Pamphlet 63 April, 1943

STATE OF IDAHO
C. A. Bottolfsen, Governor

IDAHO BUREAU OF MINES AlID GEOLOGY

A. W. Fahrenwald, Director

FLOTATION TESTS ON FLUORITE ORE

FROM LEMHI COUNTY~ IDAHO

lewis S. Prater

University of Idaho
Moscow, Idaho
 TABLE OF CONTENTS
-----

Page
INTRODUCTION • • • • • • • •.... . .. • • •
• • 1
GENERAL DESCRIPTION OF S~~LE .... . . . . . . . 2
TESTING. PROCEDURE . . . . . . . . . . . . . . . . . 2

Temperature of the Pulp • •• • • • • • • • •• 2

Variations in pH of Pulp ••• • • • • • • •• 3

Effeot of Sodium. S"ilioate • • • .... .... 3

Grinding • • • • • • • • • • • • • • • • • •• 3
SUMMARY .. . .......... ......... 5
TEST DATA . . . . . . . . . . . . . . . . . . . . . 6
BIBLIOGRAPHY . . . . . . . . . . . . . . . . . . . . 8
 FlOTATION TESTS ON FLUORITE ORE
-
-
FROM :LEMHI COUNTY.. IDAHO

By
lewis S. Prater

INTRODUCT ION

Due to the expansion in stef)l milloper ation .. and the large inorease in
demand for hydrofluorio aoid (assential in the manufaoture of artifioial
oryolite for the produotion of aluminum) .. inoreased demands have been made on
the fluorspar industry_ Domestic produotion for 1940 (01) was seo~nd high$st in
the history of the industry and, although figures are not available since then,
there is every reason to believe that there will be no deorease, at least for
the duration of the war. Present stooks of fluorspar are at a low level .. and
in order to stimulate produotion . the government has reoently permitted a price
inorease on crude ore (2).
Deposits of fluorspar have been looa.ted in Lemhi County, Idaho, (3) whioh
show promise of becoming oonunercial. Since these will require milling to be
brought up to thespecifioations of the industry, it was thought desirable to
oonduot an investigation of the possibility of oonoentrating these by flota-
tion. The objeot of the testing program was to determine the grade of the oon-
oentrate, and the peroentage. reoovery that could be expeoted from a milling
operation. .
The speoifioations for the three oommeroial grades of fl~orspar are given
in the follow.ing table:

TABLE I. THE CHIEF COMMERCIAL GRADES OF FLUORSPAR

--
Name Chief Use I Form CaF2
Specification %
8i02 Fe 203
:Minimum Maximum Maximum
Washed gravel, less
Metallurgical B. o. H. Steel
I
than 1 inoh & not
; over 15% fines I
85 5 --
Ground: Coarse,
Ceramio Glass a.nd Enamel fine .. &: extra fine j 95 3 0.12
Lump, gravel, and
Aoid Hydrofluorio aoid t ground' __
I 98 1 --
Although the steel industry consumes approximately 70 per oent of the total
produotion, under normal conditions there is a suffioient supply of this grade
of material near the large oenters of steel produotion. The supply of acid

1
 grade spar, however, is muoh more limited and there is .. oonsequently a greater
demand for it. The ooncentrate from a milling operation, being finely divided,
'Would be aooeptable for the manuta.oture ot hydrofluorio aoid, but c01:lld.not be
used in the steel furnaoe without briquetting or similar treatment. For these
reasons and also beoause aoid sparcownands a higher price than fluxing
material, the desirability of produoing a oonoentrate of this grade oan be
readily seen.
The writer wishes to aoknowledge the work of Mr. Clarenoe Zeuoh, Analyst,
Idaho Bureau of Mines and Geology, for the assays made on the samplas from the
various tests. Also to Mr. A. W. Fahrenwald, Direotor, Idaho Bureau· of Mines
and Geology, for his many suggestions and help in conduoting this work.

GENERAL DESCRIPT ION OF SAMPLE

A sample of approximately 100 pounds of oro was sent to the laboratory by

A. L. Anderson for milling tests in oonjunotion with work on tho geology of the
distriot. In general appearanco, the material is well crystallized and has a
vitroous luster. Piecos ranged in sizo from 9 inchos dawn to finos. Freshly
broken surfaces arc a pale groen color, although the older faoes are stained
a brownish-yellow by iron oxido. Tho sample oarries only a small amount of
oaloium aarbonato; tho ohiof ganguo material baing quartz and othor sillicate
minerals. Andorson reports tho presenoe of barite (3) in some of the doposits
of tho distriot, but no approoiablo amount was found in this partioular sample.
Tho spooifio gravity of a hand-pioked speoiman was found to bo 3.2. The hoad·
sample assayed as follows:

• 1.85%
= 20.6%

• 74.2%

TESTING PROCEDURE

Tomperature of ~~·Pul~

Preliminary tests were run to determine the effect of temperature varia-

tions in the flotation pulp_ At 200 C., fluorite can be oolleoted with ole io
aoid, but the aotion is quite sl~ggish. Long conditioning periods are needed
at this temperature, in~icating that the ohemioal reaotion at the mineral
surfaoes proceeds slowly. Heating to 300 C. notioeably inoreases the rate of
flotation and also decreases the amount of oleio aoid required. Heating still
higher to 45 0 C. again inoreases the amount of mineral which can be ool~oted.
Since satisfaotory results oan be obtained at 300 C., however, it was deoided
that all" following tests would be :made at this temperature. In praotioe,
heating to 45 0 C. would be deoidedly uneoonomioal and also more gangue mater-
ial would be oollected by the oleio aoid.

The following table gives the amount of oonoentrate oolleoted from 500-
gram head samples at various temperatures.

.. -.-.. -. __ _----
.. -. ----
 TABlE II. EFFECT OF PULP TElIPERATURE ON FLUORITE. FLOTAT :tON

Teat No. Temperature of Pulp Amount ofOleio Aoid Weight of Conoentrate

Colleoted

1
-- ......
190 c.
,
267
-
10 .dr..?.£.~ gr~

2A 300 o. 7 droE8 278 ~ram

2 45 0 c. 7 dr-ops .-.
338 gram
i

Note I 1 drop of 01e10 aoid • 11.5 mg. approx. - varies with room temperature

Variations ~.E!! 2!. Pulp

A series of tests was also made to determine the effeot of varying the
pH of the pulp. The same amount of sodium silioate was used in eaoh test, and
the pH was controlled by adding sodium oarbonate or sulfuric aoid. With no
modifying reagent, the pH v~s, 7.9 and fluorite was readily floated. _By add-
ing suooessive amounts of sodium oarbonate, no appreoiable ohange in results
could be noted up to a pH of 9.5. Sodium oarbonate disperses the slimes,
however, and approximately 1 lb. per ton was added to all following tests for
this reason.
One test was run at a pH Qf 7.2 (1.8 lb. of H2S04 per ton) in whioh the
mineral was readily floated. USing 4 lbs. of sulfurio aoid per ton of ore
lowered the pH to 5.0, and no minoral could be colleotod under theso oonditions.
Effeot of Sodium Silioate
Sinoe the bulk of tho matorial to be rejeoted in the tailing is silioa,
the effect of adding inoreasing amounts of sodium silioate l1aS tested. No
approoiablo dooroase in the silioa oontent of tho conoontrate was noted in
the tests in whioh a large exooss was used. Satisfactory results were ob-
tainod, using approximately 0.5 lbs. per ton of are in tho rougher circuit.
It was also found desirable to add small amounts to the oleaner and reo leaner
oirouit.
Grindin~

If tho silioa oontent of the conoontrato is to be kept below 1 per cent

Si0 21 al~st perfoot liboration of the particlos must be acoomplished. With
this in ndnd, it oan be seon that propor grinding is tho most imb'ortant faotor
in tho problem. Sinco the sample contains only a vcrysmall amount of caloium
oarbon~te ganguo and a lnrge amount of silioa, onoe tho minorals are froe,
their separation oan be rea.dily a.ooomplishod by flotation.
For most of the'tests, the grinding was done in 2000-gram batches in the
ball mill, and in order to produoe a flotation hoad sample in whiohtho ooarse
partioles were liberatod, a largo amount of ovor-grinding was done on the fine
material. Tho grindinE time was variod botwoen tests; the final sories was
made from a batoh whioh was' 0.5% plus 65 mosh and 80.5% minus 200 mesh. The
large amount of slimos did not appear to low~r tho grado of the oonoentrate,

3
 as might be expected. In two tests, desliming before flotation was tried with
no improvement over those in whioh the ball mill prod~ct was fed direotly to
the flotation machine.
In order to more nearly approaoh a classified feed and to establish the
grind required, three groups of tests were made~ in which the head samples
were stage ground to the desired size. These were made so that all partioles
passed through 65 mesh, 100 mesh, and 200 mesh, respeotively. For eaoh series,
the desired undersize was soreened out before any grinding was done_ The
oversize was ground in the ball mill for a short time, after whioh the under-
size was again removed and the oversize vms returned for another grinding
period. This was repeated until all the material passed through the desired
soreen. Aoid grade spar was made from both the minus 100 mash and the minus
200 mesh produots.

Plotting the peroent Si02 in the ooncentrate against the CaF2 reoovery
in the oonoentrate (Fig. I) shows that the rosults are almost the same for
the minus 100 mesh feed as for the minus 200 mesh. These plots indioate that
a reoovery of approximately 63 per oent of the CaF2 oan be expeoted in a con-
centrate assaying 1 per oont Si02- In praotioe, the return of middling products
to the circuit should mntorinlly improve this.

FIGURE I.
Compar~ 2.£ Flotati.2,!!. Rosult!!. ~
---- ---
~nus

,----------~--,r_
-.--

I
...
----- _
100 Mesh and Minus 200 Mesh Products
.............. ---- ........-.-.. ........-........................
-.-.-.-.--.-------~----.~----.-.,._.-~
:

3.
~
Cd
~
I
rt------t------+----+-.-.
d
Q)
0
5:l
0
t.)
2. ·--·-+-----+------+--I
d
°M
C\l
0
ori
CI)

1. -
e •

50
---'---'
so
----------------
70 eo
---:..----,
.

%Recovery CaF2 in Conoentrate

 In all t eats made on the 65 mesh pr oduot, muoh more m1neral was floated
than with the same reagents on the finer material. This gave high reooveries
on the fluorite, but in all oases, the silioa oontent was above the limit for
acid grade spar.
A oomparison of the various grinds is given in the f~llowing table:
TABLE 111.- SIZING ANAL$IS OF BALL MILL PRODUCTS

Size, Mesh
Grind %
% % % %
+65 65/100 100/150 150/200 -200

Batoh grind (20 minutes) 0.5 2.9 4.7 11.4 80.5

-65 mesh stage grind
(4 per iods of 3 minutes)
-100 mash stage grind
- - 16.9 15.9· 16.9 50.3

(6 periods of 3 minutes)
-200 mash stage grind
-- - - 11.9 21.8 66.3

3 3-minute periOdS~
3 4-minute periods
2 6-minute periods
-- -- -- -- 100.0
1 8-minute period

SUl~Y

The following conclusions can be drawn from these tests:

1) Aoid grade spar oan be made from minus 100 mesh material, provided
too high a reoovory is not required for ooonomioal oporation.
2) Extremely fino grinding docs not materially improve the metallur-
gioal results.

3) Heating tho flotation pulp to approximately 300 C. (8Go F~) is

desirablo.

4) Fluorite will not float in an acid pulp. A pH range from 8.0 to

8.5 gives very satisfaotory results.

5) Desliming before flotation does not improv~ the grade of the co~n­
trate.

6) Cloaning and recleaning the conoontrato improves the grado, but

oleaning a third time does bot help. The addition of small amounts
of sodium silicate and sodium oarbonato to tho cleaner oircuits
appears to be desirable.

5
 7) It should also be noted that more'diffioulty may be expeoted in
making a. fatisfaotory produot from any material oontaining barite.
Fluorite and barite are both readily floated with oleic aoid, whereas
silica can be quite ea.sily depressed.

Test No. 18
- --
FLUORITE FLOTATION TEST

November 24, 1942

Ore • l/4 of 2000 gram (ground for 20 minutes in ball mill)

Rea:gents:

Na2C03 = 0.25 gram

Sodium Silioa.te • 0.14 gram (12 drops )
Oleio aoid = 0.09 gram (8 drops)
Tempera.ture of'Pulp = 300 C.
The concentrate was cleaned and recleaned, using 0.1 gram of sodium sili-
cate for oleaning and 0.05 gram for Irecleaning.

6
, .
 -----' .... -
FLUORITE FLOTATION TEST
\

January 13, 1943

Test No. 26

Ore .. 1/4 of 2000 gram (stage ground to -200 mesh)

Reagents:

Na2C03 • 0.25 gra~

Sodium Si1ioate a 0.17 gram (15 drops)

01eio, Aoid • 0.09 gram (8 drop~)

Temperature of Pulp a 300 , C.

The oonoentrate VIas oleaned and reoleaned, using 0.1 gram of sodium sili-
oate for oleaning and 0.05 gram for reo leaning.

-. - -
% %Distribution of
1 Distribution % Distribution
0

Produot Weight Weight CaC0 3 CaC0 3 8i0 2 8i02 CaF2 CaF 2

Conoentrate
-
(26-1 ) 218 46.3 0.40 9.9% 0.88 1.95% 98.3 '60.5%
-
-
Rolnr. Tail
(26-3 ) 33 7.0 1.07 4.CJ1fo 3.51 1.15% 94.8 8.8%
C1nr. Tail
(26-2 ) 40 8.5 2.34 10.7% 12.4 5.~ 83.3 9.4% '
--
~~'4%
Tailing
(26-4 ) 180 38.2 50.5 91.9% 42.0 21.3%
Composite 471 100.0 1.86 10O.cP/o 21.0 100. OJ' 75.1 100. OJ'
I
-

7
 BIBLIOGRAPHY

(1) Davia, H. W., and Trought, M. E.1 Fluorspar; 1tlnera1s Yearbook, Review
of 1940, U. S. Bureau of Mines, pp. 1295 .. 131l (1941)
(2) Engineering and 1aning Journal, Vol. 144, No.1, P. 41, January 1943.
(3) Anderson, A. L.,: The antimony and fluorspar deposits near Meyers
Cove, Lemhi County, Idaho, Idaho Bureau of lanes and Geology
Pamphlet ~o. 62, (1943)