Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.
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Detergent Composition Comprising Zeolite and Amylase Enzyme
The present invention relates to a detergent composition comprising an
amylase enzyme and a small particle size zeolite component as a
sequestering agent for water hardness.
Conventionally, water soluble inorganic phosphates, such as sodium
tripolyphosphate, have been used as builders for laundry detergents.
More recently, alkali metal aluminosilicate ion-exchangers, particularly
crystalline water insoluble sodium aluminosilicate zeolites, have been
proposed as replacements for the inorganic phosphates.
For example, EP 21 491A (Procter & Gamble) discloses detergent
compositions containing a builder system which includes zeolite A, X
or P(B) or a mixture thereof. EP 384070A (Unilever) discloses
specific zeolite P materials having, an especially low silicon to
aluminium ratio not greater than 1.33 (hereinafter referred to as zeolite
MAP) and describes their use as detergency builders.
The Applicants have now surprisingly found that a problem may occur
when a water insoluble zeolite having a small particle size, is used as a
detergency builder in a composition formulated for use in the
laundering of fabrics. The problem has been found to be particularly
pronounced when the zeolite is zeolite MAP.
The choice of a small particle size for a zeolite MAP component, that
is to say particles having a particle size, measured as a d50 value, of up
to 1.0 micrometres has previously been taught to be preferred in the art,
as represented, for example, by EP 384070 A.
The problem relates to the formation of white residues, which adhere to the
fabrics and remain thereon at the end of a laundry washing process. The
degree of residue formation may vary. On coloured fabrics the appearance
of the white residues tends to be visually more apparent than on white
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fabrics. White residues frequently folm on areas of fabric where there is a
stain present, interfering with and preventing the complete removal of the
stain. As a result of the visible contrast between the white residues and the
coloured fabric, the stained area on which white deposits have formed may
be more noticeable that the original stain.
It has been established that when an amylase enzyme is employed in
compostions containing zeolite in small particle size form that the problem
of the white residue formation on the fabrics is reduced.
Whilst the prior art, as represented for example by European Patent
Aplications, EP 384070 A, EP 448297 A, EP 522726 A, EP 533392 A, EP
544492 A, EP 552053 A, and EP 552054 A has envisaged the use of
enzymes in combination with small particle size zeolite MAP in laundry
detergent compositions, none of these prior art documents specifically
disclose the use of arnylase enzyme with a small particle size zeolite MAP
component. Furthermore, none of these prior art documents provides any
-teaching relating to the white residue deposit problem addressed by the
current invention, nor of any solution thereto involving the selection of a
particular enzyme.
According to the present invention there is provided a detergent composition
containing
(a) a zeolite builder having a particle size, expressed as a d50 value, of
less than 1.0 micrometres;
(b) an amylase enzyme;
In a preferred aspect the zeolite builder comprises zeolite P having a silicon
to aluminium ratio of not greater than 1.33 (zeolite MAP)
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Detailed description of the invention
Zeolite builder
The first essential component of the present invention is an
aluminosilicate zeolite builder, optionally in conjunction with one or
more supplementary builders.
The zeolite builder is typically present at a level of from 1% to 80%,
more preferably from 15% to 40% by weight of the compositions.
In an essential aspect the zeolite detergent builder has a particle size,
expressed as a d50 value of less than 1.0 micrometres, more preferably
from 0.05 to 0.9 micrometres, most preferably from 0.2 to 0.7
micrometres.
The d50 value indicates that 50% by weight of the particles have a
diameter smaller than that figure. The particle size may, in particular be
determined by conventional analytical techniques such as microscopic
determination using a scanning electron microscope or by means of a
laser granulometer.
Suitable aluminosilicate zeolites have the unit cell formula
Naz[(AlO2)z(SiO2)y]. XH2O wherein z and y are at least 6; the molar ratio
of z to y is from 1.0 to 0.5 and x is at least 5, preferably from 7.5 to 276,
more preferably from 10 to 264. The aluminosilicate material are in
hydrated form and are preferably crystalline, containing from 10% to 28%,
more preferably from 18% to 22% water in bound form.
The aluminosilicate zeolites can be naturally occurring materials, but are
preferably synthetically derived. Synthetic crystalline aluminosilicate ion
exchange materials are available under the designations Zeolite A, Zeolite B,
' Zeolite P, Zeolite X, Zeolite MAP, Zeolite HS and mixtures thereof.
Zeolite A has the formula
Na 12 IA102) 12 (Si02)121= xH2O
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wherein x is from 20 to 30, especially 27. Zeolite X has the formula Na86
I(A102)86(Si02)1061= 276 H20.
Zeolite MAP is described in EP 384070A (Unilever). It is defined as
an alkali metal alumino-silicate of the zeolite P type having a silicon to
aluminium ratio not greater than 1.33, preferably within the range from
0.9 to 1.33 and more preferably within the range of from 0.9 to 1.2.
Of particular interest is zeolite MAP having a silicon to aluminium ratio
not greater than 1.15 and, more particularly, not greater than 1.07.
Zeolite P having a Si:Al ratio of 1.33 or less may be prepared by the
following steps:
(i) mixing together a sodium aluminate having a mole ratio
Na20:A1203 within the range of from 1.4 to 2.0 and a
sodium silicate having a mole ratio Si02:Na20 within
the range of from 0.8 to 3.4 with vigorous stirring at a
temperature within the range of from 25 C to boiling
point usually 95 C, to give a gel having the following
composition; A1203: (1.75-3.5) Si02 : (2.3-7.5) Na20 :P
(80-450)H20;
(ii) ageing the gel composition for 0.5 to 10 hours,
preferably 2 to 5 hours, at a temperature within the range
of from 70 C to boiling point, usually to 95 C, with
sufficient stirring to maintain any solids present in
suspension;
(iii) separating the crystalline sodium aluminosilicate thus
formed, washing to a pH within the range of from 10 to
12.5, and drying, preferably at a temperature not
exceeding 150 C, to a moisture content of not less than 5
wt.%.
Preferred drying methods are spray-drying and flash drying. It appears
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that oven drying at too high a temperature may adversely affect the
calcium binding capacity of the product under certain circumstances.
Commercial sodium metasilicate pentahydrate dissolved in water and
commercial sodium silicate solution (waterglass) are both suitable
silica sources for the production of zeolite P in accordance with the
invention. The reactants may be added together in any order either
rapidly or slowly. Rapid addition at ambient temperature, and slow
addition at elevated temperature (90-95 C) both give the desired
product.
Vigorous stirring of the gel during the addition of the reactants, and at
least moderate stirring during the subsequent ageing step, however,
appear to be essential for the formation of pure zeolite P. In the
absence of stirring, various mixtures of crystalline and amorphous
materials may be obtained.
Zeolite MAP generally has a calcium binding capacity of at least 150
mg CaO per g of anhydrous aluminosilcate, as measured by the
standard method described in GB 1473201 (Henkel). The calcium
binding capacity is normally 160 mg CaO/g and may be as high 170 mg
CaO/g.
Although zeolite MAP like other zeolites contains water of hydration,
for the purposes of the present invention amounts and percentages of
zeolite are expressed in terms of the notional anhydrous material.
The amount of water present in hydrated zeolite MAP at ambient
temperature and humidity is generally about 20 wt.%.
Amylase
" The second essential component of the compositions is an amylase enzyme,
that is to say an enzyme having amylolytic activity.
The amylase enzyme is typically incorporated into the compositions in
accordance with the invention at a level of from 0.01 % to 5%, preferably
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from 0.1% to 3%, more preferably from 0.2% to 2%, most preferably from
0.3% to 1.5% active enzyme by weight of the composition, on a 60KNU/g
(Kilo Novo Units/gram) activity basis.
The units of Kilo Novo Units/gram (KNU/g)' are a well known means of
defining arnylolytic enzyme activity and are described in GB-1,269,839 A
(Novo). In more detail, 1 KNU is the amount of enzyme which breaks down
5.25 grams of starch (Merck, Amylum Solubile Erg. B.6, Batch 9947275)
per hour in the method described in GB-1,269,839 A, which has the
following standard conditions:
Substrate Soluble starch
Calcium content in solvent 0.0043 M
Reaction time 7-20 minutes
Temperature 37 C
pH 5.6
The amylase enzyme may be fungal or bacterial in origin. Amylases
obtained by chemical or genetic manipulation of finngal or bacterial derived
strains are also useful herein. The amylase enzyme is preferably an ac-
amylase.
Preferred amylases include, for example, ac-amylases obtained from a
special strain of B. licheniformis, described in more detail in GB-1,269,839
A. Reported deposit numbers for B. licheniformis strains capable of
producing a-amylases include NCIB 8061, NCIB 8059, ATCC 6634,
ATCC 6598, ATCC 11945, ATCC 8480 and ATCC 9945a.
Preferred commercially available a-amylases include for example, those
sold under the trademarksRapidase and Maxamyl by Gist-Brocades; those
sold under the -trademark Taka Therm L-340 by Miles Laboratories,
Elkhart, Indiana; those sold under the trademark Rohalase AT by Rohm and
Haas, West Philadelphia, PA; and those sold under the trademarks
Termamyl 60T and 120T, Fungamyl and BAN by Novo Industries A/S.
In a preferred aspect, the amylases have been designed to have improved
stability, particularly having improved stability to oxidation, for example in
a
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bleaching environment, and improved thermal stability. Stability can be
measured using any of the technical tests known in the art including those
referred to in WO 94/02597 A. Stability-enhanced ainylases are
commercially available from Novo Industries A/S or from Genencor
International.
Highly preferred amylases with enhanced oxidative stability are derived
using site-directed mutagenesis from one or more of the Bacillus amylases,
especialy the Bacillus a-amylases, regardless of whether one, two or
multiple amylase strains are the immediate precursors. Preferred amylases of
this type are described in WO 94/02597 A, and comprise a mutant in which
substitution is made, using alanine or threonine, preferably threonine, of the
methionine residue located in position 197 of the B. licheniformis a-
amylase, sold under the trademark Termamyl, or the homologous position
variation of a similar parent amylase, such as B. amyloliquefaciens,
B.subtilis, or B.stearothermQphilus.
Other preferred amylases having enhanced oxidative stability, derived from
B.licheniformis NCIB806, are described by Genencor International in a
paper entitled "Oxidatively Resistant a-Amylases" which was presented at
the 207th American Chemical Society National Meeting, March 13-17 1994,
by C. Mitchinson. Methionine (Met) was identified as the most likely
residue to be modified. Met was substituted, one at a time, in positions 8,
15, 197, 256, 304, 366 and 438 leading to specific mutants, particularly
important being M197L and M197T with the M197T variant being the most
stable expressed variant.
Other preferred amylases having enhanced oxidative stability include those
descn'be.d in WO 94/18314 A (Genencor International) and WO 94/02597 A
(Novo). Any other oxidative stability-enhanced amylase can be used, for
example as derived by site-directed mutagenesis from lmown chimeric,
hybrid or simple mutant parent forms of available amylases. Other enzyme
modifications are acceptable including those described in WO 95/09909 A
(Novo).
It will be appreciated that enzymes for incorporation into solid detergent
compositions are generally sold commercially as enzyme prills containing
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active enzyme supported on a variety of inert host materials, which for
example, can include alkali metal sulfates, carbonates and silicates.
Optionally, organic binder materials are also incorporated. In a preferred
aspect, the calcium content of these enzyme prilis is 1rLnimzed to ensure
good in-product storage stability of the enzyme.
Additional detergent components
The detergent composition according to the invention may contain
other detergent components such as surfactants, cobuilders, bleaches,
fluorescers, antiredeposition agents, inorganic salts such as sodium
sulphate, other enzymes, lather control agents, fabric softening agents,
pigments, coloured speckles and perfumes.
Surfactant
The detergent composition according to the invention preferably
includes a surfactant selected from anionics, nonionics, zwitterionics,
ampholytics and cationics.
The surfactant is preferably present in the detergent compositions at a level
of from 1% to 50%, preferably from 3% to 30%, most preferably from 5%
to 20% by weight of the compositions.
Many suitable detergent-active compounds are available and fiilly
described in the literature (for example "Surface Active Agents and
Detergents" Volumes I and II by Schwartz, Perry and Berch).
Examples of suitable additional anionic surfactants include anionic
sulfates, olefin sulphonates, alkyl xylene sulphonates,
dialkylsuiphosuccinates, and fatty acid ester sulphonates. Sodium salts
are generally preferred.
Anionic sulfate surfactant
Anionic sulfate surfactants suitable for use herein include the linear and
branched primary alkyl sulfates, alkyl ethoxysulfates, fatty oleoyl glycerol
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sulfates, alkyl phenol ethylene oxide ether sulfates, the C5-C 17 acyl-N-(C 1-
C4 alkyl) and -N-(C 1-C2 hydroxyalkyl) glucamine sulfates, and sulfates of
alkylpolysaccharides such as the sulfates of alkylpolyglucoside (the nonionic
nonsulfated compounds being described herein).
Alkyl ethoxysulfate surfactants are preferably selected from the group
consisting of the C6-C18 alkyl sulfates which have been ethoxylated with
from 0.5 to 20 moles of ethylene oxide per molecule. More preferably, the
allcyl ethoxysulfate surfactant is a C6-C 18 alkyl sulfate which has been
ethoxylated with from 0.5 to 20, preferably from 0.5 to 5, moles of ethylene
oxide per molecule.
Anionic sulfonate surfactant
Anionic sulfonate surfactants suitable for use herein include the salts of C5-
C20 linear alkylbenzene sulfonates, alkyl ester sulfonates, C6-C22 primary
or secondary alkane sulfonates, C6-C24 olefin sulfonates, sulfonated
polycarboxylic acids, alkyl glycerol sulfonates, fatty acyl glycerol
sulfonates, fatty oleyl glycerol sulfonates, and any mixtures thereof.
Nonionic surfactant
The nonionic surfactant is preferably a hydrophobic nonionic
surfactant, paiticularly an alkoxylated nonionic surfactant, having a
hydrophilic lipophilic balance (hlb) value of < 9.5, more preferably
< 10.5.
Examples of suitable hydrophobic alkoxylated nonionic surfactants
include alkoxylated adducts of fatty alcohols containing an average of
less than 5 alkylene oxide groups per molecule.
The alkylene oxide residues may, for example, be ethylene oxide
" residues or mixtures thereof with propylene oxide residues.
Preferred alkylene oxide adducts of fatty alcohols useful in the present
invention can suitably be chosen from those of the general formula:
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R-O-(CnH2n0)YH
wherein R is an alkyl or alkenyl group having at least 10 carbon atoms,
most preferably from 10 to 22 carbon atoms, y is from 0.5 to 3.5 and n
is 2 or 3.
Preferred nonionic surfactants include primaty C 11-C 15 aliphatic
alcohols condensed with an average of no more than five ethylene
oxide groups per mole of alcohol, having an ethylene oxide content of
less than 50% by weight, preferably from 25% to less than 50% by
weight.
A particularly preferred aliphatic alcohol ethoxylated is a primary
alcohol having an average of 12 to 15 carbon atoms in the alkyl chain
condensed with an average of three ethoxy groups per mole of alcohol.
Specific examples of suitable alkoxylated adducts of fatty alcohols are
Trd
Synperonic A3 (ex ICI), which is a C13-C15 alcohol with about three
ethylene oxide groups per molecule and Empilan KB3 (ex Marchon),
which is lauric alcoho13E0.
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Another class of nonionic sufactants comprises alkyl polyglucoside
compounds of general formula
RO(CnH2nO)tZx
wherein Z is a moiety derived from glucose; R is a saturated
hydrophobic allcyl group that contains from 12 to 18 carbon atoms; t is
from 0 to 10 and n is 2 or 3; x is from 1.1 to 4, the compounds
including less than 10% unreacted fatty alcohol and less than 50%
short chain alkyl polyglucosides. Compounds of this type and their use
in detergent compositions are disclosed in EP-B 0070074, 0070077,
0075996 and 0094118.
Cobuilders
In addition to zeolite MAP, the builder system may contain an organic
or inorganic cobuilder.
Suitable organic cobuilders can be monomeric or polymeric
carboxylates such as citrates or polymers of acrylic, methacrylic and/or
maleic acids in neutralised form. Suitable inorganic cobuilders include
carbonates and amorphous and crystalline layered silicates.
Suitable crystalline layered silicates have the composition:
NaMSixO2x+l . yH2O
where M is sodium or hydrogen, preferably sodium; x is a number from
1.9 to 4; and y is a number from 0 to 20. Such materials are described
in US Patents No. 4664839; No. 4728443 and No. 4820439 (Hoechst
AG). Especially preferred are compounds in which x = 2 and y = O.
The synthetic material is commercially available from Hoechst AG as S
-Na2 Si205 (SKS6) and is described in US Patent No. 4664830.
The total amount of detergency builder in the granular composition
typically ranges from 10 to 80 wt.%, more preferably from 15 to 60
wt% and most preferably from 10 to 45 wt.%.
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Bleach
Detergent compositions according to the invention may also suitably
contain a bleach system. This preferably comprises one or more
peroxy bleach compounds, for example, inorganic persalts or organic
peroxyacids, which may be employed in conjunction with bleach
precursors to improve bleaching action at low temperatures.
The bleach system preferably comprises a peroxy bleach compound,
preferably an inorganic persalt, optionally in conjunction with a
peroxyacid bleach precursor. Suitable persalts include sodium
perborate monohydrate and tetrahydrate and sodium percarbonate, with
sodium percarbonate being most preferred.
Preferred bleach precursors are peracetic acid precursors, such as
tetraacetylethylene diamine (TAED); peroxybenzoic acid precursors.
Physical form
The detergent composition according to the invention may be of any
physical type, for example powders, liquids and gels. However,
granular and liquid compositions are preferred.
MakingUrocess
The detergent compositions of the invention may be prepared by any
suitable method. The particulate detergent compositions are suitably
prepared by any tower (spray-drying) or non-tower process.
In processes based around a spray-drying tower, a base powder is first
prepared by spray-drying a slurry and then other components
unsuitable for processing via the slurry can be sprayed on or admixed
(postdosed).
The zeolite builder is suitable for inclusion in the slurry, although it
may be advantageous for processing reasons for part of the zeolite
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builder to be incorporated post-tower. The crystalline layered silicate,
where this is employed, is also incorporated via a non-tower process
and is preferably postdosed.
Altematively, particulate detergent compositions in accordance with
the invention may be prepared by wholly non-tower processes such as
granulation.
The granular detergent compositions of the invention may be prepared
to any suitable bulk density. The compositions preferably have a bulk
density of at least 400 g/l preferably at least 550 g/l, most preferably at
least 700 g/l and, with particular preference at least 800 g/l.
The benefits of the present invention are particularly evident in
powders of high bulk density, for example, of 700 g/l or above. Such
powders may be prepared either by post-tower densification of spray-
dried powder, or by wholly non-tower methods such as dry mixing and
granulation; in both cases a high-speed mixer/granulator may
advantageously be used. Processes using high-speed mixer/granulators
are disclosed, for example, in EP340 013A, EP 367 339A, EP 390
251A and EP 420 317A (Unilever).
The detergent composition of the invention may be formulated as a
liquid detergent composition which may be aqueous or anhydrous. The
term "liquid" used herein includes pasty viscous formulations such as
gels. The liquid detergent composition generally has a pH of from 6.5
to 10.5.
The total amount of detergency builder in the liquid composition is
preferably from 5 to 70% of the total liquid composition.
Illustrative compositions according to the present invention are
presented in the following Examples.
/
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zl,
In the detergent compositions, the abbreviated component identifications
have the following meanings:
LAS C 11-C 13 linear alkyl benzene sulfonate
45AS : Branched sodium alkyl sulfate surfactant
containing C 14-C 15 alkyl chains
246AS : Sodium a]kyl sulfate surfactant containing a alkyl
chain length weight distribution of 15% C12 alkyl
chains, 45% C14 alkyl chains, 35% C16 alkyl
chains, 5% C18 alkyl chains
TAS : Sodium alkyl sulfate surfactant containing
predominantly C 16 - C 18 alkyl chains derived
from tallow oil.
24AE3 S : C 12-C 14 alkyl ethoxysulfate containing an
average of three ethoxy groups per mole
35E3 : A C13-15 primary alcohol condensed with an
average of 3 moles of ethylene oxide
25E3 : A C 12-C 15 primary alcohol condensed with an
average of 3 moles of ethylene oxide
24EY : A C12-14 linear primary alcohol condensed with
an average of Y moles of ethylene oxide
Citrate : Sodium citrate
Carbonate : Anhydrous sodium carbonate
Perborate : Sodium perborate tetrahydrate
Percarbonate : Sodium percarbonate
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TAED Tetra acetyl ethylene diamine
Silicate : Amorphous Sodium Silicate (Si02:Na20 ratio
normally follows)
CMC Carboxymethylcellulose
Suds : 25% paraffin wax Mpt 50 C, 17%
Suppressor hydrophobic silica, 58% paraffin oil
Zeolite MAP : Hydrated sodium aluminosilicate zeolite MAP
having a silicon to aluminium ratio of 1.07 having
a particle size, expressed as a d50 value, of 0.5
micrometres
Zeolite A : Hydrated sodium aluminosilicate zeolite A having
a particle size, expressed as a d50 value, of 0.6
micrometres
MA/AA : Copolymer of 1:4 maleic/acrylic acid, average
molecular weight about 80,000.
Amylase : Amylolytic enzyme sold under the trademark
Termamyl 60T by Novo Industries A/S (60 KNiJ/
gram enzyme activity)
BSA : Amylolytic enzyme - M197T variant, having
enhanced oxidative stability (60 KNU/gram
enzyme activity)
Protease : Proteolytic enzyme sold by Novo Industries A/S
under the trademark Savinase of activity 4.0
KNPU/gram.
Lipase : Lipolytic enzyme sold by Novo Industries A/S
under the 'trademark Lipolase of activity 100,000
LU/gram
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Example 1
The following granular laundry detergent compositions were prepared (parts
by weight) in accordance with the invention. All amylase enzyme levels
relate to levels of active enzyme, expressed on a 60 KNU/g activity basis.
A B C D E
246AS 7.6 6.5 4.8 6.8 -
TAS - - - - 8.6
24AE3S 2.4 - 1.2 1.7 -
25E3 3.26 - - - 6.3
35E3 - 5.0 5.0 5.0 -
Zeolite MAP 20.0 25.0 20.0 - 16.0
Zeolite A - - - 25.0
15.0
Carbonate 15.0 15.0 20.0 10.0 12.0
MA/AA 4.25 4.25 4.25 4.25 2.0
Perborate - 16.0 - 16.0 20.0
Percarbonate 20.0 - 20.0 - -
TAED 5.0 5.0 5.0 5.0 6.7
Amylase 0.2 0.5 - 0.2 0.1
BSA - - 0.1 - -
Protease 0.04 0.08 - 0.05 0.05
Silicate (2.0 4.0 - - 4.0 3.0
ratio
Water and miscellaneous (Including suds suppressor, sodium sulphate,
perfume) to balance
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Example 2
The following granular laundry detergent compositions of density 850
gram/litre are prepared (parts by weight) in accordance with the invention.
All amylase levels relate to levels of active enzyme, expressed on a 60
KNU/g activity basis.
F G H I J
45AS 9.0 8.5 9.5 9.0 6.0
LAS - - - - 3.0
24E3 2.8 2.9 3.0 2.8 2.8
24E5 6.5 6.4 6.5 6.2 6.5
Zeolite MAP 32.0 35.0 25.0 - 16.0
Zeolite A - - - 30.0 15.0
Citrate 3.3 3.0 3.5 3.5 3.0
Carbonate 9.0 9.0 9.0 10.0 12.0
MA/AA - - - - 2.0
CMC 0.8 0.5 0.8 1.0 0.8
Perborate - - - - 16.0
Percarbonate 20.0 18.0 20.0 22.0 -
TAED 4.7 4.7 4.7 4.7 4.7
Amylase 0.1 0.3 - 0.5 0.2
BSA - - 0.4 - -
Protease 2.4 2.0 1.5 2.0 1.0
Lipase 0.35 0.35 0.4 0.3 0.2
Silicate (1.6 5.1 6.0 4.5 5.0 5.0
ratio)
Water and miscellaneous (Including suds suppressor, sodium sulphate,
perfume) to balance
