efficiency of Mn2+ ion luminescence at room temperature. It was determined experimentally that in the investigated crystals the quantum efficiency of luminescence in the Mn2+ ions is about 35%, 40%, 32% for the absorption peaks at 430 nm, 470 nm, and 510 nm, respectively, for Zn0.75Be0.2Mn0.05Se crystal.


1966 ◽  
Vol 39 (4) ◽  
pp. 1041-1052 ◽  
Author(s):  
Frederic J. Linnig ◽  
Edwin J. Parks ◽  
Robert D. Stiehler

Abstract Crystalline organic compounds containing a β-naphthyl group cause pronounced stiffening of rubber vulcanizates under certain conditions. When these materials are removed by extraction, the reinforcing effect vanishes. Reversibility of this effect indicates that the forces involved are not those associated with primary bonds. Reinforcement by at least one of these materials, PBNA, is obtained with vulcanizates made from various elastomers and vulcanizing agents, and is essentially independent of the state of cure. In some instances about five per cent of PBNA, the most effective of these, produces the same stiffness on first extension as 40 phr carbon black. Any PBNA dissolved in the rubber has no effect on stiffness. Thus, less than three per cent crystalline PBNA may produce an isotropic Young's modulus of about 20 kg/cm2 at room temperature. At higher concentrations of PBNA, strain continues to decrease but hardness does not change proportionally. The temperature coefficient of Young's modulus for PBNA reinforced rubber is negative, like that for vulcanizates containing carbon black. However, the increased solubility of PBNA with rising temperature makes quantitative determination of the temperature coefficient difficult. The PBNA-rubber structure is partly destroyed by repeated extensions to twice the original length. However after 5 extensions a substantial enhancement of modulus remains. Addition of PBNA to a rubber vulcanizate does not affect significantly the glass transition temperature. Though the reversible nature of reinforcement with PBNA strongly suggests a physical mechanism, the stiffening cannot be explained by existing theories of physical reinforcement.


Author(s):  
R. M. Anderson ◽  
T. M. Reith ◽  
M. J. Sullivan ◽  
E. K. Brandis

Thin films of aluminum or aluminum-silicon can be used in conjunction with thin films of chromium in integrated electronic circuits. For some applications, these films exhibit undesirable reactions; in particular, intermetallic formation below 500 C must be inhibited or prevented. The Al films, being the principal current carriers in interconnective metal applications, are usually much thicker than the Cr; so one might expect Al-rich intermetallics to form when the processing temperature goes out of control. Unfortunately, the JCPDS and the literature do not contain enough data on the Al-rich phases CrAl7 and Cr2Al11, and the determination of these data was a secondary aim of this work.To define a matrix of Cr-Al diffusion couples, Cr-Al films were deposited with two sets of variables: Al or Al-Si, and broken vacuum or single pumpdown. All films were deposited on 2-1/4-inch thermally oxidized Si substrates. A 500-Å layer of Cr was deposited at 120 Å/min on substrates at room temperature, in a vacuum system that had been pumped to 2 x 10-6 Torr. Then, with or without vacuum break, a 1000-Å layer of Al or Al-Si was deposited at 35 Å/s, with the substrates still at room temperature.


Author(s):  
Fumio Watari ◽  
J. M. Cowley

STEM coupled with the optical system was used for the investigation of the early oxidation on the surface of Cr. Cr thin films (30 – 1000Å) were prepared by evaporation onto the polished or air-cleaved NaCl substrates at room temperature and 45°C in a vacuum of 10−6 Torr with an evaporation speed 0.3Å/sec. Rather thick specimens (200 – 1000Å) with various preferred orientations were used for the investigation of the oxidation at moderately high temperature (600 − 1100°C). Selected area diffraction patterns in these specimens are usually very much complicated by the existence of the different kinds of oxides and their multiple twinning. The determination of the epitaxial orientation relationship of the oxides formed on the Cr surface was made possible by intensive use of the optical system and microdiffraction techniques. Prior to the formation of the known rhombohedral Cr2O3, a thin spinel oxide, probably analogous to γ -Al203 or γ -Fe203, was formed. Fig. 1a shows the distinct epitaxial growth of the spinel (001) as well as the rhombohedral (125) on the well-oriented Cr(001) surface. In the case of the Cr specimen with the (001) preferred orientation (Fig. 1b), the rings explainable by spinel structure appeared as well as the well defined epitaxial spots of the spinel (001). The microdif fraction from 20A areas (Fig. 2a) clearly shows the same pattern as Fig. Ia with the weaker oxide spots among the more intense Cr spots, indicating that the thickness of the oxide is much less than that of Cr. The rhombohedral Cr2O3 was nucleated preferably at the Cr(011) sites provided by the polycrystalline nature of the present specimens with the relation Cr2O3 (001)//Cr(011), and by further oxidation it grew into full coverage of the rest of the Cr surface with the orientation determined by the initial nucleation.


2019 ◽  
Vol 7 (2A) ◽  
Author(s):  
Camilo Fuentes Serrano ◽  
Juan Reinaldo Estevez Alvares ◽  
Alfredo Montero Alvarez ◽  
Ivan Pupo Gonzales ◽  
Zahily Herrero Fernandez ◽  
...  

A method for determination of Cr, Fe, Co, Ni, Cu, Zn, Hg and Pb in waters by Energy Dispersive X Ray Fluorescence (EDXRF) was implemented, using a radioisotopic source of 238Pu. For previous concentration was employed a procedure including a coprecipitation step with ammonium pyrrolidinedithiocarbamate (APDC) as quelant agent, the separation of the phases by filtration, the measurement of filter by EDXRF and quantification by a thin layer absolute method. Sensitivity curves for K and L lines were obtained respectively. The sensitivity for most elements was greater by an order of magnitude in the case of measurement with a source of 238Pu instead of 109Cd, which means a considerable decrease in measurement times. The influence of the concentration in the precipitation efficiency was evaluated for each element. In all cases the recoveries are close to 100%, for this reason it can be affirmed that the method of determination of the studied elements is quantitative. Metrological parameters of the method such as trueness, precision, detection limit and uncertainty were calculated. A procedure to calculate the uncertainty of the method was elaborated; the most significant source of uncertainty for the thin layer EDXRF method is associated with the determination of instrumental sensitivities. The error associated with the determination, expressed as expanded uncertainty (in %), varied from 15.4% for low element concentrations (2.5-5 μg/L) to 5.4% for the higher concentration range (20-25 μg/L).


Sign in / Sign up

Export Citation Format

Share Document