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Patent 2101651 Summary

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(12) Patent: (11) CA 2101651
(54) English Title: SURFACE CLEANING AGENT
(54) French Title: PRODUIT DE NETTOYAGE POUR SURFACE
Status: Expired and beyond the Period of Reversal
Bibliographic Data
(51) International Patent Classification (IPC):
  • C11D 01/72 (2006.01)
  • C11D 03/20 (2006.01)
(72) Inventors :
  • SAVINTSEVA, SOFIA ABDULOVNA (USSR)
  • KOLOSANOVA, VALENTINA ANDREEVNA (USSR)
  • OKHONSKAYA, JUZEFA NIKOLAEVNA (USSR)
  • BATISCHEVA, ELENA KONSTANTINOVNA (USSR)
  • SEKISOVA, IRINA MIKHAILOVNA (USSR)
  • KOLESNIKOVA, VERA SERGEEVNA (USSR)
  • SIDOROV, VALENTIN DMITRIEVICH (USSR)
  • TOCHILIN, VLADIMIR NIKOLAEVICH (USSR)
(73) Owners :
  • INSTITUT NEORGANICHESKOI KHIMII SIBIRSKOGO OTDELENIA ROSSIISKOI AKADEMII NAUK
(71) Applicants :
  • INSTITUT NEORGANICHESKOI KHIMII SIBIRSKOGO OTDELENIA ROSSIISKOI AKADEMII NAUK (Russian Federation)
(74) Agent: MARKS & CLERK
(74) Associate agent:
(45) Issued: 1999-01-19
(86) PCT Filing Date: 1991-11-29
(87) Open to Public Inspection: 1993-05-30
Examination requested: 1994-11-18
Availability of licence: N/A
Dedicated to the Public: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): Yes
(86) PCT Filing Number: PCT/SU1991/000255
(87) International Publication Number: SU1991000255
(85) National Entry: 1993-07-29

(30) Application Priority Data: None

Abstracts

English Abstract


An agent for cleaning surfaces comprises a surfactant,
an alkyl phenol, an alkali additive and water. As a
surfactant, it includes oxyethylated alkyl phenol and/or
oxyethylated fatty alcohol. The ratio of the components is
as follows, % by mass:
oxyethylated alkyl phenol and/or
oxyethylated fatty alcohol 0.1-3.0
alkyl phenol 0.005-0.003
alkali additive 0.2-0.5
water the balance.


French Abstract

Un moyen de nettoyage de surfaces comprend une substance tensio-active, un additif alcalin et de l'eau. Ladite substance tensio-active est caractérisée en ce qu'elle contient de l'alkylphénole oxyéthylé et/ou de l'alcool aliphatique oxyéthylé. Ledit moyen contient également de l'alkylphénole. Le rapport des constituants exprimés en pourcentage en poids est le suivant: alkylphénole oxyéthylé et/ou alcool aliphatique oxyéthylé 0,100 à 3,00, alkylphénole 0,005 à 0,003, additif alcalin 0,200 à 0,50, le reste étant constitué d'eau.

Claims

Note: Claims are shown in the official language in which they were submitted.


The embodiments of the invention in which an exclusive
property or privilege is claimed are defined as follows:
1. An agent for cleaning surfaces, including a
surfactant comprising an oxyethylated alkyl phenol and/or
an oxyethylated fatty alcohol, an alkyl phenol, an alkali
additive and water, the ratio of the components being as
follows, % by mass:
oxyethylated alkyl phenol and/or
oxyethylated fatty alcohol 0.1-3.0
alkyl phenol 0.005-0.03
alkali additive 0.2-0.5
water the balance
2. An agent according to Claim 1, which also
includes a hydrocarbon solvent in the amount of 0.5-55.0%
by mass of the general amount of the agent components.

Description

Note: Descriptions are shown in the official language in which they were submitted.


CA 021016~1 1998-04-08
-
SURFACE CLEANING AGENT
The present invention relates to the field of
detergents, and more particularly, to surface cleaning
agents.
The above agent can be widely used at machine-tool,
metallurgical, aircraft, radio engineering, transport,
repair and a number of other enterprises for cleaning
metal, glass, plastics, paint-and-varnish and ceramic
surfaces of carbon black and in-service fouling of
petroleum character, as well as of corrosion-preventive
lubricants, lubricant-coolants, metal and plastic chips.
Such an agent can also be used for cleaning of parts
between operations, cleaning of various surfaces of
production areas and equipment during repair and preventive
maintenance, cleaning of electric machines, various-purpose
electrical equipment of different overall dimensions, as
well as for washing overalls.
A number of requirements are imposed upon such agents
for cleaning surfaces. Along will a high detergent
ability, they must be fire- and explosion-proof, efficient
within a broad range of temperatures, non-toxic, must not
exert negative effect on the surface (cause corrosion,

CA 021016~1 1998-04-08
leave deposits, including those current-conducting), and be
convenient in mechanical and automatic cleaning. It is
also desirable that the agent be reusable and that
reclamation and utilization of it be possible.
Known in the art are various detergents. As a rule,
they contain surfactants and various additives, promoting
enhanced efficiency of detergent effect (wettability,
emulsification, solubilization, foam killing and
passivation of surface).
Thus, for example, known in the art is a detergent for
cleaning hard surfaces of fouling (SU, A, 290066). This
detergent consists of a surfactant and an alkali additive.
As a surfactant, use is made of alkyl benzene sulfonates
(C12-Cl8), and as an alkali additive - 25-50% by mass of
soda ash, 30-25% by mass of sodium tripolyphosphate and 10%
by mass of sodium silicates. Such a detergent efficiently
washes off surfaces to be cleaned; however, owing to a high
content of soda ash, it can exert aggressive effect on the
cleaned surface (it destroys the structure of paint-and-
varnish and insulating coatings), and causes corrosion of
metal surfaces. The presence of sodium tripolyphosphate in
great amounts creates a threat of dangerous ecological
consequences, since a high biological activity of
~ . ~

CA 021016~1 1998-04-08
phosphorus compounds exerts a destructive effect on flora
and fauna of water reservoirs.
Still another agent for cleaning surfaces of resin-
like fouling is known in the art (SU, A, 1325061). It
contains primary alkyl sulfates (C13-C16) or primary alkyl
sulfonates (C11-C17) as a surfactant, as well as calcium,
bentonite, sodium carbonate, zeolite and a perfume
additive. This agent is also sufficiently effective,
however, it can produce a negative effect on the surface
under washing, since it contains a great amount ~up to 80%
by mass) of abrasive (bentonite).
There exists an agent which is widely used in cleaning
equipment of in-service fouling (oil, carbon black) (DE, C,
3517458). It contains a nonionogenic surfactant, zeolite
and alkali additives: carbonate and bicarbonate of alkali
metals. This agent has a narrow field of application.
Thus, for example, when cleaning electric machines with
this agent, there is a possibility of depositing current-
conducting sediments on the surface of insulation coatings.
Sufficiently effective is an agent which represents an
aqueous zeolite suspension, stabilized with a mixture of
surfactants (oxyethylated fatty alcohol TAS and KOAS). The
agent also contains Na2O. However, in a number of cases
this agent cannot be used for cleaning windings of electric
~"~

CA 021016~1 1998-04-08
machines owing to the formation of a current-conducting
deposit (DE, A, 3330220). Besides, application of said
anionic surfactants requires the use of water with reduced
hardness and heating of the agent in the process of
cleanlng .
Known in the art is still another agent for cleaning a
metal surface of petroleum residues, which contains up to
15% by mass of surfactant: oxyethylated alkyl phenol or
fatty alcohol and sodium alkyl sulphonate and up to 94% by
mass of hydrocarbon solvent (SU, A, 541857). This agent
efficiently washes off resin-like, heavy fouling. Prior to
using this agent, it is recommended preliminarily to heat
it up to a temperature of 50-60~C. The surface to be
treated should also be heated up to this temperature. The
agent is kept on the surface for 10-15 minutes, and then
the surface is flushed with an aqueous solution of
tripolyphosphate (0.1-3.0% by mass) and oxyethylated alkyl
phenol (0.1-1.0% by mass), heated to a temperature of 60~C.
Presence of a great amount of solvent renders it
impossible to automate the cleaning process owing to an
elevated fire hazard. The necessity of preliminary heating
of a part to be cleaned and a high content of the
surfactant is economically unfavourable. A high content of
the hydrocarbon solvent is not desirable due to its
-- 4
~ ~.,.

CA 021016S1 1998-04-08
'',.._
toxicity and narcotic effect, especially in the process of
hand cleaning.
Thus, an agent for surface cleaning, meeting all the
requirements of a modern enterprise, is not known in the
art.
The invention is based on the problem to provide such
an agent for cleaning surfaces of different nature, which
would possess a sufficiently high detergency within a broad
range of temperatures, would be fire safe and non-toxic,
and that it would be possible to use manually or in a
mechanized way.
This problem is alleviated in that an agent is
provided including a surfactant (and as such contains
oxyethylated alkyl phenol and/or oxyethylated fatty
alcohol), an alkali additive and water, which, according to
the invention also contains alkyl phenols, with the
following ratio of components, % by mass:
- oxyethylated alkyl phenol and/or
- oxyethylated fatty alcohol 0.1-3.0
- alkyl phenol 0.005-0.03
- alkali additive 0.2-0.5
- water the balance.
As stated above, the agent for cleaning surfaces
includes a surfactant - oxyethylated alkyl phenol and/or

CA 021016~1 1998-04-08
oxyethylated fatty alcohol in the amount of 0.1-3.0~ by
mass. Each of these components can form part of the agent
individually or in any mixture of the selected components.
In the selected range of concentrations, in combination
with other components of the agent, these surfactants
possess good detergency. At a reduced concentration of the
surfactant below minimum level, the quality of cleaning in
the above-indicated range drops. Increase of the
surfactant content above 3.0% by mass is not expedient,
since in this case, at the increased consumption of the
component, the cleaning action of the agent becomes not
much more efficient. Besides, frothing is increased, which
complicates mechanized cleaning.
Alkyl phenol, introduced into the agent composition,
carries out a function of a codetergent. Even in small
amounts, alkyl phenols improve solubilization of washed off
fouling, which decreases a danger of a repeated fouling of
the surface. At a decrease and increase of concentrations,
indicated in the selected range, efficiency of the agent
action is reduced.
As an alkali additive, use can be made of traditional
additives for agents of this kind. For example, natural
A;~

CA 021016S1 1998-04-08
and synthetic zeolite3, sodium tripolyphosphate and sodium
silicate can serve as such additives.
- Alkali additives in the selected amount of 0.2-0.5% by
mass improve washing abilities of the surfactant, ensuring
a soft alkali effect of the agent.
Besides, the proposed combination of surfactants with
an alkali additive makes it possible to produce a
synergistic effect, ensures a high quality of cleaning,
without causing corrosion and destruction of the surface,
even that having a paint-and-varnish coating. Additives
can be used individually or in combination with each other.
In a number of cases, for example, in cleaning
surfaces of certain lubricants and oils, which undergo
changes at a high temperature and pressure, and of other
kinds of heavy fouling (mazout, viscous petroleum
fractions), it is recommended to add the agent for cleaning
surfaces with a hydrocarbon solvent in an amount of 0.5-
55.0% by mass of the general quantity of the agent
components. As a hydrocarbon solvent, it is possible to
use, for example, kerosene, white spirit, diesel fuel,
gasoline or gas condensate.
Presence of the hydrocarbon solvent in the agent
composition ensures efficient cleaning of the surface of
the above-indicated kinds of fouling.

CA 021016~1 1998-04-08
Availability in the agent composition of
simultaneously selected surfactants alkyl phenol and
hydrocarbon solvent in particular, ensures the formation of
a stable emulsion with a sufficiently high washing power.
In this case droplets of the hydrocarbon solvent are
distributed in water, which retards evaporation of the
solvent, owing to which fact fire hazard and toxicity of
the agent drop considerably.
The content of the hydrocarbon solvent in excess of
55.0% by mass of the general amount of the agent components
results in reducing the efficiency of action of the water-
soluble part of the agent, and raises its toxicity and fire
hazard.
The claimed agent for cleaning surfaces makes it
possible to clean surfaces with a sufficiently high degree
of cleanness. It can clean various metal, glass, polymeric
and ceramic surfaces with a sufficiently good effectiveness
of any kinds of fouling.
The agent is serviceable within a broad range of
temperatures (25-90~C). Its application leaves no
sediments on the cleaned surface, including those current-
conducting, which makes it possible to use this agent for,
e.g., cleaning the windings of electric machines.
-

CA 021016~1 1998-04-08
Preparation of the agent requires no scarce and
expensive raw materials and a great amount of solvent. The
use of the claimed agent requires no preliminary heating of
the agent and the surface to be cleaned.
The agent can be used for manual and machine cleaning
of surfaces.
The agent can be multiply reused.
The agent can be subjected to reclamation and used in
a closed-circuit system, which makes it possible to cut
down the consumption of components of the agent, water, and
to reduce the volume of industrial waste waters.
Oils washed off by means of the agent, in the process
of depreservation can be reused.
The method of producing the agent for cleaning
surfaces is technologically simple and is effected as
follows.
The agent components in the selected amount are
charged into a reservoir and thoroughly mixed until a
homogeneous emulsion is obtained.
In case a hydrocarbon solvent is used, it is charged
simultaneously with all the components.
The efficiency of the washing agent was determined as
follows. The gist of the method consists in evaluation of
residual fouling of the surface, washed off under definite
g _
,~
,~ ~

CA 021016~1 1998-04-08
technological conditions, of the preliminarily obtained
fouling.
As a model of fouling, use was made of an industrial
oil or mazout, which was applied onto the surface (metal,
glass, polymeric) of a plate in the amount of 1-102 g/cm2;
the plates were kept for 5 hours, then washed off by means
of an ultrasound unit during 5 minutes. The quantity of
fouling remaining on the plate is determined by a weighing
method. Cleaning is considered satisfactory, if the
residual fouling does not exceed 1-10-4 g/cm2.
For better understanding of the present invention,
given below are the following concrete examples.
Example 1:
The agent was prepared with the following ratio of
components, % by mass:
oxyethylated decyl phenol -0.1
nonyl phenol - 0.005
zeolite NaA - 0.5
water the balance.
The agent was prepared by way of mixing the components.
The mixture was thoroughly mixed until a homogeneous
emulsion was obtained. Efficiency of the effect of the
prepared compound was evaluated according to the method
described above. For this purpose, 10 standard glass
- 10 -
," .

CA 021016~1 1998-04-08
plates were preliminarily soiled with an industrial oil and
then cleaned with the prepared compound.
The averaged result of cleaning the surface at a
temperature of 25~C is 1-10-5 g/cm2, at a temperature of
40~C - 7.2-10-5 g/cm2, and at a temperature of 60~C -
6.0-10- g/cm .
Examples 2-4:
Examples 2-4 are given in Table 1, wherein given are
the compositions of the agent for cleaning the surface, the
temperature at which the agent is used, and the results of
cleaning the plates of industrial oil. The data are given
in comparison with the known agent.
.,, ~
~ '~.

CA 02101651 1998-04-08
,__
Table 1
Example Composition of Surface to Quantity of fouling
the agent for be washed remained, g/cm2, at
cleaning sur- off a temperature of
faces, % by ~.ass cleaning process, ~C
25 45 90
1 2 3 4 5 6
2 Ox~eth~lated decyl slcohol
O o5 cera- g,O.~o 5 8.0-10 5 7.0-10
mics
oxgetb~lated dodec~l
81C ohol _o.o5
isonon~l phe~ol -0.01
zeolite NaA -0.5
water - the balance
3 Qx~eth~lsted dodecgl
slcohol -0.5 tLta- 4 3~10-5 1.~-10 5
~lLUm
ox~ethylated
dacyl
phe~oL -0.5
isooct~1 phenol -0.03
zeolite NaA -0.3
wster - the balsnce
4 Ox~eth~Lated
alcobol -2.0 5.0-10 5 3.0~10 5 1~0-10 5
isodec~l phenol -0.0~ steel
zeolite clinop-
tilolite
lolite -0.2
water - the balance
~he ~nown sgent
Ox~ebh~lated fatty
alcohol -2.o
~AS -0.8 steel 1.0-10 4 8.2~10 5 1.0~10 5
EOAS -0.5
zeolite NaA -45.0
Na20 ~~ 35
water - the ba~gnce
- 12 -
,
a. ~

CA 021016~1 1998-04-08
As seen from Table 1, the proposed compositions ensure
an efficient cleaning of fouling within a broad range of
temperatures in comparison with the known agent, which is
efficient enough only at a temperature of 45~C and above.
In case of cleaning surfaces of heavy fouling (mazout,
lubricants), it is recommended to use a combination of the
two compositions of the agent, the first of which contains
a hydrocarbon solvent. The surface is cleaned in turn by
the first and second compositions.
Example 5:
The fouling model was mazout.
The first composition of the agent, % by mass:
oxyethylated decyl phenol 2.0
oxyethylated dodecyl phenol 1.0
isononyl phenol 0.03
diesel fuel 55.0
sodium tripolyphosphate 0.20
water the balance
After thoroughly mixing the agent components until a
homogeneous emulsion was obtained, a soiled cast-iron plate
was sunk therein, kept for 10-15 minutes, and then treated
with the second composition.
- 13 -

CA 02101651 1998-04-08
The second composition of the agent, % by mass:
oxyethylated ionyl phenol 0.20
isononyl phenol 0.01
sodium tripolyphosphate 0.20
sodium silicate 0.30
water the balance.
The averaged results of ten experiments show that the
quantity of fouling remained on the plate is 2.2-10-5 g/cm2.
Examples 6-9:
Examples are given in Table 2 , wherein shown are
compositions for cleaning, the nature of the washed-off
surface, and the results of cleaning. The fouling model is
mazout.
- 14 -
~ .
. . .
~ ,.~

CA 021016~1 1998-04-08
Table 2
Example Composition of Surface to Quantity of fouling
No. the cleaning be washedremained, g/cm2,
agent, ~ by off
mass
l 2 3 4
6 Compositio~ I
Ox~eth~lated dodec~l
phenol 2.50
Isodec~l phenol 0.02
Eero~ene 30.00 aluminium4.2~10
Sodium tripol~phos_
phste 0.3
Water the balance
Composition 2
Oxyethylated dodecyl
phenol 0.10
Isodec~l phe~ol 0.01
Sodium tripolyphospbate 0.20
Sodium silicate 0.~0
Water the baLance
- 15 -
~..,

CA 02101651 1998-04-08
~able 2 (cDntinued)
1 2 3 4
7 Composition I
Oxyetbylated ionyl p~enol 1.5~
O*~ethylsted oct~l phenol 0.50
Dodecyl pbe~ol 0.02
Dec~l.phenol 0.01
Sodium tripDL~pbDsphate o.50
Wbite spirit 10.00 brass 4.1.10 5
Water the balance.-
Comeositio~ 2
Oxyethylated ionyl phenol 0.25
Dodecyl pbenol 0.01
Sodium tripolyphosphate o.50
~ater tbe balance
8 Composition I
Oxyetbglated decyl phenol 1.0 metal surface
~ coated v~ith
an oil paint 5.8 10 5
Decgl pbe~ol 0~01
Isonony-l phenol 0.005
Eerosese 5.o
Sodium tripol~pbosphate 0.50
Water the balance
Composition 2
Oxyethylated decyl phenol 0.10
Decyl phenol 0.01
Sodium tripolyphosphate 0.10
Sodium silicate 0.10
Water the balance
- 16 -
. ~; ,".~.
~ ~ ,
~ ;~

CA 02101651 1998-04-08
~....
~able 2 (continued)
1 2 3 4
9 Composition I
OxyetbyLated oct~l phenol 0.80
Octyl phenol 0.01 titanium
S~nthetic zeolite,
grade NsA ~-5~ 9.2~10 5
Gas condensate o.50
Water the balance
Composition 2
Ox~eth~lated oct~l p~enol 0.10
Oct~l p~enol 0.01
Sodi~m siLicate 0.20
water the balance
Example lO:
Two compositions of the agent were prepared.
The first composition of the agent, % by mass:
Oxyethylated isononyl phenol 3.0
Isononyl phenol 0.03
Hydrocarbon solvent 40.0
Water the balance
The second composition of the agent, % by mass:
Oxyethylated alkyl phenol O.l
Isononyl phenol 0.005
Sodium Tripolyphosphate 0.2
Water the balance
. _.,
~'

CA 021016~1 1998-04-08
The claimed agents have been tested in washing the
turbo-generator set blading section, without disassembly of
the set. First, through a circular header, during suction
of the compressor, fed into the blading section as a jet by
means of the pump is the first composition for 1-2 minutes
at idle turning-over of the set. 15 minutes later the
system is washed with the second composition.
A visual inspection showed that the surfaces of guide
vanes of turbo-generator sets were fully cleaned of oil-
and-dirt deposits. The use of the agent made it possible
to improve the turbine technical-and-economic indexes: with
similar values of speed of the gas turbocompressor before
and after washing (~7,200 rpm), there is observed an
increase of the power turbine speed (by 30-60 rpm), the
exhaust temperature drops by 8-12~C, an increase in power
of the turbo-generator sets, as well as a drop in gas
pressure at the machine inlet and outlet.
- 18 -
~ ~,
f~ i

Representative Drawing

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Administrative Status

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Event History

Description Date
Inactive: IPC from MCD 2006-03-11
Time Limit for Reversal Expired 2004-11-29
Letter Sent 2003-12-01
Grant by Issuance 1999-01-19
Inactive: Final fee received 1998-10-01
Pre-grant 1998-10-01
Notice of Allowance is Issued 1998-06-11
Notice of Allowance is Issued 1998-06-11
Letter Sent 1998-06-11
Inactive: Application prosecuted on TS as of Log entry date 1998-06-03
Inactive: Status info is complete as of Log entry date 1998-06-03
Inactive: First IPC assigned 1998-05-13
Inactive: IPC removed 1998-05-13
Inactive: IPC assigned 1998-05-13
Inactive: Approved for allowance (AFA) 1998-04-30
Request for Examination Requirements Determined Compliant 1994-11-18
All Requirements for Examination Determined Compliant 1994-11-18
Application Published (Open to Public Inspection) 1993-05-30

Abandonment History

There is no abandonment history.

Maintenance Fee

The last payment was received on 1998-11-26

Note : If the full payment has not been received on or before the date indicated, a further fee may be required which may be one of the following

  • the reinstatement fee;
  • the late payment fee; or
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Patent fees are adjusted on the 1st of January every year. The amounts above are the current amounts if received by December 31 of the current year.
Please refer to the CIPO Patent Fees web page to see all current fee amounts.

Fee History

Fee Type Anniversary Year Due Date Paid Date
MF (application, 6th anniv.) - standard 06 1997-12-01 1997-10-22
Final fee - standard 1998-10-01
MF (application, 7th anniv.) - standard 07 1998-11-30 1998-11-26
MF (patent, 8th anniv.) - standard 1999-11-29 1999-10-27
MF (patent, 9th anniv.) - standard 2000-11-29 2000-10-25
MF (patent, 10th anniv.) - standard 2001-11-29 2001-10-19
MF (patent, 11th anniv.) - standard 2002-11-29 2002-11-13
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
INSTITUT NEORGANICHESKOI KHIMII SIBIRSKOGO OTDELENIA ROSSIISKOI AKADEMII NAUK
Past Owners on Record
ELENA KONSTANTINOVNA BATISCHEVA
IRINA MIKHAILOVNA SEKISOVA
JUZEFA NIKOLAEVNA OKHONSKAYA
SOFIA ABDULOVNA SAVINTSEVA
VALENTIN DMITRIEVICH SIDOROV
VALENTINA ANDREEVNA KOLOSANOVA
VERA SERGEEVNA KOLESNIKOVA
VLADIMIR NIKOLAEVICH TOCHILIN
Past Owners that do not appear in the "Owners on Record" listing will appear in other documentation within the application.
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Document
Description 
Date
(yyyy-mm-dd) 
Number of pages   Size of Image (KB) 
Description 1998-04-07 18 478
Claims 1998-04-07 1 18
Abstract 1998-04-07 1 12
Description 1994-05-06 16 567
Claims 1994-05-06 1 25
Abstract 1994-05-06 1 21
Commissioner's Notice - Application Found Allowable 1998-06-10 1 164
Maintenance Fee Notice 2004-01-25 1 175
Correspondence 1998-09-30 1 33
Fees 1996-10-17 1 65
Fees 1995-10-02 1 73
Fees 1993-11-04 1 42
Fees 1994-11-16 1 56
International preliminary examination report 1993-07-28 21 984
Examiner Requisition 1997-03-24 2 67
Prosecution correspondence 1997-09-23 2 51
Courtesy - Office Letter 1995-01-02 1 56
Prosecution correspondence 1994-11-17 1 34
Courtesy - Office Letter 1994-02-01 1 58
PCT Correspondence 1993-11-29 1 28
Courtesy - Office Letter 1993-10-24 1 36