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ON THE ESTIMATION OF SMALL QUANTITIES OF PHOS
PHORUS IN IRON AND STEEL BY THE SPECTRUM
ANALYSIS.
By Sir JOHN G. N. ALLEYNE, Bart., Butterley.
INTRODUCTION.
This is not the first time that the subject of the spectrum analysis
has been brought before the Iron and Steel Institute. At th®
London meeting of the Institute, in March, 1871, Professor Roscoe
read a paper on the subject; that paper is included in the Pro
ceedings, and will be found in Vol. II, 1871, of the Journal. The
Professor, after very fully describing the spectroscope itself, and
exhibiting and experimenting with sundry apparatus, in speaking
of the spectrum of the Bessemer flame, says, “ Why do we not see
the spectrum of phosphorus ? I think the analysis of the slag will
tell us why we do not see phosphorus in the flame, for the
good reason that it is not there. A very small quantity of it is
contained in the pig, and this we know quite well does not come
out, though many people here wish it would, but it remains in the
iron, so that I think it rather hard upon us to be told you cannot
do us any good at all, because you cannot tell us anything about
silicon or anything about phosphorus. In spite, however, of these
shortcomings, I hope what I have said will show you that spectrum
analysis is not wholly without its use, and that we may really
believe it will, in time to come, be much more largely employed
than it is at present, so that we may succeed, in the end, in doing
what we originally intended to tell you: when to stop your blow,
so as to have finished steel in your converters, without having
added any spiegel at alb”
Following at a very humble distance the great discoverers in
Solar physics, Augstrom and Kirchhoff, in Germany, Huggins and
�2
ESTIMATION OF SMALL QUANTITIES OF PHOSPHORUS
Lockyer, in our own country, the author has long been of 'opinion
that, if they, by means of the spectroscope, can analyse the sun—if
they can, by means of the cross prism or prism of comparison,
prove to demonstration that most of, or all, the metallic elements
and the various constituents of which this earth is formed, are
found in a state of incandescence in the sun; if Dr. Huggins, by
the displacement of the hydrogen line, can calculate whether a
star is approaching to or receding from the earth,—we should be
able to apply this system to our manufacturing operations. In
bringing the subject again before the Institute, the author wishes
to acknowledge the great advantage he has derived from the
study of the published investigations of the gentlemen before
mentioned, Dr. Huggins, Professors Augstrom and Kirchhoff, and
Mr. Lockyer. He would especially point out to the Institute that,
as practical manufacturers and engineers, it is their special business
to apply, and apply rightly, the powers of nature to operations
of the manufactory, it is the very basis of all improvement, the
very charter of the Institution of Civil Engineers, of which the
author and many of the members of the Iron and Steel Institute
have the honour of being members. To quote the words of the
late Mr. Thos. Tredgold, “ A society for the general advancement
of mechanical science, and more particularly for promoting the
acquisition of that species of knowledge which constitutes the
profession of a civil engineer, being the art of directing the great
sources of power in nature for the use and convenience of man.” It
is on this principle that the author invites the co-operation of the
Institute, as well as that of, as it were, the parent society, the
Institution of Civil Engineers, by whose kindness we are this day
assembled in these rooms. The subject is very large, the field of
enquiry and investigation which it opens is enormous—light, heat,
and electricity. It is impossible to say into what ramifications
a discussion may lead, bringing forward questions which in all
probability the author would be unable to answer; and which
are infinitely beyond the reasonable range of a single paper. It
is with this view that it is proposed to confine the subject
of the present paper to the estimation of phosphorus, by
means of electricity of high tension, the power of absorption of
hydrogen gas, and the spectroscope. The science of spectrum
�IN IRON AND STEEL BY THE SPECTRUM ANALYSIS,
3
analysis is a new one, one which will, if successful, be of the greatest
advantage in our blast furnace, forge, and steel manufacturing
operations, indeed to all manufactories where a qualitative or
quantitative analysis of the materials is required. If the subject
is brought before the Institute in too crude a state, the author
would plead, as his excuse, that it was his ambition that the
Institute should work it out for themselves, that a quantitative
analysis should emanate from one of themselves, and that they
should not wait until some of the great discoverers, before alluded
to, had time to turn their attention to terrestrial investigations,
and show us that the same law which applied to the absorption lines
of the sun’s atmosphere, and the effect of his rays passing through
the atmosphere of the earth, could be applied to the quantitative
analysis of the iron and steel as it passes from one process
of manufacture to another. The author does not presume
to come before the Institute and state that he has made a complete
quantitative analysis of iron by Spectrum Analysis, but hopes
that he will be able to show that he has made some progress
towards that result. Taking up the subject, then, where Professor
Roscoe left it in March, 1871, the author had first to get aspectrum
of iron, and to find the requisite apparatus. Mr. Alfred Apps, of
the Strand, furnished a powerful Grove’s Battery, an induction coil
capable of giving a spark of 12 inches between the secondary poles,
and a Leyden Battery of 4 one gallon jars. The coil was of very much
the same construction as that which he has now lent to further
illustrate this paper, and which he has kindly offered to set to work,if
the members wish to see it in operation. This offer the Council has
accepted. A spectroscope, by Mr. John Browning, with a battery
of 4 prisms of dense flint glass formed the first batch of apparatus.
The author certainly has, after a great number of experiments and
much study, formed an opinion of his own, but his wish and inten
tion is to describe a number of those experiments, showing the results
to which they lead, and leaving the members to form their own
conclusions, inviting, nevertheless, their co-operation and assist
ance. Professors Augstrom and Thalen state that there are 460
lines in the spectrum of iron. Dr. Watts, in his index of spectrum,
gives—Kirchkoff 71, Thaldn 148, Huggins 101; but there are also
present the atmospheric lines, which, in his index of spectra, give—
�4
ESTIMATION OF SMALL QUANTITIES OF PHOSPHORUS
Huggins, 32 for oxygen, and nitrogen 78. The question first to be
decided was, which of all that multitude of lines are atmospheric
lines, which sulphur, calcium, manganese, phosphorus, &c., &c. It
was very soon obvious that the spectra obtained from Geissler’s
vacuum tubes, although most beautifully made and contrived, gave
the spectra under totally different conditions from those in which
they exist in our iron. The curve recommended by Dr. Watts
was tried, but the author found that the construction of the
spectroscope was such that he could not work with certainty and
accuracy. After many trials and experiments, with the details of
which it is needless to trouble the Institute, he determined to work
wholly by spectra of comparison. But considerable difficulty arose
with silica, alumina, and sulphur, as well as phosphorus. First, as to
the means of holding them as electrodes ; secondly, they are very
bad conductors. A piece of fire brick, held in the nippers, will give
no spectrum, the spark jumps over it in the most clever way, and
gives nothing but the spectrum of the nippers, be they brass or
steel. Some of the small tubes, samples of which are on the table,
were made—they are shown at No. 7 in the drawing. The object
here was to bury the electrode in the pounded fire brick, and force
the current to pass through it. These are obviously a modifica
tion of Geissler’s tubes. The lines of silica and alumina shine out
with splendour, but they do not last long, the glass gets coated
with the material which is decomposed by the spark, and forms a
conductor, the spark only passing in fitful flashes as at X, and
giving but very little light; on the whole, the best way of charging
the tube is, as shown at the drawing No. 8, letting the platinum
electrode come through the throat of the tube, and burying the
lower electrode in the powder under examination; this has the
further advantage that the spectrum of the glass itself does not
intrude, the lines of the platinum must, of course, be noted, and
not confused with those of the powder. The spectra of iron ores
come out very well by this method. The nozzles A B are for letting
in gas. This being the most difficult spectrum with which the
author has had to deal, he has thought it better to explain it
before proceeding to phosphorus, which forms the main subject of the
paper. The phosphorus lines were got in this way—a small hole was
drilled into a piece of carbon and filled up with phosphorus, the
�IN IRON AND STEEL BY THE SPECTRUM ANALYSIS.
5
phosphorus worked over the carbon like the head of a rivet, so that
the spark could not get from one carbon electrode to the other without
volatilizing the phosphorus; but it is quite obvious that this .method
•would not do in atmospheric air, the spectrum must be taken in a
gas with which the phosphorus could not enter into combustion,
orkit would simply light in the spark, combine with the oxygen,
and fill the cylinder with phosphoric acid. Carbonic acid, hydrogen,
nr the common coal gas, all do very well for this. A special appara
tus, however, had to be fitted up, which is on the table, and is
shown on the drawing at No. 2. The lines of phosphorus on a
carbon point, taken in this way in coal gas, are shown on the
spectrum on the drawing at No. 9. It will be seen at once that
the characteristic features of phosphorus are seven broad bands in
the green, there are also three very peculiar lines in the red, like a
wicket with the middle stump thinner than the other two. There
is also the same kind of group in sulphur, but in a different position
in the red, by no means coincident. The lines of both sulphur
and phosphorus are got by comparison, that is, one pair of electrodes
were prepared with a phosphorus point, as before described, and
another pair, from exactly the same carbon, were prepared without
phosphorus; each pair was fitted into one of the glass cylinders,
the cylinders were filled with coal gas, each with a separate
branch pipe, and the gas lit, the pair of plain carbon electrodes
were arranged in front of the slit of the collimator of the spectro
scope, and the phosphorus pair were arranged opposite the cross
prism, or prism of comparison. The two spectra are seen—the
phosphorus above, and the carbon below, in the usual way. The
lines which coincide are those.of carbon and coal gas, a beautiful
spectrum well worthy of study, but one with which for the
present we have nothing to do.
The lines which do not
-coincide are those of phosphorus and anything the phosphorus
may contain; the readings on the dividing plate must be
-carefully noted.
We have now to look for phosphorus in
•our iron. The plain carbon points must be removed—the nippers
replaced with a clean pair, the cylinder covers cleaned, and the
iron electrodes, to be examined; put in. The iron is now in air,
•the phosphorus in coal gas, the lines which coincide are produced
<by phosphorus in the iron which is decomposed by the spark, taking
�6
ESTIMATION OF SMALL QUANTITIES OF PHOSPHORUS
care to note which were the readings taken as phosphorus linesin the last experiment, for there may be silicon, sulphur, and other
impurities in the carbon—there is certainly also carbon itself, all of
which are present in the iron. There is, however, little or no risk
of any confusion on this point. All the coincident lines in ordinary
pig, puddled, or bar iron, are in the green, or very near to it. The
seven lines or bands of the phosphorus are much broader, those of
fairly good iron, very fine, sharp, and bright. The idea struck theauthor, are not those iron lines brighter than the phosphorus itself,!
because they are in an atmosphere containing oxygen ? The ques-'
tion was soon put and answered, the coal gas was let into the iron
cylinder, and the lines vanished entirely; but the spectrum of coal,
gas does not do very well for this purpose. It has numerous lines of
its own, which have to be eliminated, the; part of the spectrum—the
green—where the characteristic lines of phosphorus occur, is ruled
all over by the most extraordinary number of dark absorption lines,,
through the intervals of which the brighter parts of the continuous
spectrum of the spark are seen. It is most difficult to determine
whether these are, as supposed, bright spaces of a superimposed
spectrum, or lines. Hydrogen gas is much better as an absorber,,
or as a gas in which, oxygen being absent, no combustion can take
place. It is needless to point out here that, in using hydrogen, the
greatest care must be taken to avoid explosions. The practice in
these experiments has been to fill all the cylinders and pipes withcoal gas, light it, and to displace this gas with hydrogen. It is found
that, when there are twelve cubic inches of hydrogen, as measured
by the graduated bottle hereafter to be described, the carbon
rulings (if that can be accepted as a proper term) disappear. The
lines of the spectrum, which in air are bright, and which coincide
with those of phosphorus and sulphur, are completely blotted out
or absorbed. The conclusion which the author has come to is that,
when small quantities of phosphorus or other matters are present
in the electrodes, they require oxygen in some form to bring them
out as bright lines. He is confirmed in this view by other writers.
In Schellen’s Spectrum Analysis, page 162, after describing
Professor Tyndall’s discovery of another line in Lithium, in the
intense heat of the Voltaic arc, he says : “ If a few grains of common
salt be dropped into the flame of a Bunsen burner, there is emitted.
�IN IRON AND STEEL BY THE SPECTRUM ANALYSIS.
7
an intense light of one colour, producing the spectrum of a
single yellow line. If the temperature of the flame be raised
by a further supply of oxygen, the brilliancy of this line is
immediately augmented, and the number of coloured lines so much
increased, as to approach somewhat to a continuous spectrum.” It
may be that the lines are only obscured by the spectrum of
hydrogen as a screen, or as a piece of coloured glass. If this should
prove the correct explanation, it can, just as well as the first
supposition, which the author has accepted as the true one, be used
as a means of measuring the quantity present in the spark, and
arriving at a correct estimation of that quantity by the spectrum
analysis. By the first supposition, we calculate the quantity
inversely, as the quantity of oxygen, or a compound of oxygen used;
by the second, we alter the character and condition of the screen,
it becomes less dense by admixture with the oxygen compound,
until the line is able to penetrate. If a large quantity of
phosphorus is undergoing deflagration at the electrodes, it will
penetrate a screen of considerable density. If a small quantity only
is undergoing decomposition, the density of the screen must be
reduced, until the line can penetrate it; in either case the quantity
can be estimated inversely, as the quantity of oxygen that has been
used, or on same ratio as represented by the curve on the drawing,
No. 1. In comparing a phosphide of iron with phosphorus, or a
sulphide of iron with sulphur, the quantity of sulphur and phos
phorus has power to penetrate the gas, but some of the lines at the
red end of the spectrum are missing. To return, then, to the main
subject of the paper. At No. 9 on the drawings, is shown by the
characteristic lines of phosphorus, the lines were taken as before
described on carbon electrodes tipped with phosphorus—some lines
which are exceedingly fine have been omitted as doubtful. In.
this spectrum we have 21 lines; Dr. Watt’s gives 47, as found by
Plucker, but as to how the spectrum was taken, whether as a vapour
at atmospheric pressure, or in a vacuum tube, he gives no informa
tion. The principle, which the author has introduced to the Insti
tute, of course requires further investigation; but the fact does
seem to him to be confirmed by such experiments as he has been
able to apply, which is this, that an atmosphere of hydrogen gas, or
a gas composed of the ordinary coal gas from the gas works, with
�8
ESTIMATION OF SMALL QUANTITIES OF PHOSPHORUS
an admixture of hydrogen, has power to absorb completely the
phosphorus lines in iron, even when there is as much as 3-334 per
cent, of phosphorus present—that no sign of phosphorus is seen in
the spectrum in an atmosphere of this gas—that on the admission
of a very small amount of oxygen, the line does appear—that when
very small quantities of phosphorus are present, a very much larger
quantity of oxygen must be admitted, to make the line shine out
as a bright line. The experiments which have led to this result
have spread over many months, and have absorbed almost all the
author’s leisure time; they will, however, be explained in a few
minutes. They extend over several samples of iron, from which a
selection has been made, ranging from ‘550 of phosphorus to 021.
From these samples, the curve shown at No. 1 on the drawings
has been constructed; it will be observed that they do not
proceed in a direct ratio, but in the form of a curve. If,
as the author hopes, the- principle is right—but on this
he wishes to speak with great diffidence—he has lived to see
many splendid inventions of the patent office and lecture room
blown into thin air, when they get into the practical operations of
the laboratory and the workshop, that he would use due caution.
In the present state of his knowledge on the subject he would
proceed to an analysis of iron, with the apparatus now on the table,
and set forth on the drawings, in this way :—We propose, in this
case, to deal with materials suitable for the Siemens steel furnace,
either by Dr. Siemens’ open-hearth furnace or by the SiemensMartin process. For the quality we propose to make we will
assume that we must not have more than ’050 of phosphorus. A
few pieces are chipped from the pig iron to be used, from these a
pair of electrodes are filled up, they are placed in the nippers, and
put into the glass cylinder shown at No. 2. We should place the
phosphorus electrodes themselves in the cylinder shown at No. 3,
let coal gas into No. 3, and turn on the current; when the spectro
scope is adjusted, we should see that there are seven broad lines in
the green, that the band marked 181° 6j' in the green has a decided
unmistakeable coincident in iron. The current must not be kept
on long, as the iron is in air it will be very rapidly coated with
oxide, except to satisfy the observer that it is coincident, it is better
not to turn on the current when the iron is in air, because the
�IN IRON AND STEEL BY THE SPECTRUM ANALYSIS.
9
oxide will be decomposed, and upset the subsequent calculations.
Coal gas is next let into the cylinder and pipes, and lit at such
portion of the pipes, and at the cylinder, as will ensure that all the
atmospheric air has been driven out. The hydrogen gas holder is
now connected, and the gas turned on. At No. 4 of the drawings
the graduated bottle is shown; this bottle is drawn 3|f in.
Riameter, so as to get 12 in. area. The bottle actually used
in the experiments is an old barley sugar bottle, and can be
graduated accurately to whatever its diameter may be, by
weighing twelve cubic inches, marking the space on the bottle,
and graduating it accordingly.
This bottle forms a very
important part of the apparatus. It is fitted with a syphon
pipe, shown at No. 5. When the cock at the long leg is opened,
and all the cocks to the cylinder and gas holder are also
opened, the water runs out of the bottle into the bucket shown at
pSTo. 6. The coal gas in the cylinder, No. 2, flows out and takes its
place, and the hydrogen from the gas holder follows and takes the
place of the coal gas, or mixes with it. The practice in these
experiments has been to let in, in this way, 12 cubic inches of gas
as measured by the bottle, and to examine the spectrum for air
lines; the practised eye will detect these in a moment. If the air
lines are in the spectrum, this gas is not pure, oxygen is present,
the hydrogen is unfit for use, or the pipes have not been properly
cleared of air. With 12 inches of hydrogen which has been care
fully prepared, the line, the reading of which on this particular
instrument is 181 6-J/ is completely blotted out, a continuous
hazy-looking spectrum with indications of lines at various parts,
but the line 181° 6|' has completely vanished. We have next
to ascertain what quantity of oxygen will be required to make
181° 6j' come out as a bright line. The hydrogen must be
disconnected, and carbonic acid connected, taking care, of
course, to exclude the air, 36 cubic inches are required to
bring out a bright line. This iron may with confidence be
passed and used, it drops on to the curve just at 36, showing
that it has ‘021 per cent. Supposing that we are working the
Siemens-Martin process—the next sample submitted to the
spectrum analysis we will suppose to be puddled iron, it is tried
with hydrogen and there is no line, the carbonic acid is let in as
�10
ESTIMATION OF SMALL QUANTITIES OF PHOSPHORUS
before, at short intervals, and in quantities as measured by | on
the graduated scale, which is equal to 3 cubic inches, with the
second admission of 3 inches, making in all, 6 cubic inches, the line
is bright, the iron is very bad, it contains '550 of phosphorus, and
may, with great confidence, be rejected. The curve was obtained
by only 4 samples, containing—of phosphorus
’550 H.
•301 F.
•050 I.
•021 G.
Should this system come into general use, it is very probable
that some such form of apparatus, as shown at No. 12 on the
drawings, will be found the best, because greater quantities of the
material under examination can be brought under the action of
the spark. Iron, in the form of filings, gives a very fine spectrum
in this way. Wishing to try on samples of iron containing larger
quantities of phosphorus, the author asked Mr. Edward Riley to
send him some of those from which he had made analyses—that
gentleman kindly sent him five samples—ranging from 3’334 per
cent, to '027, a sample containing ’081 was tried and fell into its
place in the curve in a very satisfactory way. The sample con
taining 3'334 was also examined, and it was found, that when such
large quantities are present, other lines must be taken into account
—the line 181'6| is wholly absorbed by the hydrogen, with six
cubic inches of carbonic acid; it came out as a great broad band,
nearly as broad as that of the phosphorus. Other lines came out
which do not appear in iron, containing *550; these lines are
nearer the blue. The special part of the apparatus for the
examination of such materials as cannot be made into electrodes
is also shown on the drawings. Samples of them are on the table.
Figure 10 is a modification of Bequerell tube, which is used
generally for the examination of solutions. A great objection has
been found to using them as open tubes, with a fluid, quantities of it
are scattered by the action of the spark, to the great injury of the
slit of the spectroscope and the eyes of the operator. The same
objection holds good with a powder. A plain glass, as shown at
No. 12, would probably be a better form of apparatus than any before
mentioned. It would be better to pass the platinum electrode
�IN IRON AND STEEL BY THE SPECTRUM ANALYSIS.
11
through a glass tube so as to insulate it from the stopper, because
the deflagration from either a fluid or a powder so coats the glass
and the face of the stopper that the current passes that way;
the glass rod, should it also become coated, is easily cleaned
by drawing it up through the cork and wiping the coating from it,
and ensuring that the circuit can be made only by passing from the
platinum electrode to the fluid or the powder. The subject of such
large quantities as 2,3, or more per cent., requires further experiment.
The time of the Institute is valuable, and must not be taken up in
dealing with suppositions. The author wishes to adhere to the
subject of the paper—the estimation of small quantities of phos
phorus in iron and steel by the spectrum analysis. As time goes on,
should he be so fortunate as to gain more knowledge and
experience, he will have great pleasure in bringing this matter
forward again, hoping that other members who have taken
up this most important subject, or who may be induced by
this introduction of it to do so, will do the same.
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On the estimation of small quantities of phosphorus in iron and steel by the spectrum analysis
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Alleyne, John [1960-]
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Collation: 11 p. ; 22 cm.
Notes: Reprinted from Iron and Steel Institute Journal, 1871. From the library of Dr Moncure Conway.
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English
Subject
The topic of the resource
Engineering
Conway Tracts
Engineering
Iron
Spectrum Analysis