Pub Date : 1963-01-01Epub Date: 1963-02-01DOI: 10.6028/jres.067A.004
Wm Bruce Olson, Harry C Allen, Earle K Plyler
Two infrared absorption bands of CH2D2 have been analyzed in the semirigid rotor approximation. These are the A-type band at 2671.67 cm-1 and the C-type band at 4425.61 cm-1. The A-type band has previously been assigned as v3+v9, and the C-type band is tentatively assigned as v3+v6 The upper state of the A-type band is perturbed presumably by the close lying level 2v5. This interaction has not been investigated. The following values were found for the rotational constants of the ground vibrational state: A0=4.303 cm-1, B0= 3.504 cm-1, C0= 3.049 cm-1.
根据半刚性转子近似分析了 CH2D2 的两个红外吸收带。它们分别是 2671.67 cm-1 处的 A 型带和 4425.61 cm-1 处的 C 型带。A 型带先前被归为 v 3+v 9，而 C 型带则暂时被归为 v 3+v 6。这种相互作用尚未得到研究。地面振动状态的旋转常数值如下：A 0=4.303 cm-1，B 0=3.504 cm-1，C 0=3.049 cm-1。
{"title":"Analysis of Two Infrared Bands of CH<sub>2</sub>D<sub>2</sub>.","authors":"Wm Bruce Olson, Harry C Allen, Earle K Plyler","doi":"10.6028/jres.067A.004","DOIUrl":"10.6028/jres.067A.004","url":null,"abstract":"<p><p>Two infrared absorption bands of CH<sub>2</sub>D<sub>2</sub> have been analyzed in the semirigid rotor approximation. These are the A-type band at 2671.67 cm<sup>-1</sup> and the C-type band at 4425.61 cm<sup>-1</sup>. The A-type band has previously been assigned as <i>v</i> <sub>3</sub>+<i>v</i> <sub>9</sub>, and the C-type band is tentatively assigned as <i>v</i> <sub>3</sub>+<i>v</i> <sub>6</sub> The upper state of the A-type band is perturbed presumably by the close lying level 2<i>v</i> <sub>5</sub>. This interaction has not been investigated. The following values were found for the rotational constants of the ground vibrational state: <i>A</i> <sub>0</sub>=4.303 cm<sup>-1</sup>, <i>B</i> <sub>0</sub>= 3.504 cm<sup>-1</sup>, <i>C</i> <sub>0</sub>= 3.049 cm<sup>-1</sup>.</p>","PeriodicalId":94340,"journal":{"name":"Journal of research of the National Bureau of Standards. Section A, Physics and chemistry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1963-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC5324955/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79279539","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}
Pub Date : 1963-01-01Epub Date: 1963-02-01DOI: 10.6028/jres.067A.003
S J Schneider, J L Waring
The phase equilibrium diagram was determined for the Sc2O3-Ga2O3 system. A quenching furnace, wound with 60 percent Pt-40 percent Rh wire, was employed for experiments conducted at temperatures up to 1,800 °C. An induction furnace, having an iridium crucible susceptor, was used to obtain higher temperatures. Temperatures in the quenching furnace were measured with both an optical pyrometer and a 95 percent Pt-5 percent Rh versus 80 percent Pt-20 percent Rh thermocouple. The melting point of Ga2O3 was determined as 1,795 ±15 °C. Experiments at temperatures as high as 2,405 °C failed to melt Sc2O3. Two intermediate binary phases, a compound believed to be 6Sc2O3·5Ga2O3 and a solid solution occur in the system. The solid solution phase appears as a single phase in the region roughly defined by the compositional limits of 55 to 73 mole percent Ga2O3 at the solidus. The 6:5 compound, stable only at high temperatures, melts incongruently at 1,770 ±15 °C and decomposes below 1,700 ±15 °C. The compound appears to have orthorhombic symmetry with a=13.85 A, b= 9.80 A, and c=9.58 A. The indicated uncertainties in the melting points are a conservative estimate of the overall inaccuracies.
{"title":"Phase Equilibrium Relations in the Sc<sub>2</sub>O<sub>3</sub>-Ga<sub>2</sub>O<sub>3</sub> System.","authors":"S J Schneider, J L Waring","doi":"10.6028/jres.067A.003","DOIUrl":"10.6028/jres.067A.003","url":null,"abstract":"<p><p>The phase equilibrium diagram was determined for the Sc<sub>2</sub>O<sub>3</sub>-Ga<sub>2</sub>O<sub>3</sub> system. A quenching furnace, wound with 60 percent Pt-40 percent Rh wire, was employed for experiments conducted at temperatures up to 1,800 °C. An induction furnace, having an iridium crucible susceptor, was used to obtain higher temperatures. Temperatures in the quenching furnace were measured with both an optical pyrometer and a 95 percent Pt-5 percent Rh versus 80 percent Pt-20 percent Rh thermocouple. The melting point of Ga<sub>2</sub>O<sub>3</sub> was determined as 1,795 ±15 °C. Experiments at temperatures as high as 2,405 °C failed to melt Sc<sub>2</sub>O<sub>3</sub>. Two intermediate binary phases, a compound believed to be 6Sc<sub>2</sub>O<sub>3</sub>·5Ga<sub>2</sub>O<sub>3</sub> and a solid solution occur in the system. The solid solution phase appears as a single phase in the region roughly defined by the compositional limits of 55 to 73 mole percent Ga<sub>2</sub>O<sub>3</sub> at the solidus. The 6:5 compound, stable only at high temperatures, melts incongruently at 1,770 ±15 °C and decomposes below 1,700 ±15 °C. The compound appears to have orthorhombic symmetry with <i>a</i>=13.85 A, <i>b</i>= 9.80 A, and <i>c</i>=9.58 A. The indicated uncertainties in the melting points are a conservative estimate of the overall inaccuracies.</p>","PeriodicalId":94340,"journal":{"name":"Journal of research of the National Bureau of Standards. Section A, Physics and chemistry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1963-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC5324953/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83140793","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}
Pub Date : 1963-01-01Epub Date: 1963-02-01DOI: 10.6028/jres.067A.005
George Marinenko, John K Taylor
A method has been developed for the precise assay of halides by constant-current coulometric titration with silver ions generated at a silver anode. It is shown that a 4 milliequivalents sample of halide can be titrated with standard deviation of 0.005 percent.
{"title":"Precise Coulometric Titrations of Halides.","authors":"George Marinenko, John K Taylor","doi":"10.6028/jres.067A.005","DOIUrl":"10.6028/jres.067A.005","url":null,"abstract":"<p><p>A method has been developed for the precise assay of halides by constant-current coulometric titration with silver ions generated at a silver anode. It is shown that a 4 milliequivalents sample of halide can be titrated with standard deviation of 0.005 percent.</p>","PeriodicalId":94340,"journal":{"name":"Journal of research of the National Bureau of Standards. Section A, Physics and chemistry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1963-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC5324956/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"72756367","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}
Pub Date : 1963-01-01Epub Date: 1963-02-01DOI: 10.6028/jres.067A.009
Carl Halpern
The effect of small quantities of methyl bromide, up to 0.5 percent by volume, on the flame speed of methane-air mixtures has been determined. Maximum flame speeds, at given experimental conditions, are reduced proportionately to the amount of methyl bromide added. Flame speeds of rich mixtures are reduced much more than are flame speeds of lean mixtures. Reaction zone thickness of methane-air flames is increased by the addition of methyl bromide and the thickness increases with the amount of methyl bromide.
{"title":"Effect of Methyl Bromide Additions on the Flame Speed of Methane.","authors":"Carl Halpern","doi":"10.6028/jres.067A.009","DOIUrl":"10.6028/jres.067A.009","url":null,"abstract":"<p><p>The effect of small quantities of methyl bromide, up to 0.5 percent by volume, on the flame speed of methane-air mixtures has been determined. Maximum flame speeds, at given experimental conditions, are reduced proportionately to the amount of methyl bromide added. Flame speeds of rich mixtures are reduced much more than are flame speeds of lean mixtures. Reaction zone thickness of methane-air flames is increased by the addition of methyl bromide and the thickness increases with the amount of methyl bromide.</p>","PeriodicalId":94340,"journal":{"name":"Journal of research of the National Bureau of Standards. Section A, Physics and chemistry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1963-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC5324960/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79565108","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}
The six elastic constants (and six elastic compliances) of rutile were determined in the kilocycle per second frequency range by a resonance method. The standard deviations range from 0.2 percent for s11 to 4.3 percent for s13.
{"title":"Elastic Constants of Rutile (TiO2)","authors":"J. B. Wachtman, W. E. Tefft, D. G. Lam","doi":"10.6028/jres.066A.047","DOIUrl":"https://doi.org/10.6028/jres.066A.047","url":null,"abstract":"The six elastic constants (and six elastic compliances) of rutile were determined in the kilocycle per second frequency range by a resonance method. The standard deviations range from 0.2 percent for s11 to 4.3 percent for s13.","PeriodicalId":94340,"journal":{"name":"Journal of research of the National Bureau of Standards. Section A, Physics and chemistry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1962-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81500930","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 relative ultraviolet stability of four chemically modified polycaprolactam (Nylon-6) systems is discussed: methylmethoxylated fibers and three other fibers having methylene, disulfide, and alkylene sulfide crosslinks, respectively. The ultraviolet degradation of these systems is studied by means of a sensitive analytical technique in which the methylene (—CH2—) groups remaining in the chemically modified fibers after irradiation are converted to formaldehyde; the liberated formaldehyde is then reacted with chromotropic acid to give a colored product, the absorbancy of which can be determined spectrophotometrically. The results indicate that the data can be expressed by first order rate equations from which the rate constants may be calculated. The scission of the crosslinks is accompanied by a decrease in the internal orientation of the networks as shown by X-ray diffraction photographs.
{"title":"Ultraviolet Stability of Crosslinked Polycaprolactam Systems","authors":"S. D. Bruck","doi":"10.6028/jres.066A.050","DOIUrl":"https://doi.org/10.6028/jres.066A.050","url":null,"abstract":"The relative ultraviolet stability of four chemically modified polycaprolactam (Nylon-6) systems is discussed: methylmethoxylated fibers and three other fibers having methylene, disulfide, and alkylene sulfide crosslinks, respectively. The ultraviolet degradation of these systems is studied by means of a sensitive analytical technique in which the methylene (—CH2—) groups remaining in the chemically modified fibers after irradiation are converted to formaldehyde; the liberated formaldehyde is then reacted with chromotropic acid to give a colored product, the absorbancy of which can be determined spectrophotometrically. The results indicate that the data can be expressed by first order rate equations from which the rate constants may be calculated. The scission of the crosslinks is accompanied by a decrease in the internal orientation of the networks as shown by X-ray diffraction photographs.","PeriodicalId":94340,"journal":{"name":"Journal of research of the National Bureau of Standards. Section A, Physics and chemistry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1962-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84039786","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}
A procedure is described for the separation of hafnium from zirconium and their individual determination. The sample is dissolved in sulfuric and hydrofluoric acids and the hydrofluoric acid removed by fuming. After dilution with water, the solution is transferred to a column containing a strong quaternary amine anion-exchange resin (Dowex-1). The hafnium is eluted with diluted (3.5 percent by volume) sulfuric acid solution. Zirconium is removed by elution with 10 percent by volume sulfuric acid solution. The elements are precipitated with cupferron, ignited, and weighed as the oxides. For samples containing from twenty to eighty percent of zirconium, a second separation of the hafnium fraction using the column is necessary.
{"title":"Separation of Hafnium from Zirconium and Their Determination: Separation by Anion-Exchange","authors":"L. A. Machlan, J. L. Hague","doi":"10.6028/jres.066A.053","DOIUrl":"https://doi.org/10.6028/jres.066A.053","url":null,"abstract":"A procedure is described for the separation of hafnium from zirconium and their individual determination. The sample is dissolved in sulfuric and hydrofluoric acids and the hydrofluoric acid removed by fuming. After dilution with water, the solution is transferred to a column containing a strong quaternary amine anion-exchange resin (Dowex-1). The hafnium is eluted with diluted (3.5 percent by volume) sulfuric acid solution. Zirconium is removed by elution with 10 percent by volume sulfuric acid solution. The elements are precipitated with cupferron, ignited, and weighed as the oxides. For samples containing from twenty to eighty percent of zirconium, a second separation of the hafnium fraction using the column is necessary.","PeriodicalId":94340,"journal":{"name":"Journal of research of the National Bureau of Standards. Section A, Physics and chemistry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1962-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88330144","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}
This paper describes the preparation, analysis, and certification of a new series of standard samples. These samples consist of commercially pure titanium containing hydrogen at three levels (32 ppm, 98 ppm, and 215 ppm) and have been designated National Bureau of Standards Standard Samples Nos. 352, 353, and 354, respectively.
{"title":"Titanium Standards for Hydrogen Content","authors":"J. Sterling, F. J. Palumbo, L. Wyman","doi":"10.6028/jres.066A.049","DOIUrl":"https://doi.org/10.6028/jres.066A.049","url":null,"abstract":"This paper describes the preparation, analysis, and certification of a new series of standard samples. These samples consist of commercially pure titanium containing hydrogen at three levels (32 ppm, 98 ppm, and 215 ppm) and have been designated National Bureau of Standards Standard Samples Nos. 352, 353, and 354, respectively.","PeriodicalId":94340,"journal":{"name":"Journal of research of the National Bureau of Standards. Section A, Physics and chemistry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1962-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88330893","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}
A batch adsorption equation was derived by integrating an irreversible rate equation obtained by neglecting the desorption term of the Langmuir adsorption-rate equation. The integrated equation was in reasonably good agreement with experiment and provided a means for determining from the data the parameters q0 and k1. These constants, namely, the adsorptive capacity and the adsorption rate constant, completely characterized the adsorption system at that temperature. Agreement was found between these batch adsorption parameters and their counterparts previously derived from column adsorption experiments when both types of adsorption were performed simultaneously.
{"title":"Batch Adsorption From Solution","authors":"W. V. Loebenstein","doi":"10.6028/jres.066A.052","DOIUrl":"https://doi.org/10.6028/jres.066A.052","url":null,"abstract":"A batch adsorption equation was derived by integrating an irreversible rate equation obtained by neglecting the desorption term of the Langmuir adsorption-rate equation. The integrated equation was in reasonably good agreement with experiment and provided a means for determining from the data the parameters q0 and k1. These constants, namely, the adsorptive capacity and the adsorption rate constant, completely characterized the adsorption system at that temperature. Agreement was found between these batch adsorption parameters and their counterparts previously derived from column adsorption experiments when both types of adsorption were performed simultaneously.","PeriodicalId":94340,"journal":{"name":"Journal of research of the National Bureau of Standards. Section A, Physics and chemistry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1962-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90636548","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}
Calorimetric measurements of the heat of solution of nitronium perchlorate (NO2ClO4) and of a mixture of potassium nitrate and potassium perchlorate in aqueous potassium hydroxide have been made. These are combined to give: NO2ClO4(c)+4KOH(in5300H2O)→KClO4(c)+KNO3(c)+2KOH(in5300H2O)+H2O(liq)ΔH=−285.80±0.38kj/mole=−68.31±0.09kcal/molefrom which the standard heat of formation of nitronium perchlorate is calculated as ΔHf°(25°C)NO2ClO4(c)=37.19±1.0kj/mole=8.89±0.25kcal/mole,in which the uncertainty represents twice the estimated overall standard deviation of the result.
{"title":"Heat of Formation of Nitronium Perchlorate","authors":"A. A. Gilliland","doi":"10.6028/JRES.066A.045","DOIUrl":"https://doi.org/10.6028/JRES.066A.045","url":null,"abstract":"Calorimetric measurements of the heat of solution of nitronium perchlorate (NO2ClO4) and of a mixture of potassium nitrate and potassium perchlorate in aqueous potassium hydroxide have been made. These are combined to give: NO2ClO4(c)+4KOH(in5300H2O)→KClO4(c)+KNO3(c)+2KOH(in5300H2O)+H2O(liq)ΔH=−285.80±0.38kj/mole=−68.31±0.09kcal/molefrom which the standard heat of formation of nitronium perchlorate is calculated as ΔHf°(25°C)NO2ClO4(c)=37.19±1.0kj/mole=8.89±0.25kcal/mole,in which the uncertainty represents twice the estimated overall standard deviation of the result.","PeriodicalId":94340,"journal":{"name":"Journal of research of the National Bureau of Standards. Section A, Physics and chemistry","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"1962-11-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89704171","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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