Determination of Free Carbon in Cured Rubber Stocks

1951 ◽  
Vol 24 (1) ◽  
pp. 224-227
Author(s):  
I. M. Kolthoff ◽  
R. G. Gutmacher
Keyword(s):  
Nitric Acid ◽  
Carbon Black ◽  
Natural Rubber ◽  
Osmium Tetroxide ◽  
Free Carbon ◽  
Vulcanized Rubber ◽  
Tert Butyl Hydroperoxide ◽  
Inorganic Fillers ◽  
Dilute Nitric Acid

Abstract A method for the determination of free carbon in vulcanized rubber stocks is described. The sample is softened in boiling p-dichlorobenzene before treatment with tert-butyl hydroperoxide in the presence of osmium tetroxide. No difficulties are encountered in the filtration of the carbon black. The carbon black is washed on the filter with dilute nitric acid to remove acid-soluble inorganic fillers. The method has been successfully applied to natural rubber, GR-S, Butyl rubber, and Neoprene. No correction is necessary.

Ozonolytic Degradation of Interpolymers of Natural Rubber with Methyl Methacrylate and Styrene

1958 ◽  
Vol 31 (1) ◽  
pp. 82-85
Author(s):  
D. Barnard
Keyword(s):  
Molecular Weight ◽  
Carbon Black ◽  
Natural Rubber ◽  
Accurate Determination ◽  
Synthetic Polymers ◽  
Polymer Chains ◽  
Low Molecular Weight ◽  
Rubber Content ◽  
Tert Butyl Hydroperoxide

Abstract The preparation of graft and block interpolymers of natural rubber and synthetic polymers has made it desirable that the number and size of polymer chains attached to rubber be readily determinate. The degradation of unsaturated polymers with tert-butyl hydroperoxide in the presence of osmium tet oxide has been used for the determination of free polystyrene in SBR and carbon black in several elastomers, and has recently been applied to the present problem. The accurate determination of the rubber content of interpolymers by quantitative ozonolysis essentially according to the method of Boer and Kooyman suggested that this might be made the basis of isolation of the attached polymer, the rubber being degraded into fragments of low molecular weight, from which the polymer could be separated by conventional techniques. The method should be applicable to any interpolymer, or mixture, of a polyunsaturated and a saturated polymer and is illustrated with reference to interpolymers of natural rubber (NR)-polymethyl methacrylate (PMM) and NR-polystyrene (PS).

Determination of Free Carbon in Rubber. The Cresol Method

1941 ◽  
Vol 14 (1) ◽  
pp. 241-248 ◽  
Author(s):  
J. B. Roberts
Keyword(s):  
United States ◽  
Nitric Acid ◽  
Carbon Content ◽  
Accurate Method ◽  
The United States ◽  
Free Carbon ◽  
Simple Apparatus ◽  
Vulcanized Rubber ◽  
Acid Method

Abstract A simple, accurate method for the determination of free carbon in either raw or vulcanized rubber is presented. It has replaced the nitric acid method entirely in the laboratory of the United States Rubber Company, Detroit, Michigan. A study of the effects of interfering substances, and numerous comparisons of results by the cresol and the nitric acid methods, are given. Results by the cresol method, in the absence of interfering substances, are within 1 per cent of the calculated free carbon content. The method requires only simple apparatus readily available.

Carbon Black. I—A Study of Its Volatile Constituents

1928 ◽  
Vol 1 (3) ◽  
pp. 485-497 ◽  
Author(s):  
C. R. Johnson
Keyword(s):  
Carbon Black ◽  
Volatile Matter ◽  
Original Sample ◽  
Missing Information ◽  
Volatile Constituents ◽  
Vulcanized Rubber ◽  
Rates Of Evolution ◽  
Temperature And Pressure ◽  
The Relationship

Abstract The rates of evolution of gas from carbon black with variation of time, temperature, and pressure have been determined. Complete analyses have been made of five types of carbon black, which involve an organic combustion of the original sample, an organic combustion of the sample after the gases have been removed, a determination of the loss in weight represented by the gases removed, analyses of the gases removed, and finally a complete accounting, or balance, of the carbon in the steps considered. In an attempt to supply some missing information not revealed by the foregoing, some special gas analyses under varying conditions were made. The relationship between the amount and composition of volatile matter evolved from carbon blacks and the properties imparted to vulcanized rubber when compounded with these blacks has been studied.

Structural Characterization of Filled Vulcanizates Part 1. Determination of the Concentration of Chemical Crosslinks in Natural Rubber Vulcanizates Containing High Abrasion Furnace Black

1967 ◽  
Vol 40 (3) ◽  
pp. 866-882 ◽  
Author(s):  
M. Porter
Keyword(s):  
Carbon Black ◽  
Natural Rubber ◽  
Volume Fraction ◽  
Exponential Relationship ◽  
Furnace Black ◽  
Simple Linear Relationship ◽  
Chemical Crosslinks ◽  
Natural Rubber Vulcanizates

Abstract The degree to which HAF black restricts the swelling of natural rubber vulcanizates in n-decane has been determined using a vulcanizing system in which the stoichiometry of crosslinking is unaffected by the carbon black. The dependence of the degree of restriction, as measured by the ratio of the volume fractions of rubber in the filled and unfilled vulcanizates swollen to equilibrium, on the concentration of carbon black follows an exponential relationship previously proposed by Lorenz and Parks. This is found to be equivalent to a simple linear relationship between the apparent and actual crosslink concentrations: napparent/nactual=1+Kϕ, where K is a constant characteristic of the filler and φ is its volume fraction in the vulcanizate. The relation has been used to determine actual crosslink concentrations in filled natural rubber vulcanizates. HAF black is found to cause increases of up to 25 per cent in the yield of polymer to polymer crosslinks in conventional sulfur vulcanizing systems, accompanied by changes in rate of cure and of crosslink reversion. All these are small compared with the effect of the filler on many physical properties.

scholarly journals Determination of carbon black in vulcanized rubber by pyrolysis technique

1972 ◽  
Vol 21 (8) ◽  
pp. 989-992
Author(s):  
Tadaoki OKUMOTO ◽  
Tsugio TAKEUCHI ◽  
Emiko NAKAJIMA
Keyword(s):  
Carbon Black ◽  
Vulcanized Rubber

Heats of Vulcanization of Synthetic Rubbers

1944 ◽  
Vol 17 (2) ◽  
pp. 404-411 ◽  
Author(s):  
P. L. Bruce ◽  
R. Lyle ◽  
J. T. Blake
Keyword(s):  
Carbon Black ◽  
Natural Rubber ◽  
Chemical Reactions ◽  
Side Reaction ◽  
Heat Evolution ◽  
Butyl Rubber ◽  
Vulcanized Rubber ◽  
Principal Reaction ◽  
Low Sulfur ◽  
Quantity Of Heat

Abstract 1. The heats of vulcanization for natural rubber and Buna-S are nearly equal. The data for both materials indicate two different chemical reactions during vulcanization. At low sulfur percentages, the principal reaction forms soft vulcanized rubber and is accompanied by little or no heat evolution. Above the 2 per cent sulfur region, a second reaction predominates, forming hard rubber and producing a relatively large quantity of heat. 2. The presence of an accelerator (Santocure) in Buna-S has little, if any, effect on heat of vulcanization. 3. The addition of carbon black to Buna-S lowers the heat of vulcanization in the region above 4 per cent sulfur. The calories evolved in a 10 per cent sulfur compound decrease linearly with percentage of carbon black. 4. The heats of vulcanization of Buna-N (Hycar OR-15) indicate the presence of two chemical reactions. Unlike natural rubber and Buna-S, the ebonite reaction does not predominate until the sulfur concentration is raised above 10 per cent. 5. The heat of vulcanization of Butyl rubber with sulfur is equal to the heat evolved with natural rubber containing 0.6 per cent sulfur. If one sulfur atom reacts per double bond, the maximum amount combining would be 0.72 per cent sulfur. During the vulcanization of Butyl rubber with p-quinone dioxime and lead peroxide, a large amount of heat is evolved by a side reaction between the vulcanizing agents. The reaction involving the Butyl rubber produces about 6 calories per gram, a considerably higher value than the 1 calorie produced by sulfur vulcanization. 6. The heat of vulcanization of Neoprene-GN without added agents corresponds to a value for smoked sheet rubber containing 4.5 per cent sulfur. The addition of zinc oxide and magnesia decreases the heat of vulcanization.

Microwave Devulcanization of Waste Rubber with Inorganic Salts and Nitric Acid

2011 ◽  
Vol 418-420 ◽  
pp. 1072-1075 ◽  
Author(s):  
Glauco Dias Paulo ◽  
Denise Hirayama ◽  
Clodoaldo Saron
Keyword(s):  
Nitric Acid ◽  
Carbon Black ◽  
Soxhlet Extraction ◽  
The Other ◽  
Inorganic Salts ◽  
Metallic Ions ◽  
Chemical Modifications ◽  
Mechanical Recycling ◽  
Vulcanized Rubber ◽  
Waste Rubber

Rubber wastes cause severe damages for the environment when unsuitably disposed in the environment and represent a challenger for mechanical recycling, because the vulcanized rubber is formed by a tridimensional network with intermolecular sulfur crosslinks. Microwave radiation can lead to the breaking of sulfur crosslinks and so enable the recycling of vulcanized rubbers. The aim of this work was to study the SBR devulcanization by microwave using inorganic salts and nitric acid. Soxhlet extraction and FTIR analyzes were carried out to evaluate the devulcanization degree and chemical modifications in the rubber structure. The results showed that the presence of carbon black in the rubber is an important factor for devulcanization and some metallic ions decrease the sulfur crosslink content. On the other hand, these ions promote the oxidation in the rubber.

Poisson's Ratio for Stretched Vulcanized Natural Rubber

1969 ◽  
Vol 42 (2) ◽  
pp. 547-556 ◽  
Author(s):  
H. Sekiguchi ◽  
M. Kakiuchi ◽  
T. Morimoto ◽  
K. Fujimoto ◽  
N. Yoshimura
Keyword(s):  
Carbon Black ◽  
Natural Rubber ◽  
Large Deformation ◽  
Poisson’S Ratio ◽  
Poisson Ratio ◽  
Poisson's Ratio ◽  
Elongation Ratio ◽  
Infinitesimal Deformation ◽  
Carbon Black Content ◽  
Vulcanized Rubber

Abstract Changes in the Poisson's ratio of natural vulcanized rubber due to elongation were investigated experimentally. The following results were obtained: If infinitesimal deformation at any instant during elongation is considered, it appears to be correct to take the Poisson's ratio at such instants as 0.5. If the apparent Poisson ratio when a certain standard mark is taken and a large deformation imparted is considered, and the elongation ratio is made α, the Poisson's ratio decreases from 0.5 in accordance with the equation log10 (1/m)=0.0204α2−0.261α−0.0628. This equation is valid for subsequent elongations, no matter what elongation situation is taken for the standard marks. These two results do not vary with the carbon black content or on repeated stretching.

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