Chemical tests for raw and vulcanized rubber. Sample preparation

2015 ◽  
1998 ◽  
Vol 71 (1) ◽  
pp. 17-25 ◽  
Author(s):  
M. Gerspacher ◽  
L. Nikiel ◽  
H. H. Yang ◽  
C. P. O'Farrell

Abstract A new method of measuring carbon black dispersion in rubber is presented. This method is based on the measurement of the light reflectivity from the rubber sample using standard equipment used in the evaluation of the tint strength of carbon black (ASTM D3265 procedure). This method can be applied for both uncured and cured samples; however, the uncured sample measurement has significant advantages in the simplicity of the sample preparation and obtaining important filler dispersion information of the compound. It is shown that samples with better dispersed carbon black reflect less light as compared to samples with poor carbon black dispersion.


1945 ◽  
Vol 18 (3) ◽  
pp. 607-609 ◽  
Author(s):  
Paul Chovin

Abstract The autoöxidation of rubber is sensitive to the action of catalysis; anti-oxygenic compounds are antagonistic to the process and retard its progress; proöxygenic compounds on the contrary promote autoöxidation, and in their presence the effects of autoöxidation are evident sooner. In the present paper, experiments are described, the object of which was to study the action of a few typical proöxygenic compounds on rubber hydrocarbon. Among the substances which accelerate the action of oxygen, certain salts of copper, iron, cobalt, and manganese are known to be very active. Various organic derivatives of these metals were studied in the present work, including (1) copper acetylacetonate, oleate, linoleate, sulforicinoleate, elaidate, stearate, enanthate, pelargonate, hendecenate, erucate, and diethylthioneethiolcarbamate; (2) iron acetylacetonate, oleate, linoleate, sulforicinoleate, and pelargonate, and the dibenzoylmethane derivative of iron; (3) cobaltous oleate, linoleate and sulforicinoleate, and cobaltic acetylacetonate; (4) manganous oleate, linoleate, sulforicinoleate and pelargonate, and manganic acetylacetonate. A study was also made of certain more complex metal derivatives, including salts of the dithizone of cupferron, of mercaptobenzothiazole, of α-nitrose-β-naphthol, of benzyldioxime, etc. The method followed involved two steps: (1) incorporation of a predetermined percentage of a proöxygenic metal compound into samples of vulcanized rubber, (2) estimation of the acceleration of autoöxidation induced by the particular proöxygenic compound. In the first step, the rubber sample was cut into small cubical pieces 2–3 mm. on a side, and these were placed in a chloroform solution of the particular salt under investigation. The average content of proöxygenic compound which was absorbed was about 0.1 per cent. The swelling of the rubber in the solution was the determinant factor in the total amount of proöxygenic compound and solvent which were absorbed.


Author(s):  
R. E. Ferrell ◽  
G. G. Paulson ◽  
C. W. Walker

Selected area electron diffraction (SAD) has been used successfully to determine crystal structures, identify traces of minerals in rocks, and characterize the phases formed during thermal treatment of micron-sized particles. There is an increased interest in the method because it has the potential capability of identifying micron-sized pollutants in air and water samples. This paper is a short review of the theory behind SAD and a discussion of the sample preparation employed for the analysis of multiple component environmental samples.


Author(s):  
T. J. Magee ◽  
J. Peng ◽  
J. Bean

Cadmium telluride has become increasingly important in a number of technological applications, particularly in the area of laser-optical components and solid state devices, Microstructural characterizations of the material have in the past been somewhat limited because of the lack of suitable sample preparation and thinning techniques. Utilizing a modified jet thinning apparatus and a potassium dichromate-sulfuric acid thinning solution, a procedure has now been developed for obtaining thin contamination-free samples for TEM examination.


Author(s):  
Earl R. Walter ◽  
Glen H. Bryant

With the development of soft, film forming latexes for use in paints and other coatings applications, it became desirable to develop new methods of sample preparation for latex particle size distribution studies with the electron microscope. Conventional latex sample preparation techniques were inadequate due to the pronounced tendency of these new soft latex particles to distort, flatten and fuse on the substrate when they dried. In order to avoid these complications and obtain electron micrographs of undistorted latex particles of soft resins, a freeze-dry, cold shadowing technique was developed. The method has now been used in our laboratory on a routine basis for several years.The cold shadowing is done in a specially constructed vacuum system, having a conventional mechanical fore pump and oil diffusion pump supplying vacuum. The system incorporates bellows type high vacuum valves to permit a prepump cycle and opening of the shadowing chamber without shutting down the oil diffusion pump. A baffeled sorption trap isolates the shadowing chamber from the pumps.


Author(s):  
Jayesh Bellare

Seeing is believing, but only after the sample preparation technique has received a systematic study and a full record is made of the treatment the sample gets.For microstructured liquids and suspensions, fast-freeze thermal fixation and cold-stage microscopy is perhaps the least artifact-laden technique. In the double-film specimen preparation technique, a layer of liquid sample is trapped between 100- and 400-mesh polymer (polyimide, PI) coated grids. Blotting against filter paper drains excess liquid and provides a thin specimen, which is fast-frozen by plunging into liquid nitrogen. This frozen sandwich (Fig. 1) is mounted in a cooling holder and viewed in TEM.Though extremely promising for visualization of liquid microstructures, this double-film technique suffers from a) ireproducibility and nonuniformity of sample thickness, b) low yield of imageable grid squares and c) nonuniform spatial distribution of particulates, which results in fewer being imaged.


Author(s):  
P. B. Basham ◽  
H. L. Tsai

The use of transmission electron microscopy (TEM) to support process development of advanced microelectronic devices is often challenged by a large amount of samples submitted from wafer fabrication areas and specific-spot analysis. Improving the TEM sample preparation techniques for a fast turnaround time is critical in order to provide a timely support for customers and improve the utilization of TEM. For the specific-area sample preparation, a technique which can be easily prepared with the least amount of effort is preferred. For these reasons, we have developed several techniques which have greatly facilitated the TEM sample preparation.For specific-area analysis, the use of a copper grid with a small hole is found to be very useful. With this small-hole grid technique, TEM sample preparation can be proceeded by well-established conventional methods. The sample is first polished to the area of interest, which is then carefully positioned inside the hole. This polished side is placed against the grid by epoxy Fig. 1 is an optical image of a TEM cross-section after dimpling to light transmission.


Author(s):  
L. Mulestagno ◽  
J.C. Holzer ◽  
P. Fraundorf

Due to the wealth of information, both analytical and structural that can be obtained from it TEM always has been a favorite tool for the analysis of process-induced defects in semiconductor wafers. The only major disadvantage has always been, that the volume under study in the TEM is relatively small, making it difficult to locate low density defects, and sample preparation is a somewhat lengthy procedure. This problem has been somewhat alleviated by the availability of efficient low angle milling.Using a PIPS® variable angle ion -mill, manufactured by Gatan, we have been consistently obtaining planar specimens with a high quality thin area in excess of 5 × 104 μm2 in about half an hour (milling time), which has made it possible to locate defects at lower densities, or, for defects of relatively high density, obtain information which is statistically more significant (table 1).


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