Analysis of minor components by ultrahigh resolution NMR. 2. Detection of 0.01% diacetone alcohol in pure acetone and direct measurement of the rate of the aldol condensation of acetone

1987 ◽  
Vol 109 (22) ◽  
pp. 6609-6614 ◽  
Author(s):  
Steven R. Maple ◽  
Adam Allerhand
RSC Advances ◽  
2018 ◽  
Vol 8 (53) ◽  
pp. 30610-30615 ◽  
Author(s):  
Xuebing Xu ◽  
Hong Meng ◽  
Yingzhou Lu ◽  
Chunxi Li

The refluxing reaction of acetone on CaC2 realizes an efficient coproduction of diacetone alcohol, mesityl oxide, isophorone and C2H2.


Author(s):  
B. J. Grenon ◽  
A. J. Tousimis

Ever since the introduction of glutaraldehyde as a fixative in electron microscopy of biological specimens, the identification of impurities and consequently their effects on biologic ultrastructure have been under investigation. Several reports postulate that the impurities of glutaraldehyde, used as a fixative, are glutaric acid, glutaraldehyde polymer, acrolein and glutaraldoxime.Analysis of commercially available biological or technical grade glutaraldehyde revealed two major impurity components, none of which has been reported. The first compound is a colorless, water-soluble liquid with a boiling point of 42°C at 16 mm. Utilizing Nuclear Magnetic Resonance (NMR) spectroscopic analysis, this compound has been identified to be — dihydro-2-ethoxy 2H-pyran. This impurity component of the glutaraldehyde biological or technical grades has an UV absorption peak at 235nm. The second compound is a white amorphous solid which is insoluble in water and has a melting point of 80-82°C. Initial chemical analysis indicates that this compound is an aldol condensation product(s) of glutaraldehyde.


Author(s):  
T. Kaneyama ◽  
M. Naruse ◽  
Y. Ishida ◽  
M. Kersker

In the field of materials science, the importance of the ultrahigh resolution analytical electron microscope (UHRAEM) is increasing. A new UHRAEM which provides a resolution of better than 0.2 nm and allows analysis of a few nm areas has been developed. [Fig. 1 shows the external view] The followings are some characteristic features of the UHRAEM.Objective lens (OL)Two types of OL polepieces (URP for ±10' specimen tilt and ARP for ±30' tilt) have been developed. The optical constants shown in the table on the next page are figures calculated by the finite element method. However, Cs was experimentally confirmed by two methods (namely, Beam Tilt method and Krivanek method) as 0.45 ∼ 0.50 mm for URP and as 0.9 ∼ 1.0 mm for ARP, respectively. Fig. 2 shows an optical diffractogram obtained from a micrograph of amorphous carbon with URP under the Scherzer defocus condition. It demonstrates a resolution of 0.19 nm and a Cs smaller than 0.5 mm.


Author(s):  
Keiichi Tanaka

With the development of scanning electron microscope (SEM) with ultrahigh resolution, SEM became to play an important role in not only cytology but also molecular biology. However, the preparation methods observing tiny specimens with such high resolution SEM are not yet established.Although SEM specimens are usually coated with metals for getting electrical conductivity, it is desirable to avoid the metal coating for high resolution SEM, because the coating seriously affects resolution at this level, unless special coating techniques are used. For avoiding charging effect without metal coating, we previously reported a method in which polished carbon plates were used as substrate. In the case almost all incident electrons penetrate through the specimens and do not accumulate in them, when the specimens are smaller than 10nm. By this technique some biological macromolecules including ribosomes, ferritin, immunoglobulin G were clearly observed.Unfortunately some other molecules such as apoferritin, thyroglobulin and immunoglobulin M were difficult to be observed only by the method, because they had very low contrast and were easily damaged by electron beam.


Author(s):  
K. Fukushima ◽  
T. Kaneyama ◽  
F. Hosokawa ◽  
H. Tsuno ◽  
T. Honda ◽  
...  

Recently, in the materials science field, the ultrahigh resolution analytical electron microscope (UHRAEM) has become a very important instrument to study extremely fine areas of the specimen. The requirements related to the performance of the UHRAEM are becoming gradually severer. Some basic characteristic features required of an objective lens are as follows, and the practical performance of the UHRAEM should be judged by totally evaluating them.1) Ultrahigh resolution to resolve ultrafine structure by atomic-level observation.2) Nanometer probe analysis to analyse the constituent elements in nm-areas of the specimen.3) Better performance of x-ray detection for EDS analysis, that is, higher take-off angle and larger detection solid angle.4) Higher specimen tilting angle to adjust the specimen orientation.To attain these requirements simultaneously, the objective lens polepiece must have smaller spherical and chromatic aberration coefficients and must keep enough open space around the specimen holder in it.


1970 ◽  
Vol 13 (1) ◽  
pp. 65-73 ◽  
Author(s):  
Mary Mira

Listening, a significant dimension of the behavior of hearing-impaired children, may be measured directly by recording childrens' responses to obtain audio narrations programmed via a conjugate reinforcement system. Twelve hearing-impaired, school-aged children responded in varying ways to the opportunity to listen. Direct and continuous measurement of listening has relevance for evaluation of remediation methods and for discovery of variables potentially related to listening.


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