measure tool wear as a function of drill speed. Kirk et al. (55D) studied grinding fluids by a modified pin-on-disk simulated test employing a hemispherical segment of a grinding wheel rubbing against steel. SEM and microprobe results from the simulated test and from actual grinding tests showed similarities in wear morphology. Raje (830)reported on development of methods for evaluating the performance of oils for traction drives and discussed various hypotheses concerning the relationshirJ of chemical comrJosition of fluids to their tractive capaciiy. The volatilitv of lubricating oils was studied bv RumDf (880)who devdoped relationshps between evapor&ion rite and atmospheric pressure, average boiling point and viscosity using the Noack (DIN 51 581) apparatus. Gardos (350)utilized a quartz-spring mass sorption microbalance in combination with an ultra high vacuum pump to measure evaporation rates of low volatility polymeric lubricating oils. Greases. Stanton (960)presented a paper covering research on analysis of greases by infrared spectrometry carried out by ASTM Technical Division G-IV-4. Of the three methods described for taking IR spectra, the slurry technique proved to be the most precise. Differential thermal, thermogravimetric, and IR analyses were used by Novoded and Bogdanov (750)to study the thermal oxidation stability of complex calcium greases. Thermal analysis was also used by Gar et al. (340)to determine the effect of base oil composition on thermal phase changes in lithium greases. In studying flow properties of greases at high temperatures, Komatsuzaki and Ito ( 5 8 0 ) found the apparent viscosity measured with a cylindrical rotational viscometer dropped sharply at a specific temperature for each grease-thickener combination. Dobson (250)made a correlation stud of grease flow properties using pipe, concentric cylinder, andlcone and plate viscometers. Culp et al. ( 2 2 0 )reported on a study of grease shear stability using extended shearing up to 96 h in the ASTM Roll Stability Tester and concluded the D 1831 2-h procedure is too short to give meaningful results. Lindeman and Polishuk (66D)reported on an investigation of the effect of internal radial clearances of 0.0003-0.0008 in. (0.008-0.02 mm) on grease life and torque in ball bearings. Equations for approximating the life of almost any long-life grease as a function of bearing temperature, bearing size, speed, load, and lease com osition were presented in a paper by Booser (1107. SchneiAr (890)presented a paper describing new test procedures for measuring water washoff resistance of greases used in extreme marine environments.
WaX D. R. Cushman and J. W. Schick Mobil Research and Development Corporation, Paulsboro, N.J.
T h e r m a l Conductivity. LeRoux, Smith et al. (9E)examined Fischer-Tropsch waxes, covering thermal conductivity at 20-130 "C, specific volume-temperature curves, average molecular masses, and clear points. The waxes were mainly C34-C150 n-paraffins. Chromatography. Four papers dealt with chromatographic analysis. Azizova et al. ( I E ) studied low-melting paraffins by gas-liquid chromatography. The concentration of n-paraffins increased with increasing melting point of the low-melting wax, and complex forming paraffinic-naphthenic fractions showed a high concentration of normal araffins. Zakupra and Kolosova (I3E)also used gas-liquicfchromatography to analyze high-molecular alkanes (to C51), obtaining more pronounced peak areas of individual compounds using calibration coefficients determined by adjusting conditions (time, temperature) and packing material to those used with model mixtures. Postnov et al. (IOE) calculated physicochemical properties of solid alkanes by programmed-temperature gas chromatography, with the aid of literature data on boiling point distribution and experimental retention temperatures. The calculated molecular weights and densities showed good agreement with standard values. Blau (3E)ap240R
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ANALYTICAL CHEMISTRY, VOL. 49, NO. 5, APRIL 1977
plied gas chromatography to the analysis of common waxes and wax mixtures, including paraffin and microcrystalline waxes. Spectrometry. Zmudzinska-Zurek (15E) used infrared spectroscopy to determine solid petroleum hydrocarbons in a slack wax fraction. Average number of methyl groups was verified, and n-alkane (from urea adduction) and isoparaffin concentrations were determined. Berthold and Staude (2E) also analyzed saturated hydrocarbon mixtures by infrared spectrometry to determine structural configurations of fractions from refined crude oil products such as n-paraffins, white oils, Vaseline, and microcrystalline wax. Zenker (14E)described an infrared method for control of paraffin wax oxidation in the presence of boric acid as a reaction control in production of alcohols from paraffins. He found a linear relation between absorption intensity of B-0 stretching vibration in the borate ester wax and the hydroxyl value of the hydrolysis product. Krivjansky et al. (BE)studied the purity of solid petroleum paraffin waxes and ceresins used in the food, cosmetic, and pharmaceutical industries, using UV spectrophotometry to determine aromatic and resinous content, and a combination of UV spectrometry and spectrofluorometry for content of aromatics having carcinogenic roperties. Concentrations as low as 1-10 pb were detected. ghiraishi and Takabatake (12E)also s t u i e d carcinogens in petroleum waxes and synthetic waxes by extraction of benzo[a]pyrene with dimethyl sulfoxide, clean-up of extract on a column of alumina, and determination by spectrofluorometry. Miscellaneous. Six papers covered subjects of general interest, or those which combined several analytical techniques. Ivanova et al. (6E)gave a review, with 33 references, on the chemical composition of peat waxes. Sekine (I1E)discussed low-temperature fluidity of waxy crudes and heavy (fuel) oils, covering changes in flow properties due to wax solidification, test methods, and preventive measures such as the use of additives. Zubarev and Nevolin (16E)studied the solubility of paraffin in etroleum. The amounts of paraffin crystallizing out of petroyeum products and crude oil and depositing on pipe walls while cooling and flowing through pipelines were determined from solubilit curves. Hanna and Mahmoudr(5E) reported on the distribution of n-paraffins in Marine Belayim wax distillate, using zeolite adsorption and gas chromatography. Fal'kovich et al. ( 4 E ) determined n- paraffins by contacting with calcium-A zeolite. Results were more accurate, with lower values than by contacting with urea. Zeolite adsorption data covered nine crudes (or mixtures). Data are also given on fractional crystallization with urea, followed by zeolite adsorption, showing the presence of branched chain and cyclic hydrocarbons. Kamita et al. (7E)made a structural analysis of liquid wax oxidates. Paraffin wax was air oxidized with catalyst and separated into liquid and solid oxidates. The liquid oxides were separated by saponification, extraction, and column chromatography. Each fraction was further characterized by gas chromatography and IR and NMR spectroscopy. Viscosity increased with increased ester content. Esters were mainly lactones and compounds with a t least two ester functions.
Asphalt James R. Couper Department of Chemical Engineering, University of Arkansas, Fayetteville, Ark. 7270 1
The majority of the research work performed during the past two years has been related to the composition of asphalt. The subheadings were arbitrarily selected to facilitate the readability and location of the information. Gel Permeation a n d Chromatography. Some type of preliminary separation of asphalt into its components is necessary prior to the use of a chromatographic separation. The initial separation usually involves a solvent separation or precipitation technique. The fractions obtained by the chromatographic methods may be further subjected to in-
