A generalized method for correcting instrument spreading in gel permeation chromatography

A general method of chromatogram correction for skewed instrument spreading in gel permeation chromatography is presented. The correction method is so general that there is no restriction on the shape of the spreading function. It admits nonsymmetric, non-Gaussian as well as nonconvolution type. Aspects of solution techniques are discussed and an illustrative example is given to elucidate the method.     

Carbon fiber structure and stability studies

A study has been made of the thermal-oxidative stability of several commercially available carbon fibers. Significant differences in the weight loss behavior were observed in air aging studies run on the bare fibers at 600°F (589 K). The stability of high temperature laminates, such as those based on NR-150 polyimide precursor solutions, was found to be directly affected by the stability of the reinforcing carbon fibers. In studies carried out to determine the reasons for carbon fiber instability, residual sodium sulfate was found to be the principle destabilizing factor. A mechanism whereby the sodium sulfate promotes the oxidation of carbon in the presence of air is proposed.     

Impact reinforcement of poly(vinyl chloride)

Several theories have been advanced to explain the toughening of glassy plastics by rubbery modifiers. These have been based primarily on studies of high impact polystyrene or ABS systems, where the crazing mechanism has been shown to be most applicable. In the present study, the effects of MBS (methacrylate-butadiene-styrene) impact modifiers on PVC have been studied, utilizing both physical and microscopic techniques. Tensile test results indicate that a primary contribution of the modifier to increased toughness is a lowering of the yield stress of the PVC. Electron microscopic studies and density determinations on strained samples indicate no crazes in these MBS-modified PVC systems. These results suggest that the mechanism of impact reinforcement in PVC is based on the enhancement of localized yielding in the vicinity of the rubbery modifier particles.     

Apparatus and procedure for measuring release rates from formulations of lepidopteran semiochemicals

An apparatus was developed wherein a vacuum source was used to pull air across a controlled-release-formulation dispenser or a planchet containing a known quantity of a semiochemical and into a collector filled with a polymeric adsorbent. After a set time, the semiochemical was eluted with solvent and was quantified by gas-liquid chromatography (GLC). High percentages of known quantities of the lepidopteran semiochemicals (Z)-7-dodecen-l -ol acetate (Z7DDA), boiling point (bp) 275 ° C/1 atm, (Z)-9-tetradecen-1-ol formate (Z9TDF), bp 289 °C/1 atm, and (Z,Z)-3,13-octadecadien-1-ol acetate (ZZODDA), bp 490 °C/1 atm, were recovered. The semiochemicals did not oxidize and were recovered quantitatively from the adsorbent. The release rates of Z9TDF from a controlled-release dispenser were found to be directly proportional to the airflow rates. Release rate measurements on the Z9TDF dispensers were made for the purpose of estimating the method's precision. The method was shown to give internally consistent results by measurements on another Z9TDF formulation. The accuracy of the method is discussed.Mention of a commercial or proprietary product in this paper does not constitute an endorsement by the USDA.     

Strain-Induced Deformation in Magnesia–Alumina Layered Composites

Ceramic beams are induced in situ to form complex shapes at elevated temperature without the application of an external stress. This process has been demonstrated for thin alumina substrates coated with a layer of magnesia. The internal strain causing the substrates to deform at elevated temperature arises as a consequence of strain mismatch accompanying the penetration of the coating into the substrate. The magnitude of the deformation depends on the amount of coating applied, on the thickness of the substrate, on the density of the substrate, and on the temperature. During exposure of the beams to elevated temperature, the magnesia coating reacts with the alumina substrate to form the spinel phase; the resulting volume change accompanying the phase transformation is likely the predominant driving force for deformation.     

Determination of water in cooked cottonseed meats by a modified indirect conductivity method

Summary The modified indirect conductivities and oven-dry moisture percentages were determined on mine Samples of cooked cottonseed meats (1.8 to 13.9% water). Statistical treatment of the data yields the following results: (1) equation of the regression line, {fx177-1} (2) correlation coefficient, 0.998; (3) standard deviation from the regression line, 0.27% water. Ten replicate determinations made on each of two samples containing 2.7 and 7.7% water showed standard deviations of 0.07 and 0.08% water. These results show that the accuracy and precision of the modified indirect conductivity method are satisfactory for practical applications. For a consecutive series of determinations the average time required per determination was about 9 min. This time could be reduced to about 5 min. by using duplicate sets of stirring apparatus. Describes data obtained in research conducted cooperatively by the Cotton Research Committee of Texas and the Texas Engineering Experiment Station.     

Thermal degradation studies of several pyrrone films

The thermal degradation of several polyimidazopyrrolone (pyrrone) films was studied in air and in vacuum over the range of 100–1000°C. by thermogravimetric analysis (TGA), with the use of both isothermal heating and programmed heating rates of 2, 3, 5, and 7.5°C./min. At pressures of 10^?6 torr or less, maximum weight losses average 30% at 800°C. Rates of volatilization and activation energies were derived to provide comparison between these ladder-type polymers. Mass spectrometric analysis of the pyrolysis gases evolved under vacuum conditions showed that CO, CO₂, and H₂O were the primary volatile products and that they were formed throughout the period of weight loss. Approximate correlation between changes in weight and changes in the total pressure for the vacuum tests indicates that mass spectrometric results could provide quantitative as well as qualitative data. The importance of sample history prior to heating and of sample geometry in developing meaningful and reproducible TGA results is aptly demonstrated. The ability of these materials to absorb readily 5–7 wt.-% of water under ambient conditions and the effect of this property upon weight loss measurements are shown.     

Characteristics of the lipase from the mold,Geotrichum candidum: A review

The moldGeotrichum candidum produces an extracellular lipase, readily concentrated by removal of the culture medium in which the microorganism is grown. The lipase is characterized by a unique, but not absolute, specificity for fatty acids containingcis-9 orcis,cis-9, 12 unsaturation, hydrolyzing both regardless of position within the triglyceride molecule. The enzyme also hydrolyzescis-9-16∶1,cis,trans-9,12-18∶2,trans,cis-9,12-18∶2, palmitoyl oleate and cholesteryl oleate. Digested at comparatively slow rates are:trans,trans-9,12-18∶2, double bond positional isomers of 18∶1 (other thancis-9), stearolic acid, oleoylpalmitate, dilinoleoyl phosphatidyl choline, and saturated acids. The enzyme has an optimum pH of 8.2, and the lyophilized powder is extremely stable, retaining activity for at least eight years when stored at-20 C. A purification of 81-fold has been achieved. One of five papers presented in the Symposium “Microbial Lipolytic Enzymes,” AOCS Spring Meeting, New Orleans, April 1973. Scientific contribution 556, Agricultural Experiment Station, University of Connecticut, Storrs, Conn. 06268.     

Polymerization mechanisms and molecular weight distribution. II. AIBN-initiated polymerization of styrene at 60°C

An experimental study was carried out on the AIBN-initiated polymerization of styrene at 60°C. The kinetic rate constants were determined by the method of moments and the MWD method, which was proposed in a previous paper. The results compared favorably with the data in the literature and the MWD method was noted to yield more consistent results than the method of moments, which indicates the importance of considering the whole molecular weight distribution. The theoretical MWD was found to approximate the experimental MWD well. The chain-transfer constant to AIBN was found to be between 0.09 and 0.14.