Note: Descriptions are shown in the official language in which they were submitted.
MUZZLER SNUG FOR OIL RECOVERY
BACKGROUND OF THE INVENTION
Field of the Invention
This invention relates to a muzzler slug suitable
for use in a muzzler drive for recovering oil
from subterranean reservoirs. More specifically,
it relates to a muzzler slug capable of recovering
oil from subterranean reservoirs containing sub-
terranean water having a very wide salt concentration
at a high oil recovery efficiency.
Description of the Prior Art
It is well known in the art that the so-called
"primary recovery methods, including pumping
methods, can recover only a portion of the
petroleum or crude oil (referred to as "oil"
hereinafter) from subterranean reservoirs and leave
substantial amounts of oil in the subterranean
reservoirs.
In order -to recover the remaining large
amounts of oil from the subterranean reservoirs,
so-called "secondary recovery" methods have been
proposed, wherein, for example, water or gas is
injected into the subterranean reservoirs from an
injection well at a pressure sufficient to
increase the flyability of oil, steam is
injected into subterranean reservoirs so as to effect
I
-- 2 --
the dispel cement of oil toward a E~oduction we l l, or oil
in subterranean reservoirs is partially burned to heat
the subterranean reservoirs so as to decrease the
viscosity of thy oil and increase the flyability of
the oil.
Furthermore, the so-called various 'Tertiary
recovery" methods, including a combination of secondary
recovery methods and Improved secondary recovery methods,
have been proposed, wherein surfactants or water-soluble
polymers are utilized. These methods æ e generally
called "enhanced oil recovery" (ERR methods.
Of the surfac~ant ERR methods, the recent "muzzler
drive" methods are to ye noted. According to these
method, a muzzler slug, that is, a clear micro-emulsion
derived from water and oil such as petroleum petroleum
distillates, or fuel oil, is injected under pressure
into the subterranean reservoirs for the recovery of oil
in the subterranean reservoirs. These ERR methods are
disclosed in, for example, So Patent Nos. 3506070,
3613786, 3740343, 3983940, 3990515, 4017405, and 4059154.
These prior arts disclose that various kinds of sun-
fact ants including anionic-, non ionic , and cationic-type
surfactants can be used alone or in any mixture thereof
in the formation of muzzler slugs. Examples of such
surfactants are petroleum sulfonates, alkylaryl sulfa-
notes, dialkyl sulfosuccinates, Al Kane sulfonates,
polyoxyethylene alkylether sulfates, alpha-olefin
sulfonate, polyoxye~hylene alkylether3, polyoxyethylene
I
alkylphenylethers, polyol fatty acid ester, alkyltri-
methyl ammonia salts, and dialkyldimethyl ammonium
salts.
The muzzler slugs should have the following kirk-
teristics to recover oil from subterranean reservoirs at
a high efficiency:
Sufficiently low m terfacial tensions between
oil and the micro-emulsions and between formation water
and the micro-emulsions; stability of the micro-emulsions
and the small ah age in the interracial tensions during
sweeping even when the salt concentration of the
formation water is changed; salinity tolerance of
the muzzler slugs at a wide salt concentration range,
since the salt concentration range of the formation
water extends widely from a low to high concentration;
and low cost availability of the muzzler slugs, since a
large amount of a muzzler slug is necessary to recover
oil from subterranean reservoirs.
SUMMARY OF TOE INVENTION
The object of the present invention is to provide,
for the recovery of oil, a muzzler slug having an
excellent oil-micro emulsion end formation water-micro-
-emulsion interracial tension decreasing capabilities
and an excellent salinity tolerance at a wide salt
concentration range and being capable of maintaining ye
stability of the micro-emulsions during sweeping in eye
subterranean reservoirs even when the salt concentration
of the formation water is changed.
_ 4 ~23~
A further object of the present invention is to
provide an oil recovery process using a muzzler slug.
Other objects and advantages of the present invent
lion will be apparent from the following description.
In accordance with one embodiment of the present
invention, there is provided a muzzler slug for use in
the recovery of oil, the slug consisting essentially of
a hydrocarbon, an aqueous medium, a surfactant, and a
cosurfactant having an alcoholic hydroxyl group, the
surfactant containing, as an essential component, an
internal olefin sulfonate having 10 to 26 carbon atoms
obtained by sulfonating internal olefins containing as a
main constituent vinylene-type monoolefin having the
general formula:
R - OH = OH - R'
wherein R and R' are independently straight- or
branched-chain saturated hydrocarbon radicals having 1
or more carbon atoms provided that the total carbon atom
numbers of R and R', is 8 to 24, followed by
neutralization.
In accordance with another embodiment of the
present invention, there is provided a process -For
producing oil from an oil-bearing subterranean reservoir
penetrated by wells which comprises the steps of:
(1) injecting into the reservoir through an
injection well a muzzler slug consisting essentially of
a hydrocarbon, an aqueous medium, a surfactant, and a
cosurfactant having an alcoholic hydroxyl group, the
surfactan-t containing, as an essential component, an
internal olefin sulfonate having 10 to 26 carbon atoms
obtained by sulfonating internal olefins containing as a
main constituent vinylene-type monoolefin hazing the
general formula:
R - OH = OH I'
I "'I
; $ I;
". "I ,.,
- pa - i23212~
wherein R and R' are independently straight- or
branched-chain saturated hydrocarbon radicals having l
or more carbon atoms provided that the total carbon atom
numbers of R and R', is 8 to 24, followed by
neutralization;
I injecting into the reservoir at least one
driving fluid; and
(3) recovering oil from the reservoir through a
production well.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
The muzzler slugs desirably used for the recovery
of oil are transparent or translucent micro-emulsions
containing about I to about 90% by weight of a
hydrocarbon, about 4% to about 95% by weight of an
aqueous medium, about 1% to about 30~ by weight of a
surfactant containing, as an essential constituent, an
internal olefin sulfonate having lo to 26 carbon atoms,
and about 0.1% to about 20% by weight of a cosurfactant.
The aqueous medium usable in the formation of the
muzzler slug of the present invention includes soft
water, water containing inorganic salts, and brine. For
example r rain water, river water, lake water, formation
water, oil stratum water, and seawater can be freely
used in the formation of the muzzler slug of the
present invention.
The muzzler slugs of the present invention contain
~r~3
I
I
-- 5 --
the internal olefin sulfonates having good salinity
tolerance and hard-water resistance as an essential
constituent of the surfactant. Therefore, brine having
a salt concentration of up to about 10% by weight can be
used in the formation of the muzzler slugs of the present
invention. Further, brine having a salt concentration
of up to about 15~ by weight can be used when other
surfactants or cosurfactants are used together with the
internal olefin sulfonate. Furthermore, the muzzler
slugs of the present invention have an excellent hard-
-water resistance. For example, brine usable in the
formation of the muzzler slugs of the present invention
can contain a relatively large amount of multivalent
metal ions, for example, about 5,000 Pam of a My ion
(i.e., about 2.6~ by weight of McCoy). Thus, waxer or
brine) usable in the formation of the muzzler slugs of
the resent invention can contain 0% to about lo by
weight, desirably about 0.5% to about 12% by weight and
more desirably about 1% to about 10~ by weight, of
inorganic salts Typical examples of the inorganic
salts contained Lo the water (or brine) are Nail, Clue,
Nazi , and K2S04. For instance, seawater contains
about OWE% by weight of inorganic salts including about
1,600 Pam, in terms of a My ion, of diva lent metal ions.
25 This salt concentration is within the desirable salt
concentration range of the present invention.
The internal olefin sulfonates Usable as an essential
sur~actant in the present invention are those obtained
AL 3
6 --
by sulfonating internal olefins containing as a main
constituent vinylene-type monoolefin having 10 to 26
carbon atoms, desirably 12 to 24 carbon atoms and having
a general formula:
R -- OH = OH - R'
wherein R and R' are independently straight- or branched-
chain saturated hydrocarbon radicals having 1 or more
carbon atoms provided that the total carbon atom numbers
of R and R' is 8 to 24, desirably 10 to 22, and optionally
10 containing about 33% by weight (about one third of the
olefins) or less of tri-substituted type monoolefins,
followed by neutralizing the sulfonated products with
appropriate bases and, then, optionally, hydrolyzing the
neutralized products. The internal olefin sup donates
thus prepared generally contain about 10~ to about 60~
by weight of alkenyl sulfonates having a double bond and
about 90~ to about 40~ by weight of hydroxyalkane sulfa-
notes and also contain about 80% by weight or more of
monosulfonates and about 20% by weigh or less of dip
sulfonates. It should be noted, however, that internal
olefin sulfonates having the compositions different from
the above-mentioned composition ratios can be prepared
by appropriately selecting the sulfonation conditions
and hydrolysis conditions. Generally speaking, the
increase in the carbon atom number of the internal ole~ln
tends to result in an increase in the composition ratio
of the alkenylsulfonate. On the other hand, the increase
in the mow ratio of the sulfonating agent to the internal
~32~
7 --
olefin during the sulfonation tends to result in an
increase in the composition ratio of the disulfonate.
The content of the disulfonate in the internal
olefin sulfonates usable in the present invention should
be about 20% by weight or less. A disulfon~te content
of more than 20~ by weight undesirably decreases the
interfaclal tension decreasing capability of the internal
olefin sulfonates and, therefore, decreases the oil
recovery efficiency of the muzzler slugs. Thus, a
small content of the disulfonate in the internal olefin
sulfonates increases the salinity tolerance and the
resistance against the change in the salt concentration
of the brine, without impairing the interracial tension
decreasing capability of the internal olefin sulfonates.
Accordingly, the content of the disulfonates in the
internal olefin sulfonates is desirably about 0.5% to
about 15~ by weight, more desirably about I to about
12~ by weight
The internal olefin sulfonates usable in the present
invention can be alkali metal salts, alkaline earth
metal salts, ammonium salts, and organic amine salts
thereof. The desirable counter cations are Nay K, go
Cay NH4 , and alkanolammonium.
Examples of internal olefin sulfonates usable in
the formation of the muzzler slugs of the present
invention are: internal olefin sulfonate having 12, 14,
16, 18, 20, 22, 24, 12-16, 13-14, 13-16, 14 I 18,
15-18, 16-18, 16-20, 17-20, 18-20, and 20-24 carbon
I
- 8
atoms. These sulfonates may be used alone or in any
mixture thereof.
As mentioned above, the muzzler slugs of the
present invention contain about 1% to about 30~ by weight
of the surfactant. However, the muzzler slugs desirably
contain about 3% to about 25~ by weight of the surfactant,
taking into consideration both low interracial tensions
and reasonable cost The amount of the higher internal
olefin sulfonates having 10 to 26 carbon atoms should be
lo at least 50% by weight, desirably 60~ by weight or more,
based on the total amount of the surfactants contained
in the muzzler slugs.
The hydrocarbons usable as an oil component in the
present invention include, for example, petroleum, pique-
fled petroleum gas, crude gasoline ~naphtha), kerosine,diesel oil, and fuel oil. The recovered petroleum it
desirably used due to its low cost and availability as
well as its composition, which is similar to that of the
oil contained in subterranean reservoirs. As mentioned
above, the muzzler slugs of the present invention can
contain about I to about 90% by weight of hydrocarbons.
The desirable concentration of hydrocarbons is within
the range of about 3% to about 40~ by weight whereby an
oil-in-water (O/W) type emulsion is formed, since the
25 use of a large amount of hydrocarbons is not economical.
The cosurfactants used in the formation of the
muzzler slugs of the present invention are an essential
constituent for forming micro-emulsions associated with
2t7
_ 9 _
the surfactants. The cosurfactants usable in the present
invention are those having an alcoholic hydroxyl group.
the desirable cosurfactants are alcohols having the
general formula:
S Rescission
wherein n is a number of from 0 to about 4 and R" is an
alkyd or alkenyl group having 4 to 8 carbon atoms when n
is zero and an alkyd or alkenyl group having 6 to lo
carbon atoms, a phenol group, or an alkylphenyl group
lo having 7 to 16 carbon atoms when n it not zero. The
aliphatic groups of R" may be straight chain or branched-
-chain groups.
Examples of such alcohols are buttonless, pentanols,
hexanols, 2-ethylhexanol or other octanols, polyoxy-
lo ethylene hexylethers (n = lo, polyoxyethylene decylethers(n = 2), polyoxyethylene tridecylethers (n = 4), polyoxy~
ethylene butylphenylethers on = 2), polyoxyethylene
nonylphenylethers (n = 3), and polyoxyethylene dodecyl-
phenylethers (n = 4).
As mentioned above, the muzzler slugs of the present
invention can contain about 0.1% to about I by weight of the cosurfactants. However, the desirable concern-
traction of the cosurfactants is within the range of
about 1% to about 15% by weight from the viewpoints of
the stability of the micro emulsions and the decreasing
capacity for the interracial tensions.
As mentioned above, the muzzler slugs of the present
invention contain internal olefin sulfonates having lo
Jo
-- 10
to 26 carbon atoms as an essential or major constituent
of the surfactants. However, other auxiliary surfactants
can alto key included, together with the internal olefln
sulfonates.
Examples of such auxiliary suxfactants are anionic
surfactants and non ionic surfactants such as petroleum
sulfonates, alkylbenzene sulfonates, polyoxye~hylene
alkylether sulfates, dialkyl sulfosuccinates, alpha-
-olefin sulfonates, paraffin gut ion ales, soaps, higher
10 alcohol ethoxylate~, alkylphenol ethoxylates, polyol
Patty acid esters, fatty acid alkylol asides, and pow-
oxyethylene fatty acid aside 5 .
The viscosity of the muzzler slugs of the present
invention can be suitably adjusted by selecting the kinds
and amounts of the component s of the micro emulsions
However, when a muzzler slug having a high viscosity is
desired, an appropriate known thickening agent such as a
water-soluble polymer can be added to the mice far slugs .
Examples of thickening agents usable in the formation of
the muzzler slugs are heteropolysaccharides produced by
microbes, naphthalenesulfonic acid-formaldehyde condemn-
sates, polyacrylamides, polyacrylates, hydroxyethyl-
cellulose, and carboxymethylcelluloses
The muzzler slugs of the present invention can be
readily obtained by any known method of production. For
example, the hydrocarbons, the surfactants, the aqueous
medium, and the cosurfactants can be mixed in any mixing
order by using conventional mixing devices, mixing
Jo
temperatures, and mixing pressures.
The recovery of oil from subterranean reservoirs
can be carried out by means of any conventional muzzler
drive method by using the muzzler slugs of the present
invention. For instance, the muzzler slugs are injected
under pressure into at least one injection well of the
subterranean reservoirs. Then, at least one driving
fluid such as flood water and/or aqueous solution of the
above-mentioned thickening agent it Injected into the
injection well so as to transfer or drive the remaining
oil toward on oil production well and to recover the oil
from the production well. The suitable amount of the
muzzler slugs injected into the injection well is about
I to about 25% by volume of the porosity of the subtler-
reunion reservoirs.
The suitable salt concentration of the subterranean water in the subterranean reservoirs where the muzzler
slugs of the present invention can be applied is 0% to
about 15~ by weight, desirably about 0.1~ to about 12%
by weight and, more desirably, about 0.5~ to about lo
by weight. Although the salt concentration of water
used in the formation of the muzzler slugs is not
necessarily the same as that of the subterranean water,
they are desirably the same prom the viewpoints that the
Walt concentration is changed during the sweeping.
As mentioned hereinabove, the muzzler slugs of the
present invention contain the internal olefin sulfonates
having a disulfonate content of about 20~ by weight or
I
-- 12 -I
Lowe as an essential component of the surfactantO The
resultant macular slugs thus haze an excellent salinity
tolerance and hereditary resistance and can form micro-
-emulsions by using water having a very wide salt consign
traction ox soft water to urine having a high salt
concentration. Furthermore, the muzzler slugs of the
present invention have very small interracial tensions
between water and the micro emulsions and between oil
and the micro-emulsions and have resistance against the
change in the salt concentrations. As a result, the
following remarkable advantageous features can be
obtained:
1) Either soft water, seawater, or subtler-
reunion water having a hush salt Concentration can be
freely used;
(2) The muzzler slugs injected into the
subterranean reservoirs are subjected to no substantial
adverse effects by inorganic salts present in the subtler-
reunion reservoirs;
(3) Thy muzzler drive method can be readily
applied in subterranean reservoirs containing oil having
a low viscosity to a high viscosity; and
(4) A high oil recovery efficiency can be
attained since stable micro-emulsions are maintained in
the subterranean reservoirs until oil banks are formed.
EXAMPLES
The present invention now will ye ~Irther illustrated
by, but is by no means limited to, the following examples,
- 13 -
in which the component ratios or amounts of samples used
are based on n % by weight" unless orioles specified.
Example 1
Micro-emulsions were prepared by weighing 10.5~ of
sodium C14-C18 internal olefin sulfonates (C14-Cl~ IOS-Na)
having various disulfonate contents or petroleum sulfonate
TRACY (manufactured by Witch Chemical Corp.) as a sun-
fact ant, 4.5~ of Amy alcohol as a cosurfactant, 17% of
fuel oil (ASTM No. 2 oil) as a hydrocarbon, and 68% of
an aqueous solution of 8% of sodium chloride dissolved
in demineralized water as a brine in a beaker. The
resultant mixture was stirred at 100 rum for 30 minutes
at a temperature of 71C.
The IOS-Na samples having various disulfonate (DO)
contents used as a surfactant were prepared by changing
the molar ratio of the starting internal olefin and S03.
The samples having a small DO content were prepared
by extracting the disulfonates from the reaction
products by isobutyl alcohol to adjust the desired DO
contents.
The micro-emulsion forming capabili~les, the inter-
facial tension decreasing capabilities, and the oil
recovery efficiencies of the micro-emulsions thus
prepared were evaluated as follows. The results are
shown in Table 1.
The micro-emulslon forming capabilities were deter-
mined from the visual appearance of the micro-emulslons
according to the following:
27
- 14 -
o ...... A transparent or translucent and home-
generous micro-emul~ion was formed
x ...... An opaque suspend ion, rather than a
micro-emulsion was formed.
The interracial tensions were measured by a spinning
drop type tensiometer at 71C in an appropriately diluted
system.
The oil recovery tests were carried out by using
err sandstone core having a size of 3.8 cm diameter
and 28 cm length and having a permeability of about
500 my and a porosity of about 20%. A core sufficiently
saturated with brine was set Lo a core holder and, then,
Lull oil was injected under pressure m to the core at a
feed rate of 6 cumin until no brine was discharged.
Then, brine was injected under pressure at the same feed
rate in a water drive method until the content of the
fuel oil in the effluent became less than 0.1%. thus,
the fuel oil was recovered. After the waxer drive method
the core holder and the micro-emulsions were placed in a
constant temperature bath at a temperature of 71C for a
muzzler drive method. The micro-emulsions were first
injected under pressure into the core in an amount of
10% by volume of the pore volumes, a polymer solution
(i.e., Lowe pup of Xanthan gum solution m a brine
solution) way when injected under pressure in an amount
of 100% by volume of the pore volume, and, finally,
brine was injected under pressure in an amount of Lowe .
by volume of the pore volume. Thus, the fuel oil was
I
- 15 -
recovered. The injection rate under pressure was
2 feet/day. The oil recovery efficiency was determined
by measuring the amount of water in the core after the
test in a Tulane azeotropic method to convert the
recovery amount of the fuel oil.
Table l
A B C D E F G
Surfactant 14 18
Petroleum
Disul*nabe ccnbent 0* 4 712l9 24 sulfcnate
(% effective component)
Micro-emulsion rang
c~pabili~ O o x
In racial tension 3.5 4.4 5.2 6~4 9.8 19.3
(x 10 dyne/cm)
Oil recovery 93 92 91 82 72
* Diaphaneity content: less than 0.1
Example 2
Micro-emulsions were prepared by weighing 10.5% of
Cluck IOS-Na containing 7% (based on the effective
component) of the disulfonate as a surfac~ant, 4.5~ of
Amy alcohol as a cosurfactant, 17% of fuel oil (ASSET
No. 2 oil) as a hydrocarbon, and 68~ of an aqueous
solution of a given amount of sodium chloride dissolved
in demineralized water, or an aqueous solution of a
given amount of Coequal or Meekly dissolved in the above-
I
- 16 -
-prepared aqueous sodium chloride solution in a beaker.
The resultant mixture was stirred at 100 rip for 30
minutes at a temperature of 71C.
The micro-emulsion forming capabilities, the inter-
facial tensions, and the oil recovery efficiencies of the
micro-emulsions were evaluated in the same manner as in
Example 1. The results are shown in Table 2 below.
Table 2
.
Sample No H I J K L
S~riactant 14 18 a
Ermine Nail 1 12 15 5 5
(%)
Cook - - - 0.5
McCoy - - _ _ owe
M~xo-emulsion no O O O O O
capability
Interracial tension 6.2 5.1 4.8 4.6 4.6
(x 10 dyne/cm)
Old wreck (~)90 91 91 91 91
. .
Example 3
Micro-emulsions were prepared by weighing Lowe
of C -Clue IOS-Na, C18-C20 ITS My, or C20 22
a surfactant, 4.5~ of Amy alcohol as a cosurfactant,
17% of fuel oil (ASTM No. 2 oil), and 68% of an aqueous
solution of 8% of sodium chloride dissolved in definer-
alized water in a beaker The resultant mixture was
I
- - 17 -
stirred at 100 rum for 30 minutes at a temperature
of 71C.
he micro-emulsion forming capabilities, the inter-
facial tensions, and the oil recovery efficiencies of
the mlcro-emulsions were evaluated in top same manner
as in Example l. The results are shown in Table 3 below.
Table 3
_ .
_ Same No. M_ N JO
Surfactant C13 C14 IOS-Na C18-C20 IOS,M~ C20 C22
Disulfonate content
(I For effective 6 8 7
camFonent)
Micro~lsion arming
capability
In facial Zion 9 9 6.5 3.8
(x 10 3 dyne/cm)
Oil recovery (~) 81 90 92
Example 4
Muzzler slug compositions containing anionic
surfactants, cosurfactants, hydrocarbons, and aqueous
media were prepared.
The anionic surfactna~ used was sodium C14-Cl~
IOS-Na ADS = 7%), C20-C2~ IOS-Na ADS = 9%), petroleum
sulfonate TRACY (manufactured by Witch Chemical Corp.).
The cosurfactants used were Amy alcohol or isopropyl
alcohol. The hydrocarbons used were kerosene or fuel
Lo
- 18 -
oil (ASTM No. 2 fuel oil). The aqueous media used were
seawater having a saline content of about 3.5~ and an
alkaline earth metal ion concentration of about 1,600 Pam,
or soft water.
S The muzzler slugs were prepared by first mixing
the surfactant and the aqueous medium and, then, adding
the cosurfactant and the hydrocarbon to the mixture,
while stirring it.
The compositions and properties ox the muzzler
slugs thus obtained are shown in Table 4. Visual
appearance was determined according Jo the following:
o ...... A micro-emulsion was formed
x ...... A suspension, rather than a micro-
emulsion was formed.
~3~7
- 19 -
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us o I o
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Jo
Ye ,,~ tl, '0 o I -
. ....
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r I O o r
D I I O o O
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o I o Jo
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- 21 -
Example 5
Muzzler slug samples were prepared in the same
manner as descried in Example 4 except that various
brines obtained by dissolving sodium chloride in de-
mineralized water to predetermined saline concentrations were used.
The compositions and the properties of the samples
are shown in Table S.
Example 6
Muzzler slug samples were prepared in the same
manner as described in Example 4 except that various
brines were obtained by adding I by weight of sodium
chloride and magnesium chloride and/or calcium chloride
so as to provide the predetermined bivalent metal ion
concentration to demineralized water.
The compositions and the properties of the samples
are shown in Table 6.
~3~27
-- 22
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rJ Jo I I I ED O Lo I
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I O N I
I our I I 1` I I I O I
Jo ¦ I I D I clue:) I I I I X
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x 2 8
b o 3
Ye to o s
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-- 23 --
Jo I o I
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M i I I n I I o O
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D I I I I I O I
Jo I I l l l O us I
I I I I I I I I x
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Muzzler slug samples were prepared in the same
manner as described in Example 4 except that the counter
ion s o f the internal olefin sup ion a toes were changed.
The compositions and the properties of the samples
are shown in Table PA (monovalent cations) and Table 73
diva lent cations).
Example 8
Muzzler slug samples were prepared in the same
manner as described in Example 4 except that two or more
internal olefin sulfonates were used together.
The compositions and the properties of the samples
are shown in Table 8.
-- 25 --
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