WO2001098558A2 - Corrosion control utilizing a hydrogen peroxide donor - Google Patents
Corrosion control utilizing a hydrogen peroxide donor Download PDFInfo
- Publication number
- WO2001098558A2 WO2001098558A2 PCT/US2001/019783 US0119783W WO0198558A2 WO 2001098558 A2 WO2001098558 A2 WO 2001098558A2 US 0119783 W US0119783 W US 0119783W WO 0198558 A2 WO0198558 A2 WO 0198558A2
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- acid
- corrosion
- metal
- electrolyte
- hydrogen peroxide
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
- C02F5/08—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents
- C02F5/10—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents using organic substances
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
- C02F5/08—Treatment of water with complexing chemicals or other solubilising agents for softening, scale prevention or scale removal, e.g. adding sequestering agents
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
- C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
- C23F11/12—Oxygen-containing compounds
- C23F11/124—Carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
- C23F11/10—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using organic inhibitors
- C23F11/173—Macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23F—NON-MECHANICAL REMOVAL OF METALLIC MATERIAL FROM SURFACE; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL; MULTI-STEP PROCESSES FOR SURFACE TREATMENT OF METALLIC MATERIAL INVOLVING AT LEAST ONE PROCESS PROVIDED FOR IN CLASS C23 AND AT LEAST ONE PROCESS COVERED BY SUBCLASS C21D OR C22F OR CLASS C25
- C23F11/00—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent
- C23F11/08—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids
- C23F11/18—Inhibiting corrosion of metallic material by applying inhibitors to the surface in danger of corrosion or adding them to the corrosive agent in other liquids using inorganic inhibitors
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/02—Non-contaminated water, e.g. for industrial water supply
- C02F2103/023—Water in cooling circuits
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/02—Temperature
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/06—Controlling or monitoring parameters in water treatment pH
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/40—Liquid flow rate
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/04—Flow arrangements
- C02F2301/046—Recirculation with an external loop
Definitions
- This invention relates to a method of inhibiting corrosion as well as inhibiting scale and deposit formation resulting from the saturation of mineral salts, and buildup of corrosion byproducts.
- the invention generally relates to the inhibition of corrosion of metals in contact with an electrolyte and the reduction of insulating films owing to scale formation/deposition.
- the invention most particularly relates to the inhibition of corrosion on metals which experience active-passive transition by application of a hydrogen peroxide donor- Illustrative of such metals are steel (s), aluminum, titanium or mixtures thereof; however the instant invention contemplates the treatment of any metal which is capable of experiencing active/passive transitions when exposed to passivating agents.
- Corrosion of metals are of critical concern.
- water from rivers, lakes, ponds, wells, wastewater treatment plant effluent etc. is employed as the cooling media for heat exchangers .
- Such waters can contain a variety of either dissolved and/or suspended materials such as mineral salts, metals, organics, silt, mud etc.
- the cooling water from a heat exchanger is typically passed through a cooling tower, spray pond or evaporative system prior to discharge or reuse.
- cooling is achieved by evaporating a portion of the water passing through the system.
- anionic ions such as chlorides and sulfates can increase the rate of corrosion of the metals making up the cooling system. This is especially true with the metals making up the heat exchangers that are experiencing higher temperatures.
- contaminates such as hydrogen sulfide can also increase corrosion rates.
- mineral salts for example those of calcium and magnesium can induce scaling of the heat exchanger.
- a scale common in cooling systems is calcium carbonate.
- the corrosion cell consist of two half cells, the cathode, and the anode.
- the cathode is defined as the point where the reduction of a reducible substance takes place.
- the primary reducible substance is oxygen.
- the steps involved with the cathode include: oxygen diffusion to the metal surface, adsorb by either physical or chemical adsorption, electron transfer, rearrangement with other adsorbed materials (i.e.
- the anode is defined as the point where dissolution of metal ions occurs.
- the dissolution of metal ions at the anode is a chemical process.
- the reaction forms ferrous hydroxide. Initially, the potential at the anode is low; however with time, the electrical potential at the anode increases. The increased potential is the result of the increased concentration of metal ions (result of dissolution) in the immediate vicinity of the anode.
- the increased concentration of metal ions induces the formation of a Metal Ion Concentration Cell, as well as the reduction of oxygen.
- the increasing concentration of cationic charged ions at the anode increases the electrical potential of the anode.
- General corrosion is defined as a state where the potential of the cathode decreases with time while the potential at the anode increases. At some point, the potentials of the cathode and anode shift or find neighboring electrodes of stronger or weaker potential. This shifting or jumping is the result of the mechanisms already described.
- As the hydroxide concentration at the cathode increases oxygen adsorption decreases, and the cathodes potential goes down.
- the concentration of cationic ions increases, the demand for electrons increases, so the potential goes up.
- Pitting corrosion refers to a condition where the potential surrounding the anode is high (cathodic) and electron flow is not distributed across many anodes, therefore the electron comes from a local anode.
- Pitting corrosion is of great concern because of the high loss of metal from a localized area.
- MPY mils per year
- general corrosion would take many decades of continued corrosion before resulting in failure of the part, e.g. of a heat exchanger.
- the electron flow and subsequent metal loss is from a localized area. Pitting corrosion often results in equipment failure long before reaching the expected life of the equipment, e.g.
- the mechanism of passivation involves the dissolution of metal ions, followed by formation of a ferrous hydroxide layer, followed by conversion to an insoluble ferric oxide by reaction with oxygen.
- Analysis of passive films indicates a layered structure with an outer layer of gamma iron oxide and an inner layer of magnetite. Passivation occurs when we have established sufficient oxidation potential. At low oxidation potential, insufficient concentrations of oxidizer exist to establish a homogenous oxide layer; distinct anodes and cathodes exist. When sufficient oxidizer is present, the electrical potential of the entire surface is increased. The concentration of oxidizer is sufficient to induce the flash" formation of an oxide layer.
- the oxidizer concentration is sufficiently high to react with the ferrous hydroxide across the entire metal surface.
- the current density increases.
- the current density required to induce passivation is called the critical current.
- the transpassive region is a process requiring oxygen. Therefore, inhibitors that induce passivation must increase the oxidizing potential or make better use of the oxidizer present .
- Inhibitors such as chromate, nitrite and hydroxide raise the oxidizing potential of the solution by directly supplying oxygen to the anode to react with the metal ions thereby reducing the formation of a metal oxide.
- Inhibitors such as phosphate, silicate, borate and molybdate are non-oxidizing inhibitors which form complexes with iron (III) species so as to stabilize them from disproportionation (the transformation of a substance into two or more substances by oxidation or reduction) to the more soluble Fe (II) species until reaction with dissolved oxygen creates the more immune oxides.
- iron (III) species the transformation of a substance into two or more substances by oxidation or reduction
- II iron
- These inhibitors do require the presence of oxygen to promote passivation.
- Their performance can be enhanced with the addition of a peroxide compound where peroxide is used to enhance the formation of a passive oxide film.
- Concentrations of peroxide and peroxycarboxylic acids can be reduced with the addition of a cathodic inhibitor such as zinc.
- a cathodic inhibitor such as zinc.
- polymers are commonly fed to help prevent fouling from precipitation.
- zinc has environmental implications.
- Using existing treatment methods operating cost increased, and in many operating conditions such as high heat flux and/or high chlorides, results are less than desirable.
- a treatment program that is effective at inhibiting corrosion -under various heat flux and water chemistry conditions, as well as being environmentally innocuous.
- US Patent No. 5,800,732 describes the use of hydrogen peroxide as a means of controlling microbial activity in an all-in-one treatment for cooling water.
- US Patent No. 4,977,292 describes the development of an organic phosphorous compound using hydrogen peroxide as an oxidizer to initiate the oxidation reaction.
- US Patent No. 5,382,367 describes the use of hydrogen peroxide in cooling water systems to control microbiological activity in said systems.
- US Patent Nos. 5,980,758, 5,785,867, 5,658,467 and 5,494,588 describe the use of peracetic acid with non- oxidizing biocides to inhibit growth of microorganisms.
- the instant invention is directed toward a method which provides superior corrosion inhibition, particularly to those areas experiencing heat transfer; namely the heat exchangers where corrosion and scale potential is most prevalent.
- the instant process recognizes the fact that both hydrogen peroxide and peroxycarboxylic acids are strong oxidizing agents having important similarities to chromate (VI) in that they are anionic oxidizers. Since they function as anionic oxidizers, these compounds have high solubility in water and readily diffuse to the metal surface. Being strong oxidizers as well as oxygen donors, they are able to directly supply the oxygen needed to induce passivation.
- the instant process utilizes these compounds as corrosion inhibitors and passivators to achieve performance equal to or exceeding that obtained by chromate.
- Such performance has been demonstrated under high heat load conditions and/or in the presence of corrosion inducing ions such as chlorides. These compounds also provide an environmentally innocuous treatment that eliminates the need for other corrosion inhibitors such as zinc and phosphate based treatments, as well as their supporting polymer treatment .
- the instant invention teaches an innovative treatment technology having application wherever removal of scale or deposits in contact with an electrolyte is required.
- the invention also teaches effective removal of insulating films while inhibiting corrosion (especially under heat transfer) and can be effectively used to improve operational performance without suffering loss of system integrity or production time.
- the chemistry selected for removal of the insulating layers is based on the composition of the deposits.
- ferrous oxide was the primary composition and therefore, peroxycitric acid solution or mineral acid was affective at removing the deposit.
- Other chelating, sequestering, and dispersing agents could also provide effective results when used in conjunction with peroxycarboxylic acid(s) solutions. Accordingly, it is an objective of the instant invention to utilize hydrogen peroxide donors as corrosion inhibitors and passivators to achieve performance equal to or exceeding that obtained by chromate . It is a further objective of the instant invention to provide an environmentally innocuous treatment that eliminates the need for other corrosion inhibitors such as zinc and phosphate based treatments, as well as their supporting polymer treatment.
- Figure 1 is illustrative of a circulating system useful for conducting tests replicating a typical cooling water treatment application
- Figure 2 illustrates a cross-sectional view of a MENTOR CHx device
- Figure 3 is a graphical representation of Electro Chemical Noise (ECN) in the presence of Chromate
- Figure 4 is a graphical representation of ECN in the presence of Hydrogen Peroxide
- Figure 5 is a graphical representation of ECN in the presence of Peroxide-Citric Acid
- Figure 6 is a graphical representation of Heat Transfer During Cleaning
- Figure 7 is a graphical representation of ECN During Cleaning
- Figure 8 is a graphical representation of Activity Factor (AF) During Cleaning.
- ECN Electro Chemical Noise
- Figure 1 is illustrative of a circulating system useful for conducting tests replicating a typical cooling water treatment application.
- the instant device is comprised of a system that incorporates: a MENTOR CHx heat transfer device (more particularly described in Figure 2) 110 that is made of the metallurgy to be tested.
- the metallurgy under heat transfer is in contact with an electrolyte which is pumped via pump 116 through a heat exchanger 112 through which electrolyte from electrolyte reservoir 114 is passed.
- a block 210 is comprised of a series of pieces of the desired metallurgy 212 that are joined with an insulating material 214 placed between each adjoining piece. This series of adjoined pieces will be designated the "block". A hole (not shown) is incorporated at some part of the construction process through which the electrolyte will contact the block.
- the metal pieces making up the block are equipped with appropriate sensing apparatus (not shown) for the sensing of ECN and LPR.
- Other sensing apparatus for determination of temperature gradients, heat transfer coefficients, etc. can be applied in a way that does not interfere with the performance of ECN and LPR sensing apparatus.
- the block is equipped with a device 216 to provide heat thru the block.
- the block is combined with other supporting equipment necessary for replicating the operational environment of the heat transfer equipment in question. This can include, but is not limited to, equipment necessary for replicating electrolyte flow rate, electrolyte chemical parameters, and skin temperature at the heat exchanger electrolyte interface, etc.
- the process control parameters are adjusted and controlled to replicate the operational environment at the heat exchanger metal-electrolyte interface.
- the heated element was made of 1010 carbon steel.
- a circulation pump was attached to a reservoir pump the water of desired chemistry through the testing element, a cooling coil and back to the reservoir.
- the chemistry selected for removal of the insulating layers is based on the composition of the deposits. Therefore, in the following tests, since ferrous oxide was the primary composition, a peroxycitric acid solution or mineral acid was chosen for effectively removing the deposit.
- Other chelating, sequestering, and dispersing agents could also provide effective results when used in conjunction with peroxycarboxylic acid(s) solutions.
- Peroxycarboxylic acids are formed from acids selected from the group consisting of formic acid, acetic acid, citric acid, oxalic acid, gluconic acid, glucoheptonic acid, succinic acid, acrylic acid, polyacrylic acid, maleic acid, polymaleic acid, polyepoxysuccinic acid, ethylene-diamine-tetraacetic acid, malonic acid, adipic acid, phosphonobutanepolycarboxylic acid and mixtures thereof.
- peroxycitric acid is an equilibrium product of hydrogen peroxide and citric acid (a "solution" of a peroxycarboxylic acid is comprised of the peroxycarboxylic acid, hydrogen peroxide and the carboxylic acid) .
- a solution of peroxycitric acid was prepared by combining a solution of citric acid, with 30% laboratory grade hydrogen peroxide. The ratio of the blend was 2:1 hydrogen peroxide to citric acid based on actives. After flushing the system, 130ppm of the blend was added to the water. The pH was measured at 6.8. After allowing the system to reach steady state, the ECN corrosion rate was monitored and recorded as illustrated in Figure 5.
- the lower heat transfer value indicates a 19.46% reduction in heat transfer efficiency due to the presence of corrosion byproducts (ferric oxide) .
- the electrolyte was initially treated with lOOOppm of a peroxycitric acid solution made from a 2:1 actives weight ratio of hydrogen peroxide and citric acid.
- Figure 6 illustrates the heat transfer increased (data point 4) while ECN ( Figure 7) showed a corresponding rise in corrosion fate. ECN corrosion rates then dramatically drop (data point 5) , followed by the onset of a, passive-steady state condition (data points 8-13) .
- data point 12 Fig. 6
- heat transfer recovered 22% of the lost heat transfer resulting from the removal of much of the insulating ferric oxide.
- Data point 13 shows the affects of adding lOOOppm of HCl (based on active(s)). Heat transfer is completely restored while maintaining unprecedented control of ECN corrosion rate and Activity Factor (Figure 8) .
- the "Activity Factor” (AF) is calculated using the equation: where O ⁇ is the standard deviation of the electrochemical current noise data, and l rms is the root mean square of the electrochemical current noise. The AF detects changes in current and highlights the deviation from the steady state condition. Test results clearly illustrate the cleaning and corrosion inhibition capabilities of peroxycarboxylic acid solutions . Even in the presence of high chlorides and low pH ( ⁇ 4.0), pitting corrosion was averted, and corrosion rates were controlled while regaining 100% efficiency.
- This technology can also be utilized in conjunction with other corrosion inhibitors to improve their performance.
- corrosion inhibitors include but are not limited to orthophosphates, polyphosphates, phosphonates, zinc and azoles.
- the instant treatment technology could, and in many cases would be utilized with other water treatments such as deposit control agents, corrosion inhibitors and microbiological control agents. It is to be understood that while a certain form of the invention is illustrated, it is not to be limited to the specific form or arrangement of parts herein described and shown. It will be apparent to those skilled in the art that various changes may be made without departing from the scope of the invention and the invention is not to be considered limited to what is shown and described in the specification and drawings.
Abstract
Description
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Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
AU7001901A AU7001901A (en) | 2000-06-22 | 2001-06-21 | Corrosion control utilizing a hydrogen peroxide donor |
MXPA02012886A MXPA02012886A (en) | 2000-06-22 | 2001-06-21 | Corrosion control utilizing a hydrogen peroxide donor. |
CA002413888A CA2413888A1 (en) | 2000-06-22 | 2001-06-21 | Corrosion control utilizing a hydrogen peroxide donor |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US60376400A | 2000-06-22 | 2000-06-22 | |
US09/603,764 | 2000-06-22 |
Publications (2)
Publication Number | Publication Date |
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WO2001098558A2 true WO2001098558A2 (en) | 2001-12-27 |
WO2001098558A3 WO2001098558A3 (en) | 2002-07-04 |
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Application Number | Title | Priority Date | Filing Date |
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PCT/US2001/019783 WO2001098558A2 (en) | 2000-06-22 | 2001-06-21 | Corrosion control utilizing a hydrogen peroxide donor |
Country Status (5)
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US (1) | US6645400B2 (en) |
AU (1) | AU7001901A (en) |
CA (1) | CA2413888A1 (en) |
MX (1) | MXPA02012886A (en) |
WO (1) | WO2001098558A2 (en) |
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Also Published As
Publication number | Publication date |
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US20020043650A1 (en) | 2002-04-18 |
WO2001098558A3 (en) | 2002-07-04 |
MXPA02012886A (en) | 2003-05-14 |
CA2413888A1 (en) | 2001-12-27 |
AU7001901A (en) | 2002-01-02 |
US6645400B2 (en) | 2003-11-11 |
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