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Nano Carbon Film Coated Water Wettable Graphite And A Process For Its Manufacture.

Abstract: The present invention relates to providing water wettable graphite and a process of its manufacture. More particularly, the present invention is directed to providing nano carbon coated graphite wherein nano carbon form a film over it and making it wettable in water by treating with a solution comprising selective combination of surfactants, dispersants and pigment black and drying, which would not come out even in alkaline water at the time of casting so as to facilitate making of carbon containing refractory castable. Advantageously, the nano carbon coated water wettable graphite according to the present invention is also useful as coating on slide gate plates of steel ladles and electrodes for lithium and other battery favouring wide industrial application.

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Patent Information

Application #
Filing Date
30 August 2013
Publication Number
10/2015
Publication Type
INA
Invention Field
METALLURGY
Status
Email
niloygupta@rediffmail.com
Parent Application
Patent Number
Legal Status
Grant Date
2020-01-15
Renewal Date

Applicants

STEEL AUTHORITY OF INDIA LIMITED
RESEARCH & DEVELOPMENT CENTRE FOR IRON & STEEL, DORANDA, RANCHI-834002, INDIA

Inventors

1. KUMAR KAUSHLESH
RESEARCH & DEVELOPMENT CENTRE FOR IRON & STEEL, DORANDA, RANCHI-834002, INDIA
2. SINGH RAKESH KUMAR
RESEARCH & DEVELOPMENT CENTRE FOR IRON & STEEL, DORANDA, RANCHI-834002, INDIA
3. BARUA PULAK
RESEARCH & DEVELOPMENT CENTRE FOR IRON & STEEL, DORANDA, RANCHI-834002, INDIA

Specification

FIELD OF THE INVENTION
The present invention relates to providing water wettable graphite and a process of its
manufacture. More particularly, the present invention is directed to providing nano carbon
coated graphite wherein nano carbon form a film over it and making it wettable in water
which would not come out even in alkaline water at the time of casting so as to facilitate
making of carbon containing refractory castable. Advantageously, the nano carbon coated
graphite according to the present invention is also useful as coating on slide gate plates of
steel ladles and electrodes for lithium and other battery favoring wide industrial application.
BACKGROUND OF THE INVENTION
At present graphite is used in making carbon containing bricks or castables. Graphite is a
flaky material that is not wettable in water. Wettability is the basic criteria for making water
based refractory materials like bricks and castables with water. At the time of pressing the
brick the flaky graphite comes to the surface of the brick. The main hurdle in developing
carbon containing castable is graphite which is non wettable in water and comes to the
surface at the time of casting. If graphite become water wettable then using of it for
making carbon based refractory will be easier.
There has been thus a need in the art to produce graphite which would be water wettable.
The present invention attempts to coating graphite particles with appropriate combination of
surfactant, dispersant and carbon black based solution so that the nature of graphite
changed from non-wettable to wettable. The nano carbon which forms a film over it and do
not come out even in alkaline water thereby the problems experienced in making carbon
containing castable can be solved.
OBJECTS OF THE INVENTION
The basic object of the present invention is directed to providing nano carbon coated
graphite which form a film over it making it wettable in water and a process for its
manufacture.

A further object of the present invention is directed to providing nano carbon coated
graphite which is wettable in water and do not come to the surface at the time of casting
making carbon based refractory easier.
A still further object of the present invention is directed to providing nano carbon coated
graphite wherein nano carbon which forms a film over graphite and do not come out even in
alkaline water , thus facilitating making of carbon containing castable.
A still further object of the present invention is directed to providing nano carbon coated
water wettable graphite wherein graphite particles are coated with solution of optimum
combination of surfactant, dispersant and carbon black nano particles.
A still further object of the present invention is directed to providing nano carbon coated
water wettable graphite wherein coated graphite when put in alkali solution or water the
coating of carbon does not come out from the graphite, which is favourable for development
of carbon containing castables.
A still further object of the present invention is directed to providing nano carbon coated
water wettable graphite wherein carbon black forms a film over the graphite which is
insoluble in water.
A still further object of the present invention is directed to providing nano carbon coated
water wettable graphite wherein coated graphite does not react with alkali solution and
carbon is not coming out from the grain once coated.
A still further object of the present invention is directed to providing nano carbon coated
water wettable graphite wherein dried coated graphite easily settled down in water so that
mixing graphite is easier for making carbon based refractory bricks and castables or any
other ceramic carbon containing materials.
SUMMARY OF THE INVENTION
The basic aspect of the present invention is thus directed to water wettable graphite
comprising:
graphite coated with nano carbon comprising nano carbon film coated graphite.

A further aspect of the present invention is directed to water wettable graphite wherein
said nano carbon comprises carbon black having particle size of 24-36 nm.
A still further aspect of the present invention is directed to water wettable graphite wherein
said nano carbon film comprises a solution of carbon black.
A still further aspect of the present invention is directed to water wettable graphite wherein
said solution of carbon black comprises :
Nano Carbon black 10 to 15 % by wt.
2 - pyrrolidine 3 to 6 % by wt.
1,5 pentanediol 3 to 5 % by wt.
Multranol 4012 4 to 7 % by wt.
Ethylene glycol 4.5 to 6.5 % by wt.
Proxcel TM Ultra 5 0.6 to 1.0 % by wt.
Surfynol 104H 0.05 to 0.12 % by wt.
Water soluble resin 1 to 3 % by wt.
(Fevicol SH)
Water 55 to 75 % by wt.
Yet another aspect of the present invention is directed to a coatable/film forming nano
carbon black solution comprising:
Nano Carbon black 10 to 15 % by wt.
2 - pyrrolidine 3 to 6 % by wt.
1,5 pentanediol 3 to 5 % by wt.
Multranol 4012 4 to 7 % by wt.
Ethylene glycol 4.5 to 6.5 % by wt.
Proxcel TM Ultra 5 0.6 to 1.0 % by wt.
Surfynol 104H 0.05 to 0.12 % by wt.
Water soluble resin 1 to 3 % by wt.
(Fevicol SH)
Water 55 to 75 % by wt.

A further aspect of the present invention is directed to a solution suitable for producing
coatable/film forming nano carbon black solution comprising:
Nano Carbon black 10 to 15 % by wt.
2 - pyrrolidine 3 to 6 % by wt.
1,5 pentanediol 3 to 5 % by wt.
Multranol 4012 4 to 7 % by wt.
Ethylene glycol 4.5 to 6.5 % by wt.
Proxcel TM Ultra 5 0.6 to 1.0 % by wt.
Surfynol 104H 0.05 to 0.12 % by wt.
Water soluble resin 1 to 3 % by wt.
(Fevicol SH)
Water 55 to 75 % by wt.
A still further aspect of the present invention is directed to a process for manufacturing
solution for coating nano carbon black on graphite comprising:
providing selectively a solution comprising of
Nano Carbon black 10 to 15 % by wt.
2 - pyrrolidine 3 to 6 % by wt.
1,5 pentanediol 3 to 5 % by wt.
Multranol 4012 4 to 7 % by wt.
Ethylene glycol 4.5 to 6.5 % by wt.
Proxcel TM Ultra 5 0.6 to 1.0 % by wt.
Surfynol 104H 0.05 to 0.12 % by wt.
Water soluble resin 1 to 3 % by wt.
(Fevicol SH)
Water 55 to 75 % by wt.
A still further aspect of the present invention is directed to a process for producing water
wettable graphite comprising:
i) providing a coatable /film forming nano carbon black solution comprising:

Nano Carbon black 10 to 15 % by wt.
2 - pyrrolidine 3 to 6 % by wt.
1,5 pentanediol 3 to 5 % by wt.
Multranol 4012 4 to 7 % by wt.
Ethylene glycol 4.5 to 6.5 % by wt.
Proxcel TM Ultra 5 0.6 to 1.0 % by wt.
Surfynol 104H 0.05 to 0.12 % by wt.
Water soluble resin 1 to 3 % by wt.
(Fevicol SH)
Water 55 to 75 % by wt.
(ii) Mixing about 10 to 15 % by wt of said solution as obtained in step (i) with 85
to 90 % by wt of water;
(iii) Adding 20 to 30 % by wt. graphite powder into the above mix of (ii) and
mixing with a stirrer ;
(iv) Allowing all the graphite powder settled down in the vessel after 30 to 40
minutes,
(v) Screening out the wetted and coated graphite from the solution,
(vi) Drying the coated graphite at 100 to 120 °C preferably 110°C in a drier for 2
to 4 hrs. preferably 3 hours to thereby obtain the water wettable graphite.
Another aspect of the present invention is directed to a process for producing nano Carbon
coated water wettable graphite, wherein ratio of nano carbon, organic compound and water
vary with varied type of graphite.
A further aspect of the present invention is directed to a process for producing nano Carbon
coated water wettable graphite, wherein said nano carbon used is Carbon black which is a
nano material being 99.9 % pure carbon amorphous in nature with particle size in the
range of 24-36nm.
A still further aspect of the present invention is directed to Refractory bricks/castables
comprising water wettable graphite which is graphite coated with nano carbon preferably
nano carbon film coated graphite.
Yet another aspect of the present invention is directed to said Refractory bricks/castables
wherein said nano carbon comprises carbon black having particle size of 24-36 nm.

The objects and advantages of the present invention are described hereunder in greater
details with reference to the following non limiting illustrative drawings and example.
BRIEF DESCRIPTION OF THE ACCOMPANYING FIGURES
Figure 1: is the photograph showing the behavior of uncoated graphite powder as well as
coated graphite powder according to the present invention wherein (i) Bekar 1 : Graphite
powder floating above water, (ii) Bekar 2 : Graphite powder mixed in developed solution,
(Mi) Bekar 3 : Treated graphite powder settled down at bottom of water.
Figure 2: is the photograph showing (i) natural graphite and (ii) nano carbon treated water
wettable graphite according to the present invention.
DETAILED DECSRIPTION OF THE INVENTION WITH REFERENCE TO THE
ACCOMPANYING FIGURES
The present invention is directed to providing nano carbon coated graphite which form a
film over it making it wettable in water and a process for its manufacture.
It is well known that Carbon black is a nano material, amorphous in nature, which is 99.9 %
pure carbon. The particle size of carbon black used for the purpose of the present invention
is 24-36nm. This carbon black is admixed with some organic compound and water to form a
solution. Several solution of different combination of different type of surfactant (acrylate
resin, Propylene glycol, monostyrene, acrylic acid), and pigment black have been tried out
for desired activity. An optimum combination of these with varied water ratio was obtained.
Nano carbon black of different ratio was also added in the solution. Some Alkali like NaOH
or KOH was also mixed, in the solution. An accurate solution of optimum combination of
surfactant, dispersant and carbon black was thus obtained.
When graphite is put into this solution for some time then all the graphite settled down and
coated with this nano carbon based solution. As the graphite is taken out from the solution
a film of nano carbon is coated over it and the nature of graphite changed from non
wettable to wettable. Now the graphite become water wettable. It forms carbon thin film

over the graphite. The nano carbon coated graphite is then dried in oven at 110°C for one
hour. The ratio of nano carbon, organic compound and water vary with varied type of
graphite.
The process of producing the nano carbon coated graphite powder which would be wettable
in water to favour produing carbon containing refractory castables/bricks is illustrated with
the following Example:
Example I:
(A) As already stated in the preceding paragraph, different types of materials and
organic compounds were tried to coat graphite with carbon black by using surfactant
and dispersant with water.
The organic compounds of four variety were used to coat the graphite with carbon black
namely Formaldehyde, Ethylene glycol, Ethyl alcohol and furancarbinol. Several solution of
different combination of different type of surfactant (acrylate resin, Propylene glycol,
monostyrene, acrylic acid), dispersant of R-O-(CH2CH2O) - CH2COONa group or
C18H35O(CH2CH2O)12CH2COONa and pigment black, were tried.
It was observed from the above experimental trials that:
Formaldehyde, Ethylene glycol makes a solution well with carbon black but could
not coat the grains which can stick on the graphite.
Ethyl alcohol could not make a solution with carbon black.
Furancarbinol make a solution better with carbon black and coat the graphite but
not wettable in water.
Thus through the trial of different combination with different surfactant and dispersant, the
following combination of solution was arrived at which could provide the desired result:
Nano Carbon black 10 to 15 % by wt.
2 - pyrrolidine 3 to 6 % by wt.
1,5 pentanediol 3 to 5 % by wt.
Multranol 4012 4 to 7 % by wt.
Ethylene glycol 4.5 to 6.5 % by wt.
Proxcel TM Ultra 5 0.6 to 1.0 % by wt.
Surfynol 104H 0.05 to 0.12 % by wt.

Water soluble resin 1 to 3 % by wt.
(Fevicol SH)
Water 55 to 75 % by wt.
(B) After preparing the solution of above components, following steps are followed to
produce the nano carbon coated graphite according to the present invention:
(i) About 100 gm solution were mixed with 900ml water.
(ii) 200 gm of graphite powder were put into the above solution and mixed with
a stirrer manually for 5 minutes,
(iii) After 30 to 40 minutes all the graphite powder settled down in the vessel,
(iv) The wetted and coated graphite were screened out from the solution,
(v) The coated graphite dried preferably at 110°C in a drier, preferably for 2
hours.
(vi) The dried coated graphite when put into the water. It easily settled at the
bottom of the vessel as shown in the accompanying Figure 1.
(vii) The solution can be used again for coating the graphite.
Accompanying Figure 2 is the photograph showing (i) natural graphite powder and (ii)
nano carbon treated water wettable graphite obtained according to the present invention.
(C)The dried nano carbon coated graphite so produced found to have the following
properties:
(i) The nano carbon coated the surface properly and forms a film over the
graphite.
(ii) When it dried the film is not coming out from the graphite that confirms
carbon coated the graphite well.
(iii) The coated graphite is glazy in appearance.
(iv) The coated graphite when put in alkali solution or water the coating of
carbon is not comes out from the graphite.
(v) The coated graphite when put in water no carbon is coming out from the
graphite that is good for development of carbon containing castables.

It is thus possible by way of the present invention to providing nano sized Carbon coated
water wettable graphite and process of its manufacture wherein nano carbon coated
graphite form a film over it and making it wettable in water which would not come out even
in alkaline water at the time of casting so as to facilitate making of carbon containing
refractory castable/bricks. Advantageously, the nano carbon coated graphite obtained
according to the present invention is also useful as nozzle filling compound of steel ladles
and electrodes for lithium and other battery favouring wide industrial application.

We Claim:
1. Water wettable graphite comprising:
graphite coated with nano carbon comprising nano carbon film coated graphite.
2. Water wettable graphite as claimed in claim 1 wherein said nano carbon comprises
carbon black having particle size of 24-36 nm.
3. Water wettable graphite as claimed in anyone of claims 1 or 2 wherein said nano
carbon film comprises a solution of carbon black.
4. Water wettable graphite as claimed in claim 3 wherein said solution of carbon black
comprises :
Nano Carbon black 10 to 15 % by wt.
2 - pyrrolidine 3 to 6 % by wt.
1,5 pentanediol 3 to 5 % by wt.
Multranol 4012 4 to 7 % by wt.
Ethylene glycol 4.5 to 6.5 % by wt.
Proxcel TM Ultra 5 0.6 to 1.0 % by wt.
Surfynol 104H 0.05 to 0.12 % by wt.
Water soluble resin 1 to 3 % by wt.
(Fevicol SH)
Water 55 to 75 % by wt.
5. A coatable/film forming nano carbon black solution comprising:
Nano Carbon black 10 to 15 % by wt.
2 - pyrrolidine 3 to 6 % by wt.
1,5 pentanediol 3 to 5 % by wt.
Multranol 4012 4 to 7 % by wt.
Ethylene glycol 4.5 to 6.5 % by wt.
Proxcel TM Ultra 5 0.6 to 1.0 % by wt.
Surfynol 104H 0.05 to 0.12 % by wt.
Water soluble resin 1 to 3 % by wt.
(Fevicol SH)
Water 55 to 75 % by wt.

6. A solution suitable for producing coatable /film forming nano carbon black solution
comprising:
Nano Carbon black 10 to 15 % by wt.
2 - pyrrolidine 3 to 6 % by wt.
1,5 pentanediol 3 to 5 % by wt.
Multranol 4012 4 to 7 % by wt.
Ethylene glycol 4.5 to 6.5 % by wt.
Proxcel TNI Ultra 5 0.6 to 1.0 % by wt.
Surfynol 104H 0.05 to 0.12 % by wt.
Water soluble resin 1 to 3 % by wt.
(Fevicol SH)
Water 55 to 75 % by wt.
7. A process for manufacturing solution for coating nano carbon black on graphite
comprising:
providing selectively a solution comprising of
Nano Carbon black 10 to 15 % by wt.
2 - pyrrolidine 3 to 6 % by wt.
1,5 pentanediol 3 to 5 % by wt.
Multranol 4012 4 to 7 % by wt.
Ethylene glycol 4.5 to 6.5 % by wt.
Proxcel TM Ultra 5 0.6 to 1.0 % by wt.
Surfynol 104H 0.05 to 0.12 % by wt.
Water soluble resin 1 to 3 % by wt.
(Fevicol SH)
Water 55 to 75 % by wt.
8. A process for producing water wettable graphite as claimed in anyone of claims 1 to
4 comprising:
i) providing a coatable /film forming nano carbon black solution comprising:
Nano Carbon black 10 to 15 % by wt.
2 - pyrrolidine 3 to 6 % by wt.

1,5 pentanediol 3 to 5 % by wt.
Multranol 4012 . 4 to 7 % by wt.
Ethylene glycol 4.5 to 6.5 % by wt.
Proxcel TM Ultra 5 0.6 to 1.0 % by wt.
Surfynol 104H 0.05 to 0.12 % by wt.
Water soluble resin 1 to 3 % by wt.
(Fevicol SH)
Water 55 to 75 % by wt.
(ii) Mixing about 10 to 15 % by wt of said solution as obtained in step (i) with 85 to
90 % by wt of water;
(iii) Adding 20 to 30 % by wt. graphite powder into the above mix of (ii) and mixing
with a stirrer ;
(iv) Allowing all the graphite powder settled down in the vessel after 30 to 40
minutes.
(v) Screening out the wetted and coated graphite from the solution.
(vi) Drying the coated graphite at 100 to 120°C preferably 110°C in a drier for 2 to 4
hrs. preferably 3 hours to thereby obtain the water wettable graphite.
9. A process for producing nano Carbon coated water wettable graphite as claimed in
claim 8, wherein ratio of nano carbon, organic compound and water vary with varied
type of graphite.
10. A process for producing nano Carbon coated water wettable graphite as claimed in
anyone of claims 8 or 9, wherein said nano carbon used is Carbon black which is a
nano material being 99.9 % pure carbon amorphous in nature with particle size in
the range of 24-36nm.
11. Refractory bricks/castables comprising water wettable graphite which is graphite
coated with nano carbon preferably nano carbon film coated graphite.
12.'Refractory bricks/castables as claimed in claim 11 wherein said nano carbon
comprises carbon black having particle size of 24-36 nm.

ABSTRACT

The present invention relates to providing water wettable graphite and a process of its
manufacture. More particularly, the present invention is directed to providing nano carbon
coated graphite wherein nano carbon form a film over it and making it wettable in water by
treating with a solution comprising selective combination of surfactants, dispersants and
pigment black and drying, which would not come out even in alkaline water at the time of
casting so as to facilitate making of carbon containing refractory castable. Advantageously,
the nano carbon coated water wettable graphite according to the present invention is also
useful as coating on slide gate plates of steel ladles and electrodes for lithium and other
battery favouring wide industrial application.

Documents

Orders

Section Controller Decision Date

Application Documents

# Name Date
1 1006-KOL-2013-(30-08-2013)-SPECIFICATION.pdf 2013-08-30
1 1006-KOL-2013-IntimationOfGrant15-01-2020.pdf 2020-01-15
2 1006-KOL-2013-(30-08-2013)-FORM-3.pdf 2013-08-30
2 1006-KOL-2013-PatentCertificate15-01-2020.pdf 2020-01-15
3 1006-KOL-2013-Annexure (Optional) [11-01-2020(online)].pdf 2020-01-11
3 1006-KOL-2013-(30-08-2013)-FORM-2.pdf 2013-08-30
4 1006-KOL-2013-Written submissions and relevant documents (MANDATORY) [11-01-2020(online)].pdf 2020-01-11
4 1006-KOL-2013-(30-08-2013)-FORM-1.pdf 2013-08-30
5 1006-KOL-2013-FORM 13 [07-01-2020(online)].pdf 2020-01-07
5 1006-KOL-2013-(30-08-2013)-DRAWINGS.pdf 2013-08-30
6 1006-KOL-2013-RELEVANT DOCUMENTS [07-01-2020(online)].pdf 2020-01-07
6 1006-KOL-2013-(30-08-2013)-DESCRIPTION (COMPLETE).pdf 2013-08-30
7 1006-KOL-2013-HearingNoticeLetter-(DateOfHearing-10-01-2020).pdf 2019-12-13
7 1006-KOL-2013-(30-08-2013)-CORRESPONDENCE.pdf 2013-08-30
8 1006-KOL-2013-CLAIMS [06-11-2018(online)].pdf 2018-11-06
8 1006-KOL-2013-(30-08-2013)-CLAIMS.pdf 2013-08-30
9 1006-KOL-2013-(30-08-2013)-ABSTRACT.pdf 2013-08-30
9 1006-KOL-2013-COMPLETE SPECIFICATION [06-11-2018(online)].pdf 2018-11-06
10 1006-KOL-2013-(05-09-2013)-FORM-1.pdf 2013-09-05
10 1006-KOL-2013-FER_SER_REPLY [06-11-2018(online)].pdf 2018-11-06
11 1006-KOL-2013-(05-09-2013)-CORRESPONDENCE.pdf 2013-09-05
11 1006-KOL-2013-OTHERS [06-11-2018(online)].pdf 2018-11-06
12 1006-KOL-2013-FER.pdf 2018-05-22
12 1006-KOL-2013-FORM-18.pdf 2013-11-14
13 1006-KOL-2013-(27-12-2013)-CORRESPONDENCE.pdf 2013-12-27
13 1006-KOL-2013-(27-12-2013)-PA.pdf 2013-12-27
14 1006-KOL-2013-(27-12-2013)-CORRESPONDENCE.pdf 2013-12-27
14 1006-KOL-2013-(27-12-2013)-PA.pdf 2013-12-27
15 1006-KOL-2013-FER.pdf 2018-05-22
15 1006-KOL-2013-FORM-18.pdf 2013-11-14
16 1006-KOL-2013-(05-09-2013)-CORRESPONDENCE.pdf 2013-09-05
16 1006-KOL-2013-OTHERS [06-11-2018(online)].pdf 2018-11-06
17 1006-KOL-2013-FER_SER_REPLY [06-11-2018(online)].pdf 2018-11-06
17 1006-KOL-2013-(05-09-2013)-FORM-1.pdf 2013-09-05
18 1006-KOL-2013-(30-08-2013)-ABSTRACT.pdf 2013-08-30
18 1006-KOL-2013-COMPLETE SPECIFICATION [06-11-2018(online)].pdf 2018-11-06
19 1006-KOL-2013-(30-08-2013)-CLAIMS.pdf 2013-08-30
19 1006-KOL-2013-CLAIMS [06-11-2018(online)].pdf 2018-11-06
20 1006-KOL-2013-(30-08-2013)-CORRESPONDENCE.pdf 2013-08-30
20 1006-KOL-2013-HearingNoticeLetter-(DateOfHearing-10-01-2020).pdf 2019-12-13
21 1006-KOL-2013-(30-08-2013)-DESCRIPTION (COMPLETE).pdf 2013-08-30
21 1006-KOL-2013-RELEVANT DOCUMENTS [07-01-2020(online)].pdf 2020-01-07
22 1006-KOL-2013-(30-08-2013)-DRAWINGS.pdf 2013-08-30
22 1006-KOL-2013-FORM 13 [07-01-2020(online)].pdf 2020-01-07
23 1006-KOL-2013-(30-08-2013)-FORM-1.pdf 2013-08-30
23 1006-KOL-2013-Written submissions and relevant documents (MANDATORY) [11-01-2020(online)].pdf 2020-01-11
24 1006-KOL-2013-(30-08-2013)-FORM-2.pdf 2013-08-30
24 1006-KOL-2013-Annexure (Optional) [11-01-2020(online)].pdf 2020-01-11
25 1006-KOL-2013-PatentCertificate15-01-2020.pdf 2020-01-15
25 1006-KOL-2013-(30-08-2013)-FORM-3.pdf 2013-08-30
26 1006-KOL-2013-IntimationOfGrant15-01-2020.pdf 2020-01-15
26 1006-KOL-2013-(30-08-2013)-SPECIFICATION.pdf 2013-08-30

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