Note: Descriptions are shown in the official language in which they were submitted.
WO 95/27771 ~ ~ PCT/EP95/01085
- 1 -
The present invention relates to fabric softening
compositions. In particular the invention relates to fabric
softening compositions that have excellent stability,
dispensing and dispersing properties.
Backaround and Prior Art
Rinse added fabric softener compositions are well known.
Typically such compositions contain a water insoluble fabric
softening agent dispersed in water at a level of softening
agent up to 7o by weight in which case the compositions are
considered dilute, or at levels from 7~ to 30~ in which case
the compositions are considered concentrates. Fabrics can
also be softened by the use of sheets coated with softening
compound for use in tumble dryers. In more detail the
commercially available fabric softening compounds generally
form stacked lamellar structures in water which have
characteristic L~ to L0c phase transition temperatures.
The rinse added fabric softening compositions of the prior
art soften by depositing dispersed colloidal particles of
softening compound onto fabrics, whilst dryer sheets soften
fabrics by direct transfer of molten softening compound, as
taught by the review by R. G. Laughlin in "Surfactant Science
Series 2 Volume 37 Cationic surfactants Physical Properties
Pages 449 to 465. (Marcel Decker, inc, 1991)
Conventional liquid fabric softening compositions are in the
form of dispersed colloidal particles of the fabric softening
compound. Fabric softening compositions comprising dissolved
WO 95/27771 ~ PCT/EP95/01085
- 2 -
fabric softening compound in organic solvent and powder or
granular compositions have also been described.
Fabric softening compositions formed from dispersed colloidal
particles have complex, unstable structures. Because of this
instability there are many problems associated with
conventional fabric softening compositions. The principal
problems are: physically instability when stored at high and
low temperatures; when frozen they are converted irreversibly
to gels; it is difficult to obtain compositions that exhibit
good dispersibility into the wash liquor, deposition onto the
fabrics and dispensability from the washing machine dispenser
drawer. Poor dispersibility results in uneven coating of
fabric softener onto the laundry and in some cases spotting
can occur. These problems are exacerbated in concentrated
fabric softening compositions and on the addition of perfume.
Physical instability manifests itself as a thickening on
storage of the composition to a level where the composition
is no longer pourable, and can even lead to the irreversible
formation of a gel. The formation of a gel can also occur in
the dispensing drawer of- a washing machine when the
temperature of the drawer is increased by the influx of warm
water. The thickening is very undesirable since the
composition can no longer be conveniently used. Physical
instability can also manifest itself as phase separation into
two or more separate layers.
Concentrated products, good dispersibility and
dispensability, and storage stability at low or high
temperature are however desired by the consumer.
The problems associated with conventional dispersed colloidal
particles are addressed by the prior art.
.. WO 95/27771 p ~ ~ PCT/EP95/01085
- 3 -
US 4 789 491 (Chang) discloses a specific process for the
formulation of aqueous dispersions of cationic softening
compounds. The process is said to overcome the difficulties
of product viscosity and poor dispensing and dispersing on
storage.
EP 0 239 910 (Procter and Gamble)) discloses compositions
containing dispersions of either diester or monoester
quaternary ammonium compounds in which the nitrogen has
either two or three methyl groups, stabilized by maintaining
a critical low pH.
The physical stability of rinse added fabric softener
compositions has been improved by the addition of viscosity
control agents or anti-gelling agents. For example in
EP 13 780 (Procter and Gamble) viscosity control agents are
added to certain concentrated compositions. The agents may
include Clo-C18 fatty alcohols. More recently in EP 280 550
(Unilever) it has been proposed to improve the physical
stability of dilute compositions comprising biodegradable,
quaternary ammonium compounds and fatty acid by the addition
of nonionic surfactants. EP 507 478 (Unilever) discloses a
physically stable fabric softening composition comprising a
water insoluble, biodegradable, ester-linked quaternary
ammonium compounds and a nonionic stabilising agent.
Various proposals have been made to supply fabric softener in
granular or powdered form. EP 111074 is typical and uses a
silica to carry the softener. A disadvantage of using a
carrier such as silica is that it bulks up the product and
serves no function beyond making the powder compatible with
other ingredients that may be contained in a washing powder.
. ,0 95~2~~~1 218 4 0 6 9 pC'f/EP95/01085
- 4 -
EP 569 184 (Unilever) discloses use of a granular composition
to form a pre-dilute which is then added to the dispenser
drawer of the washing machine.
WO 92/18593 (Procter and Gamble) discloses a granular fabric
softening composition which can be added to water to form an
aqueous emulsion. The composition contains a nonionic fabric
softener such as a sorbitan ester and a mono-long chain alkyl
cationic surfactant.
WO 93/23510 (Procter and Gamble) discloses liquid and solid
fabric softeners comprising biodegradable diester quaternary
ammonium fabric softening compounds and a viscosity and/or
dispersibility modifier, the application also discloses
specific processes for making these products. The viscosity
and/or dispersibility modifier may be a single long chain,
alkyl cationic or a nonionic surfactant. The solid
composition when added to water fozrns an emulsion or
dispersion.
WO 95/13346 discloses the use of
a tegobetaine to overcome the problem of instability induced
by perfume in concentrated fabric softeners.
In an attempt to overcome the problems associated with
dispersed colloidal particles the prior art has turned to
fabric conditioners in the form of solutions of fabric
softening compounds in organic solvents. Compositions of
this type are exemplified by our copending application
WpA-94/17169. However on contact with water dispersed
colloidal particles are still formed.
A further way of making solutions of fabric conditioners is
by specific structural modifications.
a
218 4 0 6 9 p~''~~'o
- 5 -
US 3 892 669 (Lever Brothers) discloses a clear, homogeneous.
aqueous based liquid fabric softening composition and is
limited to solubilised tetraalkyl quaternary ammonium salts
having two short-chain alkyl groups and two long-chain alkyl
groups, the longer chain groups having some methyl and ethyl
branching. The solubilisers comprise of aryl sulphonates,
diols, ethers, low molecular weight quaternaries.
sulphobetaines, and nonionic surfactants. The specification
teaches that nonionic surfactants and phosphine oxides are
not suitable for use alone and only have utility as auxiliary
solubilisers.
We have surprisingly found that a novel fabric softening
composition can be formed without the disadvantages of the
prior art. The present invention discloses fabric softening
compositions having excellent softening properties yet which
exhibit excellent storage stability at both high and low
temperatures, good freeze thaw recovery and excellent
dispensability and dispersibility when the composition is
concentrated and even when the fabric softening compound is
concentrated to levels greater than 30 wt%. Furthermore
compositions prepared according to our invention do not
suffer from loss of softening performance.
pef~n~t~on of the Tnvention
Thus according to one aspect of the invention there is provided a fabric
softening
composition comprising
i) a substantially water insoluble fabric softening compound
3 0 com risin a com ound havin two C alk 1 or alken 1 ou s connected to a
P g P g i2-22 Y Y ~' P
quaternary ammonium head group via at least one ester link or a quaternary
ammonium compound comprising of a single chain with an average chain
length equal to or greater than C2o and;
A
wo 95i2~~~i 21 8 4 0 6 9 p~T~~s~~~~gs
- 6 -
ii) a solubilising agent comprising an amphoteric surfactant;
characterised in that the weight ratio of (ii) solubilising agent to (i)
fabric
softening compound is greater than 1:6, and when the fabric softening
composition is diluted in water to a concentration of 5 wt% of (i) and (ii),
at least
70 wt% of the fabric softening compound is in solution.
A further aspect of the invention provides the use of self-
size-limiting molecular aggregates (as defined below) as a
fabric softening composition.
Without wishing to be bound by theory it is believed that the
fabric conditioner of the invention is not in conventional
lamellar form, and when contacted with water may be
solubilised partially in the form of self-size-limiting
molecular aggregates, such as micelles or micellar solutions
with solid or liquid interiors or mixtures thereof. Where
the composition is in a form containing water the composition
itself may be at least partially in the form of self-size-
limiting molecular aggregates. It is thought that it is this
new structure of the fabric softening compositions that
overcomes the problems of the prior art.
Suitably the fabric softening compound and solubilising agent
form a transparent mix. However, the following tests may be
used to determine definitely whether or not a composition
falls within the present invention.
a) The,fabric softening composition is diluted with water
at a concentration of 5 wt% (of the fabric softening
compound and the total solubilising agent ie the
A
° ~ 2 ~ ~ ~ Q 6 9 PCT/EP95/01085
W O 95/27771
_ 7 _
nonionic surfactant and any non-surfactant
cosolubiliser). The diluate is warmed to between 60 - 80
°C then cooled to room temperature and stirred for 1
hour to ensure equilibration. A first portion of the
resulting test liquor is taken and any material which is
not soluble in the aqueous phase is separated by
sedimentation or filtration until a clear aqueous layer
is obtained. (Ultarcentrifuges or ultrafilters can be
used for this task.) The filtration may be performed by
passing through successive membrane filters of 1 dun,
0.45 u.m and 0.2 dun.
b) The concentration of the fabric softening compound in
the clear layer is measured by titrating with standard
anionic surfactant (sodium dodecyl sulphate) using
dimidiumsulphide disulphine blue indicator in a two-
phase titration with chloroform as extracting solvent.
c) The titration with anionic surfactant is repeated with a
second portion of fabric softening composition which has
been diluted but not separated.
d) Comparison of b) with c) should show that the
concentration of fabric softening compound in b) is at
least 70 wt$ (preferably 80 wt~) of the concentration of
fabric softening compound in c). This demonstrates that
the fabric softening compound was in solution.
a) The fabric softening composition is diluted as for Test
I.
b) The viscosity of the diluate at a shear rate of 110s-1
is measured.
21~4~69
WO 95/27771 PCT/EP95/01085
g _
c) The diluate is warmed to 60°C and held at this
temperature for 1 day.
d) The diluate is cooled to 20°C and the viscosity is once
again measured at a shear rate of 110s-1.
e) Comparison between the viscosities of b) and c) should
show that they differ by less 5 mPas.
It is preferable if the fabric softening compositions of the
invention conforms to the following test:
a) The fabric softening composition is diluted as for Test
I.
b) The viscosity of the diluate at a shear rate of 110s-1
is measured.
c) The diluate is frozen and thawed.
d) The viscosity is once again measured at a shear rate of
110s-1.
e) Comparison between the viscosities of b) and c) should
show that they differ by less than 10 mPaS.
The fabric softening compositions according to the invention
may be translucent. Translucent in the context of this
invention means that when a cell lcm in depth is filled with
the fabric softening composition, "Courier 12 point" typeface
can be read through the cell.
A further advantage of the present invention is that the
softening of the composition is enhanced over compositions of
the prior art comprising similar levels of fabric softening
compound.
T_T _ _ __ ._._._ .... _
WO 95/27771 ~ ~ ~ ~, ~ ~~ ~ PCT/EP95/01085
_ g
The present invention has the advantage that high levels of
perfume can be tolerated without adversely effecting the
stability of the product.
The Fabric Softening Compound
The fabric softening compound is suitably a water insoluble
quaternary ammonium material comprising a single alkyl or
alkenyl chain length equal to or greater than Czo or, more
preferably, the softening compound comprising a polar head
group and two alkyl or alkenyl chains each having an average
chain length equal to or greater than C12 such as a quaternary
ammonium material having two Cla-22 alkyl or alkenyl groups
connected to the quaternary ammonium head group via at least
one ester link.
Preferably the fabric softening compound of the invention has
two long chain alkyl or alkenyl chains with an average chain
length equal to or greater than C,q. More preferably each
chain has an average chain length equal or greater than'Cls~
Most preferably at least 50~ of each long chain alkyl or
alkenyl group has a chain length of C18.
It is preferred if the long chain alkyl or alkenyl groups of
the fabric softening compound are predominantly linear.
The fabric softening compounds used in the compositions of
the invention are molecules which provide excellent
softening, characterised by chain melting -L~ to La -
transition temperature greater than 25°C, preferably greater
than 35°C, most preferably greater than 45°C. This L~ to La
transition can be measured by DSC as defined in "Handbook of
Lipid Bilayers, D Marsh, CRC Press, Boca Raton Florida, 1990
(Pages 137 and 337).
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WO 95/27771 PCT/EP95/01085
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Substantially insoluble fabric softening compounds in the
context of this invention are defined as fabric softening
compounds having a solubility less than 1 x 10-3wt~ in
demineralised water at 20°C. Preferably the fabric softening
compounds have a solubility less than 1 x 10-' Most
preferably the fabric softening compounds have a solubility
at 20°C in demineralised water from 1 x 10-8 to 1 x 10-6~
Preferred fabric softening compounds are quaternary ammonium
compounds.
It is especially preferred if the fabric softening compound
is a water insoluble quaternary ammonium material which
comprises a compound having two C1z_le alkyl or alkenyl groups
connected to the molecule via at least one an ester link. It
is more preferred if the quaternary ammonium material has two
ester links present. The especially preferred ester-linked
quaternary ammonium material for use in the invention can be
represented by the formula:
Ri
2 5 R1 N' ( CHz ) ~-T-R2
35
CHz ) n-T-R2
wherein each R1 group is independently selected from C1_4
alkyl, hydroxyalkyl or C2_Qalkenyl groups; and wherein each
R2 group is independently selected from C8_28 alkyl or alkenyl
groups;
O O
T is -O-C- or -C-O-; and
n is an integer from 0-5.
_..__.______..r.,r _ _...._n~__.__...
v 218409
WO 95/27771 PCT/EP95/01085
- 11 -
Di(tallowyloxyethyl)dimethyl ammonium chloride, available
from Hoechst, is especially preferred.
A second preferred type of quaternary ammonium material can
be represented by the formula:
OOCRZ
( R' ) 3N' - ( CHZ ) n CH
CHzOOCR2
wherein R1, n and Rz are as defined above.
It is advantageous for environmental reasons if the
quaternary ammonium material is biologically degradable.
Preferred materials of this class such as 1,2 bis[hardened
tallowoyloxy]-3- trimethylammonium propane chloride and their
method of preparation are, for example, described in
US 4 137 180 (Lever Brothers). Preferably these materials
comprise small amounts of the corresponding monoester as
described in US 4 137 180 for example 1-hardened tallowoyloxy
-2-hydroxy -3-trimethylammonium propane chloride.
The solubilising agent is an amphoteric surfactant, and is
characterised in terms of its phase behaviour. Suitable
solubilising agents are amphoteric surfactants for which,
when contacted within water, the first lyotropic liquid
crystalline phase formed is normal cubic (I1) or normal
cubic-bicontinuous (V1) or hexagonal (H1) or nematic (Nel),
or intermediate (Intl) phase as defined in the article by G J
T Tiddy et al, J Chem Soc. Faraday Trans. 1., 79, 975, 1983
and G J T Tiddy , "Modern Trends of Colloid Science in
~1~~G~9
WO 95/27771 PCT/EP95/01085
- 12 -
Chemistry and Biology", Ed. H-F Eicke, 1985 Birkhauser Verlag
Basel). Surfactants forming La phases at concentrations of
less than 20 wt~ are not suitable.
In the context of this invention amphoteric surfactants are
defined as substances with molecular structures consisting
of a hydrophilic and hydrophobic part. The hydrophobic part
consists of a hydrocarbon and the hydrophilic part consists
of both a positive and a negative group. Preferred
amphoteric surfactants include amine oxides, betaines
including sulphobetaines and tegobetaines, phosphine oxides
and sulphoxides.
Mixtures of solubilising agents may be used.
For compositions in solid form, especially powder, the
solubilising is desirably solid at room temperature as this
provides crisp composition particles.
It is particularly advantageous if the solubilising agent
further comprises a non-surfactant co-solubiliser. Preferred
co-solubilisers include propylene glycol, urea , acid amides
up to and including chain lengths of C6, citric acid and other
poly carboxylic acids as disclosed in EP 0 404 471
(Unilever), glycerol, sorbitol and sucrose. Particularly
preferred are polyethylene glycols (PEG) having a molecular
weight ranging from 200 - 6000, most preferably from 1000 to
2000.
It is preferred if the ratio of co-solubiliser to amphoteric
surfactant is from to 2:1 to 1:40. Preferably the ratio of
co-solubiliser to nonionic surfactant is less than 1:1, more
preferably 1:5.
_._~._.~_.. __..._. _ _.____.w~.._._~_._..
--rr
WO 95/27771 O ~ ~ PCT/EP95101085
- 13 -
It is advantageous if the weight ratio of solubilising agent
twhere relevant this would also include the co-solvent) to
fabric softening compound is greater than 1:6, preferably
greater than 1:4, more preferably equal to or greater than
2:3. It is advantageous if the ratio of solubilising agent to
fabric softening compound is equal to or below 4:1, more
preferably below 3:2.
It is beneficial if the solubilising agent/ co-solubiliser is
present at a level greater than 5 wt~ of the total
composition, preferably at a level greater than 10 wt~.
The solubilising agent/ co-solubiliser may be present at a
level greater than 20 wt~ of the total composition, or even
at a level greater than 30 wt%. Such higher levels are
especially preferred where the fabric softening composition
is a solid.
The compositions of the invention preferably have a pH of
more than 1.5, more preferably less than 5.
The composition can also contain fatty acids, for example
Ce - C24 alkyl or alkenyl monocarboxylic acids, or polymeric
carboxylic acids. Preferably saturated fatty acids are used,
in particular, hardened tallow C16-C18 fatty acids.
The level of fatty acid material is preferably more than 0.1%
by weight, more preferably more than 0.2~ by weight.
Especially preferred are concentrates comprising from 0.5 to
20~ by weight of fatty acid, more preferably 1~ to 10~ by
WO 95/27771 ~ rj 6 ~ PCT/EP95/01085
- 14 -
weight. The weight ratio of fabric softening compound to
fatty acid material is preferably from 10:1 to 1:10.
Compositions according to the present invention may contain
detergency builders and/or anionic surfactants as desired.
However it is especially preferred that the composition is
substantially free of builders. It is also preferred that
the composition be substantially free of anionic surfactant.
Suitably the composition is substantially free of nonionic
hydrophobic organic materials such as hydrocarbons and
hydrocarbyl esters of fatty acids.
The composition can also contain one or more optional
ingredients, selected from non-aqueous solvents, pH buffering
agents, perfumes, perfume carriers, fluorescers, colorants,
hydrotropes, antifoaming agents, antiredeposition agents,
polymeric or other thickeners, enzymes, optical brightening
agents, opacifiers, anti-shrinking agents, anti-wrinkle
agents, anti-spotting agents, germicides, fungicides, anti-
oxidants, anti-corrosion agents, drape imparting agents,
antistatic agents and ironing aids.
The product may be in any product form. Particularly
preferred forms are liquid and solid compositions and
compositions suitable for coating onto a dryer sheet. Solid
composition in this context includes compositions in the form
of a tablet, a gel, a paste and preferably granules or a
powder.
The composition may be used in a tumble drier but is
preferred for use in a washing machine for example by
dispensing the composition via a drawer of a washing machine
T--T-- _
2i8~~69
WO 95/27771 PCT/EP95/01085
- 15 -
optionally with dilution prior to dosing into the dispensing
drawer.
The invention further provides a process for preparing a
rinse conditioner, as described above, which comprises the
steps of:
i) mixing the substantially water insoluble fabric
softening compound and the solubilising agent,
preferably by co-melting;
ii) adding the resulting mixture to conventional
ingredients for example, water.
Alternatively the composition may be prepared by the
independent addition of the water insoluble fabric softening
compound and the solubilising agent to conventional
ingredients.
Compositions in solid form may be prepared by spray drying,
freeze drying, milling, extraction, cryogenic grinding or any
other suitable means.
The invention will now be illustrated by the following non-
limiting examples. In the examples all percentages are
expressed by weight.
Comparative Examples are designated by letters, while
Examples of the invention are designated by numbers.
WO 95/27771 ~ ~ ~ ~ PCT/EP95/01085
- 16 -
The following examples were prepared by one of the following
methods:
1) co-melting the fabric softening compound in the
solubilising agent and adding the resulting dispersion in the
required amount of hot water.
2) Sequentially adding the fabric softening compound and the
solubilising agent to hot water.
In the comparative cases where there is no solubilising agent
present the cationic is dispersed in hot water (liquid
compositions).
In the Examples:
HT TMAPC = 1,2 bis[hardened tallowoyloxy]-3-
trimethylammonium propane chloride
DEQA = di(tallowyloxyethyl)dimethyl ammonium chloride
,
Softening performance was evaluated by adding 0.1g of fabric
softening compound (2m1 of a 5o a.d. dispersion) for liquids
to 1 litre of tap water, 10°FH, at ambient temperature
containing 0.001 (w/w) sodium alkyl benzene sulphonate (ABS)
in a tergotometer. The ABS was added to simulate carryover
of anionic detergent from the main wash. Three pieces of
terry towelling (8cm x 8cm, 40g total weight) were added to
the tergotometer pot. The cloths were treated for 5 minutes
at 65 rpm, spin dried to remove excess liquor and line dried
overnight.
Softening of the fabrics was assessed by an expert panel of 4
people using a round robin paired comparison test protocol.
_ _._.__..._.~._.. __..~._ _. w_.... _... ~_. _ . .
2784~~9
WO 95/27771 PCT/EP95/01085
- 17 -
Each panel member assessed four sets of test cloths. Each
set of test cloths contained one cloth of each test system
under a evaluation. Panel members were asked to assess
softness on a 8 point scale. Softness scores were calculated
using an "Analysis of Variance" technique. Lower values are
indicative of better softening.
The following examples were made according to either of the
standard methods.
Example
wt (g)
Ingredient 1 2 3
HT TMAPC 1.2 1.2 0.9
C10 Sulphobetaine 0.3 - -
C14 Sulphobetaine - 0.3 0.6
Water 8.5 8.5 8.5
The Examples dispersed and dispensed well.
Examples 4 to 7 and A and B
Compositions having a range of fabric softening compound to
solubilising agent ratios were prepared according to the
either of the methods described above in Preparation of
Examples. The softening performance was determined.
Z~g4069
WO 95127771 PCT/EP95101085
- 18 -
Softening Results
HT TMAPC:*L5351 Softness Score
(wt ratio)
A 5:0 2.5
4 4:1 2.75
5 3:2 3.0
6 2:3 3.25
7 1:4 5.5
B 0:5 7.25
* Fatty acid amido alkyl betaine ex Th Goldschmidt.
Compositions 4 to 7 all exhibited good softening performance
and good stability. Composition A set under a freeze/thaw
test as described under Test III above.
The compositions were prepared by either one of the methods
described for Preparation of Examples.
T r. ___....._....__.
2184~~9
WO 95/27771 PCT/EP95/01085
- 19 -
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218069
WO 95/27771 PCT/EP95/01085
- 20 -
The storage stability of compositions 8 to 14 was determined
by storing the compositions under a variety of conditions
including a freeze/thaw regime and measuring the viscosity
thereof using a Carri-med rheometer at a shear rate of
110 sec-1. The results are shown below.
The comparative compositions all set or the components
separated illustrating poor stability.
_..___~.T..~. _~~.__...~ _...~__. _ .
2184069
WO 95/27771 PCT/EP95/01085
- 21 -
lf1 01 01 01 N 00 N
l0 I~ ri 01 lf1
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WO 95/27771 ~ ~ PCT/EP95/01085
- 22 -
The compositions according to the invention all exhibited
acceptable storage stability and did not set under the
freeze/thaw regime.
Compositions were analysed in accordance with Test 1
described above and were filtered by being consecutively
passed through filters of pore sizes 1 um, 0.45 um and 0.2 um
to achieve separation. The cationic material remaining was
measured by standard titration.
Nonionic used o Cationic remaining
0.2um filter
8 85
9 90
10 97.1
11 94.9
12 86.3
13 84.6
14 94.1
C 50
D 56
E 16
F Too viscous to filter
T._~ .__..._.. _....... .,. _-
WO 95!27771 ~ ~ ~ ~' 0 6 9 pCT~P95101085
- 23 -
The compositions were analysed under Tests II and III
described above. The viscosities were measured on a
Carri-med rheometer at shear rate of 110 sec-1.
Product Initial Test II Test III
Viscosity/ mPas 24 hrs @ F/Thaw / mPas
60C / mPas
8 3.2 3.4 3.8
9 6.8 4.1 2.7
2.7 1.9 2.8
10 11 2.6 2.0 1.8
12 2.0 4.2 3.5
13 2.6 2.5 2.1
14 1.8 1.7 2.3
C 7.4 Separated
D Separated Separated
E 57 95
F 111 Separated
The softening effect of compositions was determined. The
results are shown below using a 5~ solution of fabric
softening compound and solubilising agent (ratio 3:2)..
L Sample ~ Softness Std.
5~ HEQ 5:0 3.0
10 2.75
13 3.75
