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LOS ALAMOS SCIENTIFIC LABORATORY of the UNIVERSITY of CALIFORNIA LOS ALAMOS NEW MEXICO REPORT WRITTEN: March 1959 REPORT DISTRIBUTED: August 27, 1959

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LOS ALAMOS SCIENTIFIC LABORATORY of the UNIVERSITY of CALIFORNIA LOS ALAMOS NEW MEXICO REPORT WRITTEN: March 1959 REPORT DISTRIBUTED: August 27, 1959 LEGAL NOTICE ThlB report was prepared as an account of Government sponsored work. Neither the United States, nor the Commission, nor any person acting on behalf of the Commission A. Makes any warranty or representation, expressed or Implied, with respect to the accu­ racy, completeness, or usefulness of the information contained In this report, or that the use of any InformaUon, apparatus, method, or process disclosed in this report may not Infringe privately own^ rights, or B. Assumes any liabilities with respect to the use of, or for damages resulting from the use of any information, a^iaratus, method, or ptocess disclosed la this report As used in the above, "person acting on behalf of the Commission" Includes any em­ ployee or contractor of the Commission, or employee of such contractor, to the extent that such employee or contractor of the Commission, or employee of such contractor prepares, disseminates, or provides access to, any Information pursuant to his employment or contract with the Commission, or his employment with such contractor. LA-2306 CHE MISTRY- - GENERAL (TID-4500, 14th edition) LOS ALAMOS SCIENTIFIC LABORATORY OF THE UNIVERSITY OF CALIFORNIA LOS ALAMOS NEW MEXICO REPORT WRITTEN: March 1959 REPORT DISTRIBUTED: August 27, 1959 THE ANALYSIS OF REFRACTORY BORIDES, CARBIDES, NITRIDES, AND SILICIDES by Owen H. Kriege This report expresses the opinions of the author or authors and does not necessarily reflect the opinions or views of the Los Alamos Scientific Laboratory. Contract W-7405-ENG, 36 with the U. S. Atomic Energy Commission - 1 - DISCLAIMER This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency Thereof, nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof. DISCLAIMER Portions of this document may be illegible in electronic image products. Images are produced from the best available original document. ABSTRACT Methods are presented for the analysis of kl refractory materials. An evaluation of the accuracy and the precision of these techniques is also given. The materials studied are the borides of hafnium, molybdenum, niobium, rhenium, tantalum, thorium, titanium, tungsten, uranium, vanadium, and zirconium; the carbides of hafnium, molybdenum, niobium, silicon, tantalum, thorium, titanium, tungsten, uranium, vanadium, and zirconium; the nitrides of boron, hafnium, niobium, silicon, tantalum, titanium, uranium, and zirconium; the silicides of molybdenum, rhenium, tantalum, titanium, tungsten, vanadium, and zirconium; and mixed carbides of uranium with hafnium, niobium, tantalum, or zirconium. ACKNOWLEDGMENTS The author is indebted to N. H. Krikorian, C. P. Kempter, J. C. McGuire, and W. G. Witteman for the preparation of many of the materials studied in this investigation. C. P. Kempter and N. H. Krikorian assisted greatly by identifying the phases present in refractory samples by X-ray studies. In addition, the author wishes to thank 0. R. Simi and coworkers for spectrographic analyses, and M. E. Smith and coworkers for oxygen determinations. CONTENTS Page ABSTRACT 5 ACKNOWLEDGMENTS 5 1. INTRODUCTION AND GENERAL DISCUSSION 9 Characteristic Properties of Refractories Which Are 10 Important to the Analyst Reliability 11 Preparation of Samples for Analysis 12 2. THE ANALYSIS OF REFRACTORY BORIDES 13 The Determination of Boron in the Borides of Hafnium, 13 Molybdenum, Niobium, Rhenium, Tantalum, Thorium, Titanium, Tungsten, Vanadium, and Zirconium The Determination of Boron in Uranium Boride Ik The Determination of Hafnium and Zirconium in Hafnium 15 and Zirconium Borides The Determination of Molybdenum in Molybdenum Boride 15 The Determination of Niobium and Tantalum in Niobium l6 and Tantalum Borides The Determination of Rhenium in Rhenium Boride 17 The Determination of Thorium in Thorium Boride 18 The Determination of Titanium in Titanium Boride 18 The Determination of Tungsten in Tungsten Boride 19 The Determination of Uranium in Uranium Boride 19 The Determination of Vanadium in Vanadium Boride 20 -5- Page The Determination of Carbon in the Borides of Hafnium, 20 Molybdenum, Niobium, Rhenium, Tantalum, Thorium, Titanium, Tungsten, Uranium, Vanadium, and Zirconium THE ANALYSIS OF REFRACTORY CARBIDES 2k The Determination of Total Carbon in the Carbides of 2k Hafnium, Molybdenum, Niobium, Tantalum, Thorium, Titanium, Tungsten, Uranium, Vanadium, and Zirconium, and the Mixed Carbides of Uranium with Hafnium, Niobium, Tantalum, or Zirconium The Determination of Total Carbon in Silicon Carbide 26 The Determination of Graphite in the Carbides of Hafnium, 27 Molybdenum, Niobium, Tantalum, Thorium, Titanium, Tungsten, Uranium, Vanadium, and Zirconium, and the Mixed Carbides of Uranium with Hafnium, Niobium, Tantalum, or Zirconium The Determination of Graphite in Silicon Carbide 28 The Determination of Total Metal in the Carbides of 28 Hafnium, Niobium, Tantalum, Thorium, Titanium, Tungsten, Uranium, Vanadium, and Zirconium The Determination of Molybdenum in Molybdenum Carbide 29 The Determination of Silicon in Silicon Carbide 50 The Determination of Hafnium and Zirconium in Mixed 31 Carbides of Uranium with Hafnium or Zirconium The Determination of Uranium in Mixed Carbides of Uranium 31 with Hafnium or Zirconium The Determination of Niobium, Tantalum, and Uranium in 32 Mixed Carbides of Uranium with Niobium or Tantalum The Determination of Nitrogen in the Carbides of Hafnium, 33 Niobium, Tantalum, Titanium, Tungsten, Uranium, Vanadium, and Zirconium, and the Mixed Carbides of Uranium with Hafnium, Niobium, Tantalum, or Zirconium Pag THE ANALYSIS OF REFRACTORY NITRIDES 38 The Determination of Nitrogen in the Nitrides of Hafnium, 38 Niobium, Tantalum, Titanium, Uranium, and Zirconium The Determination of Nitrogen in Boron Nitride and 38 Silicon Nitride The Determination of Boron in Boron Nitride 39 The Determination of Total Metal in the Nitrides of kO Hafnium, Niobium, Tantalum, Titanium, Uranium, and Zirconium The Determination of Silicon in Silicon Nitride kl The Determination of Total Carbon in the Nitrides of k2 Hafnium, Niobium, Tantalum, Titanium, Uranium, and Zirconium The Determination of Total Carbon in Boron Nitride and k2 Silicon Nitride The Determination of Graphite in the Nitrides of Hafnium, k'^ Niobium, Tantalum, Titanium, Uranium, and Zirconium THE ANALYSIS OF REFRACTORY SILICIDES I+7 The Determination of Silicon in the Silicides of ^+7 Molybdenum, Rhenium, Tantalum, Titanium, Tungsten, Vanadium, and Zirconium. The Determination of Molybdenum in Molybdenum Silicide kQ The Determination of Rhenium in Rhenium Silicide k8 The Determination of Tantalum in Tantalum Silicide k^ The Determination of Titanium in Titanium Silicide 50 The Determination of Tungsten in Tungsten Silicide 50 The Determination of Vanadium in Vanadium Silicide 5I The Determination of Zirconium in Zirconium Silicide 5I Pag 6. SUMMARY 5^ REFERENCES 58 TABLES Table I Results of the Analysis of Refractory Borides 22 by Recommended Procedures Table II Recommended Combustion Temperatures for Carbides 25 Table III Results of the Analysis of Simple Refractory Carbides 35 by Recommended Procedures Table IV Results of the Analysis of Mixed Refractory Carbides 36 by Recommended Procedures Table V Results of the Analysis of Refractory Nitrides by k"^ Recommended Procedures Table VI Results of the Analysis of Refractory Silicides 55 by Recommended Procedures FIGURES Figure 1 Detailed drawing of a combustion train for the 23 determination of carbon Figure 2 Detailed drawing of the Dumas apparatus for the 57 determination of nitrogen Figure 5 Detailed drawing of the caustic fusion apparatus k6 for the determination of nitrogen 1. INTRODUCTION AND GENERAL DISCUSSION The use of various oxides and silicates as refractory materials has been widespread for many years; however, since World War II there has been a rapid increase of interest in other types of refractory materials among chemists, chemical engineers, metallurgists, and, more recently, nuclear engineers. Because of interest in research involving temperatures as high as 35^0° C, refractories of types other than oxides and silicates have become of increasing importance. It seems logical to conclude that demands for better and special refractories will greatly increase in the future. The property most generally sought is chemical inertness at very high temperatures. This requires that the material have a high melting point, that it not react with its environment at high temperatures, and in many cases that it maintain considerable structural strength at these temperatures. The types of materials that hold the most promise of generally fulfilling many present day needs are the borides, carbides, nitrides, and silicides of certain transition metals. This paper describes methods that have been satisfactorily applied to the analysis of refractory
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