Reliable procedures are given for the preparation and purification of hexahydroxybenzene (benzenehexol), tetrahydroxy-p-benzoquinone, rhodizonic acid, triquinoyl (cyclohexanehexone), croconic acid, and leuconic acid (cyclopentanepentone). Certain derivatives and color tests, as well as infrared and ultraviolet spectra, are reported for their identification.
{"title":"Cyclic Polyhydroxy Ketones. I. Oxidation Products of Hexahydroxybenzene (Benzenehexol).","authors":"A. Fatiadi, H. Isbell, W. Sager","doi":"10.6028/JRES.067A.015","DOIUrl":"https://doi.org/10.6028/JRES.067A.015","url":null,"abstract":"Reliable procedures are given for the preparation and purification of hexahydroxybenzene (benzenehexol), tetrahydroxy-p-benzoquinone, rhodizonic acid, triquinoyl (cyclohexanehexone), croconic acid, and leuconic acid (cyclopentanepentone). Certain derivatives and color tests, as well as infrared and ultraviolet spectra, are reported for their identification.","PeriodicalId":94340,"journal":{"name":"Journal of research of the National Bureau of Standards. Section A, Physics and chemistry","volume":"39 1","pages":"153-162"},"PeriodicalIF":0.0,"publicationDate":"1963-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74739292","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
The theory for frustrated total reflection has been developed for the case where the third medium is metallic of complex index. Using parallel polarized light a unique minimum in reflectance occurs at a definite film thickness. Experimental verification of the theory is made and indicates the theory applicable to the precise measurement of thin contact films existing between metallic and dielectric surfaces.
{"title":"Theory of Frustrated Total Reflection Involving Metallic Surfaces.","authors":"T. R. Young, B. Rothrock","doi":"10.6028/JRES.067A.012","DOIUrl":"https://doi.org/10.6028/JRES.067A.012","url":null,"abstract":"The theory for frustrated total reflection has been developed for the case where the third medium is metallic of complex index. Using parallel polarized light a unique minimum in reflectance occurs at a definite film thickness. Experimental verification of the theory is made and indicates the theory applicable to the precise measurement of thin contact films existing between metallic and dielectric surfaces.","PeriodicalId":94340,"journal":{"name":"Journal of research of the National Bureau of Standards. Section A, Physics and chemistry","volume":"582 1","pages":"115-125"},"PeriodicalIF":0.0,"publicationDate":"1963-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77212777","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
The Pd III spectrum has been observed from 688 to 2991 A, and the earlier analysis has been revised and extended. The number of Pd III lines here reported is 1,110, of which 917 are classified as combinations of 57 even energy levels with 111 of odd parity. The interpretation has been aided by theoretical predictions of the approximate positions of expected energy levels. Spectral terms from the 4d 8, 4d 7 ns 1, and 4d 6 5s 1 5p 1 configurations are designated. Eight limit terms are in the 4d 7 ns 1 configurations. The earlier ionization potential, 33.0 electron volts derived from the (ns 1) 3,5 F series (n=5,6) by means of a Ritz formula, remains unchanged.
{"title":"Third Spectrum of Palladium (Pd III).","authors":"A. G. Shenstone","doi":"10.6028/JRES.067A.010","DOIUrl":"https://doi.org/10.6028/JRES.067A.010","url":null,"abstract":"The Pd III spectrum has been observed from 688 to 2991 A, and the earlier analysis has been revised and extended. The number of Pd III lines here reported is 1,110, of which 917 are classified as combinations of 57 even energy levels with 111 of odd parity. The interpretation has been aided by theoretical predictions of the approximate positions of expected energy levels. Spectral terms from the 4d 8, 4d 7 ns 1, and 4d 6 5s 1 5p 1 configurations are designated. Eight limit terms are in the 4d 7 ns 1 configurations. The earlier ionization potential, 33.0 electron volts derived from the (ns 1) 3,5 F series (n=5,6) by means of a Ritz formula, remains unchanged.","PeriodicalId":94340,"journal":{"name":"Journal of research of the National Bureau of Standards. Section A, Physics and chemistry","volume":"254 1","pages":"87-112"},"PeriodicalIF":0.0,"publicationDate":"1963-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76332467","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Robert D Goodwin, Dwain E Diller, Hans M Roder, Lloyd A Weber
Experimental data are presented at closely spaced intervals of temperature and density. The range of experimental densities is from 0.064 to 2.8 times the critical density. There are presented, in addition, tables interpolated uniformly in arguments density and temperature, and also in pressure and temperature.
{"title":"Pressure-Density-Temperature Relations of Fluid Para Hydrogen From 15 to 100 °K at Pressures to 350 Atmospheres.","authors":"Robert D Goodwin, Dwain E Diller, Hans M Roder, Lloyd A Weber","doi":"10.6028/jres.067A.017","DOIUrl":"10.6028/jres.067A.017","url":null,"abstract":"<p><p>Experimental data are presented at closely spaced intervals of temperature and density. The range of experimental densities is from 0.064 to 2.8 times the critical density. There are presented, in addition, tables interpolated uniformly in arguments density and temperature, and also in pressure and temperature.</p>","PeriodicalId":94340,"journal":{"name":"Journal of research of the National Bureau of Standards. Section A, Physics and chemistry","volume":"67A 2","pages":"173-192"},"PeriodicalIF":0.0,"publicationDate":"1963-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC6640577/pdf/jres-67A-173.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41224877","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Three independent velocities of sound can be measured along any direction of propagation in a cubic crystal except the [100] and [111] directions. These three velocities suffice to determine the three elastic constants and for the [110] direction, the calculation of these constants is easy. For all other directions, the calculation is more difficult; the only existing method appears to be a perturbation technique developed by Neighbours. The present paper presents a method using exact equations and an iterative procedure to solve these equations and to calculate both the elastic constants and their standard deviations from the sound velocities and their standard deviations. The method is illustrated with new data on SrTiO3 which give c11=3.156±0.027, c12=1.027±0.027, c44= 1.215±0.006×1012 dynes/cm2 at 25 °C. The importance of including covariance terms in calculations of the standard deviations is emphasized.
{"title":"A Method for Determining the Elastic Constants of a Cubic Crystal from Velocity Measurements in a Single Arbitrary Direction; Application to SrTiO3.","authors":"J. B. Wachtman, M. Wheat, S. Marzullo","doi":"10.6028/JRES.067A.018","DOIUrl":"https://doi.org/10.6028/JRES.067A.018","url":null,"abstract":"Three independent velocities of sound can be measured along any direction of propagation in a cubic crystal except the [100] and [111] directions. These three velocities suffice to determine the three elastic constants and for the [110] direction, the calculation of these constants is easy. For all other directions, the calculation is more difficult; the only existing method appears to be a perturbation technique developed by Neighbours. The present paper presents a method using exact equations and an iterative procedure to solve these equations and to calculate both the elastic constants and their standard deviations from the sound velocities and their standard deviations. The method is illustrated with new data on SrTiO3 which give c11=3.156±0.027, c12=1.027±0.027, c44= 1.215±0.006×1012 dynes/cm2 at 25 °C. The importance of including covariance terms in calculations of the standard deviations is emphasized.","PeriodicalId":94340,"journal":{"name":"Journal of research of the National Bureau of Standards. Section A, Physics and chemistry","volume":"31 1","pages":"193-204"},"PeriodicalIF":0.0,"publicationDate":"1963-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75883973","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
An interferometer for measuring change in index of refraction with pressure is described. Absolute indices of refraction are reported to five decimals for benzene, carbon tetrachloride, and water at pressures as high as 1100 bars over a small temperature range. The results of replicate measurements agree to within ±0.0001. Various equations relating index and specific volume show systematic deviations in all cases. At constant specific volume, the index of carbon tetrachloride increases with increasing temperature, while the index of water decreases with increasing temperature. The refractive index of benzene shows no effect due solely to temperature within the experimental error. Possible explanations for this behavior are discussed.
{"title":"Effect of Pressure and Temperature on the Refractive Indices of Benzene, Carbon Tetrachloride, and Water.","authors":"R. Waxler, C. Weir","doi":"10.6028/JRES.067A.016","DOIUrl":"https://doi.org/10.6028/JRES.067A.016","url":null,"abstract":"An interferometer for measuring change in index of refraction with pressure is described. Absolute indices of refraction are reported to five decimals for benzene, carbon tetrachloride, and water at pressures as high as 1100 bars over a small temperature range. The results of replicate measurements agree to within ±0.0001. Various equations relating index and specific volume show systematic deviations in all cases. At constant specific volume, the index of carbon tetrachloride increases with increasing temperature, while the index of water decreases with increasing temperature. The refractive index of benzene shows no effect due solely to temperature within the experimental error. Possible explanations for this behavior are discussed.","PeriodicalId":94340,"journal":{"name":"Journal of research of the National Bureau of Standards. Section A, Physics and chemistry","volume":"53 1","pages":"163-171"},"PeriodicalIF":0.0,"publicationDate":"1963-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80655342","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Accurate quantitative data pertinent to the structure of solid materials at the micro size level, which are difficult or prohibitive to obtain by traditional manual measurements, are now obtained directly by a digital computer which uses a photomicrograph as the information input. The history of picture interpretation experiments at the National Bureau of Standards is reviewed. The fundamental computer operations are illustrated, together with a description of 24 image processing routines now functional at a practical level. A micrograph of a specimen of Nb-Sn superconductor wire is exhaustively analyzed. This specimen is found to contain approximately 70 percent Nb3Sn, nearly all of which is mutually interconnected. It is also found that in this specimen the mean free path in the Nb3Sn superconducting phase is only 26.5 microns. This small value results from the spongy structure of the material and numerous interruptions caused by voids and by particles of four other solid phases. The comparative importance of the several types of interruptions is measured. It is determined that small voids are the most important single cause of the short mean free path, and deduced that these voids appear to have formed mainly from the reaction during heat treatment.
{"title":"Quantitative Metallography With a Digital Computer: Application to a Nb-Sn Superconducting Wire.","authors":"G. Moore, L. Wyman","doi":"10.6028/JRES.067A.013","DOIUrl":"https://doi.org/10.6028/JRES.067A.013","url":null,"abstract":"Accurate quantitative data pertinent to the structure of solid materials at the micro size level, which are difficult or prohibitive to obtain by traditional manual measurements, are now obtained directly by a digital computer which uses a photomicrograph as the information input. The history of picture interpretation experiments at the National Bureau of Standards is reviewed. The fundamental computer operations are illustrated, together with a description of 24 image processing routines now functional at a practical level. A micrograph of a specimen of Nb-Sn superconductor wire is exhaustively analyzed. This specimen is found to contain approximately 70 percent Nb3Sn, nearly all of which is mutually interconnected. It is also found that in this specimen the mean free path in the Nb3Sn superconducting phase is only 26.5 microns. This small value results from the spongy structure of the material and numerous interruptions caused by voids and by particles of four other solid phases. The comparative importance of the several types of interruptions is measured. It is determined that small voids are the most important single cause of the short mean free path, and deduced that these voids appear to have formed mainly from the reaction during heat treatment.","PeriodicalId":94340,"journal":{"name":"Journal of research of the National Bureau of Standards. Section A, Physics and chemistry","volume":"71 1","pages":"127-147"},"PeriodicalIF":0.0,"publicationDate":"1963-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"73012624","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Moiré fringes produced by soft X-rays passing through crossed gratings of fine wire mesh are demonstrated. Regular systems of bands appearing superimposed on radio-micrographs of oriented cellulosic structures may also be moiré fringes. These fringes could be formed by fibrillate structures acting as crossed diffraction gratings.
{"title":"Moiré Fringes Produced by a Point Projection X-ray Microscope.","authors":"S. Newman","doi":"10.6028/jres.067a.014","DOIUrl":"https://doi.org/10.6028/jres.067a.014","url":null,"abstract":"Moiré fringes produced by soft X-rays passing through crossed gratings of fine wire mesh are demonstrated. Regular systems of bands appearing superimposed on radio-micrographs of oriented cellulosic structures may also be moiré fringes. These fringes could be formed by fibrillate structures acting as crossed diffraction gratings.","PeriodicalId":94340,"journal":{"name":"Journal of research of the National Bureau of Standards. Section A, Physics and chemistry","volume":"73 1","pages":"149-151"},"PeriodicalIF":0.0,"publicationDate":"1963-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77871090","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
The present work deals with the broadening of rotational lines of the carbon monoxide 2-0 band by both argon and hydrogen chloride. A high resolution grating spectrometer with a spectral slit width of 0.07 cm-1 was used, necessitating only a small correction in observed half-width values. Sufficiently small contributions of CO self-broadening were obtained by using long pathlength cells of 12 meters for CO-argon mixture and 1 meter for CO-HCl mixture. Half-width results, which are considered accurate to within ±5 percent, are presented in the form of a table and by a graph.
{"title":"Broadening of the Rotational Lines of Carbon Monoxide by HCl and by Argon.","authors":"R. J. Thibault, J. H. Jaffe, E. K. Plyler","doi":"10.6028/JRES.067A.011","DOIUrl":"https://doi.org/10.6028/JRES.067A.011","url":null,"abstract":"The present work deals with the broadening of rotational lines of the carbon monoxide 2-0 band by both argon and hydrogen chloride. A high resolution grating spectrometer with a spectral slit width of 0.07 cm-1 was used, necessitating only a small correction in observed half-width values. Sufficiently small contributions of CO self-broadening were obtained by using long pathlength cells of 12 meters for CO-argon mixture and 1 meter for CO-HCl mixture. Half-width results, which are considered accurate to within ±5 percent, are presented in the form of a table and by a graph.","PeriodicalId":94340,"journal":{"name":"Journal of research of the National Bureau of Standards. Section A, Physics and chemistry","volume":"21 1","pages":"113-114"},"PeriodicalIF":0.0,"publicationDate":"1963-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82744019","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
The complex bulk compliance (dynamic compressibility) of a commercial sample of poly (vinyl acetate), AYAT, was measured at frequencies from 50 to 1,000 cycles per second, temperatures from 0 to 100 °C, and static hydrostatic stresses from 0 to 981 bars (gage pressure) using an alternating hydrostatic stress generated and detected by piezoelectric transducers mounted in an essentially noncompliant cavity with dimensions small in comparison to a wavelength. The above temperature range was more than sufficient to cover the dispersion region in which an inflection in the storage compliance and a maximum in the loss compliance were observed. The data were reduced to functions of reduced variables using the WLF Equations extended to include static pressure with the “universal” WLF Constants and dT/dP = 0.020 °C/bar. The difference in limiting compliances at zero and infinite frequencies was larger than that predicted from the dT/dP shift using the free volume concept. A discussion is presented on possible processes that might contribute to an excessive value between limiting compliances.
{"title":"Dynamic Compressibility of Poly (Vinyl Acetate) and Its Relation to Free Volume","authors":"J. McKinney, H. .. Belcher","doi":"10.6028/jres.067A.007","DOIUrl":"https://doi.org/10.6028/jres.067A.007","url":null,"abstract":"The complex bulk compliance (dynamic compressibility) of a commercial sample of poly (vinyl acetate), AYAT, was measured at frequencies from 50 to 1,000 cycles per second, temperatures from 0 to 100 °C, and static hydrostatic stresses from 0 to 981 bars (gage pressure) using an alternating hydrostatic stress generated and detected by piezoelectric transducers mounted in an essentially noncompliant cavity with dimensions small in comparison to a wavelength. The above temperature range was more than sufficient to cover the dispersion region in which an inflection in the storage compliance and a maximum in the loss compliance were observed. The data were reduced to functions of reduced variables using the WLF Equations extended to include static pressure with the “universal” WLF Constants and dT/dP = 0.020 °C/bar. The difference in limiting compliances at zero and infinite frequencies was larger than that predicted from the dT/dP shift using the free volume concept. A discussion is presented on possible processes that might contribute to an excessive value between limiting compliances.","PeriodicalId":94340,"journal":{"name":"Journal of research of the National Bureau of Standards. Section A, Physics and chemistry","volume":"4 1","pages":"43 - 53"},"PeriodicalIF":0.0,"publicationDate":"1963-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84102650","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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