the determination of magnetite in metallurgical products ... · 1 electrical diagram of the...

65
The determination of magnetite in metallurgical products by an electromagnetic method Item Type text; Thesis-Reproduction (electronic) Authors Doan, Donald Jay, 1910- Publisher The University of Arizona. Rights Copyright © is held by the author. Digital access to this material is made possible by the University Libraries, University of Arizona. Further transmission, reproduction or presentation (such as public display or performance) of protected items is prohibited except with permission of the author. Download date 05/02/2021 08:04:08 Link to Item http://hdl.handle.net/10150/553124

Upload: others

Post on 30-Sep-2020

1 views

Category:

Documents


0 download

TRANSCRIPT

Page 1: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

The determination of magnetite in metallurgicalproducts by an electromagnetic method

Item Type text; Thesis-Reproduction (electronic)

Authors Doan, Donald Jay, 1910-

Publisher The University of Arizona.

Rights Copyright © is held by the author. Digital access to this materialis made possible by the University Libraries, University of Arizona.Further transmission, reproduction or presentation (such aspublic display or performance) of protected items is prohibitedexcept with permission of the author.

Download date 05/02/2021 08:04:08

Link to Item http://hdl.handle.net/10150/553124

Page 2: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

THE DETERMINATION OF MAGNETITE IN METALLURGICAL PRODUCTS

BT AN ELECTROMAGNETIC METHOD

By

Donald J&y Doan

Submitted in p a r t i a l fu lf i l lm e n t of the

requirem ents f o r the degree of

Master of Soienoe in M etallurgy

in the College of Mines and Engineering of the

U niversity of Arizona

1 9 3 2

A

Page 3: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance
Page 4: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

/ /

ACKNOWLEDGMENT

The au tho r wishes to acknowledge the a s s is ta n c e of

Dr. V. H, G ottsohalk and Mr. F. S. Wartman who, as

w ell as d ire c tin g the re se a rc h , made a l l of the chem­

ic a l analyses p resen ted . The au thor a lso wishes to

express h is indebtedness to Dr. T. G. Chapman fo r

advice and cooperation in the p rep a ra tio n of th is

th e s is . This th e s is p resen ts the r e s u l ts of work

done under a cooperative agreement between the United

S ta te s Bureau of Mines and the U niversity of Arizona.

< 5

85739

Page 5: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

OOTETOS

Page

In tro d u c tio n .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

The B a l l i s t i c M ethod.............................................. 9

The D eterm ination of "Average Size" B a r t ic le . 23

M ateria ls U sed ....................................................... 27

The I& gnetic-Balanoe Method............ .. 30

S u m m a r y . . . . . . . . . . . . . . . . . . . . . . . . . . . .................. M

Page 6: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

ILLUSTRATIONSFig .NO.

1 E lectr ica l diagram of the apparatus used fcy S tu tzer,Grozt and B o r n e a a n . 5

: ' . ■ -2 The magnetic balance used by Seaman................................. 6

2 Diagram of th e m agnetic f i e ld through a s o le n o id .. . . 10

4 Diagram of th e b a l l i s t i c a p p a r a tu s . . . .............................. IS

5 E ffec t of "average s iz e " p a r t i c le upon magnetica t t r a c t io n , using th e solenoid magnetic b a la n c e .. . 21

6 The e f f e c t of "average s iz e " o f p a r t i c le s upon mag­n e t ic a t t r a c t io n , u sing th e p o le-type magnetic b a lance ............................... 34

7 The e f fe c t of d i lu tin g m agnetite No. 11b, -356 mesh,and No. 11b, -100 +150 mesh, w ith q u artz , -350mesh and -100 +150 mesh, r e s p e c t i v e l y . . . . . . ............. 37

8 The e f f e c t of d i lu t in g m agnetite No. 4, -360 mesh(lower curve) and No. 4 , -100 mesh, w ith quartz ,-350 mesh and -100 +160 mesh, re sp e c tiv e ly ............... 37

9 Photograph of the "d en sito m ete r" .. . . . . . . . . . . . . . . . . . . 40

10 The r e la t io n between density and com position, usingm agnetite -quartz m ix tu res........................ 41

11 Photograph of the magnetic balance f in a l ly adopted*• 42

12 The e f f e c t of volume of m agnetite m ixtures upon mag­n e t ic a t t r a c t i o n . ....................... 43

13 The re la tio n between magnetite content and magnetic attract ion a t constan t volume.. . . . . . . . . . . . . . . . . . . 4 4

Page 7: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

TABLES

Table Ho. : ...... .. .............. - • ■ Bilge

1 B eprofluo lb llity of the b a l l i s t i c instrum ent* . 19

Sa Grain s in e measurements u sing Sample Ho. 10,IBLnerille m a g n e tite .; ......... .... 26

8b Grain s iz e measurements u sing Sample Ho. 11a,M ineville m a g n e tite ...................... . 26

. S . Summary of the m a te ria ls u s e d .. . . . . . . . . . . . . . . 27

4 A com ^.risen of the m agnetite con ten ts o f a i z - ,.. tu re s as measured by th e balance method and as determined c h e m i c a l l y . . , . . . . . , . * . , . , . , , . ,47

6 . Comparative m agnetite co n ten ts of s la g s ........... .. 60

Page 8: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

THE DETERMINATION OF MAGNETITE IN METALLURGICAL PRODUCTS

BY AN ELECTROMAGNETIC METHOD

INTRODUCTION

The presence of m agnetite (FegO^ In r e ­

verb era to ry and een v erte r s la g s r e s u l t in g from copper sm elt­

ing operation i s g en e ra lly known. I t has been widely recog­

n ised th a t th e presence- of th i s m agnetite caw ee c e r ta in

d i f f i c u l t i e s in copper sm elting o p e ra tio n s , among which the

fo llow ing are n o ted : increased lo s s of copper in th e s la g s ,

the g re a te r the m agnetite content th e h igher th i s lo s s ; th e

troublesom e "m agnetite mush" la y e r between the s la g and th e

m atte is a t t r ib u te d to th e presence of m agnetite; the b u ild ­

ing up of the re v e rb e ra to ry furnace bottom encountered a t some

p la n ts i s due to m agnetite . I t i s , th e re fo re , of th e utmost

im portance th a t an accu ra te and r e la t iv e ly simple method of

a n a ly s is be developed which can be used in sm elter co n tro l

work and to fu r th e r the study of s la g s . The ob jec t of th is

in v e s tig a tio n i s the study and development of a sim ple and

r e l ia b le method fo r the determ ination of m agnetite in re v e r ­

b e ra to ry and converter s lag s r e s u l t in g from copper sm elting

operations* :

Page 9: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

This problem may be attem pted from e i th e r

the chemical s id e o r , since m agnetite la known to be m agnetic,

from a p hysica l view point. Inmerous papers on th e measurement

of e i th e r magnetic perm eab ility or s u s c e p t ib i l i ty have been

pub lished ; from th e se a few which a re ap p licab le to th is prob­

lem a re no ted . The chemical method fo r th e determ ination of

m agnetite i s a lso described and d iscussed .

A method of measuring magnetic s u s c e p t ib i l ­

i t y which is based on th e p r in c ip le of a simple transform er i s1

advanced by S tu ts e r , Grog, and Bomeman. The magnitude of

the induced elec trom otive fo rce produced by a transfo rm er i s

a fu n c tio n of the magnetic perm eab ility of the eore th a t i s

used; i f an apparatus is s e t up in which the core may be in t e r ­

changed, the perm eab ility of the core can be determ ined. A

diagram of th e appara tus used i s shown in Figure 1. R eferring

to th i s F igure , two tran sfo rm ers , each being in th e form of

two concen tric so len o id s , a re arranged so th a t the induced

cu rren ts a re opposite ; i f both transfo rm ers a re id e n t ic a l ,

e l e c t r i c i t y w ill not flow through the secondary c i r c u i t when

an a l te rn a t in g cu rren t i s passed through the primary c i r c u i t .

S tu tze r p laced the sample of th e m a te ria l to be te s ted a t th e

cen te r of one tran sfo rm er, and th e perm eab ility of the core

was e i th e r increased or decreased , which in tu rn caused an

a l te rn a t in g cu rren t to flow in the secondary c i r c u i t . The

1S tu tz e r , F . , Groz, W., and Borneman, K ., Uber Magnetisohe E lgeneohaften der Zinkblende und e in ig e r anderer M ineralien : Me t a l l , und Erz, v o l. 15, 1918, pp. 1 -9 .

Page 10: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

AMMETER GALVANOMETERAMMETER'

PRMARYCIRCUrr

SOLENOOS'

5ECOCARYCIRCUIT

COMMUTATNG

DEVICE

Figure 1 .—E le c tr ic a l diagram showing the appara tus used toy S tu tz e r , Groz, and Borneman.

a l te rn a t in g cu rren t in the primary c i r c u i t was produced toy a

ro ta t in g sw itch which co n tin u a lly reversed the d ire c tio n of

the c u r re n t, as may toe noted in Figure 1. This arrangement

y ielded a corresponding induced a l te rn a tin g cu rren t through

the secondary c i r c u i t . For the purpose of changing th is sec­

ondary a l te rn a tin g cu rren t to d ire c t c u rre n t, a c i r c u i t Breaker

was placed on the sh a ft th a t operated the a l te rn a to r fo r the

primary c i r c u i t , thus p e rm ittin g only the cu rren t of one-half

a cycle to toe tran sm itted through the secondary c irc u it (see

Figure 1 ) . A D'Arsonval galvanometer was used to measure the

transform ed secondary c u r re n t. S tu tzer pointed out two main

e rro rs r e la t in g to th is work. The ncommutating device" was

operated toy a small e l e c t r ic motor which revolved a t a speed

Page 11: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

of 1,200 r .p .m .; th e Inoenstaney of th e motor v/as +1.5 per c e n t.

The demagnetizing e f fe c t of the sample introdmeed considerab le

e rro rs th is e r ro r I s dependent upon the r a t io of le n g th to d ia - 2m eter of the sam ple, but i s only Im portant when ab so lu te meas­

urements of the perm eab ility a re made, and i t need not be con­

sidered when com parative s tu d ie s a re d e s ire d , provided the r a t io

o f le n g th to diam eter i s m aintained constant*

Wait used two methods fo r the determ ination

of ab so lu te p e rm e a b ilit ie s o f iro n and m agnetite . Aside from

the complexity of the ap p ara tu s , eaoh method has the disadvan­

tage th a t th e samples to be te s te d must be worked in to wax and

a lso be made to assume d e f in i te shapes* Wait did not d iscuss

the percentage accuracy of these methods.

Mendenhall and Lent have advanced a method

fo r the determ ination of magnetic s u s c e p t ib i l i t i e s of diam agnetic

and param agnetic m a te r ia ls . The apparatus used i s very d e l i ­

c a te , and consequently i f placed in r e la t iv e ly u n sk ille d hands

the maximum e r ro r of 1 .5 per cen t obtained by Mendenhall and

le n t would be increased . A fu r th e r disadvantage of th i s method

is due to the fa c t th a t i t is not ap p lio ab le to m a te ria ls th a t

possess high magnetic p e rm e a b ilit ie s . * 3 *

S ta r l in g , S. G ., E le c t r ic i ty and magnetism: London, 1924, p . 2T03Wait, G. R ., Magnetic P erm eab ility of Iron and M agnetite in

High Frequency A lte rn a tin g F ie ld s : Phy. l e v . , vo l. 29, 1927, pp. 866—878. . ■

^M endenhall, C.B., and Lent, W. F . , A Method of Measuring the S u s c e p tib il i ty of Weakly Magnetic Substances: Phy. Rev., vo l.82, 1911, pp. 406-417.

Page 12: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

6Wilson has m odified the Curie type of

instrum ent fo r th e determ ination of magnetic s u s c e p t ib i l i ty .

The general p r in c ip le of the l a t t e r type i s th a t th e fo rc e

exerted upon a sample of magnetic m a te ria l by a magnet i s

measured and the s u s c e p t ib i l i ty then ca lcu la ted from the r e -6

s u i t s ob tained . Soaman and H o s te tte r used a Ruepreeht

a n a ly tic a l balance fo r th e measurement of th is magnetic fe ra e ,

while Wilson used magnetic means to balance the fo rc e . The '

advantages and d isadvantages of th e Curie type of instrum ent

eq u a lly apply to bo th methods noted , and as the Sosman modi­

f ic a t io n w ill be described in some d e ta i l , a d iscu ss io n of

the Wilson type i s om itted .

The Magnetic Balance Method

The p r in c ip a l exponent of the magnetic

balance method of app ly ing the Curie p r in c ip le fo r the d e te r­

m ination of magnetic p e rm e a b ilitie s and s u s c e p t ib i l i t i e s has

been Robert B. Sosman. Seaman*s o r ig in a l procedure5 6 7 employed

an electrom agnet of the pole type; th is apparatus is shown in

F igure 2. I t consisted "simply of a Ruepreeht a n a ly t ic a l

5 :Wilson, E rn e s t, On the Measurement of lew S u s c e p tib il i ty by an Instrum ent of a Hew Type: F ree . Roy. So©, of London, (A), v o l. 98, 1931, pp. 274-284.

6Sosman, R. B ., and H o e te tte r , J . C ., The Ferrous Iron Content and Magnetic S u s c e p t ib i l i t ie s o f some A r t i f i c i a l and N atural Oxides of I re n i Trans. Am. I n s t . Min. Eng., v o l. 58, 1918, pp. 404-433.

7Sosman, R. B ., and H o s te tte r , J . C ., oj). o l t .

Page 13: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

• 6 -

balanoe , from one pan of which was suspended a g la ss p latfo rm

on which the charge of oxide was p laced , a sho rt d is tance above

an electrom agnet. The oxide was contained in a small f l a t -

bottomed g lass pan; the p a r t ic le s a re kept from moving by a8

g la ss plunger which pressed down upon the powder." E rro rs

caused by ou tside d istu rbances such as the presence of s te e l

in the balance were remedied or computed m athem atically . In

using the method as described i t is obviously im possible to ob­

ta in ab so lu te values fo r the s u s c e p t ib i l i ty because of many unde­

term inable fa c to rs r e la t in g to the f i e ld , but as only comparative

r e s u l ts a re re q u ired , these fa c to rs are not im portant. Sosman

Figure 2 .--The magnetic balance used by Sosman*

3Sosman, R. B ., and H o s te tte r , J. C ., oj>. c l t .

Page 14: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

l a t e r changed h is o r ig in a l apparatus by re p lac in g the pole type

electrom agnet by a se t of a d e n o id # , thus p e rm ittin g th e a t ­

tainm ent of ab so lu te r e s u l t s . The solenoid magnetic balance

has a maximum accuracy of 2 p e r cent fo r param agnetic su b stan ces ,

and "only somewhat crude comparative r e s u l t s a re ob tainab le9

w ith ferrom agnetic powders." The Sosman a p p a ra tu s , though

not of g re a t accuracy , has been in s ta l le d in th e la b o ra to r ie s

of two sm elting p la n ts (United Terde, CLarkdale, A r ia . , and

Copper Queen, Douglas, A r iz . ) fo r the comparative study of

rev erb e ra to ry and converte r s la g s . In Sosman*s and E e s te t te r 's 10o r ig in a l paper th e au th o rs have shown an approximate r e la t io n ­

sh ip between the magnetic s u s c e p t ib i l i ty and th e fe rro u s iro n

content in various oxides of Iron . The s u s c e p t ib i l i ty was de­

term ined as the weight re q u ire d , in m illig ram s, per gram of

m a te ria l to balance the magnetic fo rc e . The idea of d e te r ­

mining the con ten t of a m agnetic substance in a given m a te ria l

by electrom agnetic measurements is th e re fo re not new. 9 10

9Sosman, R. B ., and Posnjak, E ., Ferrom agnetic F e rr ic Oxide, A r t i f i c i a l and n a tu r a l : J . Wash. Acad, of Science, v o l. 18, 1925, pp. 329-342.

10Sosman, R. B ., and H o s te tte r , J . C ., 0£. o i t .

Page 15: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

Chemical Method f o r the Determ ination o f M agnetite

fhe most r e l ia b le chemical method fo r the

determ ination of m agnetite i s probably th a t advanced by Eawley1*

in 1919 and which Roberts and Hugent12 modified in 1901 w ith

improved r e s u l t s . The p r in c ip le involved in th is method i s the

s e le c tiv e d isso lv in g a c tio n of n i t r i c ac id and potassium ch lo r­

a te so lu tio n , which sep a ra tes th e r e la t iv e ly in a c tiv e m agnetite

from the more r e a d i ly a ttacked iro n and sulphur compounds.

Roberts and Hugent l i s t the fo llow ing p o s s ib i l i t i e s of e r r o r ;

"1. The su lph ides may not be com pletely removed and

th e ir reducing a c tio n during the so lu tion of the sample cause

low r e s u l t s .

2. The ox id iz ing m ixture m y d isso lve m agnetite .

3 . The o x id is in g m ixture m y oxidize so lid fe rro u s

compounds in th e undissolved re s id u e ” to m agnetite , "g iv ing

h igh r e s u l t s .

4. Atmospheric oxidation may occur during th e so lu ­

tio n of the sample.

5. Traces of o ther elem ents may reduce iro n during

the so lu tio n of the sam ple, or may oxid ize the stannous chloride

in th e t i t r a t i o n ” of the iron from m agnetite .

TE ' ” 'Hawley, F. 0 . , D eterm ination of M agnetite in Matte and S lag;Eng. and Min. Jo u rn a l, vo l. 108, 1919, pp. 308-310.

12R oberts, L. E«, and Hugent, R. L . , D eterm ination of M agnetitein Copper Slags? Report of In v e s tig a tio n s , S e ria l 3180, U. S.Bureau of Mines, S e p t., 1931, 14 pp.

Page 16: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

9

They estim ate the accuracy of the Improves

Hawley method to be about 2 per een t. The method i s q u ite

e lab o ra te and requires eonaiderable s k i l l in technique to ob­

ta in eoneietent r e s u l t s . Roberts and liugent have compared the

chemical method with the magnetic balance f o r determ ining mag­

n e t i t e in copper fu rnace s lag s and the re s u l ts agree "within

about 2 per e e n t." This l a t t e r r e f e r s to d iffe ren ce in p er

een t.

THE BALLISTIC MflOD

The b a l l i s t i c method, in so f a r as the

w riter could determ ine, has never been used to measure the

magnetic s u s c e p t ib i l i ty o r perm eability of pu lverized mate­

r i a l s w ith . the d e f in i te o b jec t of determining magnetite con­

te n t . The method has been ou tlined in several t r e a t i s e s on

e l e c t r i c i t y and m a g n e t i s m , b u t i t u su a lly is app lied to

the study of uniform so lid s such as s te e l s and iro n s . Y/elo16

and Baudisoh used the b a l l i s t i c method to determine the p e r­

m eability of powdered m agnetite and o ther iron oxides. The

p resen t in v e s tig a tio n i s not concerned with th e ab so lu te value

13Spooner, T ., P ro p e rtie s and T esting of Magnetic M ateria ls : Hew York, p . 207, 1987.

14S ta r l in g , S. E le c t r ic i ty and Magnetism: London, 1924, p . 271.

Welo, L ., and Baudisoh, A ., The Two-Stage Transform ation of M agnetite in to Hem atite: P h il . Mag. (6 ), v o l. 50, 1926, pp. 599-408.

1 6

Page 17: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

- 1 0 -

of the magnetic perm eab ility or s u s c e p t ib i l i ty of the m a te ria ls

u sed , but only w ith the comparative values which a re a func­

tio n of the ab so lu te q u a n ti t ie s . The b a l l i s t i c instrum ent16

may, however, be c a lib ra te d by various means, and thus be

used to ob tain abso lu te r e s u l t s .

D iscussion of the B a l l i s t i c Method

The theory concerning th is method is not

new and is r e la t iv e ly sim ple. I f a uniform elec trom otive fo rce

is maintained through a so le n o id , a magnetic f ie ld w ill r e s u l t .

R eferring to Figure 3, th is magnetic f ie ld is denoted by l in e s

Figure 3. — Diagram of the magnetic f ie ld through a solenoid .

To "S ta r l in g , S. G ., Oj3. c i t . , p . 256

Page 18: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

1 1 -

of fo rc e . I f a second so lenoid is in se rted in to th e f i r s t ,

th e term inals being connected to a galvanom eter, a momentary

cu rren t w ill be induced in th e secondary c o il when the cu rren t

in th e prim ary c i r c u i t i s in te rru p te d . S im ila rly , i f th e cu r­

re n t i s "made" through the prim ary solenoid in the opposite

d ire c tio n , th e induced cu rren t in th e secondary solenoid w il l

be in the same d ire c tio n a s th e f i r s t induced secondary c u rre n t•

In th i s manner a double Induced cu rren t may be obtained by use

of a commutating sw itch , which sim ultaneously breaks the cu rren t

In the prim ary c i r c u i t and s t a r t s i t in the opposite d ire c tio n .

Thus:

. . . . ; . • ~ M # / . 1 7 .. . . , . ..

where e ia th e induced elec trom otive fo re # ,M ie the c o e f f ic ie n t of mutual inductance,£ i s th e cu rren t in the prim ary c i r c u i t .

This equation in d ic a te s th a t when th e cu rren t L i s constan t or

ae ro , the induced elec trom otive fo rc e i s ze ro ; the quan tity

of induced c u rren t produced i s a lso p ro p o rtio n a l to the ra te

of change of the prim ary c u rren t w ith tim e. In the p resen t

in v e s tig a tio n th i s r a te of change was kept constan t and no a t ­

tempt was made to determine i t .

S ta r l in g , S. G. , op. o i t . , p . m .

Page 19: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

In any magnetio o ir e u it , eozjpeeponding to

Oto-a tow: u = e R 18 ' : ' ^

where u i s th e m agnetic p o te n t ia l in am pere-tarns, e i s the

magnetic f la x in wefcere, and R i s the to t a l magnetle re lu e tan ee

in am pere-tarns per weber# I f R*, R*,—— rs>-----a re the separa te

relaotam eea of the p a r ts o f th e magnet io c i r o u i t , then RA4- R&,+--+

, i f p ro v is io n is made in the wcomdary solenoid for

the p lacing of a c y lin d e r , which in turn serves to hold the sam­

p le of magnetic substance to be te s te d , them

/ -/where A ,is th e c ro ss -se c tio n a l a rea of the sample, L*the depth

of the sam ple, and i s equal to 4 w l 0 when/t- i s the p e r-. ' 80

m eab ility of th e m a te ria l. S u b s titu tin g U* N,I where I

i s the cu rren t through th e prim ary and N pIs the number of

tu rn s of the prim ary, in equation 1 : 0 = , and d ifferen ­

t i a t in g :III .

The m utually induced elec trom otive fo rc e through the secondaryjh 21i s expressed by: * 19

Bennett, E, K ,, and Crother, H. M., Introductory E lec tro ­dynamics fo r E ngineers: Hew York, 1926, sec . 010, p. 644.

19 - ;Bennett and Crother, op. c i t . , sec . 314, p. 644.

80 -----Bennett and Crother, o£. c i t . , sec. 312, p. 642.

Bennett and C ro ther, 0£. c i t . , sec . 298-b, p. 577.

Page 20: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

and, since th e t o t a l linked magnetic f l a x , A , i s equal to

the number of tu rn s on the seeen la ry , Ns , m u ltip lied hy the .22

t o t a l magnetic f lu x , 6 , e = .

S u b s titu tin g equation I I I in th is equation ,

6 = - ^ ^ • IV-

By Ohm’s Law e = 1 h # where r i s th e r e s is ta n c e .o f th e sec -

ondary so leno id , c i s the c u r re n t , and e i s the e lec trom otive

fo rc e . Then:

U t = _£U_Nfct[ T.

and since i d t — where d y i s the charge c irc u la te d through

the solenoid when a cu rren t t flows fo r a time d t . In te ­

g ra tin g th e equation V:>

> = - N r ‘ r, ^ ' = "r "since Ai, i s held co n stan t throughout th e in v e s tig a tio n , where

f" — Ns N»aI.r •

I f two se ts of id e n tic a l so leno ids a re oonneeted in

s e r ie s so th a t th e induoed c u rren ts a re opp o site , then :

v i i .

Bennett and C ro ther, 0£ . o l t . , s e e . 278, p . 481.82

Page 21: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

•1 4 * '

K. does not e v m l ze ro , because of the d i f f i c u l ty in manufac­

turing th e so len o id s , hut by a l te r in g th e re lu c ta n c e , Rz ,

of c e i l s Re. 2 the charge c i r c u la t in g through the secondary

c i r c u i t may be made sm all and equal to K. Solenoids l e . 2

a re not a l te re d a f t e r s e t t in g and therefore the re lu c ta n c e ,

Ra , i s a co n s tan t. The q u an tity fo r so lenoids Ho. 1 i s

a constan t when th e sample container of the secondary i s empty,

s ince th e reluctance does no t change; and th e re fo re the quan-

tityYtf,-$i) = K where K i s a co n stan t.

When th e sample of m a te ria l to be te s te d i s placed

in secondary c o i l Ho. 1 , thenz % — % = “ "r2

and su b tra c tin g equation VII (fs—%) — K = ^ ^ V III.

From t h i s equation the fo llow ing conclusion may be drawn:

(% -& ) “ K = FUNCTION (Rs)

A b a l l i s t i c galvanom eter la uael t . maaanr.

and a lso K, and s in ce 0 = fad where ^ i s charge put through

the galvanometer, ^ is the gal van easier constant and c t i s

the d e f le c tio n , and th e re fo re

Ad/ = FUNCTION (Rg) ' IX.

where A c/is th e difference between th e galvanometer d e f le c tio n

with and w ithout the sample in the c o i l . . Using equation l i t

Ac/ = FUNCTION (%) or Ad/ = FUNCTION X.

w h e re y ^ is . th e perm eab ility of the sample. ......

Page 22: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

- 1 5 -

A lt hough I t may he considered obvious th a t

the magnetic perm eab ility is a fu n c tio n of the m agnetite content

of any p a r t ic u la r sample, a curve re p resen tin g th i s r e la t io n

is presented w ith the d e sc r ip tio n of the experim ental work.

VARIABLE RESISTANCE 7 KEY 7

Figure 4 .—Diagram of the b a l l i s t i c ap p a ra tu s .

F igure 4 rep resen ts a diagram of the appa­

ra tu s used. R eferring to th i s f ig u r e , i t may be noted th a t

w ith both keys c lo sed , a snap of the commutating sw itch r e ­

verses the curren t in the primary c i r c u i t , thereby causing

the magnetic f ie ld to rev e rse in prim ary so leno id , which in

tu rn induces a corresponding instan taneous e le c t r ic cu rren t

through th e secondary c i r c u i t . This secondary charge is

Page 23: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

me##mr#d by the b a l l i s t i c galvanom eter. The v a ria b le re s is ta n e e

ia connected in the prim ary c i r c u i t so th a t th e cu rren t may be

m aintained a t a given va lue . The m a te ria l to be te s te d i s

placed w ith in a b ra ss cy lin d e r and i s lowered in sid e a desig ­

nated secondary so leno id .

The B a l l i s t i c Apparatus

The galvanometer is a Leeds and ITorthrup

type which had a period of 5 .5 seconds, but because of th i s

r a p id i ty , a r o l l o f platinum f o i l was f ix ed upon the top of

moving c o i l ; th is improved galvanom eter has a period of 10.6

seconds and may now be convenien tly used as a b a l l i s t i c type

instrum ent. The so leno id se ts may each be subdivided in to p ri­

mary and sooondary so len o id s . The prim ary c o ils a re r ig h t

cy lin d ers having an in s id e d iam eter of 2.2 cen tim ete rs , a

le n g th of 9 ce n tim e te rs , and approxim ately 40 tu rn s per cen­

tim e te r of No. 12 enameled copper w ire . The secondary so len ­

oids a re a lso r ig h t cy lin d ers having an in sid e diam eter of

0.7-centim eter, a le n g th of 1 .7 cen tim ete rs , and approxim ately

1,600 tu rn s per cen tim eter of Ho. 38 enameled copper wire.

Each secondary c o i l f i t s r ig h t ly in to i t s prim ary so leno id .

The v a r ia b le re s is ta n c e i s a Genoo typo

having a maximum re s is ta n c e of 5 .8 ohms and cu rren t cap ac ity

o f 8*7 amperes. The commutating sw itch m s made from two

e le c t r ic l ig h t "snap" sw itches. These were mounted so th a t

a connecting bar of aluminum could be made to throw the two

Page 24: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

- 1 7

sw itches sim ultaneously , which in tu rn reversed the cu rren t.

The ammeter i s a Weston d .o . ammeter, model 45, Ho* £0098.

I t i s equipped w ith an ap p ro p ria te shunt which i s in th is case

a 5 0 - a i l l i v e l t , f * 5-aapere shunt. th i s ammeter has the degree

of accuracy necessary to l im it the e r ro r of the f in a l galvan­

ometer read ing to w ith in 1 p e r c e n t, the b a t te r ie s a re fo u r

Edison c e l l s arranged in s e r ie s , and they gave s a t is fa c to ry

se rv ice under the experim ental cond itions used.

P relim inary Knowledge R ela ting to th e A p p lic a b ility

of the B a l l i s t i c Method

Work was s ta r te d to in v e s tig a te th e p o ss i­

b i l i t i e s of u t i l i z i n g th e b a l l i s t i c type of magnetic apparatus

fo r the determ ination of magnetic perm eab ility of m agnetite ,

m ainly because of the wide a p p lic a tio n of an instrum ent e f28

the same p r in c ip le fo r the t e s t in g of s te e ls and iro n s .

At th e s t a r t of th i s work i t was conceded th a t the method i s

sim ple, and as used w ith iro n and s te e ls i s f a i r l y accu ra te .

As no ted , the use of the b a l l i s t i c method

has been lim ited to homogenous s o l id s . I t was re a l is e d th a t

the a p p lic a tio n e f th i s m ethod.to f in e ly ground m a te ria l p re ­

sented serious; o b s ta c le s . From the work of Seamen and Hoe-'04

t e t t e r i t was p red ic ted th a t the "g rain s ize" of the m a te ria l

S U • I' ' • ■ , r r , r V ' T ' ' ' . . . . . . . . . . . . . . . - ; T ' r 1 T ' ’ r r i T 1 , T " ' . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . * . . . . . . . . . . . . . . . . . . . ' * r " r n r ^ r ~ '

W all, T. F . , Applied Magnetism: Hew York, 1927, chape. IX and X, pp. 129-166.

24 . ■ . . . . . . . . . ■ : • . 'Seaman, R* B ;, and H o s te tte r , J . 0 . , The Ferrous Iron Con­te n t and ISagnetle S u s c e p t ib i l i t ie s of Seme A r t i f i c i a l and n a tu ra l Oxides of I re n : Trans. Am. I n s t . Min. E ng ., vo l. 58, 1918, pp. 404-433.

Page 25: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

to be te s te d would have a narked e f fe c t upon th e magnetlo p e r­

m eab ility of th e l a t t e r . I t i s a ls o known th a t p rev ious mag­

net io h is to ry , a s w ell as heat trea tm en t of magnet io m a te r ia ls ,

have some e f fe c t upon th e i r magnetic p ro p e r tie s .

In te rp re ta t io n of R esults

A bsolute values fo r the perm eab ility or

s u s c e p t ib i l i ty of m ate ria ls tested has not been determ ined.

I t i s , th e re fo re , im portant th a t an explanation be given th a t

w i l l enable the data presen ted to be in te rp re te d . The magnetic

p e r m e a b i l i t y ,^ , from equation X, page 14, i s a fu n c tio n of

the d iffe re n c e in galvanom eter d e f le c tio n s , and th i s read ing

i s recorded in cen tim eters f o r a given weight of sample.

Weight measure is used to determine the amount of m a te ria l to

be t r e a te d ra th e r than volume measure, because of the ease

and accuracy of weighing.

The Container

C onstruction and development of th e appa­

ra tu s o ffe red many d i f f i c u l t i e s . Three s e ts of so leno ids were

construc ted of which the th i r d and l a s t s a t i s f i e d the re q u ire ­

ments of the method. The shape of the sample co n ta in er was

se lec ted a s long and narrow, to decrease the dem agnetization

e f f e c t . The l a t t e r does not e f fe c t the desired com parative 25

25S ta r l in g , 3. G ., E le c t r ic i ty and Magnetism: London, 1924,p. 270.

- 1 8 -

Page 26: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

1 9

v a lu e s , tu t only le e re a se s the true magnetlo p erm eab ility

which f o r a c e r ta in perm eab ility i s ecn s tan t. Aluminum, g la s s ,

and brass co n ta in ers were t r i e d . These m a te ria ls a re non­

magnetic w ith in the experim ental error. One very im portant

f a c t which was found ea rly in th e work i s th a t th e samples

must be of .th e , same id e n t ic a l s iz e and shape* The aluminum

being s o f t and the g la s s d i f f i c u l t to shape, the b rass was se ­

lected as the best a v a ila b le container m a te r ia l, s ince i t could

be. machined in a la th e to th e required s iz e w ith the desired

accuracy . Six b ra ss capsu les were made, but only th ree were

found to produce r e s u l t s to an accuracy w ith in 1 per cent.

The fo llow ing data shown in Table 1 give r e s u l ts which in d i­

ca te th e fo re g o in g conclusions.

Table 1 .—R eprod u c ib ility of the B a l l i s t i c Instrum ent.

dapsule ; Galvanometer d e f le c tio n , cen tim eters50#

P C: %est So. I I : T e s tt io . 12 :1 l i s t i o . "1 8 1 Test lie. 14

i■ • r

: 21.19 : 21.08 ; 21.05 : 21.05

2:: 21.10 $ 21.11 \ 21.10 : 21.16

6«: 21.01 : 21.09 : 21.10 : 21.01

■ ■ i

A sample of fu rnace accretion m agnetite

produced in copper sm elting , weighing 1 .0 grams, was used in- ' . •' » % ' " , ' ' • - • - ' ' ■ • -

1 ■ I • • -.v ■ ' ' *1 '

these t e s t s , and a prim ary cu rren t of 2 amperes was employed.

The maximum percentage error i s 0 .9 .

Page 27: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

Used to Control Volume of Sample

To ob ta in a volume f a c to r , uniform as poss­

ib le , tapping of th e m ate ria l was p ra c tic e d . The tapping pro­

cedure comprised (1 ) p lac in g th e sample in a capsule and tapping

the co n ta in er w ith a modified "b e ll buszer" which was arranged

so as to s t r ik e the capsule in such a way so as to ro ta te i t

and ja r the sample a t the same tim e. This process was continued

fo r about a 6-m inute p e rio d , a f te r which the capsule was removed

(2 ) The sample co n ta in e r was placed w ith in a so lenoid which

has approxim ately 80 tu rn s per cen tim eter of copper w ire . An

a l te rn a t in g c u r re n t , 5 amperes a t 60 c y c le s , was then caused

to pass th rough the so lenoid fo r th e purpose of p reparing the

sample so th a t constan t va lues could be ob tained . This proce­

dure was continued fo r a period of approxim ately 3 minutes $

the capsule was then placed w ith in th e te s t in g solenoid and

the galvanom eter d e f le c tio n was read . /

Steps (1) and (2) were repeated fo r sh o rte r

time periods u n t i l successive galvanom eter d e f le c tio n s were

co n stan t. This c o n s ta n t:value was accepted as th e f in a l meas­

u re of magnetic p e rm eab ility . .

The ob ject of p lac in g th e sample con ta iner

w ith in the a l te rn a t in g magnetic f i e ld i s not q u ite c le a r ly

e s ta b lish e d , but i t i s necessary from e i th e r a tapp ing in f lu ­

ence in a d d itio n to th a t obtained by the mechanical tapp ing

or the n e c e ss ity of dem agnetising o f the m a te ria l te s te d .

The p lac in g of the sample in th i s c o i l in creases the galvan­

ometer d e f le c tio n ; th e re fo re the tapping in fluence appears to

Page 28: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

be g re a te r than the dem agnetization e f f e c t , M eans# Shis l a t ­

t e r redmees the p e rm eab ility . Some m agnetite m ineral has an

app rec iab le h y s te re s is e f f e c t26 * and, provided the m agnetizing

f i e ld i s le s s th an th a t required to sa tu ra te th e m agnetite ,

demagnetizing would decrease the perm eab ility and th e re fo re

the galvanom eter d e f le c tio n . A marked disadvantage of th e

complete tapp ing procedure a s described is the len g th of time

re q u ire d . This am ounts 'to from 1 to 3 hours per th ree samples

in order to ob ta in f iv e to s ix constan t values of th e galvan­

ometer d e f le c tio n s f o r each sample.

m ane t i e V iscosity

A co n d itio n which may or may not be p resen t

in m agnetite i s termed by Wall as "Magnetic V isc o s ity ." I t

i s conceivable th a t th e re v e rs a l of a magnetic f i e ld through

a magnetic m a te ria l would take a c e r ta in d e f in i te measurable

period of tim e. This period may prove to be so long th a t the

b a l l i s t i c method may be in v a lid a ted f o r perm eab ility measure­

ments. 28 R eferring to the d e sc rip tio n of the theory as p re ­

sented on page 14, i t may be noted th a t in order to o b ta in a

W — 1 - ! 1 " 1 """"Seaman, R. B ., and Peanjak, E . , Ferrom agnetic F e rr ic Oxide, A r t i f i c i a l and n a tu ra l : Jour. Wash. Acad, o f S o l . , v e l. IS ,

, 1928, pp. 329-342.

W all, T. F , , Applied Magnetism* Bew York, 1927, pp. 90-91.

W all, T* F#, op. o i t ♦

Page 29: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

tru e measurement of the charge, , by the b a l l i s t i c g a l-

vanometer, th e charge must be proameea p r a c t ic a l ly In s ta n ta ­

neously. I f th e value of th e magnetic f i e l d th rough the

m agnetite in c reases or decreases g ra d u a lly , th e re would be.a

"leakageM of the charge, which would not be f u l ly measured by

the f i r s t galvanom eter d e f le e tio n .

The e f f e c t of magnetic v ie e e e ity should be

determined or shown to be in e f f e c t iv e , but u n fo rtu n a te ly the

b a l l i s t i c method can not be used f o r th i s purpose and the w rite r

did not have the opportunity to develop any o ther means of

proving or d isprov ing th e e ffec t#89

%11 suggests th e magnetometer method

fo r "Magnetic V iscosity" measurements, but the apparatus used• ; .* .

in th is method i s qu ite d i f f i c u l t to co n stru c t and opera te .

Conclusions from th e Work on the B a l l i s t i c Method

Taking in to co n sid e ra tio n the leng thy

tapp ing time re q u ire d , the: "magnetic v is c o s ity " f a c to r , and

th a t the ammeter was found to be d e fec tiv e and was shipped to

the fa c to ry to be re c a lib ra te d and re p a ire d , work progressed

along two l i n e s —f i r s t , aeo u ra te determ inations of th e s iz e s

of p a r t ic le s were made on screen f r a c t i o n s s e c o n d , in v e s t i ­

g a tio n of the p o s s ib i l i t i e s of th e Sosman or magnetic balance

type of instrum ent was s ta rted * - -) ' . - . ;

Wall, T. P . Vo ^ . o i t . , chap. X llle pp. S01-814*

Page 30: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

35PI ATION OF "AVERAOE SIZE" PARTICLETHE DE®

In any method f o r th e determ ination of mag­

n e tic p erm eab ility of pu lverized m a te r ia l , th e e f fe c t of v ar­

ia b le g ra in s iz e i s extrem ely im portan t. The general procedure. ' . — • ■- - - :; : ■ • r. '. : '

of p reparing s ized magnetic m a te ria l i s to crush or grind the

m a te ria l and then s iz e w ith Tyler standard s ie v e s . The average

s iz e of p a r t i c le fo r each sc reen f ra c t io n may not n ec e ssa rily

be the average o f the diam eter o f th e ho les of th e l im itin g

sc reen , and th e re fo re determ ination of the average g ra in s iz e

becomes necessary . Determ inations were made by th ree methods,

denoted "A", "B", and "0".

- ̂ Method "A"

A sample of a screen f r a c t io n was mixed

w ith some liq u id Canada Balsam on a g la ss s l id e ; a cover g la ss

was then pressed upon th e m ix ture. This s l id e was mounted upon

a mechanical stage o f a microscope equipped w ith a micrometer

ocu lar and th e g ra in diam eters were measured, u sing tran sm itted

l i g h t . From 50 to 160 g ra in s were measured in order to ob tain

a f a i r average , which n e c e s s i ta te s a system being adopted , using

the mechanical s tag e , whereby no p a r t ic le would be measured

tw ice. The "average s in e" p a r t i c l e , as used in th i s paper,

i s defined a s the num erical average of the measurements of 50- . - ■ • • • • • ‘ ' < •

to 150 g ra in s ; two measurements must be made on each p a r t i c le —

one along the g re a te s t and the o ther a long the sm a lle s t dimen­

s io n v is ib le . A f a i r average was obtained by averag ing th e

Page 31: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

f i r s t ana l a s t h a lf of the read ings and i f th ese two values

were co inc iden t w ith in the experim ental accuracy , the t o t a l

average was re p e rted as th e "average e ia e M p a r t i c le .

: ' ' ; - ; Method "B" : "

This method co n sis ted in the working of a

sm all m agnetite sample in to Canada Balsam on a cover s l i p .

A b rass r i n g .0 .26-inch long and 0 .50-inch diam eter was placed

around th e m ixture and the b rass contaizm r f i l l e d w ith Canada

Balsam. A g la ss s l id e was then placed on th e open end of the

r in g , the Canada Balsam adhering to th e g la s s . The m agnetite

sam ple, w ith the g la s s cover s l ip upperm ost, was examined by

tran sm itte d l i g h t . By u sing old Balsam, which i s r e la t iv e ly

viscous when cold but which becomes f a i r l y liq u id when warmed,

the s l id e specimen w as.made permanent. The method of measure­

ment was the same as described under method "A".

..... -. . . -.......’ ' ' ;. Method "0" ■;..... :: ; . - . 7 . ... -.. ■;" ■; :■:. " . - . ■ , ■ " .. - ' ! ; v; **. -• -r

A sample of the m a te ria l was s t i r r e d in to

visooua C h asse r^ cement contained in a r in g of b rass tubing

approxim ately l /2 - i i i s h long . The m ixture i s allowed to see l

and harden, a f t e r which the su rface of the specimen i s ground

and p o lish ed . The " b r iq u e tte " i s then mounted fo r examine-

t io n w ith a m etallographio m icroscope. The measurementa were

c a rr ie d out the same as ou tlined under method "A".

Page 32: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

Experiments were made with th e eb jee t of

determ ining which of the methods described o ffered th e g re a t­

e s t promise of y ie ld in g th e " tru e" value of th e "average s iz e "

p a r t i c le . Tables 2-a and b p resen t the r e s u l t s of measure­

ments u sing methods "A", and "G".

3ample- H°J

Screen s iz e , .mesh

O bjective ~ used .

Average Size1* of p a r t i c l e , m illim ete rs

Through : mm. : • t "B" : nC"

180 1 • 0.002 0*011i :

200 $ 380 0.002 0.088 $ :■ ■ 180 v t 200 0.000 0.144.

100 : 160 0.004 0.188 s 0.177 : 0.07416 t 100 0.0189 0.29148 $ 66 I> ' .. - . . '

Table 2 - t . —Grain Size Measurements Using Sample Ho.

. ./ .

11a. M ineville M agnetite.■ \ ' . : , .

Screen e ls e ,mesh

i Objee- % t t iv e i

"Average S ize" of p a r t i c l e , m illim e te rs Ratio

Through | On s used , $ »A» | "B" ; wCw i* * « rc*- : '

360 :J 0*0009)1t 0.002 )$

3 0.006)88 0.012)8 0.008 1 .6

200 i 360 - t 0*002 i 3 0.076 : 0.034 2 .2160 s 200 S 0.004 % 3 0.134 3 0.056 2 .4100 t 180 ; 0.004 $ 3 0.180 3 0.079 2 .3

66 t 100 8 0.0189 8 8 0.258 8 0.132* 1.9648 J

200 ! 250 $270 :

65260270860

s 0.0189 s : 0.002 $ 8 0.002 3 3 0.002 8 :

8 0.315 s3 0.098 8s 0.081 3 3 0.069 3

:

0.181 1 .74

*0b je e tiv e used was 0.004-mm.

Page 33: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

The screens used as l is t® ! in the f i r s t

two columns, Tables 2-a and 2-b , a re Tyler standard sieves#

The s ig n if ic a n c e of th e f ig u re s l i s te d in the column "Objec­

t iv e used" i s th e value of each sca le d iv is io n of the micro­

meter d isc in the ocu lar o f th e microscope w ith the o b jec tiv e

used fo r th a t p a r t ic u la r screen f r a c t io n . .

I t i s th e w r i te r ’s opinion th a t of the

th re e methods t r i e d , method ”B" approaches the " tru e r value

of the "average s iz e " or p a r t ic le as defined above. The r e ­

s u l t s obtained by each method a re r e la t iv e ly c o rre c t, but the

ab so lu te values of "average size*! probably approach those of

method "B". The r e s u l t s obtained by employing method "B"

a re used throughout as th e "average s iz e " p a r t i c l e . The r e a ­

son fo r th is apparent v a r ia t io n of values f o r the "average

s iz e " in method "A" probably i s due to th e e f fe c t of fo rc in g

the cover s l ip down upon the g ra in s , thereby causing an a l ig n -i • !.ment p erp en d icu la r to the l in e s of force* In method .^C" th e i ; " “ ' ' i r | ■ •"read ings a re made by measuring sections; of p a r tic le s ^ which,

in the opinion of the w r ite r , tends to cause low r e s u l t s fo r

th e "average s iz e " p a r t i c le .

Page 34: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

.MATERIALS USED

- ‘ - . Table S g ives a d e se r ip tio a in summary form of>

the m a te ria ls used . ; : -

Table 3 . . .Summary of the M ateria ls Used

M agnetiteeentent Den­ Methods of

Ho. B eslg- Source Per - Grams s i ty preparationn a tio n cent * *

0. 0.

10 Magne- Witherbee-Sherman Co., See page 28t i t * M inev ille , H.Y. - ■

11a do. " do. '■ • - ' • 90 See page 28l i b do. ... . do. 91.6 2,836 See page 28

2A Magne­ H o .lib , Ho. 3 73.8 2.255 80^ H o.libt i t e

m ixture2 # Ho. 3

SB do. do. -: ; ;z V- " 55.8. _ -*;*». . • • . .... -■

1.850 60=5 HO.lib 40̂ 5 Ho.3

■ " ; *20 do. do. . 27.7 1.455

■ .Ho. 11b

7 # He. 3

SD do. do. ' " - - - ' 46.2u v /• / •

0.787 1,704 SSS S:i". . . \ .2E do. 32.3 0,488 1.510 35^ H o .lib

. '■>. 665$ Ho.3

2F do. do. 25.0 0.3645 1.421 27J5 Ho. 11b• . 7356 Ho.3

EG do. do. • 12 .9 0,1680 1.298 145S Ho. 11b 86=5 Ho.3

2H do. '4@# 7 .4 O.OfSl 1.246 8.0% H o .lib 92% Ho.3

3 Quartz Ottawa, 111. 0 ' 0 1.186 See page 294 Magne­ Hevada Cons.Copper Go., See page 29

t i t e Hurley, II.M.5 do. Calumet & A ria . Copper

Co., Dou^lae, A ria .See page 29

6 R u tile 0 0 m u m ' See page 29

Page 35: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

Kethoas of P reparing IS a teria ls

Ho. 10 :

The m ineral m agnetite was s ized as fo llow s: -65 +100^

-100 +150, -150 +500, -200 .*350, -550 mesh. A ll s iev es used

were Tyler standard s ie v e s . This m a te ria l was used only in

the pre lim inary work f o r the determ ination of "average s ize"

p a r t i c le and magnetic da ta were not obtained*

HQ. 11a :

The o r ig in a l specimen of m ineral m agnetite was ground

through 48 mesh, m agnetica lly concen tra ted , and s ized . The

f r a c t io n , minus 48 p lu s 65 mesh, was d igested in 10 per cent

so lu tio n of f e r r i c su lphate to remove the m e ta llic iro n , a f t e r

which i t was washed, d r ie d , and ground in an agate mortar to

secure th e fo llow ing sized fraction s: -48 +65, -65 +100,

-100 +150, -150 +200, -200 +250, -250 +270, -270 +550, -550

mesh. Each of these sized f r a c t io n s was analyzed fo r magne­

t i t e content. The potassium dlehrornate and the potassium p er­

manganate methods fo r fe rro u s iron were used fo r th ese analyses

The r e s u l t s of bo th methods were averaged to ob tain the magne­

t i t e co n ten t. The value repo rted in Table 3 i s the average

value of m agnetite co n ten ts of a l l the fr a c tio n s .

Ho. 11b:

This m a te ria l i s th e o r ig in a l sized f r a c t io n minus 100

p lu s 150 mesh obtained as described under Ho. 11a. Half of

th i s f r a c t io n was ground through 350 mesh* These two s iz e s ,

-100+ 150 and -350 mesh, were se p a ra te ly d igested in a 10 per

cent copper su lpha te so lu tio n to remove m e ta llic iro n . They

Page 36: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

were then washed, d r ie d , and resereened* The m agnetite een-

te n t of th e -100 t-150 meah was 90.8 per c e n t, and th a t of the

-880 meah 92.4 per c e n t. The d e n s ity a s used in Table 3 la

defined oh page 40.

Boa. 2A to 2H. in e lu a iv e :

The m agnetite con ten ts as rep o rted in Table 3 were ob­

ta in ed by c a lc u la tio n from those known fo r the o r ig in a l sub-

etanoea. The d e n s i t ie s of m a te ria ls numbered SB to 2H, in ­

c lu s iv e , were ob tained from the curve shown in F igure 10.

Pure quartz was. ground through 350 meah, d i l a t e d in

d i lu te hydroohlerio a c id , w a s h # , ig n i te d , and resize#*

M ineral m agnetite was tre a te d to remove any m e ta llic

iro n p re se n tj i t was then ground to -100 *150 mesh s iz e in

an ag a te m ortar, and a p o rtio n of th e product was then ground

to -350 mesh.

Ho. 5 :

Furnace a c c re tio n m agnetite was ground through a 200-

mesh s ie v e , d igested in copper su lphate s o lu tio n , and re s iz ed

to -200 *350 meah. I t was then analyzed fo r m agnetite con­

te n t and a p o rtio n was ground to -350 mesh in an ag a te m o rta r |

the l a t t e r was used fo r magnetic balance work.

Ho. 6 :

R u tile was ground through 350 mesh, d igested in d i lu te

hydroch lo ric a c id , washed, ig n i te d , and re s iz e d .

Page 37: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

- 20 -

M&.6HETIC BALAJICI METHOD

On aooGnnt of the aforem entionea d i f f i c u l ­

t i e s concerning th e use o f th e b a l l i s t i c a p p a ra tu s , a study was

s ta r te d fo r th e purpose of in v e s tig a tin g th e p o s s ib i l i ty of

applying the-m agnetic balance method f o r th e com parative meas­

urement of th e magnetic s u s c e p t ib i l i t i e s of magnetic m a te r ia ls .

The Curie p r in c ip le i s th e b a s is of a l l types of magnetic b a l­

ances te s te d by th e w r i te r , th e only v a r ia t io n being th e means

of m agnetically a t t r a c t in g th e magnetic m a te r ia l. Two methods

of producing th e magnetic f ie ld s were used by Sosman; iro n -co reSO 31

elec tro -m agnetio p o le s , and a so lenoid magnetic f i e l d .

Instrum ents using both o f Sosman*s methods were assembled and

experim ents were ca rried out in order to determine which offered

the most prem ise.

The Solenoid Type of Magnetlo Balance

Figure 2 , page 6 , re p re se n ts a diagrammatic

view of the appara tus, w ith the exception th a t the pole p ieces

shown were rep laced by a so len o id , approxim ately 16 centim eters

long and 1 centim eter d iam eter. By allow ing a constant e l e c t r ic' V ' •

30 — — —Sosman, R. B ., and H o s te tte r , J . C ., op. c l t .

31Sosman, R, B ., and Poanjak, E . , op. p i t .

Page 38: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

- 3 1 -

cu rren t to flow through th i s solenoid a magnetic f i e ld was pro­

duced so th a t a capsule con tain ing magnetic m a te ria l would be

a t t r a c te d . The in te n s i ty of the a t t r a c t io n was measured by an

assay ba lance , accurate to 0, 02-m illig ram , and re s u l ts could be

reproduced w ith in 1 per c e n t.

The f i r s t experim ental work to be ca rried

out was to determine the e f fe c t of various s iz e s of p a r t ic le s

upon the magnetic a t t r a c t io n . The methods fo r determining the

"average s iz e " p a r t ic le have been described and the data a re

presented in Table 2-b. The r e s u l ts of the magnetic determ in­

a tio n s on various p a r t ic le s iz e s , using the various sized f r a c ­

tio n s of m agnetite No. 11 -a , a re shown in Figure 5.

r i,3------------ -------------U______ L___________________ 1___

Figure 5 . —E ffec t of "average s ize " p a r t ic le upon the magnetic a t t r a c t io n , using the solenoid magnetic balance.

Page 39: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

- 3 8 -

$he r e s u l t s o f measuring the magnetic a t t r a c ­

t io n of vario u s s iz e p a r t ic le s in d ic a te a d iffe re n c e of 2*7

m illig ram s between p a r t ic le s of average s iz e , 0.006 m illim ete rs

and 0.315 m illim e te rs . Expressing th ese re s u l ts in term s of

per eent based on the magnetic a t t r a c t io n of the la rg e r s iz e

p a r t i c l e , th e sm aller s iz e p a r t ic le s have a magnetic a t t r a c ­

t io n 21 per cen t l e s s than th e la r g e r . I t may be noted th a t

due to low in te n s i t i e s o f th e magnetic f ie ld s th a t th e d i f f e r ­

ences in a t t r a c t io n as measured in m illigram s a re sm all and

th e re fo re the balance must be s e n s i t iv e ; the balance used in

th i s work was ad ju sted fo r a high degree of s e n s i t iv i ty and

therefore n ec ess ita te d freq u en t checking of th e zero p o in t.

As p rev iously m entioned, m agnetite has an appreciab le h y s te re ­

s i s e f fe c t which n e c e s s i ta te s the use of a so lenoid having a

uniform magnetic f i e l d . Sue to th e d i f f i c u l t i e s mentioned sad

in view o f the f a c t th a t the po le -ty p e m agnetic balance de­

creased these d i f f i c u l t i e s , th e so leno id-type instrum ent was

not f u r th e r used in th i s work.

The Pole-Type Magnetic Balance

R efe rrin g aga in to F igure 2, page 6 , the

po le-type apparatus used followed t h i s diagram w ith a few mod­

i f i c a t io n s . The appara tu s used f o r t h i s work was a sm all

la b o ra to ry balance having an accuracy of approxim ately 1 to

2 m illig ram s, which req u ired the use of a correspondingly

greater magnetic f i e l d . The l a t t e r was obtained by means of

a s o f t iro n -co re p o le -ty p e electromagnet. The co n ta in e r f o r

Page 40: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

the m a te ria l m s made of b rass and con sis ted of a cup 1 .35

cen tim eters in d iam eter and 1.26 cen tim eters h igh , w ith a

sm all screw on the s id e which served to hold a c lo s e - f i t t in g

p lunger, 2 .3 cen tim eters long , t ig h t ly once the plunger had

been ad ju sted . A sm all ey e le t was a ttach ed to the top of the

p lunger, to which th e balance arm was connected. When in use

th e co n ta in e r capsule was ad justed so as to r e s t d i r e c t ly upon

th e pole p ieces of th e magnet.

A constan t e le c t r ic c u rren t of approxim ately

0. 49-ampere was used to induce th e magnetic f i e l d , which in

tu rn produced an a t t r a c t in g fo rc e of th e o rder of 10 to 12

grams f o r pure m agnetite m a te ria l weighing 0.500-gram. This

fo rce was measured by a llow ing sand to slow ly r m upon the b a l­

ance pan u n t i l the capsule was pu lled away from the pole p ie c e s ,

the capsule being f i r s t balanced without th e a t t r a c t in g f i e l d .

A fte r each sample was placed in th e co n ta in er th e l a t t e r was

tapped u n t i l successive determ inations y ie lded re s u l ts which

were ecn stan t w ith in an experim ental e r ro r of 1 per c e n t.

This co n stan t r e s u l t was the repo rted value of the magnetic

a t t r a c t io n f o r th a t p a r t ic u la r magnetic m a te ria ls

Using the method described, the e f fe c t of

"average g i s t ” p a r t ic le upon m agnetic a t t r a c t io n was determined

and is p resen ted in F igure 6.

Page 41: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

- 3 4 -

Figure 6 . —The e f fe c t of "average s ize" of p a r t ic le s upon magnetic a t t r a c t io n , using th e po le-type

of magnetic balance.

By comparison of Figure 6 w ith Figure 5,

i t may he observed th a t the sen s itiv en ess of the po le-type

balance is not as great a s th a t of the so len o id -ty p e , the

v a r ia tio n of th e 0 .006-m illim eter m ateria l being only 6 per

cent as compared w ith la rg e r s iz e 0 .316-m illim eter m aterial

while th is amounts to 21 per cent fo r the so len o id -ty p e .

Page 42: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

fhese curves dem onstrate the f a c t th a t v a r ia tio n in s ize of

p a r t ic le in flu en ces th e magnetic m a te ria ls and therefore i f

comparable r e s u l t s a re to be obtained on d i f f e r e n t magnetic

m a te ria ls the g ra in s iz e of th ese m a te ria ls must be id e n tic a l .

A fte r th e work upon e f fe c t of g ra in s ize

was completed the po le-type balance was improved. The pole

p ieces were moved f a r th e r a p a rt in o rder to e lim in a te the use

of sand to balance the p u l l , and th i s reduced th e a t t r a c t io n

to be measured from about 11 to 1 .5 grams, the s iz e of the

sample being a ls o reduced from 0.50 to 0 .25-gram. A marked

g la ss s l id e was a ttach ed to th e pole p ieces to f a c i l i t a t e th e

centering of th e container over the pole p io ees . The a t t r a c ­

t io n was th en measured d i r e c t ly w ith standard weights. The

procedure fo r th e p re p a ra tio n of th e m a te ria l was a lso modi­

f ie d and comprised i

1 . In tim ate m ixing of th e m ate ria l in the capsu le .

2 . Demagnetization of the m ateria l in a decreasinga l te rn a t in g magnetic f i e ld , thus in su rin g the e f fe c ts due to h y s te re s is were absen t.

3 . The m ate ria l was aga in mixed.

4. The m a te ria l was leve led by g e n tle shaking andby f ix in g th e p lunger in p lace and then r o ta t­ing i t .

6. The co n ta in e r was tapped 10 to 20 tim es w ith hard blows upon a so lid p iece of wood while ho ld ing the p lunger f irm ly down upon the m a te ria l and then th e plunger was made f a s t by means of the screw. - •

The co n ta in e r was next placed over th e

polo p ieooe, the current turned on, the balance connected, and

weights added to th e balance pan u n t i l the magnetic p u l l was

Page 43: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

ju s t enough, to hold the co n ta in e r . The weighings were d e te r -

mined to the order of 1 m illigram . Using th i s improved p o le -

type in strum en t, th e e f f e c t of d i lu t io n was stud ied using

q uarts as the d i lu tin g agen t.

The E ffec t of D ilu tio n of M agnetite w ith Quartz

The procedure fo r determ ining th e e f fe c t

of d i lu t io n upon magnetic a t t r a c t io n when u sin g m agnetite m s

as fo llo w s ;

1, The m agnetite and quartz were weighed d i r e c t ly

in to the sample co n ta in e r in the proper p roportion to make a

t o t a l weight of 0#2600-gram.

2. The m ixture was tre a te d and te s te d m agnetica lly

a s o u tlin ed on page 36. R esults were rep roducib le w ith in 1

p er cen t using th e same m agnetite m ixture j th i s dem onstrates

the la ck of segregation of th e components in the m ix tu re . The

m agnetite content was re p o rted as th a t determined by chemical

means in th e in te rp re ta t io n of these r e s u l t s . The r e s u l t s of

th i s work appear in th e form of cu rv es , which fo llow .

Page 44: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

r - 3 7 -

L - - - " JFigure 7 .—The e f fe c t of d ilu tin g m agnetite H o .lib , -350 meah and H o .lib , -100 +150 meah, w ith q u a r tz , -350 mesh and -100

+150 mesh, re sp e c tiv e ly .

10 20 30 4090 80 70 60

COMPOSITION

Figure 8 .—The e f fe c t of d ilu tin g m agnetite Ho. 4 , -350 mesh (lower cu rve), and Ho. 4, -100 mesh, with quartz -350 mesh

and -100 mesh, re sp e c tiv e ly .

Page 45: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

Several observations may be noted from a

co n sid e ra tio n of these cu rves. The most s ig n if ic a n t f a c t i s

th a t the curves a re not s t r a ig h t l in e s ; th i s variance from the

expected s t r a ig h t - l in e curves may be explained from th e type of

magnetic f i e ld which a t t r a c t s the m a te ria l and a lso from th e

v a r ia tio n of the d e n s it ie s of th e mixtures* The f ie ld becomes

weaker as the d is tan ce away from th e pole p ieces in c re a se s ,

and consequently , i f th e d en sity e f the p u lv e ru len t m a te r ia l

decreases o r , since th e d iam eter of th e co n ta in e r i s c o n s ta n t,

the heigh t in c re a se s , th u s producing a more than p ro p o rtio n a te

decrease in magnetic a t t r a c t i o n w ith d i lu t io n . The f a c t th a t

in Figure 7 the curves fo r th e -100 +i80-me#h and -3§0-mesh

m a te ria ls do net show a p ro p o rtio n a te decrease may a lso be

explained by th e v a r ia tio n in pulp d en sity . This d en sity is

not only a fu n c tio n of th e "massive d en sity " of the m a te r ia ls ,

but a lso r e l i e s upon the amount of v e ld s , which in tu rn de­

pends upon packing of the mixed substances. I t was, th e re fo re ,

im portant th a t accura te knowledge be obtained oeneerning den­

s i t i e s of the ground m agnetite and s i lu t lo n s of m agnetite , and

th e re su lta n t e f f e c t upon magnetic a t tra c tio n * I t i s known

th a t when a m ixture of m inerals i s ground the in d iv id u a l min­

e r a ls a re not u su a lly d is tr ib u te d in the same r a t io in a l l th e

sized f ra c t io n s . Therefore in a l l the fo llow ing work i t was

decided to g rin d to minus 360-mesh in order to e lim in a te as

much a s p o ssib le the e f fe c t upon th e magnetic a t t r a c t io n caused

by th e v a r ia tio n s of m agnetite con ten ts fo r the d if fe re n t p a r­

t i c l e s iz e s . That i s , a m ixture which produces a preponderance

of minus 360-mesh m agnetite when ground w ill have a le s s

Page 46: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

a t t r a c t l e a than one which producea the m agnetite in th e ocareer

s iz e s , even though the two have equal m agnetite co n ten ts .

The Penalty of P u lveru len t M ateria ls

A photograph of the apparatus designed by

the w r i te r to measure th e d en sity of dry pu lverized m aterial®

i s p resen ted in Figure 9, and c o n s is ts of a c a p illa ry tu b e ,

closed a t one end by fu s in g . A sm all funnel was sealed to the

o ther end in order t e f a i i l t t a t e th e t r a n s f e r of m a te ria l to the

c a p il la ry . This tube f i t s in to a rack which has a s ta tio n a ry

s c a le , graduated in m illim e te rs along one edge. The m a te ria l

i s weighed in to th e funnel and tapped u n t i l the heigh t of the

column is eonstant as read w ith th e aid of a movable piece @f

paper w ith a f in e l in e drawn upon i t . The tube was c a lib ra te d■

by p lac in g v a ria b le amounts of mercury in i t and measuring the

heigh t of each mercury column and then weighing the tube te

ob ta in the weight of mercury contained by d if fe re n c e ; th e abso­

lu te volume was ca lcu la ted and the d en sity of any m ate ria l c f

known weight and placed in the tube i s then o b ta in ab le . The

accuracy of the density determ ination was of the order of 1 per

Page 47: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

-4 0

Figure 9•—Photograph of th e "densitom eter*"

From th i s d iscu ssio n i t fo llow s th a t th e

term "d e n s ity ” as app lied to pu lveru len t m a te ria l when used in

th i s paper i s the number of grams of m ate ria l which w ill occupy

a volume of 1 cubic centim eter when tapped u n t i l no fu r th e r

in crease in den sity is observed.

The d e n s itie s of m a te ria ls Ros. 2 , 2A, 2B,

2C, and 3 t which a re described in Table 3 , were determ ined and

the r e s u l ts a re in d ica ted in Figure 10.

Page 48: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

•41

IF THEl a w o r

100-MAGNETITE NO 1^-350 MESH0 -Q U A RTZ, -3 5 0 MESH0 60 * 50 4 0 3(

COMPOSITION BY WEIGHT, PER CENT

Figure 10#--The r e la t io n between density and com position, using m agnetite -quartz mixtures*

I t is observed from Figure 10 th a t the

u sual law of m ixtures a s app lied to d en sity does not hold fo r

the m ixtures u sed , and the d ensity of a m agnetite -quartz mix­

tu re is not the weighted average of th e component densities*

This is presumably due to the d iffe ren ce in r e la t iv e packing

of the quartz and m agnetite which in tu rn might be caused by

the d iffe ren ce in shape of t h e i r re sp e c tiv e g ra in s .

Page 49: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

- 42 -

Development of a C a lib ra tio n Curve fo r Determining

the M agnetite Content of Substances

Magnetic measurements were made according

to the procedure ou tlined on page 55 w ith the exception th a t the

a t t r a c t in g c o ils and pole p ieces were changed in order to in ­

crease the s e n s i t iv i ty of the magnetic balance fo r dea ling w ith

m a te ria ls of small m agnetite co n ten ts . A photograph of th i s

f in a l apparatus i s shown in Figure 11.

Figure 1 1 .—Photograph of the Magnetic Balance f in a l ly adopted.

Page 50: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

V aria tions In the d e n s it ie s of magnetic

m a te ria ls in fluence the magnetic r e s u l t s in two ways—f i r s t ,

the a c tu a l volume of the m ateria l taken to determine th e mag­

n e tic a t t r a c t io n , and second, the amount of m agnetite (FegC^)

per u n it volume of m aterial# In order to study the f i r s t

e f f e c t , m a te ria ls Nos. 2d , 2E, 2F, 2G, and 2h, which a re de­

scribed in Table 3, were used and the magnetic a t t r a c t io n of

various volumes of th ese m a te ria ls were determined and p lo tte d ,

as shown in Figure 12#

14 00

ooool OS 5? 5aVOLUME, CUBC CENTIMETERS

Figure 12 . —The e f fe c t of volume of m agnetite m ixtures uponmagnetic a t t r a c t io n .

Page 51: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

- 4 4 -

In order to ob tain a s e r ie s of curves which

would account fo r both these e f fe c ts due to d en s ity , the degree

of magnetic a t t r a c t io n was obtained from Figure 11 where the con­

s ta n t com position curves cut the volume o rd in a te s : 0.080, 0.120,

0 .170, and 0.210 cubic cen tim eters. The com positions of each of

these m a te ria ls being known in grams of m agnetite per cubic cen­

tim e te r (see Table 3 ) , curves were drawn showing th e r e la t io n

between m agnetite (Fe^O^) content and magnetic a t t r a c t io n a t

sev e ra l constant volumes. These curves a re presented in Figure 13.

1.400

0.600

0.200

08000400 0.600

, P C O S * CENTIMETER Of MATERIAL0000

g ram s or m a o c t it c ,

Figure 1 3 .—The r e la t io n between m agnetite conten t and magnetica t t r a c t io n a t constan t volume.

Page 52: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

To determ ine th e m agnetite con ten t of any

m a te r ia l , the d en sity of th e m a te ria l a f t e r g rin d in g through

350-mesh being known, a weight is se lec ted such th a t the volume

occupied i s th a t fo r which a curve has been p lo tte d as shown in

Figure 13, and the magnetic a t t r a c t io n fo r th i s volume is then

measure*$ th e eom peeition i s next obtained d i r e c t ly from the

proper curve. A fte r th e com position in grams of m agnetite per

cubic cen tim eter has been determ ines, the per cen t by weight

Is obtained by d iv id in g th e grama of m agnetite (FegO^) per

cubic cen tim eter by th e d en s ity and m u ltip ly ing by 100. The

reason fo r th e above curves being constan t-v e lu m curves ra th e r

than density i s th a t th i s procedure e lim in a tes the n ec ess ity

of in te rp o la t io n .

I t may be observed from th i s d iscu ssio n

th a t th e method i s dependent upon th e fo llow ing p o s tu la te :

That a constant amount of pure m agnetite w i l l show the same

magnetic a t t r a c t io n (or s u s o e p t ib i l i ty ) independent of what

th e composition of th e in term ediary components may be (except,

of cou rse , i f th e l a t t e r a re a lso m agnetic), provided th a t the

t o t a l volume of th e m a te ria l remains equal.

The TJae of th e C a lib ra tio n Curve

In order to t e s t th e v a l id i ty of th e fo re ­

going c a lib ra tio n curve i t was, of cou rse , necessary to d e te r­

mine the m agnetite con ten ts by th e m agnetic-balance method of

substances of known chem ically determined m agnetite co n ten t.

Page 53: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

From a eo n s ld e ra tio a of th e ea rv is shown In Figure 13 th e re a re

th z te measmrahle v a r ia b le s which f i x th e magnetic a t t r a c t io n —

namely, th e d en sity , the a c tu a l volume of th e m a te ria l used ,

and the m agnetite co n ten t. F u rth e r, the in d iv id u a l m agnetite

m a te r ia l s , , whether m ineral or fu rnace p roducts, m ight have some

e f fe c t upon the value fo r the m agnetite con ten t a s .determined by

th e magnetic balance method* The c a lib ra tio n curves {Figure 13)

were determined by u sin g m ineral m agnetite . As, i t i s planned'• i , ■ : ■ . • !

to use th ese curves fo r the determ ination of m ag n e tite -in furnaoe

products as w ell as in m inera ls , m agnetite contents o f m ixtures

of fu rnace m agnetite and a lso m ineral m agnetite w ith quartz

and r u t i l e of known chem ical m agnetite © intents were determined , - - ' :- ■ ; . . ■

Krith th e magnetic balanoe. I t i s noted th a t a l l the v a r ia b le s

which a f f e c t the determ ination of m agnetite by the balance methodf:.- : ' : ■' :. ;■ ' . : ■' !

have been a lte re d in order to te s t th e accuracy of th e c a lib ra -- : ■■ ; ; - ■ ■- . • - : • :t io n curves* The r e s u l t s of t h i s work a re shown in Table 4.

Page 54: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

oh an lo a l l y .

Mixture cotnpositiewi, ’by weight nature of Density, Volume used for liagnetlte ise^eart. PercentageMat*- M agxeMte BllutjLog agent magnetite grama the magnetite per cent b: weight differenceH A5## Ho. Per cent Ho. Per cent

per o.o. determination,0. 0.

Oaloalated

chemloal

Magnetic H=HL V 100 71

i I I XII IV T VI VII f i l l

4A 4 27.00 8 78.## MSsma. 1.884 0.120 24.3 24.2 0.4

4B 4 sf.eo 6 73.00 * 8.874 0.120 24.3 24.0 1#8

40 4 13,50 3 86.60 1.883 @.170 38 OS 12.1 0.4

49 4 13.50 6 86.50 2.586 #•18# 12.15 11.8 2.9

4E 4 6.75 3 93.25 1.4fiL 0.210 6.08 5.75 w

4V 4 6.73 6 #8.87 2.587 0.120 4»#6 5.79 4.5

5A s 87.00 3 78.## Pumaoe 1.677 0.120 88.6 25.3 1.4

SB 6 87.00 6 73.00 * 2.667 0.120 25.6 25.3 1.4

50 5 13.50 3 86.50 1.676 0.170 12.80 12.2 4.7

5D 5 13.50 6 86.50 2.577 0.120 12.80 12.2 4.7

SB 5 6.75 3 93.25 1.464 ©.81# 6.41 5.98 6.7

5F 5 6.75 6 93.25 * 8 .m #.120 6.41 5.94 7.8

'It?-

Page 55: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

•48

I t i s noted from Table 4 th a t th e magnetic

balance method need is capable of y ie ld in g co n s is te n t r e s u l ts

when compared to chem ically determined m agnetite con ten ts of

th e m ixtures used. R eferring aga in to Table 4 , columns I I I ,

IT, V, and VI rep resen t th e "v a riab le s" p rev iously d iscu ssed ,

and i t i s noted th a t th ese have been a l te re d w ith in wide l im i t s .

The percentage accuracy given in column T i l l v a r ie s from 0*4 in

the case of h ig i m agnetite con ten ts to 7 .3 fo r low m agnetite

co n ten ts . Those f ig u re s in d ic a te th e probable accu rac ie s of

the magnetic balance instrum ent by v ir tu e of th e f a c t th a t they

a re lim ited by th e accuracy of th e c a lib ra tio n curves. C ertain

e r ro rs in th e mechanical mixing of d ilu tin g substances combined

w ith the e r ro rs involved in th e chemical determ ination in d ic a te

th a t accu rac ies of th e m agnetic 'balance g re a te r than those noted

can not be expected. I t i s In te re s t in g to no te , however, th a t

the magnetto balance is capable of reproducing values fo r the

m agnetite content of m ixtures of th e same com position very

c lo se ly . Another very im portant conclusion which may be drawn

from the r e s u l t s presented in Table 4 i s the r e la t iv e magnetic

p ro p e rtie s of n a tu ra l m ineral m agnetite and th a t formed by

furnace reactions* These da ta show l i t t l e , i f any , v a r ia tio n

in m agnetite con ten t a s determined from t h e i r magnetio prop­

e r t i e s u t i l i s e d by the m agnetic-balance method. I t i s f a r th e r

seen th a t the d i lu tin g medium does net have any e f fe c t upon

th e determ ination of m agnetite content when q u arts or r u t i l e

a re used.

Page 56: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

- 4 9 -

The s lag s used hy Roberts and Hageat

In th e i r etufly o f th e Hawley chemical method fo r the d e te r­

m ination of m agnetite were found to be a v a ila b le and were

te s te d by means of the magnetic balance as used by the w rite r .

The r e s u l ts of th i s work a re presented In Table 5, page 60.

I t i s noted from a co n s id e ra tio n of the

r e s u l t s presented in Table 5 th a t th e m agnetite co n ten ts of

s lag s nos, 11, 4 , and 8 a s obtained by the chemical method

(column I I ) agree w ith th o se determined by the magnetic b a l -

anee (column IT) w ith in the experim ental e rro r of both methods $

a l l o ther r e s u l t s do not show the requ ired agreement. I t i s ,

however, noted th a t both magnetic balance re s u l ts (columns I I I

and IV) show a marked consistency . The d iffe ren ce in m agnetic-

balance r e s u l ts obtained by th e w rite r from those repo rted by

Roberts and Nugent might p o ss ib ly be due to th e f a c t th a t th e

"d e n s ity ” of th e p u lveru len t m a te ria l was taken in to consider­

a t io n . The probable experim ental percentage d iffe ren ce of

determ ining m agnetite con ten ts by th e m agnetio-balanoe method

as compared to chemical methods fo r converter s lag s i s l e s s

than 8 per cent and fo r re v e rb e ra to ry s la g s is le s s than 8

per c e n t. The v a r ia tio n of m agnetite con ten ts fo r the m ajo rity

of s la g s a s obtained by the eheaieal and magnetic balance

methods i s d i f f i c u l t to exp lain from th e b a s is of experim ental

e r ro r g iven . Several p o ss ib le exp lana tions of th i s marked

82 ...

52 • • .R oberts, L. E . , and Nugent, R, L ., op. p i t .

Page 57: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

pQfefaiTable 5

I IX I I I 17 TSlag Ho.

(R.I.3120)

kagrotite content reported by Roberts and Hugent,

Magnetite oonteat from magnetic balance re-

Magnetite content from magnetic balance re­ported by writer,

per cent

Per cent differenceM t . 100

' \\- '18.2 17.7 . 11. . :''

25.78 26.2 24.6 4.6

2^48 22.8 22.0 18.25.12 25.8 24.0 4.5

9> 18.82 17.2 16.1 14.

11 28.05 *8.8 88.7 2.3IS 25.32 *6.* 84.4 5.6

2 4.48 4.0 3.88 . ;12.. .4 IMS 8.7 10.1 0.2

6 9.61 S.S W.4 8.5

• 1.79 1.5 1.80 0.6

10 5.76 ; s - 5 ■ .v : 4.56 21.

12 ' 4.94 2.0 .3.02 39.

-09-

Page 58: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

-SI*

v a r ia tio n p resen t them selvess

1* The e f fe c t of s iz e of m agnetite g ra in

upon m agnetic a t t r a c t io n and th e re fo re on the determined magne­

t i t e con ten t has been prev iously e s ta b lish e d , from which i t i s

seen th a t i f th e s iz e of m agnetite g ra in f a l l s app rec iab ly be­

low 850-mesh, th e magnetic a t t r a c t io n w il l be reduced. This

e f fe c t may or may not be p resen t in s la g s , depending upon the

r a te of cooling of th e s la g . Thus, i f time is allowed fo r the

growth of m agnetite c ry s ta ls to such a s iz e th a t when the slhg

is ground, th e m agnetite g ra in s w il l be 350»®esh s i z e , the *

m agnetic-balance method r e s u l t s w il l not be a ffe c te d from th i s

cause. Some s la g s , however, a re ra p id ly cooled by pouring them

in to w ater, whieh p reven ts ap p rec iab le g ra in growth of the

m agnetite p a r t i c le s , th e g ra in size of which was undetermined

by th e w r i te r .

2, There i s a p o s s ib i l i ty of copper f e r r i t e

(CuO.PegOjj) being formed as a s id e re a c tio n in th e converter

and reverbera to ry fu rn a c e s . I f t h i s be the ease th e m agnetite

content determined by th e chemical method w ill probably include

the iro n p resen t as copper f e r r i t e , and so w il l be h igher than

th e tru e value . The magnetic perm eab ility of copper f e r r i t e

i s l e s s th an th a t of m agnetite and th e re fo re m agnetite con ten ts

as obtained by th e magnetic balance w ill be h igh , but w ill net

be as high a s th a t probably obtained by the- chemical method.

I t may be observed from Table 5 th a t th e re is a d e f in ite ten ­

dency fo r the m agnetite contents as determined by the m agnetic-

balance method to y ie ld lower r e s u l t s than these obtained by

Page 59: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

- 52*»

aeans of th e chemical method. E ith e r the sm aller m agnetite

g ra in s iz e in th e s la g s or th e presence of copper f e r r i t e in

the s la g s , o r both , o ffe r two p o s s ib i l i t ie s fo r explain ing the

d iffe re n c e .

3. The p o s s ib i l i ty of the presence of mag­

n e t ic substances o ther than Ire n o r i t s compounds i s u n lik e ly ,

s in ce i f t h i s %as the case th e magnetic balance r e s u l t s fo r

the m agnetite content would be c o n s is te n tly h igher than these

obtained from the use of th e chemical method u n less th is e f f e c t

m s obscured by the o ther p o s s ib i l i t i e s of e r ro r .

Page 60: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

summer

Two methods fo r th e determ ination of magne­

t i t e con ten t have been in v e s tig a te d . The b a l l i s t i c method was

deemed worthy of t r i a l , bat was shown to be lack in g in c e r ta in

fundamental c h a ra c te r is t ic s e s s e n t ia l f o r a sim ple and an aeon*

r a te method. The m agnetic-balance method w as.believed to show

promise fo r use in measuring m agnetite content and was used to

study the p ro p e r tie s of magnetic m a te ria ls which,might have

some in fluence on the determ ination of m agnetite . The r e s u l t s

of th ese s tu d ie s fo llow ;

1* Reproducible r e s u l t s fo r magnetic a t t r a c ­

tio n s were obtained by packing to a constan t volume to w ith in

1 per cen t.

2. The e f fe c t of g ra in s ize upon magnetic

perm eab ility was investigated and th e r e s u l t s dem onstrated th a t

uniform s iz e of m agnetite p a r t ic le i s neeessary fo r consisten t

magnetic a ttra ctio n . The s iz e of g rind ing was standard ized as

minus 250-mesh to avoid e r ro rs in too wide ranges of m agnetite

p a r t ic le s iz e s .

3* The v a r ia tio n of density of pulverulent

m a te ria l w ith com position was determ ined. With t h i s inform ation

the e f f e c t of volume of m a te ria l and density upon th e d e te r­

m ination of m agnetite conten t was in v e s tig a te d . From th is

the ca lib ration curves expressing magnetic a t t r a c t io n , volume

of m a te r ia l , and grams of m agnetite (Fe30^) per cubic cen tim eter

o f m a te ria l were p lo t te d .

Page 61: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

4» M agnetite conten t of m ixtures of chem­

ic a l ly known m agnetite conten ts were determined by means' of

the c a lib ra tio n omrree ana a comparison of th e chemical and

magaetie-fcalanoe r e s u l t s has been given and shows th a t fo r

m agnetite con ten ts of about 25 per cen t th e v a r ia tio n is near

1 per c e n t, and fo r m agnetite contents of about 5 per cen t the

methods vary le s s than 8 per c e n t.

5* By determ ining the m agnetite con ten ts

of known m ixtures of fu rnace m agnetite w ith the c a lib ra tio n

ourve, i t was shown th a t the mode of form ation of th e m agnetite

did not have any e f fe c t upon the r e s u l t s of th e m agnetic-

balance determ ination .

t». M agnetite conten ts of s la g s , analyzed

chem ically by Roberts and Hugent, were determined by the mag­

n e tic -b a la n ce method and very l i t t l e agreement was observed

between the r e s u l t s of th e modified Hawley chemical and the

m agnetic-balance methods. A discussion of the p o s s ib i l i t ie s

of e rro r between the two methods has been given.

fhe use of the magnetio balance for the

determination of m agnetite con ten ts of s la g s can not be re e -

ommended except when agreement w ith the r e s u l t s obtained by

the ohemloal method, such as those given in Table 5, a re de­

s ire d . The writer b e lie v e s , however, th a t th e m agnetio-balanoe

method would be s a t is fa c to ry in general i f th e cond itions which

have been presen ted a re c lo se ly observed. Lacking tim e, the

Page 62: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

- 8 8 -

w riter eonia not continue the work of d e fin ite ly estab lish ­

ing the reason fo r the lack of agreement "between magnetite

contents determined hy the magnetic-balance method and those

by means of the chemical method for s la g s .

Page 63: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

BIBLIOGrRAPHT

BEME5I, E. E . , and CROWTHER, H. H ., In troduc to ry E le c tro ­dynamics fo r Engineers i Hew York, 1926.

HiWLEY, F. Q ., Determ ination of liagne tite in %&tte and Slags Eng. & m n . Jo u r ., vol» 108, 1919, pp. 308-310.

ROBERTS, L. 1 . , and HUGEHT, R. 1 . , Determination of M agnetite in Copper S la g s : Rent, of I n f . , Ser. 3120, tr. S. Bureau of Mines, S e p t . , 1931, 14 pp*

3P001BR, T ., P ro p e rtie s and T esting of Magnetic M ate ria ls :Hew York, 1927.

SOSMO, R. B . , and HOSTETTEH. J. C ., The Ferrous Iron Content and Magnetic S u s c e p t ib i l i t ie s of Some A r t i f i c i a l an# n a tu ra l Oxide# of Iro n : Trans. Am. In s t . Min. Eng., vo l. 5 8 , 1 9 1 8 , p p . 4 0 4 -4 3 3 .

S0SM1H, 1 . B ., and POSEJAK, E . , Ferrom agnetic F e rr ic Oxide, A r t i f lo ia l and n a tu ra l: J. Wash. lo a d , o f S ciences, f o l . 15, 1926, pp. 329-342.

STARLIHC, S. G ., E le c t r ic i ty and Magnetism: London, 1924.

STUTZER, F . , GROZ, W., and BORKMU, E», Uber Magnetisohe E igensohaften der Zinkblenle i n i a n ie re r M ineralien:Me t a l l , und E rz, v o l. 15, 1918, pp. 1-9 .

MUDWMLL, C. E ., and LENT, W. F . , A Method of Measuring the S u s c e p tib il i ty of Weakly Magnetic Substances: Bay. Rev., vo l. 38, 1911, pp. 406-417.

WAIT, 0. R ., Magnetic P erm eab ility of Iron and M agnetite in High Frequency A lte rn a tin g F ie ld s : Phy. R ev ., vo l. 29, 1927, pp. 666-578.

WALL, T. F . , Applied Magnetisms Hew York, 1927.

WELO, L ., and B AUDI SCI, A ., The Two-Stage Transformation of M agnetite in to Hem atite: P h il . Mag., (6 ) , v o l. 60, 1926, pp. 399-408.

WILSON, ERNEST, On th e Measurement of Low S u s c e p tib i l i ty by an Instrum ent of a Hew Type: proo. Roy. goo. o f London, (A), VOl. 98, 1931, pp. 274-284.

Page 64: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance

-

I 0&Z‘% 3til , w8 «■a * •'. ’ *1 / »C 0

t »> l%8 | i t W : »■-. ,. iot tdf tsioS lo . ' so / .d%e

. .. , -^1 , '^

. \ . - t o ! v . - ■ P - f " t • ’ * : : r

< ft: e '0 • » * ( * ■ !.‘ ** • ;■•/.' j- . . : I . : .

- . ; , . v *x i ^ ^zu; '.•• • •,.j

.vnei , noV ;p . i w 3 . ^ : £C;*/ t . 1 % J a l i .

3s ; v sf* .: -C , . . . t *>5 . c? t O; , » . - ' i : ■ M

.

4 8 0 7

Page 65: The determination of magnetite in metallurgical products ... · 1 Electrical diagram of the apparatus used fcy Stutzer, Grozt and B o r n e a a n . 5: ' . - 2 The magnetic balance