Title of Invention

A WATER ELECTROLYSER DEVICE AND A METHOD THEREOF

Abstract

The invention relates to a flame based method for analyzing a sample by introducing the sample into an enclosure including a combustible gas mixture, comprising the steps of: generating by means of a water electrolyser a premixed hydrogen and oxygen gas mixture, said water electrolyser being capable of providing the gas mixture require for sustaining a flame; stabilizing the output flow rate of said premixed gas mixture for reducing the flame background noise; heating said enclosure to a temperature sufficient for preventing water condensation in said enclosure; feeding said mixture via a flame source having an opening sufficiently small for preventing a flame flashback towards said electrolyser; igniting said gas mixture to produce a flame, and detecting a characteristic of the resulting flame to determine the identity and/or concentration of one or more chemical substances in the sample.

Full Text

FORM 2 THE PATENT ACT 1970 (39 Of 1970) The Patents Rules, 2003 COMPLETE SPECIFICATION (See Section 10, and rule 13) TITLE OF INVENTION A METHOD FOR ANALYZING A SAMPLE BY INTRODUCING THE SAMPLE INTO AN ENCLOSURE INCLUDING A COMBUSTIBLE GAS MIXTURE; 2. APPLICANT(S) a) Name b) Nationality c) Address CHEMITO TECHNOLOGIES PVT. INDIAN Company 8, MOHATTA BHAVAN, OFF DR. E. MOSES ROAD, WORLI, MUMBAI - 400 018 MAHARASHTRA LTD. 3. PREAMBLE TO THE DESCRIPTION The following specification particularly describes invention and the manner in which it is to be performed : the The invention relates to a new Gas Chromatographic detector based on the provision of a low flow rate of a premixed gas mixture of oxygen and hydrogen, provided by a water electrolyzer device. Basic Principle The Electrolyser powered Flame Ionization Detector (EFID) is based on the combustion of a premixed, stoichiometric, hydrogen and oxygen gas mixture, at a low flow rate, without make-up gas. This gas mixture is provided from a water electrolyser, without any gas separation or compression. The water electrolyser is very reliable (no moving parts and no gas separation or compression) and it can be integrated into the GC. Its sensitivity is even slightly improved as compared to a FID due to higher flame chemical ionization yield. Introduction The flame ionization detector (FID) is the most widely used detector for gas chromatography (GC) and is also used as a stand-alone monitor of the total hydrocarbon concentration in air. Although very effective, the FID typically consumes 30 ml/min of hydrogen, 30 ml/min of helium make-up gas and 300-400 ml/min of pure air. Clearly, it is highly desirable to eliminate these gases, their cylinders, pneumatics and safety hazards from the FID and GC. A new type of FID was developed, based on the provision of a low flow rate of an unsprayed gas mixture of oxygen and hydrogen, provided by a water electrolyser. This electrolyser-powered FID (EFID) considerably simplifies the gas logistics of GC-FID, improves its operational safety, reduces the cost of analysis and significantly improves its transportability. The EFID is operated with a combustible gas mixture produced by water electrolyser, without gas separation or compression. The Electrolyser powered FID 2 (EFID) is based on the combustion of a premixed, Stoichiometric, hydrogen and oxygen gas mixture, at a low flow rate, without make-up gas. The EFID gas exit is heated to a temperature above 100°C. The small water electrolyser has a diameter of 150 mm, a height of 235 mm. This electrolyser typically requires 2.3 Ampere at 2.0 Volts (4.5 Watts) consumes ~ 15 ml water per day and enables 30 days of continuous operation. The electrolyser requires only water, with no drying material, and enables full EFID automation for years of unattended operation. The water electrolyser can be fully integrated with the GC and replace the FID three channels electronic flow control. The EFID efficiency is about 60 milli Coulomb/gram C. The EFID shows close to uniform carbon response with linear dynamic range of Six orders of magnitude. Accordingly there is provided; A flame detector for analyzing a sample based on the provision of a combustible gas mixture, comprising the steps of: generating by means of a water electrolyser a premixed hydrogen and oxygen gas mixture, said water electrolyser being capable of providing the gas mixture required for solely sustaining a flame; stabilizing the output flow rate of said premixed gas mixture for reducing the flame background noise; heating said detector to a temperature sufficient for preventing water condensation ; feeding said mixture via a jet having an opening sufficiently small for preventing a flame flashback; igniting said gas mixture to produce a flame, and detecting a characteristic of the resulting flame to determine the identity and/or concentration of one or more chemical substances in the sample. The invention will now be described with figure 1 in the accompanying drawing. Figure 1 is the perspective view of the electrolyser; Referring to figure 1 consists of an electrolyser cell (1) with water inlet (2) and studs for electric connection (6). The released gases; premixed hydrogen and oxygen gas mixture is passed through a silica gel filter unit at (3). A 6-way Bakelite connector (4) is attached to the body of the cabinet. 3 Basic Specifications • Base temp.: 200 to 450°C • Gas outlet temp.: 100 to 160°C • Sensitivity: 2pg/sec • Dynamic range: 107 • Water consumption: ~15ml/24hrs at 2.3 Amp. • Water capacity: ~ 520 ml • Air pump flow rate: 70 to 80 ml/min Description of Electrolyses parts: 1) Electrolyser Cell 2) Water Inlet 3) Silica Gel filter unit 4) Bakelite 6 way Connector 5) Condenser unit 6) Studs for electric connection Operational particulars/ description of manufacturing process Following is the procedure of manufacturing process. In manufacturing process, there are sub processes like material purchasing process, inward inspection process, process of production, calibration and chemical testing process etc. a) Material Purchasing Process 1. Obtain Production plan and stock order. 2. Give requisition to purchase. 3. Place purchase order to the supplier. 4. Receive the material at stores Dept. 5. If there is any commercial discrepancy, then give feedback to purchase Dept. and follow up with the supplier for necessary action. 6. If everything is ok, then send material to QA for inward inspection. 4 7. If the material is accepted as per quality plan, then update records and give to Stores for raw material storage. 8. If material is rejected then give feedback to purchase Dept. and follow up with the supplier for necessary action. b) PCB Manufacturing and testing process 1. Send bare PCB's for assembling with bill of material and components. 2. After receiving PCB's, send to QA for inspection as per quality plan. 3. If PCB's are as per requirements, then test it module wise. c) Process of Production 1. Plan the production activities. 2. Check that adequate resources are available. 3. If all resources are not available, then give input to process of provision of resources. 4. If all resources are available, then start manufacturing. 5. In-process inspection of the product will be done at designated stages of production. 6. If product is not accepted then take necessary corrective action and retest. 7. If product is ok / valid, then start further process. 8. After completion of product, final inspection to be done. 9. If inspection results are not valid, then provide input to process of control of non-conforming product. d) Calibration & chemical testing process 1. Identify test & measurement requirement 2. Identify equipment required, 3. Prepare master list of solution and any other material required for Chemical testing and 5 plan for calibration. 4. Once calibration is done, start to analyze the samples 5. After completion of analysis, store the result and update the records. 6. If all results are valid & ok then send it for evolutions. 7. Check confirmation of product against customer requirement is fulfilled. 8. Once evaluation is through, arrange delivery to customer. The water electrolyser device having water mist and vapor pressure management system comprises a solid state Peltier cooling element. The water electrolyser device having Peltier cooling element is operative to reduce the temperature of the cooled volume by 5 or more degrees C below the room temperature. The water electrolyser device having Peltier cooling element is cooled through heat conductivity to the electrolyser external box surface, which surface is air cooled by heat conductivity to the room air. The water electrolyser device having water mist and vapor pressure management system further comprises means for the removal of dust and/or small droplets produced by the drying of water mist. The water electrolyser device having means for the removal of dust produced by the drying of water mist is based on porous material. Water electrolyser further comprises means for measuring the amount of residual water inside said water electrolyser, to enable replenishment thereof before its total consumption. The water electrolyser device further comprises means for automated water replenishment. 6 The water electrolyser device comprises check valve means, at least indirectly connected to said water container, for increased safety. The water electrolyser device wherein said water electrolyser further comprises means for stabilizing the flow rate of the output premixed oxygen and hydrogen gas mixture. The water electrolyser device wherein said water electrolyser further comprises means for provision of room air into said flame ionization detector. A water electrolyser device for generating hydrogen gas and for directing said. hydrogen gas into a flame ionization detector, said device comprising:00,nb water container means for performing water electrolyser; electrode means for passing electrolyser current in the water; means for separating hydrogen from co-produced oxygen; and a water mist and vapor pressure management system for the elimination of water mist and reduction of the water relative humidity below the saturation point, said system being located between said water electrolyser and said flame ionization detector. A method based on water electrolyser for the provision of a combustible gas mixture for the operation of a flame ionization detector, said method comprising the steps of: generating, by means of a water electrolyser, a premixed, combustible hydrogen and oxygen gas mixture; reducing water mist and relative humidity below saturation level, without the use of replaceable adsorbing material, in order to prevent water condensation in the flow path of said gas mixture to said flame ionization detector; and irecting flow of combustible gas mixture into said flame ionization detector. 7 The water electrolyser based method wherein said flow of combustible gas mixture is passed through an adsorbing material for the removal of dust and/or small droplets produced by the drying of said water mist. A method based on water electrolyser wherein said flow of combustible gas mixture is stabilized. Comparison of New Invention over Conventional one A conventional FID operates with a hydrogen diffusion flame, which has a central flow of pure hydrogen and column effluents, surrounded by a much higher coaxial flow of pure air. In contrast, the EFID is based on the combustion of a premixed hydrogen and oxygen, stoichiometric gas mixture. This premixed gas mixture is provided by a simple water electrolyser with low power and water consumption, without separation, compression, or pressure stabilization of the hydrogen and oxygen. The EFID has two modifications: (a)The flame tip must have a narrow hole (250 um) to prevent flame flash-backs. (b)The entire detector structure is maintained above 100°C to prevent water condensation due to the lack of diluting air. Up to twice improved detection can be achieved with the EFID. The flame chemical ionization yield of the EFID linearly increases with the electrolyser current. The EFID response is linear over almost 7 orders of magnitude. The response is selective to carbon compounds where the response in aliphatic compounds is ~ 30% lower than with aromatic compounds, and no observable difference for N-, S-, P-, and Cl-containing compounds. The use of split less solvent injections with a mega bore column (0.53 mm i.d.) quenches the flame. This flame extinction is eliminated by the use of a miniature air pump during the solvent elution time. Typical electrolyser operating parameters are current of 2.3 A, ~15 mL/day water consumption and 4.5 W electrolyser power requirements. 8 Benefits of invention Over Conventional One The benefits of the EFID compared to the conventional FID are: • The EFID Eliminates all the gas cylinders from the FID, while retaining all its features that made FID the GC industry standard detector. • Saves gases and maintenance cost more than the price of the GC in its lifetime • Frees precious laboratory space occupied by gas cylinders and their service path. • Considerably simplifies the purchase and installation of GC-FID • Simplifies GC-FID maintenance and makes it much easier to use. • Enables a new dimension of GC-FID transportability. • Is slightly more sensitive than the standard FID • The EFID does not require any makeup gas. • Enables full gas cylinder free GC-FID operation for gases, VOCS and breath analysis applications. 9 WE CLAIM: 1. A flame based method for analyzing a sample by introducing the sample into an enclosure including a combustible gas mixture, comprising the steps of: generating by means of a water electrolyser a premixed hydrogen and oxygen gas mixture, said water electrolyser being capable of providing the gas mixture require for solely sustaining a flame; stabilizing the output flow rate of said premixed gas mixture for reducing the flame background noise; heating said enclosure to a temperature sufficient for preventing water condensation in said enclosure; feeding said mixture via a flump source having an opening sufficiently small for preventing a flame flashback towards said electrolyser; igniting said gas mixture to produce a flame, and detecting a characteristic of the resulting flame to determine the identity and/ or concentration of one or more chemical substances in the sample. 2. A water electrolyser device for generating a premixed hydrogen and oxygen gas mixture and for directing said gas mixture into a flame ionization detector, said device comprising: water container means for performing water electrolyser; electrode means for passing electrolyser current in the water; and a water mist and vapor pressure management system for the elimination of water mist and reduction of the water relative humidity below the saturation point, said system being located between said water electrolyser and said flame ionization detector. 3. The water electrolyser device according to claim 1, wherein said water mist and vapor pressure management system comprises a solid state Peltier cooling element. 10 4. The water electrolyser device according to claim 2, wherein said Peltier cooling element is operative to reduce the temperature of the cooled volume by 5 or more degrees C below the room temperature. 5. The water electrolyser device according to claim 2, wherein said Peltier cooling element is cooled through heat conductivity to the electrolyser external box surface, which surface is air cooled by heat conductivity to the room air. 6. The water electrolyser device according to claim 1, wherein said water mist and vapor pressure management system further comprises means for the removal of dust and/or small droplets produced by the drying of water mist. 7. The water electrolyser device according to claim 5, wherein said means for the removal of dust produced by the drying of water mist is based on porous material. 8. The water electrolyser device according to claim 1, wherein said water electrolyser further comprises means for measuring the amount of residual water inside said water electrolyser, to enable replenishment thereof before its total consumption. 9. The water electrolyser device according to claim 1, wherein said water electrolyser further comprises means for automated water replenishment. 10. The water electrolyser device according to claim 1, wherein said water electrolyser further comprises check valve means, at least indirectly connected to said water container, for increased safety. 11 11. The water electrolyser device according to claim 1, wherein said water electrolyser further comprises means for stabilizing the flow rate of the output premixed oxygen and hydrogen gas mixture. 12. The water electrolyser device according to claim 1, wherein said water electrolyser further comprises means for provision of room air into said flame ionization detector. 13. A water electrolyser device for generating hydrogen gas and for directing said hydrogen gas into a flame ionization detector, said device comprising:00,nb water container means for performing water electrolyser; electrode means for passing electrolyser current in the water; means for separating hydrogen from co-produced oxygen; and a water mist and vapor pressure management system for the elimination of water mist and reduction of the water relative humidity below the saturation point, said system being located between said water electrolyser and said flame ionization detector. 14. A method based on water electrolyser for the provision of a combustible gas mixture for the operation of a flame ionization detector, said method comprising the steps of: generating, by means of a water electrolyser, a premixed, combustible hydrogen and oxygen gas mixture; reducing water mist and relative humidity below saturation level, without the use of replaceable adsorbing material, in order to prevent water condensation in the flow path of said gas mixture to said flame ionization detector; and directing flow of combustible gas mixture into said flame ionization detector. 15. The water electrolyser based method according to claim 13, wherein said flow of combustible gas mixture is passed through an adsorbing material for the 12 removal of dust and/or small droplets produced by the drying of said water mist. 16. A method based on water electrolyser according to claim 13, wherein said flow of combustible gas mixture is stabilized. Dated this 10th day of April, 2007. 13

Documents:

749-MUM-2007-CANCELLED PAGES(10-06-2010).pdf

749-MUM-2007-CANCELLED PAGES(14-3-2011).pdf

749-MUM-2007-CANCELLED PAGES(30-11-2010).pdf

749-MUM-2007-CANCELLED PAGES(7-6-2012).pdf

749-MUM-2007-CLAIMS(AMENDED)-(10-06-2010).pdf

749-MUM-2007-CLAIMS(AMENDED)-(14-3-2011).pdf

749-MUM-2007-CLAIMS(AMENDED)-(30-11-2010).pdf

749-mum-2007-claims.pdf

749-mum-2007-claims.rtf

749-MUM-2007-CORRESPONDENCE(17-8-2010).pdf

749-MUM-2007-CORRESPONDENCE(29-09-2010).pdf

749-MUM-2007-CORRESPONDENCE(7-6-2012).pdf

749-mum-2007-correspondence-received.pdf

749-mum-2007-description (complete).pdf

749-mum-2007-drawings.pdf

749-MUM-2007-FORM 1(10-06-2010).pdf

749-MUM-2007-FORM 1(30-11-2010).pdf

749-MUM-2007-FORM 1(7-6-2012).pdf

749-MUM-2007-FORM 13(7-6-2012).pdf

749-MUM-2007-FORM 2(TITLE PAGE)-(10-06-2010).pdf

749-MUM-2007-FORM 2(TITLE PAGE)-(30-11-2010).pdf

749-MUM-2007-FORM 5(7-6-2012).pdf

749-mum-2007-form-1.pdf

749-mum-2007-form-2.doc

749-mum-2007-form-2.pdf

749-mum-2007-form-3.pdf

749-MUM-2007-GENERAL POWER OF ATTORNEY(14-3-2011).pdf

749-MUM-2007-REPLY TO EXAMINATION REPORT(10-06-2010).pdf

749-MUM-2007-REPLY TO EXAMINATION REPORT(30-11-2010).pdf

749-MUM-2007-REPLY TO HEARING(14-3-2011).pdf