The analysis of tungsten and arsenic in steels

480 Pages·2017·10.77 MB·English

Loughborough University
Institutional Repository
The analysis of tungsten and
arsenic in steels
ThisitemwassubmittedtoLoughboroughUniversity’sInstitutionalRepository
by the/an author.
Additional Information:
• A Doctoral Thesis. Submitted in partial fulfilment of the requirements
for the award of the degree of Doctor of Philosophy at Loughborough
University.
Metadata Record: https://dspace.lboro.ac.uk/2134/36080
Publisher: (cid:13)c D.R. Marriott
Rights: This work is made available according to the conditions of the Cre-
ative Commons Attribution-NonCommercial-NoDerivatives 4.0 International
(CC BY-NC-ND 4.0) licence. Full details of this licence are available at:
https://creativecommons.org/licenses/by-nc-nd/4.0/
Please cite the published version.
LOUGHBOROUGH
UNIVERSITY OF TECHNOLOGY
LIBRARY
AUTHOR ',?
I F'_
MA~RIO, J) -
i
I
I
••••• , .................................... ~ ..........................................................................• •••••••••••••••••••• ................... •• ••••• · •• ·1
, ! iJ~GIJ+{" i
COpy NO.
.... ".. .................................. ...................................... ............................................................................. .
~ I..~
! VOl NO. CLASS MARK
FOR
R~fERENCE O~LY
002 2134 01
I
111 1111\ I11

/
TI1E ANALYSIS OF TUNGSTEN
AND ARSENIC IN STEELS
By
D. R. MARRIOTT
Supervisors
Dr. D. Thorburn Burns. and Dr. A. G. Fogg
Submitted for the degree of Doctor of
Philosophy of Loughborough University
of Technology
October. 1970.
Loughborough University
Of To ch/lOI0'n library
70
Date J)EC,.
Clasl
OZ:2IJJr
~~'
TO MY FATHER
E. R. MARRIOTT
\
PROGREDIAMUR
------------------------------
--- - - ._- ---
SUMMARY
The literature pertaining to the analysis of tungsten
and arsenic has been reviewed and methods developed for the
colorimetric determination of these elements in steels .
.
.
CONTENTS
I
CHAPTER 1 Preface 1
TUN G S TE N
CHAPTER 2 Introduction 3
CHAPTER 3 General Review 5
CHAPTER 4 Dissolution of Steels 68
CHAPTER 5 Determination by Gravimetry 99
CHAPTER 6 Calorimetric determination using Heteropoly Acids 125
CHAPTER 7 Calorimetric determinatiotl using Thiocyanate 169
CHAPTER 8 Final Discussion and Conclusions 222
A R S E N I C
CHAPTER 9 Introduction 227
CHAPTER 10 General Review 229
CHAPTER 11 Dissolution of Steels 297
CHAPTER 12 Solvent Extraction from Steel Solutions 303
CHAPTER 13 Calorimetric determination using M,olybdenum Blue 342
CHAPTER 14 Final Discussion and Conclusions 378
APPENDIX 1 Recommended Procedure for Tungsten 383
APPENDIX 2 Recommended Procedure for Arsenic 391
APPENDIX 3 Steel Analyses Tungsten 399
APPENDIX 4 Steel Analyses Arsenic 402
CHAPTER I
PREFACE
., J
· -------------
1.
, I
!
PREFACE
This thesis is a report of research ;,nto chemical methods for
the determination of tungsten and arsenic in steels. Of the series of
British Standard Methods devoted to the analysis of steels, several
of the proposed procedures are not completely satisfactory. This is
the case with the calorimetric methods proposed for tungsten and
arsenic.
The terms of reference for this work were to produce precise,
aocurate methods for these elements, suitable for use in
steelworks laboratories. Procedures investigated were to be capable
of being used by non-skilled laboratory personnel and to require
relatively inexpensive equipment. This negates the use of techniques
such as spectrograph'ic analysis, X-ray fluorescence, neutron activation,
'etc., for which satisfactory methods for tungsten and arsenic are
well documented. Possible techniques, in addition to gravimetry and
colorimetry, are flame emission, atomic absorption, and polarography,
,
although the latter was considered unsuitable due to its lack of
acceptance within the industry.
The approach adopted was to survey the literature for accepted
and less well known methods for the analysis of these elements in any
sample matrix. By consultation with representatives of the steel
industry, selected plausible approaches were investigated towards the
applicability of these to the specific problems associated with the
analysis of steels.
In this way, methods have been developed for the determination
of tungsten and arsenic in steels.