AN INVESYIGATSON AND CQMPAMSON
02" VARIOUS FECHNIQUES Q? fiiSAGGRiGATWN
A3 A?'§?LEE§E TC} SHALES

flwests £0? {“510 Degree 0? M. 5.
WCBEGAN SM?" Ufi‘é’i’fig‘il‘i’

William Fay Bradford
1958

 

THESIS

LIBRARY

Michigan Scam
University

 

AN INVESTIGATION AND COMPARISON
OF VARIOUS TECHNIQUES OF DISAGGREGATION
AS APPLIED TO SHALES

by
WILLIAM FAY mADFORD

Submitted to the College of Science and Arts of Michigan
State University of Agriculture and Applied Science
in partial fulfillment of the requirements
for the degree of

MASTER OF SCIENCE

Department of Ghology

1958

ACKNOWLEDGEMENTS

The author wishes to express his sincere appreciation to
Dr. B. T. Sandefur for his direction and suggestions which
aided greatly in the completion of this project.

He also wishes to thank Dr. H. B. Stonehouse and Dr.
C. E. Prouty of the Geology Department of Michigan State
University for their helpful suggestions pertaining to this
problem, and Dr. M. Breazeale of the Physics Department of
Michigan State University who made the use of the ultrasonic
vibrator possible.

The writer is deeply indebted to his wife Meriel, who
was responsible for the typing of this manuscript and who

gave much encouragement during the entire project.

11

AN INVESTIGATION AND COMPARISON
OF VARIOUS TECHNIQUES OF DISAGGREGATION
AS APPLIED TO SHALES

WILLIAM FAY BRADFORD

ABSTRACT

The purpose of this project was to employ a number of
disaggregation techniques on shales to determine which
techniques produced the best results.

The disaggregation methods employed in this research
were both physical and chemical. The physical included
ultraSOnic vibration, mortar and pestle, and oak board. The
chemical included potassium hydroxide and perchloric acid.

.Eight rock samples were selected; they included six
shales, one sandstone and one siltstone. These samples were
treated by the various disaggregation techniques and then
pipette analyses were run on each sample. The results of
the analyses were compared to determine which methods were
most effective.

The results of this research indicate that for the most

successful disaggregation of a shale, the ultrasonic vibration

111

method should be employed. However, the perchloric acid
method produced the best results on the coarser-grained

siltstone and sandstone.

iv

CONTENTS

INTRODUCTION . . . . . . .
Purpose ........ . . . .
Methods and Scope . .
Sample Selection . . .

PHYSICAL METHODS . . . . .

Introduction . . . . . .

Ultrasonic Vibration Method

Equipment . . . . . .
Sample Preparation . .
Disaggregation . . . .
Pipette Analysis .

Data Analysis . . . .
Data Interpretation .

Mortar and Pestle Method

Equipment . . . . . .
Disaggregation . . . .
Pipette Analysis . . .
Data Analysis . . .
Data Interpretation

Oak Board Method . .‘. .

Equipment . . . . . .
Disaggregation . . . .
Pipette Analysis . . .
Data Analysis . . . .
Data Interpretation

CHEMICAL METHODS . . .

Introduction . . . . . .

Potassium Hydroxide Method

Sample Preparation . .
Disaggregation . . .
Pipette Analysis . . .
Data Analysis . . . .
Data Interpretation .

"U
A

\nCDOvPIfla u: \0 x» so +4 +4 l4

Perchloric Acid Method
Sample Preparation
Disaggregation . . .
Pipette Analysis . .
Data Analysis . .
Data Interpretation

CONCLUSIONS . . . . . .
RECOMMENDATIONS . . .

REFERENCES . . . . . .

v1

TABLE
I.

II.
III.

IV.

VI.

VII.

VIII.

IX.

XIII.
XIV.

XVI.
XVII.
XVIII.

ILLUSTRATIONS

Rock Samples . . . . . . .

UITRASONIC VIBRATION METHOD

Sample Treatment . . .

Weight and Percentage of Sample larger
than 0.0625 mm ,

Size Analysis

Percentage by Weight .

Cumulative Percentage

MORTAR AND PESTLE METHOD

Sample C

OAK BLOCK METHOD

Sample C .

POTASSIUM HYDROXIDE METHOD

Weight and Percentage of Sample larger
than 0.0625 mm

Uncorrected weight in Grams

Corrected weight in Grams . , . .
Corrected weight in Grams times 50 . ,
Percentage . . . . . . . . . . . . . .
Cumulative Percentage . . . . . . . .

PERCHLORIC ACID METHOD

Weight and Percentage of Sample larger
than 0.0625 mm o o o o o e e c o o o e

Uncorrected Height in Grams . . . . .

Corrected weight in Grams ,

Corrected Weight in Grams times 50 .

vii

Page

12
16

21

2h

27
29
30
31

33
3h

35
37
38
39

TABLE
XIX.
XX.

XXI. Percentage of Samples larger than

Percentage

Cumulative Percentage

Cumulative
Cumulative
Cumulative
Cumulative
Cumulative
Cumulative
Cumulative

Cumulative

Curves
Curves
Curves
Curves
Curves
Curves
Curves

Curves

for
for
for
for
for
for
for

for

Sample
Sample
Sample
Sample
Sample
Sample
Sample

Sample

viii

EQ’UWUOEIb

Page
#1
42
H6

1&7
48
49
50
51
52
53
5:.

AN'INVESTIGATION AND COMPARISON
OF VARIOUS TECHNIQUES OF DISAGGREOATION
AS APPLIED TO SHALES

INTRODUCTION

Purpgse

The purpose of this research was to employ various dis-
aggregation methods on a number of shales and analyze the
results to determine which method of disaggregation produced

the best results.

Methgds agd Scope

The methods used in this research were both physical
and chemical. The physical were ultrasonic vibration,
mortar and pestle, and oak block. The chemical means
utilized potassium hydroxide and perchloric acid.

The scope of the research was to disaggregate the
samples, run a phpette analysis, interpret the results, and

determine which method gave the best results.

ngple Selectigg

Eight rocks were selected; they included six shales,
one sandstone, and one siltstone (Table I).

1

Sample

EQWFJUOW

TABLE I
ROCK SAMPLES

Egg;
Marshall sandstone
glazed argillaceous shale
bituminous shale
Saginaw shale
petroliferous shale
siltstone
carbonaceous shale

Antrim shale

urce
Grindstone City, Michigan
Cohoes, New York
Leroy, New York
Grand Ledge, Michigan
Fossil, Wyoming
Mexico.
Moscow, New York

Charlevoix County, Michigan

PHYSICAL METHODS

Igtrgdgctigg

Because of the lack of information about the ultrasonic
vibrator, it was decided to explore the use of this machine
extensively to determine if it would be successful in this
application. It was not decided to add the mortar and
pestle method and the oak block method until after the
chemical methods had been started. Because of the lack of
sample material after starting the chemical methods, the
mortar and pestle method and the oak block method could only
be run on one rock type. However, the sample that was used
in these two methods was one of the toughest of the samples
and it was felt that if disaggregation was successful on

this sample, it would also be successful on other shales.

Ultrasonic Vibrgtigg

Eguipgggt

The ultrasonic vibration machine had a maximum frequency
of 300 kc, with an oscillator plate power output of 300 watts.
The power supply was full wave, producing 1500 volts at full
power.. The vibrations were produced by a disc-shaped quartz
crystal transducer about four inches in diameter and about

one-half inch thick.

The transducer was located inside a heavy lucite cylinder.
The cylinder was filled with oil which transmitted the
vibrations produced by the quartz crystal transducer to the
samples. Various other transducers are obtainable which
would increase the effectiveness of the treatment, however
none of them were available. Because of the power loss due
to the shape of the transducer, it was decided to use one

gram samples in this machine.

Sample Preparatigg

Because of the lack of knowledge and information about
this machine, three samples of each of the eight rocks were
subjected to a treatment of five minutes, ten minutes, and
fifteen minutes respectively (Table II). The rocks were
crushed with a hammer to a maximum diameter of approximately I
one—sixteenth of an inch and three samples of 1.000 gram
each were taken from each of the eight pulverized rocks.
The samples were placed in water in a small glass test tube

and then treated.

Disaggregatiog

During the treatment of the samples the machine was run
at full power for five minute periods whenever possible.
The glass test tube containing the pulverized sample was
suspended in'the oil during the treatment. At times the

machine became so hot the water in the test tube boiled.

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machine to cool. On one occasion a fuse burned out. The'
addition of an air cooling unit and a strong fan helped
prevent overheating so that most of the samples could be
treated for the full five minute periods. This process took
'longer than the prescribed time because the machine had to
cool between treatments. After the air cooling unit was
added the average timing was to treat the sample for five

minutes and then allow the machine to cool for ten minutes.

Pipptte Applysip

After all the samples were vibrated, each sample was
wet sieved through a 230 mesh sieve to separate the sand
from the silt and clay particles. During the sieving many
of the samples had aggregates about one-sixteenth of an inch
in diameter. In most of the samples these aggregates could
be crushed by attrition between the fingers. However, in
some samples they could not be separated. The washing was
continued untilgall of the clay and silt particles passed
through the sieve. The amount of sample larger than the
230 mesh sieve was dried, weighed, and recorded (Table III).

Due to the small amount of sample used, standard
pipette analysis procedures could not be employed. That
part of the samples smaller than the 230 mesh sieve was
washed into a 600 m1 beaker and enough distilled water was
added to make the total height 10 cm. The beaker was

TABLE III
UDTRASONIC VIBRATION METHOD

WEIGHT AND PERCENTAGE or SAMPLE
LARGER THAN c.0625 MILLIMETERS

Weight of Sample

Larger than Percentage of
ngple 9.0625 mm Tpta; Sapple
A-1 .hh9 nu.9
A-2 .u92 49.2
A-3 .5h6 54.6
3.1 .733 73.3
3-3 0749 7409
0.1 .231 23.1
C-2 .146 - 10.6
0-3 .041 4.1
D—l .008 0.8
D-2 .000 0.0
D-3 .032 3.2
E-l .046 4.6
E-3 .017 .l.7
F-l .697 69 O7
F-3 .689 68.9
0-1 .468 #6.8
0.2 .471 “7.1
0-3 .399 39.9
H-l .201 20.1
H-2 .098 9.8
III-3 .103 1003

agitated and then allowed to settle for the standard periods
of time according to Stokes‘ law (Krumbein and Pettijohn,
1938). At the end of the designated periods of time the
liquid was decanted off, leaving the sediment which had
settled. This sediment was washed into another beaker,
dried, weighed, and recorded. Enough distilled water to
make a total height of 10 cm was added and the process was
repeated for each of the times specified in Stokes' Law
(Table IV).

We

Table II, which shows the flow sheet for the sample
treatment is self-explanatory, except to note that the
fluctuation of milliamperes could not be controlled by the
author. The milliamperes increased as the temperature of
the machine increased.

‘In Table III, the percentage of sample larger than 230
mesh in diameter was calculated directly from the weight of
the material because the original size of each of the
samples was 1.000 gram.

Table IV lists the weight of each portion of each
sample which settled according to their diameter in
millimeters. The depth of settling was 10 centimeters in
all cases.

Table V lists the percentage by weight of each portion

of each sample according to the diameter in millimeters.

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TABLE V

ULTRASONIC VIBRATION METHOD

PIPETTE ANALXSIS OF MATERIAL TREATED

PERCENTAGE BY WEIGHT

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TABLE V (Continued)

ULTRASONIC VIBRATION METHOD

PIPETTE ANALYSIS OF MATERIAL TREATED

PERCENTAGE BY WEIGHT

6

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TABLE V (Continued)

ULTRASONIC VIBRATION METHOD

PIPETTE ANALXSIS OF MATERIAL TREATED

PERCENTAGE BY HEIGHT

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15

The percentage was calculated by subtracting the weight of
the material in the sample larger than 0.0625 mm from the
original sample of 1.000 gram size. This value was used to
calculate all of the percentages for the certain sample.
This results in the value of a certain size representing the
percentage of material of this size in the total weight of
all the material which is less than 0.0625 mm in diameter.
In short, the percentage value represents the percent of
material in the silt and clay sizes only.

The cumulative percentage for each sample was obtained
by adding each of the percentages for each sample to the
percentages above it (Table VI).

Data Interpretation

In examining the portion of the sample larger than
0.0625 mm (Table III), it is evident that the disaggregation
method was successful on some of the samples. Sample C, the
bituminous shale, shows a definite decrease in the amount of
sand particles which varies indirectly with the length of
treatment. Sample D, the Saginaw shale, indicates that most,
if not all, of the silt and clay particles have been sepa-
rated from the sand particles. The results obtained by
treating sample E, the petroliferous shale, indicates that
most, if not all, of the silt and clay particles have been
separated from the sand particles. The results of sample H,
the Antrim shale, indicates that the majority of the silt

TABLE VI

ULTRASONIC VIBRATION METHOD

PIPETTE ANALYSIS OF MATERIAL TREATED-

CUMULATIVE PERCENTAGES

21
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TABLE VI (Continued)

ULTRASONIC VIBRATION METHOD

PIPETTE ANALYSIS OF MATERIAL TREATED

CUMULATIVE PERCENTAGES

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N

TABLE VI (Continued)

UUTRASONIC VIBRATION METHOD

PIPETTE ANALYSIS OF MATERIAL TREATED

CUMULATIVE PERCENTAGES

1mm

2:1

Nl
I
:1:

;1

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19

and clay particles have been separated after 10 minutes of
treatment. What is indicated by the trend in sample A, the
Marshall sandstone, is not known. Sample B, the glazed
argillaceous shale, and sample F, the siltstone, do not show
any definite trend. Lack of any definite trend indicates
that disaggregation has not begun to any large degree.
Sample G, the carbonaceous shale, shows that disaggregation
may have begun after the treatment exceeded 10 minutes.

The wide variations in total percentage in Tables IV
and V'were probably due to unavoidable errors in the
unorthodox technique employed for the pipette analysis.
However, even though the technique employed was unorthodox
due to the extremely small size of the sample and the lack
of available information on executing pipette analyses on
such small samples, the author feels that the data obtained
may be at least partially indicative of the true results
obtained with this disaggregation method.

Mortar and Pestle Methgd

 

Equipment

The equipment used in this method consisted of a large

steel mortar and pestle.

Disaggregatigg

The rock used in this method was sample C, the bituminous

20

shale from Leroy, New Ybrk. The rock was pulverized in the

mortar and then a sample of 25.000 grams was taken.

Pipette Analysis

The sample was both dry sieved and wet sieved through
the 230 sieve to separate the sand particles from the silt
and clay particles. The wet sieving was continued until all
the silt and clay particles were washed through the sieve.
The part of the sample which did not pass through the sieve
was dried, weighed, and recorded (Table VII). That portion
of the sample which passed through the sieve was washed into
a 1000 m1 graduated cylinder. To minimize coagulation 0.670
grams of sodium oxalate was added to the solution and enough
water was added to make exactly 1000 ml. The procedure
determined by Stokes' Law for a pipette analysis was followed.

The suspension was agitated thoroughly, and after the-
designated time period a 20 cc pipette was inserted to the
designated depth and exactly 20 cc of the solution was with-
drawn. This was dried in a beaker of predetermined weight.
The weight of the material in the beaker was recorded.

This weight represents one-fiftieth of the amount of material
of a certain diameter present in the suspension. This
process was repeated for each of the times designated by

Stokes' Law.

21

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22
Data Analysis

The data for this method is shown on Table VII. The
uncorrected weight in grams was obtained by weighing the
beakers of predetermined weight which contained the various
sizes of sample. In the pipette analysis 0.670 grams of
sodium oxalate was added to the graduated cylinder to
minimize coagulation. Because of this addition, the weights
had to be corrected. This was done by subtracting 0.013
grams from each of the uncorrected weights. The corrected
weights were each multiplied by 50 because the 20 m1 sample
taken represented one-fiftieth of the total suspended
material. The percentages represent the percent of silt and
clay only. The cumulative percentages were obtained by
adding each of the percentages to those above it in the
table. I

Data Interpretatign

The percentage of the sample larger than 0.0625 mm is
still quite large, which indicates that disaggregation by

this method has not been very successful.

Oak Bgard Methgd

Equipment

The equipment used in this method consisted of a hand

Jaw crusher and two oak boards. The machine was made of two

23

grooved plates, one solidly fastened and the other attached
to an eccentric camshaft. Turning the crank produced a
back and forth movement of the plate attached to the cam-
shaft. There was very little up and down movement of the
plate. It wassfelt that the use of this machine in crushing
the rock would result in very little attrition. The oak
boards were two pieces four inches wide, twelve inches long,
and about three-quarters of an inch thick. The two largest.

surfaces on each board were sanded until they were smooth.

Disgggregatipn

The rock used in this method was sample C, the bituminous
shale from Leroy, New York. The rock was first crushed in
the Jaw crusher. After crushing with this machine, the
largest remaining particles were thin, platy-shaped, and
approximately one-quarter of an inch long and one-eighth of
an inch.wide. The rock was then placed between the large
flat surfaces of the oak boards, pressure was applied and
as little rotary motion as possible was used to further dis-
aggregate the rock. A 16.000 gram sample was then weighed

out.

Pipette Analysis

The procedure followed here was the same as that of the

pipette analysis of the mortar and pestle method (Table VIII).

20

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25
Data Analysis

The procedure followed was the same as the procedure

in the data analysis of the mortar and pestle method
(Page 19).

Data Interpretation

The percentage of sample larger than 0.0625 mm is 20.0
percent of the original sample weight, which indicates that

disaggregation by this method has not been very successful.

CHEMICAL METHODS

Introduction

For the chemical methods of disaggregation it was
decided to use potassium hydroxide and perchloric acid, two
methods which have been utilized before (Ross, 1957 and
Kropschot, 1953). It was felt that these previously used
methods would provide the necessary basis for a sound com-

parison of disaggregation techniques.

Pgtassium Hydrgxide Method

 

Sample Preparation

All samples to be chemically disaggregated were prepared
by crushing them down to a maximum diameter of approximately
one-sixteenth of an inch with a hammer. The weight of the
sample used depended on the amount of rock available (Table
IX). The amount of crushed sample available was divided ap-
proximately in half so as to insure having enough left to use
in the perchloric acid method.

The potassium hydroxide solution was prepared by using
a ratio of ten grams of dry potassium hydroxide and ten ml
of water to each gram of sample (Ross, 1957). The solution

was then placed in a 600 ml beaker and the sample was added

26

27

TABLE IX
POTASSIUM HYDROXIDE METHOD

wsrcar AND PERCENTAGE or SAMPLE
LARGER THAN 0.0625 mm

 

 

Original Weight of Sample Ercentage

Sample Weight larger than 0.0625 mm Larger than

Sample 113, grams in gramsa 0.0625 mm
A 30.000 16.960 56.5
3‘ 25.000 7. 30 29.3
C 30.000 13. 79 (+5.0
0 25.000 10.996 00.0
E 30.000 1.073 (4.9
F 30.000 16.140 53.8
0- 20.000 7.065 35.3
H 20.000 13.535 67.8

28

to the solution. In some cases there was a mild effervescence

when the sample was added.

Dispggregatipp

The disaggregation method consisted of heating the
beaker and contents slowly until most of the liquid was
driven off, then adding more water and evaporating that.
water was added to each beaker several times. This process
took about 2h hours of slow heating. The beakers containing
the sample were weighed both before and after the disag-
gregation to determine if a part of the beaker had been
taken into solution. Nb appreciable difference in weight

was noted.

Pipptte Analysis

The procedure followed was the same as that used in the
pipette analysis of the mortar and pestle method, except
that the sample was wet sieved only (Table X).

W

The procedure followed was the same as the procedure
described in the data analysis of the mortar and pestle
method.

29

omo.
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30

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31

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32

Data Inter ret t o

Upon examining the percentage larger than 0.0625 mm
as shown in Table IX, it is evident that disaggregation was
much more successful on sample B, the petroliferous shale,
than any of the other samples. The other samples still have
a high percentage of sand particles which indicates that
disaggregation was not complete when using this method.

The variation in percentages in Tables XIII and XIV

is little; the largest error is one percent.

Perchipric Acid Metgpd

Sapple Preppratipn

All of the samples used in this process were prepared
by crushing them with a hammer to a maximum diameter of ap-
proximately one-sixteenth of an inch. The weight of the
sample used varied, depending on the amount of rock left
after dividing the sample in half for use in the potassium
hydroxide treatment (Table XV).

The solution used in this method consisted of one ml of
perchloric acid, one ml of sulfuric acid, and 10 ml of nitric
acid to each gram of shale (Kropschot, 1953). This ap-
proximate ratio must be maintained to prevent the precipi-
tation of calcium sulphate. This solution was placed in a

600 ml beaker and the sample was added to the solution.

TABLE XIII

POTASSIUM HYDROXIDE METHOD

PERCENTAGE

Dia-

Height

meter

Time
Hr, Min, SecI

in
Centi-

in
Milli-

meters

ml

6|

ml

MI

QI

CH

ml

A

meters

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0

TABLE XV

PERCHLORIC ACID METHOD

WEIGHT AND PERCENTAGE OF SAMPLE
IARGER THAN 0.0625 mm

Original
Sample Weight

ip grgmp

30.000
30.000
30.000
24.000
25.000
25.000
20.000
18.000

Weight of Sample
Larger than 0.0625 mm

111 grams a

 

5.965
2.h07
1.211
1.362
5.670
5.980
0.006
1.723

Percentage
Larger than

.219éaissa_

19-9
8.0

a
5
22
23
2
9

muwflfl O

35

36
D s re t

The disaggregation method consisted of heating the
beaker and contents slowly. The perchloric acid was given
off as a white vapor and the nitric acid was given off as
nitrogen dioxide. It was essential to use a hood with a
‘strong exhaust system to draw off the fumes. When there was
very little liquid remaining, water was added to the beaker
and allowed to evaporate. Water was added to each beaker
several times. This process took about 72 hours of slow

heating to complete.

Pipette Analysis

The procedure followed was the same as the procedure
used in the pipette analysis following disaggregation by the
mortar and pestle method, except that the sample was wet

sieved only (Table XVI).

Data Analysis

The procedure followed was the same as that described

in the data analysis of the mortar and pestle method.

Data Interpretation

Upon examining the percentage larger than 0.0625 mm in
Table XV, it is evident that disaggregation was not very

successful on sample E, the petroliferous shale. Sample A,

37

3N0”

cmc. ch mac.
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39

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no

the Marshall sandstone, and sample F, the siltstone, still
have a high percentage of material larger than 0.0625 mm, but
since these two rocks are coarser grained, disaggregation
may be complete. All of the remainder of the samples have a
small percentage of sand particles, which indicates that dis-
aggregation has been successful.

The variation in percentages as shown in Tables XIX
and XX is little with the exception of sample G-where the

'error is slightly over five percent.

PERCENTAGE

TABLE XIX

PERCHLORIC ACID METHOD

Height
in
Centi-

meter
in
Milli-

Dia~

ml

6|

kd

MI

9|

0|

m!

:5.

52"Mig. SgcI

meters

——h

meters

000 00...... O
mmgommdmmszNH m

omNmNNMJQMHHHQN m
HH 4®

ommmmmmmmmmommwm

.0000.
&NNOHHNMNNNMMNNM
HHHHHHH g

NCV:ADSWDOAOrdF“OWD ax

F1“). 0 e e o e o o o o .
HMNNH¢3NWMMHHH o
HHHHH o

.ooooeoeeoo
«wwounvnifififiFfithfi
HH

0\

mmmommwnmomm4a
m

1h.8
lh.1

.g...eoooeeOOo
mwommWW-S’NNHHNQ

mmOQOHMNwdedr
H H m

12.1
22.8

NHMHBmHmNaim

someone-o 0

CD cmmnxo manna N N 8
H

(I)

H
H

12.5
10.9
10.7

“HWHNHWQWN-fiwwéfilw

mmammmmmmmmmmnma

®\O\ON:T

mmmm:
HHMaMHH m HHNm
Hm m 33 N470)
HNQ‘ \ONVN
mgflmm
ooocoooooooommm

NNHHHHHHHHHH

wmwwmm
mNNHmommmnmmmw:
Nzfiwmflmmmwfifiooo
wgmmflaooooooooo
ooooooooooooooo
.geeooeooeooooe

TABLE XX

PERCHLORIC ACID METHOD

CUMULATIVE PERCENTAGE

afl

0|

fid

h"

OI

Ln

ml

A

Time
fig; M49. 809.

Height
in

meters

Centi-

meter
in

Milli-

meters

D13-

0 mnmvuao: Nuxxo caooxom

. O O O O C O O O O O I C O O
‘00 MO ONQ) monnmmdxooo O\
H m: WWW cab-0000 O\O\O\O\O\

Od’H-fiOQNmmHJ-fifimm

0.000.000.0000.
NJBBQCNWCDHC'VOQNW
HNC'WWNQCDCDQQQQSS

\Ofi-mmaomemNzoml—l
0.000000000000-
NQNNMOO\\OOWO\NWK\H

H©®03033HB®HNMM

000.000.00.000.
HQNOHHanI—ljwumo
memmbhmoommcxmmg

\

m N30” MHWO\O\NK\C\
e o o o
N

O\
.0
awn
HN

o o e e e e o e
:MHBNme-if‘OF-Q
:MWNNCDK)C)O\O\O\O\O\

HON®®33WON®3®O

. O O C O O O C . O O . O C .
Nd'm-fid'mexmmH-imbm
HMWWWBBCDQmO‘mCha

\n-d‘NO‘.l—‘NV\\O\'\HN®OO‘
oooooooooeooo

NMWWJHWHCDNWO

HCQMJW\O\OI\I\®CDO\O\

5
97.
100.3

“\OHNWWNCod'womNWCO
Cece-0000000000
@03NO0WHNNwmm-fl'm
HNm-znwmfiflwmefi

.0625
.ouuz
.0312
.0221
.0156
.0110
.0078
.0055
.0039
.00276
.00195
.00138
.00098
.00069
.00009~

CONCLUSIONS

For the purposes of drawing accurate conclusions from

the results, we shall consider complete disaggregation to

be composed of two parts, primary disaggregation and secon-
dary disaggregation. Primary disaggregation shall be
defined as separating the particles larger in diameter than
0.0625 mm (Table XXI). Secondary disaggregation shall be
defined as separating the particles smaller in diameter than
0.0625 mm (Refer to the cumulative curves of the samples).

The cumulative curves of sample A rock type show that
the perchloric acid method was much more successful in
primary disaggregation than any of the other methods. The
perchloric acid method was also most effective in secondary
disaggregation.

The cumulative curves of sample B show that the per-
chloric acid method was most successful in primary disag-
gregation, with the potassium hydroxide method second. The
potassium hydroxide method and the perchloric acid method
were about equally successful in secondary disaggregation.

The cumulative curves of sample 0 show that the per-
chloric acid method and the 15 minute vibration method were
equally successful in primary disaggregation. The 10
minute vibration method was most effective in secondary dis-

aggregation with the 15 minute vibration method second.

43

 

an

The perchloric acid method was sixth out of seven in
effectiveness.

The cumulative curves of sample D show that all three
vibration methods and the perchloric acid method were
successful in primary disaggregation. The vibration methods
were most successful in secondary disaggregation.

The cumulative curves of sample E show that the 15
minute vibration method was most successful in primary dis-
aggregation. The 5 and 10 minute vibration methods and the
potassium hydroxide method were about equally effective,
but less so than the 15 minute vibration method. The
vibration methods were the most successful in secondary dis-
aggregation with the potassium hydroxide method the least
effective.

The cumulative curves of sample F show that the
perchloric acid method was much more successful in primary
disaggregation than any of the other methods.. The three
vibration methods and the perchloric acid method were about
equally effective in secondary disaggregation.

The cumulative curves of sample G show that the per-
chloric acid method was much more successful in primary
disaggregation than any of the other methods. The three
vibration treatments were most successful in secondary dis-
aggregation with the perchloric acid method second.

An examination of the cumulative curves of sample H
shows the 10 and 15 minute vibration methods and the per-

chloric acid method to be about equally successful in primary

‘45

disaggregation. The cumulative curves show the potassium
hydroxide method as the most successful, with the vibration
methods second and the perchloric acid method last in secon-
dary disaggregation.

The ultrasonic vibration method was successful in
primary disaggregation in four of the shale samples. This
method was successful in secondary disaggregation in four of
the shale: and in the siltstone.

The mortar and pestle method and the oak board method
were not successful in either primary or secondary disag-
gregation.

The potassium hydroxide method was surprisingly un-
successful. It was successful in primary disaggregation in
only one shale sample and in secondary disaggregation in
only two shale samples.

The perchloric acid method was the most successful of
all the methods in primary disaggregation. It was successful
in primary disaggregation in five of the shale samples and
in both the sandstone and siltstone samples. This method
was successful in secondary disaggregation in two of the
shale samples and in both the sandstone and siltstone
samples.

On the basis of the above results, the following con-
clusions can be drawn:

1. If a sandstone or siltstone is to be disaggregated,
the perchloric acid method should be used.

2. If a shale is to be fully disaggregated, the ultra-
sonic vibration method should be used. However, if
only primary disaggregation is desirei,the perchloric
acid method is recommended.

TABLE XXI

PERCENTAGE OF SAMPLE
LARGER THAN 0.0625 MILLIMETERS

SAMPLE A

Marshall Sandstone, Michigan
1-1 M-9
A-2 “9.2
A-3 5h.6
Perchloric acid 19.9
Potassium Hydroxide 56.5

SAMPLE B
Glazed argillaceous shale,
Leroy, New York

B-l

B-2

B-3

Perchloric acid
Potassium Hydroxide

8 VVV
mtxiu
e e o e e

UOWQU

SAMPLE C ,
Bituminous shale,
Ieroy, New York

C-1

C-2

C-3 .
Perchloric acid
Potassium Hydroxide
Oak Board

Mortar and Pestle

HM

tvcnmjrthtu)
O
maoor-ono-o

NM?

SAMPLE D
' Saginaw shale, Michigan

D-l
Da2
D-3
Perchloric acid‘
Potassium Hydroxide h .

o e o
OVNOOJ

tang)
O

SAMPLE E

Petroliferous shale, Fossil, Wyo.

E—l

E—Z

E—B

Perchloric acid
Potassium Hydroxide

SAMPLE F
Siltstone, Mexico

F-l

F—2

F-3

Perchloric acid
Potassium Hydroxide

SAMPLE G
Carbonaceous shale,
Moscow, New York

Perchloric acid
Potassium Hydroxide

SAMPLE H

‘Antrim shale, Michigan

H-l

H~2

H-B

Perchloric acid
Potassium Hydroxide

\JRNChO‘Os
Uh.) CD\O\O
O
(IROWCD'Q

U31?

MNWVQ
o

WWWHQ

w

P4 to
avocamwo
O
cnoumcnpa

O\

A-3

A-l

A-Z

Potassium

4'7

CUMULATIVE CURVES FOR SAMPLE A

 
  

O
T.
2
.C
0 -l
L-
0
0..
q
to
.4
D
0.

’

 

IOO_.

Perchloric

 

I
o
9

48

CUMULATIVE CURVES FOR SAMPLE B

/
J

 

/

/
/Potcssuum

 

 

49

CUMULATIVE CURVES FOR SAMPLE C

mmooo.

 

 

low

 

I 00.

50

CUMULATIVE CURVES FOR SAMPLE D

E
3
'57!
W
E ..
m
I
O H
G
. 01
‘0
O
o.
. -
o

 

 

 

 

\
\ E
\ ‘0:
\\ .‘i’
\ m
\ E.
~55
.2 so
.5.
‘5
o H
:5
0.
4r
L_ I I I I I A? I g, I
8° 8 8 e N o

1N3083d

 

 

.22 Z. mmhmzda

 

 

51

 

CUMULATIVE CURVES FOR SAMPLE E

28.5ch

 

ON

0
<1-
.LNEIOHBd

8

 

Perchloric

Potassium

IOO F

 

52

CUMULATIVE CURVES FOR SAMPLE F

 

 

I | I
.0078
IA R I

 

I
.0625

 

 

53.

CUMULATIVE CURVES FOR SAMPLE G

 

.22 z. awhw2<5
mmmoo H .4 _ _ _ _ mrwwH .4 H _ .H IJ

 

 

.16
nuoiIIII

N16

 

£3328
0.3229.

ON

0
<r
lNEOHBd

O
(D

Om

 

00.

54

CUMULATIVE CURVES FOR SAMPLE H

 

.22 z. mm...m2<.o
maOO.
1% H

_ A 4 q

 

52320.”.

3.6.5.8;

 

ON

00

 

00.

RECOMMENDATIONS

As a result of this research, the author feels there

are several further investigations that would be interesting

and valuable. These are:

1.

3.

H

The use of the perchloric acid method for
primary disaggregation and then the use of
ultrasonic vibration for secondary disag—
gregation may prove to be more successful
than either of the methods by themselves.

-An investigation of more intensive treat-
ment with the ultrasonic vibrator.

A study of the application of the ultra-
sonic vibrator to other fields, such as
freeing fossils.

Possibly a longer treatment in the oak

block and the mortar and pestle method
would make these methods successful.

55

REFERENCES

Goodrich, D. L., (1957). “A Sedimentary Analysis of the
Lower Devonian Bois Blanc Formation in Michigan,“ Master's
Thesis, Michigan State University.

Grim, R. 3., (1953). Clay Mineralogy, McGraw-Hill Book
Company, Inc., New Yerk.

Kropschot, R. 3., (1953). 'A Quantitative Sedimentary
Analysis of the Mississippian Deposits in the Michigan
Basin,“ Master's Thesis, Michigan State University.

.

Krumbein, W. C., and Pettijohn, F. J., (1938). Mangal g;
Sedimentary Petrographz. Appleton-Century-Crofts, New
York.

Ross, Roy, Jr., (1957). “A Quantitative Sedimentary Analysis

of the Middle Devonian Traverse Group in the Michigan
Basin,‘ Master's Thesis, Michigan State University.

56

n 3'”:

we

I

{fl

 

‘L‘.~ 44.

 

MICHIGAN STATE UNIVERSITY LIBRAR

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