Note: Descriptions are shown in the official language in which they were submitted.
~L~LC~i3Z9
HIGH CONCENTRAT~ON METERED AEROSOL
ANTIPERSPIRANT PRODUCT
.,':
This invention relates to an aerosol antiperspirant
suspension system and, more particularly, to an aerosol
antiperspirant of this type employing a propellant,
preferably a hydrocarbon propellant, and active antiper-
spirant materials at relatively large concentrations.
The use of aerosol systems for applying antiper-
spirant materials to the underarm has proven to be one
of the most convenient ways of delivering these materials.
In these systems, fluorocarbon propellants ware previously
found to be most suitable since they were thought to be
; safe because of their non-flammability.
~ evertheless, there were certain limitations in
the practical application of these systems in delivering
` antiperspirant materials. One item that was constantly
a problem was the fact that in these systems, aerosol
valve clogging-problems were encounterad. To deliver
a commercially satisfactory product in which the
clogging~problem was controlled within acceptable limits,
it was necessary to limit the antipers~irant material
in the system to a level of from about 4-5% of active
antiperspirant material suspended in the system.
~ To obtain satisfactory antiperspirant activity
;~ by underarm application, it was necessary to deposit
the antiperspirant material under the arm in a suffici-
~; 25 ently large dose to be effective. It has been deter-
~ mined and it has been adopted~as an industry standard
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that a dose of between 100-130 milligrams of active anti-
perspirant material e.g. aluminum chlorhydrate is an
effec~ive dose. The prior art fluorocarbon propellant
systems containing 4-5% of active antiperspirant
have a product delivery rate of 1200 mg/sec which
delivers about 48-60 milligrams of active antiperspirant
material per second. To deliver an efective dose of
antiperspirant material in these systems, it was necessary
then to apply the material for a period of two seconds.
Because of the character of the spray dispensed from
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these aerosol systems, this two second spray did not
present too much of an inhalation problem. The product
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did not stay suspended in the air forming a fog or mist
- but rather settled quite promptly.
With the advent of the environmental concern with
the fluorocarbon propellants, the search for a substitute
propellant was undertaken by the industry. It was soon
- found that hydrocarbon propellants could be employed in
the antiperspirant aerosol suspension systems. However,
; 20 new problems were encountered. It was found that when
the hydrocarbon propellant was substituted for the
fluorocarbon propellant and the material was dispensed
for two-seconds as per the prior art procedure, a cloud
of product was produced that stayed suspended in the
air for relatively long periods of time. This intro-
- duced a potential for inhalation problems.
: It has now been found that the aforesaid potential
inhalation problems can be significantly diminished by
incorporating a relatively large quantity of powdered
active antiperspirant material distributed in a substan-
tially anhydrous oil system, suspending this in a relatively
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small quantity of propellant (preferably a hydrocarbon
propellant) and dispensing the same from an aerosol
container having a meterecl valve designed to deliver
uniform dosages of active antiperspirant ingredients
when the aerosol valve is actuated. This system has
the virtue that notwithstanding the relatively high
concentrations of powderecl active antiperspirant mater-
, ials suspended in the syst:em, substantially no clogging
or malfunction of the valve occurs.
It is accordingly an object of the present inven-
tion to provide an aerosol antiperspirant system of
the suspension type having relatively high concentra~
tions of active antiperspirant material suspended in
the system but with a relatively low potential for
producing persistent clouds of product when sprayed
into the atmosphere.
It is also an object of the present invention to
provide a system of the type described in the above
object in which the potential for clogging or malfunction
of the aerosol valve is minimal.
It is a further object of the present invention to
provide an article of manufacture comprising an aerosol
container provided with a metered valve and containing
powdered active antiperspirant material in relatively
high concentrations suspended in a substantially anhydrous
liquid containing a propellant; said propellant as compared
with prior art products constitutin~ a relatively small
proportion of the composition contained in the aerosol
` ~ container~
Other and more detailed objects of this invention
will be apparent from the following description, claims
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and drawings wherein:
Fig. 1 is a longitudinal elevation partly in sectlon
of a metered aerosol valve and container that may be employed
in practicing the present invention.
Thus the present invention provides as an article
. of manufacture an aerosol container having enclosed therein
a composition comprising an active antiperspixant material
under pressure and means for discharging said composition
from said container, said composition comprising based on
the total weight of the composition: (a) from about 20% to
about 50~ of an active antiperspirant material; (b) from
about 20% to about 50% of an oily material; and (c) from
about 20% to about 50% of a propellant said composition
discharging means including a metered valve designed to
deliver said active antiperspirant material in metered doses;
the concentration of the ingredients in said container and
the dimensions of said metered valve being such as to deliver
a dose of ~rom about 40 to about 80 mg of active ingredient
with each discharge.
The propellant may preferably be a hydrocarbon
propellant. The oily material may in a preferred em~odiment
be a li~uid oil having a vapor pressure no greater than
about 1 mm of ~g at body temperature. Preferably such an
article of manufac~ure is provided in which said oily material
is a li~uid oil selected from the group consisting of liauid
hydrocarbons; fatty acid monoesters; diesters of dicarboxylic
acids; polyoxyalkylene glycol esters; propylene glycol
diesters of short chain fatty acids (C8-ClO); polyoxyethylene
; ethers; polyoxypropylene ethers; higher fatty alcohols;
propoxylated monohydric alcohol M.W. 880-930; silicone oils
and mixtures thereof. Also preferably such an article
includes from about 0.1% to about 5.0% by weight based on
the total weight of the composition of a suspenaing agen~.
In ano~her embodiment the present invention provides,
as an article of manufacture, an aerosol container having
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: enclosed therein a composltion comprising an active anti-
perspirant material under pressure and means for discharging
said composition from said container in the form of a
spray, said composition comprising based on the total weight
of the composition: (a) ~rom about 30~ to about 40% of an
-~ active antiperspirant material; (b) from about 30% to about
40% of an oily material; and (c) from about 25~ to 35% of a
propellant said composition dischar~ins means including a
metered valve designed to deliver said active antiperspirant
- lO material in metered doses; the concentration of the
ingredients in said container and the dimensions of said
metered valve being such as to deliver a dose in the range
of from about 48 mg to about 65 mg o~ active ingredient with
each discharge.
As noted above, it is a feature of the present
invention to provide an aerosol antiperspiran~ composition in
; which the active antiperspirant in powdered form is suspended
in the fluid system in relatively high concentrations. The
; quantity of antiperspirant material may vary somewhat but
it will be in the range of about 20 to about 50% and pre~erably
between about 30 to about 40~ by weight based on the total
weight of the composition.
The active antiperspirant material that may be employed
- in the present invention may be any one of a number of
materials known in this art to exhibit this property which
may be prepared as a powdered material capable of bei.ng
~ suspended in the fluid medium in accordance with the present
: invention. By way of examples, we mention aluminum chlor-
; hydroxide, aluminum chloride, aluminum chlorohydrex propylene
glycol complex, aluminum zirconium complexes, sodium aluminum
- chlorohydroxy lactate of mixtures thereof. Typical of the
mixed active antiperspirant materials that may be emploved
herein are ~he aluminum chloride-aluminum chlorhyd~oxlde
` powdered materials described in Canadian Patent 958,338; said
r'` ' 35 patent being incorporated herein by way of reference.
' It is also a feature of the present invention to provide
` an oily material, preferably a liquid, which
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will serve as a vehicle for suspending the powdered anti-
perspirant material employed herein. Aside from this
function, the oily material will serve as an emollient
to ~ive the skin a good ~eel when the product is deposited
on it from the aerosol can and serve as a means for
retaining the active mater:ial at the site on which it is
deposited. For the latter reasons, it is advantageous
to employ oily materials that are not especially volatile
under the conditions under which it is applied to the
skin e.g. one that does not have a vapor pressure above
about 1 mm of Hg at body temperature. By way of illus-
tration of the oily materials that may be employed herein,
the following may be mentioned: liquid hydrocarbons
(mineral oil); fatty acid monoesters (isopropyl myristate,
isopropyl palmitate); diesters of dicarboxylic acids
(diisopropyl adipate); polyoxyalkylene glycol esters (poly-
propylene glycol 2000 monooleate); propylene* glycol diesters
of short chain fatty acids (C8-C10) (Neobee M20); polyoxy-
ethylene ethers ((polyoxyethylene(4)1auryl ether (Brij 30~,
polyoxyethylene(2)ole~1 ether (Brij 92), polyoxyethylene
(lO)oleyl ether (Bri~ 96, Volpo 10~ ; polyoxypropylene
. .
cetyl ether (Procetyl); higher fatty alcohols (oleyl,
` hexadecyl, lauryl); propoxylated monohydric alcohol M.W.
880-930 (Fluid AP); silicone oils (dimethyl polysiloxane
10-1000 centistokes). Mixtures of the above liquids are
equally suitable for the purposes of this invention.
- The quantity of oily material that will be contained
; in`the composition of the present invention may also vary
somewhat depending on the results desired. For the most
part, it wil~l comprise from about 20% to about 50% by
weight and preferably from about 30~ to about 4~ by
weight based on the total weight of the composition.
It is also desirable to incorporate in ~he aerosol
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compositions of this invention suspending agents to fur-
ther prevent caking of the powder and to enable redisper-
sing the powder by simple agitation. A variety of
materials may be used (alone or in combination) for this
purpose, among wh*ich may be mentioned:
~a) Cab-O-~il (Cabot Co.) (Fumed Silica)
` (b) Bentone 34 or Bentone 38
(dimethyl dioctadecyl ammonium bentonite
or he~torite, respectively)
(c~ Veegum F (R. T. Vanderbilt Co.)
(microfine magnesium aluminum silicate)
` (d) Microthene (U.S.I.)
(polyethylene powder)
(e) Metal soaps of fatty acids (e.g.
powder aluminum stearate, aluminum
octoate)
The quantity of suspending agent that will be con-
tained in the present composition may also be employed
over a range of concentrations. Usually, this will fall
; 20 within the range of from about 0.1 to about 5.0~ by weight
based on the total weight of the composition. The pre-
ferred range for these materials, however, will be from
` about 0.5 to about 1.5% by weight based on the total
weight of the composition.
A further aspect of this invention is that the
"
present compositions contain relatively small quantities
~; ~ of propellant. This too may vary somewhat but, in general,
this will amount to from about 20 to about 50% by weight
based on the total weight of the composition. In the
; 30 preferred form of this invention, the propellant will
constitute in the range of from about 25~ to about 35~
by weight based on the total weight of the composition.
~ As previously indicated, because of environmental
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considerations, it is desirable to use a hydrocarbon pro-
pellant in the present invention. The h~drocarbon propel-
lants that are useful herein are those that are well known
in the art. These are the liquified normally gaseous
aliphatic hydrocarbons i.e. those that are gaseous at
ambient pressures and temperatures. Generally, these
propellants should have a boiling point lower than about
75F and a vapor pressure from about 25 to 70 pounds
- per square inch gauge (psig) at 70F, preferably between
30 and 40 pounds psig. A suitable vapor pressure can
also be produced by blending two different propellants
such as propane and isobutane. By way of illustrating
those hydrocarbon propellants that are useful herein,
mention may be made of n-butane, isobutane, propane,
pentane, isopentane and mixtures thereof. However, the
propellants of choice are isobutane and n-butane.
Although the hydrocarbon propellants described
above are preferred in practicing the present invention,
; other types of propellants can be employed. Thus, the
` 20 well-known liquified normally gaseous halogenated hydro-
carbon and particularly, the chlorofluorohydrocarbons
may be utilized herein. These include such ~aterials
as 1,2-dichloro-1,1,2,2-te*trafluoroethane (Freon 114);
trichloxofluoromethane (Freon 11~; dichlorodifluoro-
methane (Freon }2); trichlorofluoroethane tFreon 113);
chl~orodifluoroethane ~Freon 14~B); chlorodifluoromethane
(Freon 22); methylene chloride and mixtures thereof.
In addition to the aforesaid ingredients, other
auxilliary agents well known to those skilled in the art
may be incorporated in th~ present co~position in
effective quantities. These additives include:
1. Antibacterial and~antifungal agents such
as hexachlorophene, quaternary nitrogen compounds
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(benzethonium chloride), benzoic acid, resorcinol mono-
acetate, chlorobutanol, Vancide 89RE, zinc omadine, etc.
2. Fragrance
3. Slip Agents (e.g. talc, zi~c stearate)
4. Surfactants (e.g. Arlacel 80 sorbitan mono-
oleate)
5. Pigments (e.g. titanium dioxide)
6. Fabric Damage Reducing Agents (e.g. urea,
glycine) *
7. Anticorrosion Agents: Gafac RM 510 (ethoxylated
dinony~ phenyl mono and diester of phosphoric acid);
Crodafos CAP (propoxyl*ated cetyl mono and diesters of
phosphoric acid); Epoxol 8-2B (epoxidized butyl esters
of linseed oil fatty acids).
Another feature of the present invention is the
use of a metered valve on the aerosol container contain-
ing the composition described above. A typical valve that
may be employed herein is shown in Fig. 1, although this
is by no means the only construction that is useful for
~;~ 20 our purposes.
Referring to Fig. 1 the valve mounting cup is shown
~, at 2 and is employed to mount the assembly shown in this
Fig. 1 onto an aerosol can containing product and is secured
thereto by crimping lip 4 to the can.
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The metered valve comprises a metering chamber 6
formed by genexally cylindrical housing 8. The upper end
of metering chamber 6 is closed off by top gasket 10
- which forms an airtight seal. The lower end of metering
chamber 6 is formed by the upper end dip tube 12 which
is provided with valve seat 14 adapted to receive the
end of valve stem 16 described in more detail below.
The internal diameter of the lower portion of
metering chamber 6 is smaller than the internal diameter
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of the upper portion of metering chamber 6 thereb~ form-
ing a flange 18 for support of lower gasket 20. Lower
gasket 20 is provided with a centrally disposed hole
which has a diameter which is larger than the external
diameter of valve stem 16 below the valve stem stop 22.
Because of the size of the opening in lowex gasket 20,
the upper portion 24 of metering chamber 6 is in communi-
cation with the lower portion 26 of metering chamber 6.
Furthermore, because o~ the size of the opening in lower
gasket 20 when valve stem 16 is depressed, the major
portion of valve stem 16 below stop 22 may pass through
the opening in gasket 20.
~ In assembling the metered valve employed herein,
-~ a coiled spring 28 is inserted so that its lower end
~.
. 15 rests on gasket 20 and its upper end lies just below
stem stop 22. When spring 28 is in its extended position,
it urges stem stop 22 upwardly against the under surface
o upper gasket 10.
Valve stem 16 is hollow; open at the top but closed
at its lower en~ by stem end 30. Stem 16 is also pro
vided with a hole 32 that is bored through the stem
.. wall and into the hollow o~ stem 16. When assembled,
a valve button 34 is provided having internal channels
~hat co~municate with the internal hollow o~ stem 16
and to the atmosphere through opening 36.
In operation, when the valve stem 16 is in its
extended position as shown in Fig. lj the product under
pressure filIs metering chamber 6. When valve stem is
depressed, it is depressed until the valve stem end 30
::~ 30 engages and seats in valve seat 14, thereby cutting
~:~ off the communication between the interior of the
aerosol can and metering chamber 6. At the same time,
the measured quantity of product in metering chamber 6
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, is expelled since it is under pressure. The volume of
metering chamber 6 can be varied by changing the length
of cylindrical housing 8 and/or lowering the top end of
dip tube 12 disposed inside cylindrical housing 8.
The quantity of product delivered and as a con-
~; sequence, the quantity of antiperspirant material that
will be deposited at the site of application with each
discharge will be dependent on the volume of the metering
chamber, the density of the product that is contained in
the metering chamber and the concentration of the active
antiperspirant materials in the product. These parameters
may vary within the following ranges:
i (l) volume of metering chamber about
: 50 to 250 microliters;
~; 15 (2) density of product about 0.9 to 1.2; and
(3) concentration of active about 20~ to
50% by weight based on the total weight of
product
~ These parameters are adjusted to deliver between about
,i; 20 40 to 80 mg by weight of actives and preerably between
about 48 t~ 65 mg of actives with each discharge.
The metered valve system of this invention allows
a uniform dosage each time the actuator is depressed,
but at the same time causes all the product held in the
~ 25 metering chamber to be totally expelled or purged. By
,~ this purging no buildup is allowed in the stem or
hctuator portion of the system, the main areas of valve
~ clogging problems.
i The metered dose with high solids content delivered
in accordance with the present invention gives a non-
~fogging spray. ~imiting the amount of propellant sprayed
as per the instant invention reduces the flammability.
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In addition, since we concentrate the actives, we can
- obtain more uses per given can volume. Moreover, the
product goes on as a dry, warm and gentle spray.
The valve systems now used in the standard antiper-
spirant aerosol all contain a vapor tap. The vapor tap
mixes gaseous propellant with the product inside kh0 valve
at the stem orifice. The resultant spray is fine and
dry, causing the suspended antiperspirant powder to fly
; into a cloud which floats in the air. This cloud of
suspended antiperspirant powder is the cause of choking
`~ and inhalation problems.
The metered valve systems employed herein have no
vapor tap; therefore, the resultant spray particles are
large and fall to the ground rather than be suspended in
the air. This tends to eliminate inhalation problems.
Furthermore, the metered system of the present
invention uses a concentrated dosage. Because we use,
for example, between 30-40% of active antiperspirant
material in our metered aerosol as compared to around 10
in standard vapor tap antiperspirant aerosols, we will
spray about 75~ less can contents into the air than the
standard aerosol system. This, along with our non-vapor
tap metered system, will give a spray with lessened
~ inhalation problems.
;; 25 The following Examples are given to further illus-
trate the present invention. It is to be understood,
however, that this invention is not limited thereto.
The ~ollowing terms used in the Examples given
below have the following meanings:
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Bentone 38: dimethyl dioctadecyl hectorite
Emollient 60: isopropyl palmitate/isopropyl
myristate (60/35)
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Alcohol SDA 40: denatured ethyl alcohol
amino acetic acid
EXAMPLE 1
- Preparation of Concentrate % by Wt.
5Aluminum chlorhydrol
; (Macrosphericals 9';) 50.0
~ Emollient 60 25.0
~
; *Bentone Gel 25 0
~".,:
'; 100. 0
~, * Bentone Gel ~ by Weight: 10.0% Bentone 38; 10.0%
i~ 10 Alcohol SDA-40; 80.0% Emollient 60
^~ The Bentone Gel is added to a Hobart pot while mix-
;~ ing slowly. The Emollient 60 is then added thinning out
gel. The actives are added slowly when the gel is thoroughly
mixed. The mixture is placed in a Warlng blender and
blended for 1 minute at medium speed. This concentrate
is then packaged as described below.
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Sixty-six parts by weight of the above concentrate
- were charged into each of eleven aerosol cans which had
a diameter of 202 centimeters~and a height of 314 centi-
meters. These were equipped with B-l~M metered valves
(Ethyl Corp.) shown in Fig. 1 having a ~etering chamber
; ~ with a volume of 175 microliters (measured by the de~livery
of 175 mg of water). These cans were then filled with 34
parts by weight of~either isobutane or n-butane~using
the under cup filling technique. The cups were then
crimped to the tops of the cans.
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~; The furthsr specifications of the metering valves
employed are as follows: .030 stem, B18-5J spring,
buna N seal and diaphram, dip tube I.D. ~040.
The following experiments were carried out to
compare the degree of foggi;ng or product cloud formation
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that follows the use of the present product as compared
with prior art products.
Experimental Procedure:
Prior to the experiment, two filter pad holders per
subject were equipped with tared Gelman Metricel DM-800
filter pads. Each pad was weighed on an analytical balance,
sensitive to 0.01 mg. The subject wearing the particle
sampler holder (Gelman in line filter holder) connected
to a HASL cyclone (Model 1~) which eliminates particles
10 ug, entered a simulated home bathroom (5' x 5' x 8').
The cyclone and filter holder are secured to the subject's
head so that the cyclone portion of the apparatus is sus-
pended in the breathing zone of the panelist. A tygon
vacuum tube connects the filter pad holder via the door
sill to a wet test meter, vacuum pump and electric timer
located outside of the test room. A specific air sampling
flow rate of 9 liters/minute maintained by adjustment
of vacuum pump.
Upon entering the room a panelist is equipped with
the first tared filter pad. A 15 minute control sample
of ambient air from the breathing ~one is collected.
He is then fitted with the second ~ilter pad, instructed
to hold the test product 6" from the exposed underarm,
and spray twice to each axilla and remain seated for
the 15 minute treatment collection.
At the end of the sampling periods, the tared filter
pad is removed from the sampler and weighed to determine
the amount of respirable material in the breathing zone.
In addition to the gravimetric method of determining
the amount of respirable residue deposited, a ferron method
for aluminum analysis was employed. Aluminum forms a
colored complex with ferron (8 hydroxy-7 iodo-5 quinolene
sulfonic acid~ which has a maximum absorbance at 3~0 mu.
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; (Davenport, W.H., Anal. Chem. 21: 710 (1949). An ex~osed
filter pad is placed in a 50 ml beaker with 5 ml o~ a
~, 0.5N HC1 solution. Both are heated (almost to boiling) for
10-15 minutes. After making appropriate dilutions, the
' 5 solution is reacted with ferron and read at 370 mu vs. the
; reagent blank in absorption cells o the Beckman D B-G
Spectrophotometer.
Four test products were used in the experiments
s;~ identified by the codes F #1072~ F ~769, F ~1039 and
Triad metered A/P spray. The compositions of these
formulas are given below:
F #1072
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Ingredients % by Wt.
Isopropyl Palmitate-Myristate
(60~-35%) 2.00
Isostearamide DEA
; (Monami*d 150 IS-Mona Industries) 0.80
Dimethicone 500 Centistokes
;~ (Silicone SWS-101, 500 CSTK
~ 20 Stau~fer Wacker Silicone Corp.) 0.40
; Perfume 1833-W (IFF) 0.15
.
'; Aminoacetic Acid (Glycine Crystal
~i (USP - Robeco) 0.60
~ Water, deionized 8.05
;~ ~ 25 Aluminum chlorhydroxide 50%22.90
Aluminum chloride hexahydrate
solution 50% * 5.10
Talc 2755, Lo-Micron 5.00
Isobutane (CP Grade) 55.00
100.00
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F #769
Ingredlents % by Wt.
*BM Special Aluminum Chlor-
hydroxide Type II 5.50
Colloidal Silicon Dioxide, M-5 0.23
Dimethyldioctadecyl Ammonium
: Bentonite 0.23
Isopropyl Palmitate-Myristate
~0%-35%) 7.00
~ 10 Perfume 4216T (IFF) 0.30
; Propellant 11 56.38
Propellant 12 30.36
: 100. 00
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* Spray dried aluminum chlorhydroxide (80~)
aluminum chloride (20%) mix
F #1039
: Ingredients % by Wt
.
Alu~inum chlorohydrate complex
(Rehydrol-Reheis) 15.00
Alcohol SD-40, Anhydrous
::~ (Brucine Sulfate) 69.25
Isopropyl Palmitate-Myristate
(60%-35%) 10.00
Isostearic Acid (Emery 871-
- 25 Emery Ind.) 1.00
Polyoxyethylene(4)lauryl ether 0.75
~: Polyoxyethylene(23)lauryl ether 0.25
Aluminum Chloride Hexahydrate
Solution 50% 2.00
:~ 30 Aminoacetic Acid (Glycine Crystal
~F-Robeco) 0.50
Water, deionized 0.75
Perfume 1758-Y (IFF) 0.50
100.00'
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Triad Metered A/P Spra~
Concentrate ~ by Wt.
: *BM Special Aluminum
Chlorhydroxide Type II 50.0
- 5 Emollient 60 47.0
Bentone 38 1.5
Alcohol SD 40 1.5
'' 100.O
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Aerosol
-
Concentrate ~ 66.0
Isobutane 34.0
', 100.O
* Spray dried aluminum chlorhydroxide (80%)
aluminum chloride (20%) mix
Formulas F ~1072 and F #769 were dispensed from conven-
tional aerosol cans; whereas formula F #1039 was dispensed
from a pump spray container. The Triad metered A/P
` spray composition was dispensed from the metered aerosol
container shown in Fig. 1
The results of these studies are summarized in
Tables I and II below.
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