TR201613170A1 - AN ELECTRODE FOR USING PHOSPHATE DETERMINATION AND A METHOD FOR ELECTRODE PRODUCTION - Google Patents

AN ELECTRODE FOR USING PHOSPHATE DETERMINATION AND A METHOD FOR ELECTRODE PRODUCTION Download PDF

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TR201613170A1
TR201613170A1 TR2016/13170A TR201613170A TR201613170A1 TR 201613170 A1 TR201613170 A1 TR 201613170A1 TR 2016/13170 A TR2016/13170 A TR 2016/13170A TR 201613170 A TR201613170 A TR 201613170A TR 201613170 A1 TR201613170 A1 TR 201613170A1
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electrode
molybdenum blue
blue
molybdenum
modified
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Şahi̇n Yücel
Beşi̇r Arvas(%33) Meli̇h
Koyun(%33) Özge
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Melih Besir Arvas %33
Oezge Koyun %33
Yuecel Sahin
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Priority to TR2016/13170A priority Critical patent/TR201613170A1/en
Priority to GB1902974.3A priority patent/GB2567993B8/en
Priority to DE112017004744.7T priority patent/DE112017004744T5/en
Priority to PCT/TR2017/000089 priority patent/WO2018056931A2/en
Publication of TR201613170A1 publication Critical patent/TR201613170A1/en

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28Electrolytic cell components
    • G01N27/30Electrodes, e.g. test electrodes; Half-cells
    • G01N27/333Ion-selective electrodes or membranes
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D9/00Electrolytic coating other than with metals
    • C25D9/04Electrolytic coating other than with metals with inorganic materials
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/416Systems
    • G01N27/4166Systems measuring a particular property of an electrolyte
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/416Systems
    • G01N27/48Systems using polarography, i.e. measuring changes in current under a slowly-varying voltage
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/18Water
    • G01N33/182Specific anions in water

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  • Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)
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Abstract

Buluş, fosfat tayinini istenilen her yerde, hızlı, düşük maliyetli ve kolay gerçekleştirmek üzere enzim kullanılmadan geliştirilmiş bir yöntem(500) ve bu yöntem(500) ile üretilen bir molibden mavisi elektrot ile ilgilidir.The invention relates to an improved method 500 and a molybdenum blue electrode produced by this method 500 to perform phosphate determination wherever desired, quickly, cost-effectively and easily.

Description

TARIFNAME FOSFAT TAYININDE KULLANILMAK UZERE BIR ELEKTROT VE ELEKTROT URETIMI IÇIN BIR YONTEM Bulusun Ilgili Oldugu Teknik Alan: Bulus, fosfat tayininde kullanilmak üzere üretilinis bir elektrot ve bu elektrodun üretiin yöntemi ile ilgilidir. DESCRIPTION AN ELECTRODE FOR PHOSPHATE DETERMINATION AND A METHOD FOR ELECTRODE PRODUCTION Technical Field of Invention: The invention is an electrode manufactured for use in phosphate determination and the production of this electrode. relates to method.

Onceki Teknik: Göl, gölet ve biyolojik yasam parklarinda canlilarin hayat döngüsü ve tür çesitliliginin kalitesini artirmak için fosfat kontrolünün yapilinasi gerekmektedir. Ayrica tarimda tahillarin ve diger ürünlerin gelismesinde fosfatin önemi büyüktür. Fosfat miktarinin fazla Oldugu topraklarda bitki zarar görmekte, verim azalmakta ve yapilan sulamalar sonucunda bitki bünyesinde artan fosfat sebebiyle su, bitki bünyesinde dogru tasinainainakta ve bitkide çürüme gerçeklesmektedir. Fosfat miktarindaki eksiklik durumunda ise bitki türüne ve eksiklik oranina bagli olarak farkli belirtiler görülse de genel olarak; özellikle yasli yapraklarda sararma, kalin ve dik yaprak görünümü, bodur büyüme, mavimsi yesil veya mor renk olusumu tipiktir. Bitkilerde fosfat yetersizligi sebebiyle bitkilerin meyve tutumlari zayiflamakta ve meyvelerin olgunlasmasi erken olmakta, meyvelerde sekil bozuklugu ve çatlaklar olusmaktadir. Sayilan tüin bu sebeplerden fosfatin tayin edilmesi önemli olmaktadir. Previous Technique: The life cycle of living things and species diversity in lakes, ponds and biological life parks. Phosphate control should be done in order to improve its quality. Also in agriculture Phosphate is of great importance in the development of cereals and other products. Too much phosphate The plant is damaged in the lands where it is located, the yield decreases and as a result of the irrigations. Due to the increased phosphate in the plant, the water is transferred to the correct transport within the plant and rotting occurs in the plant. In case of deficiency in the amount of phosphate, the plant Although different symptoms are seen depending on the type and deficiency rate, in general; especially yellowing of old leaves, appearance of thick and upright leaves, stunted growth, bluish green or purple color formation is typical. Fruiting of plants due to phosphate deficiency in plants attitudes are weakening and the ripening of the fruits is early, the shape of the fruits defects and cracks occur. Determination of phosphate for these reasons becomes important.

Teknolojide sensörlerin kullanimi yayginlasmadan önce fosfat tayini yas (wet) analiz ve spektroskopik yöntemler kullanilarak yapilmaktaydi. Ancak kullanilan bu geleneksel yöntemler fosfat tayini için yüksek maliyet ve uzman personel gerektiren, zaman alici, sarf ihtiyacinin fazla oldugu, tayin bölgesinin (yani yöntemin Ölçebilecegi en küçük konsantrasyon miktarinin) yeterli olmadigi ve yerinde analiz imkâni sunamayan yöntemlerdir. Bu yöntemlerin uygulandigi cihazlar pratik ve tasinabilir yani portatif olmadigindan fosfat tayinini spektroskopik yöntemler ile yerinde analiz etmek zordur. Before the use of sensors in technology became widespread, phosphate determination, wet analysis and was done using spectroscopic methods. However, this traditional The methods are time consuming, consumable, requiring high cost and expert personnel for phosphate determination. where the need for the determination is greater (i.e. the smallest that the method can measure) concentration amount) is not sufficient and cannot provide on-site analysis. are methods. The devices in which these methods are applied are practical and portable. It is difficult to analyze the phosphate determination in situ by spectroscopic methods because there is no

Teknigin bilinen durumunda yer alan bu spektroskopik yöntemlere ek olarak teknigin bilinen durumunda yer alan bir diger yöntemde tüm dünyada kullaniini giderek artan sensörler ile elektro-inaktif ve inorganik bir tür olan fosfatin belirlenmesi de mümkündür. In addition to these spectroscopic methods, which are in the state of the art, the technique Another method, which is in its known state, is increasingly used all over the world. It is also possible to detect phosphate, an electro-inactive and inorganic species, with sensors.

Ancak, mevcut bu tip sensörlerin üretilniesinde enzim veya enzim sistemleri kullanildigi için bu sensörlerin kullanimi, sicaklik ve pH degisimlerinden kolaylikla etkilenmektedirler. Dolayisiyla fosfat tayini için kullanilan enzim temelli potansiyometrik sensörlerin, kullaiiim anina kadar oda kosullarinda yapisi bozulmadan muhafaza edilmeleri güçtür. However, it is known that enzyme or enzyme systems are used in the production of these types of sensors. The use of these sensors for temperature and pH changes easily they are affected. Therefore, enzyme-based potentiometry used for phosphate determination Keep the sensors intact under room conditions until the moment of use. they are difficult to get.

Onceki teknikte her ne kadar fosfat tayini sensörler ile yapilsa da fosfatin elektro-inaktif bir tür olmasi sebebiyle elektrokimyasal olarak tayini zordur. Although phosphate determination was made with sensors in the previous technique, phosphate is electro-inactive. It is difficult to determine electrochemically because it is a species.

Teknigin bilinen durumunda yer alan U85252486 numarali patent dokümaninda inorganik fosfat için akis enjekte analizi yönteminden bahsedilmektedir. In the patent document numbered U85252486, which is in the state of the art, inorganic The flow-injection analysis method for phosphate is mentioned.

Bulusun Kisa Açiklamasi: Bulusun amaci fosfat oldugu düsünülen çözeltilerde fosfat tayiiiiiii elektrokiinyasal olarak dogru ve hizli yapabilmesi için bir elektrot ve bu elektrodun üretim yöntemini gerçeklestirmektir. Brief Description of the Invention: The aim of the invention is to detect phosphate transport electrochemically in solutions thought to be phosphate. an electrode and the production method of this electrode so that it can be made accurately and quickly. is to perform.

Bulus konusu yöntemle(500) enzim kullanilmadan fosfat tayininde kullanilmak üzere bir inolibden mavisi modifiye elektrot üretilmistir.. To be used in the determination of phosphate without using enzymes with the method of the invention (500), Inolybdenum blue modified electrode has been produced.

Amaca yönelik olarak bulus ile bir uygulamada çalisma elektrodu olarak karbon temelli elektrot kullanildiginda elde edilen elektrot molibden inavisi modifiye karbon temellidir. Carbon-based as a working electrode in an application with the invention for purpose. The electrode molybdenum invisibility obtained when the electrode is used is based on modified carbon.

Bulusun bir diger uygulamasinda çalisma elektrodu olarak inert metal elektrot kullanildiginda elde edilen elektrot molibden mavisi modifiye inert metal elektrottur. In another embodiment of the invention, an inert metal electrode as a working electrode The electrode obtained when used is a molybdenum blue modified inert metal electrode.

Uygulamalara göre bu elektrotlardan herhangi biri fosfat tayini yapilmak istenen çözeltiye daldirilarak ve diferansiyel puls voltainetri yöntemi kullanilarak fosfat tayini hizli ve ucuz bir sekilde yapilmaktadir. Diferansiyel puls voltametrisi, dönüsümlü voltametri yöntemi ile hazirlanan elektrodun sensör cevabinin incelendigi yöntemdir. According to the applications, any of these electrodes can be applied to the solution for which phosphate determination is desired. Determination of phosphate by immersion and using differential pulse voltainetry is fast and inexpensive. is done in one go. Differential pulse voltammetry, alternating voltammetry method It is the method in which the sensor response of the electrode prepared with

Bulus konusu yöntem ile elektro-inaktif bir tür olan fosfat tayini enzim kullanilinadan yani non-enzimatik olarak yapilmaktadir. Çesitli nuinunelere bulusun uygulamalarina göre molibden mavisi modifiye karbon temelli elektrot veya molibden mavisi modifiye inert metal elektrot daldirilarak yapilan ölçümlerde es zamanli, hizli ve uzman personel gerektirmeden fosfatin tayini yapilabilmektedir. With the method of the invention, the determination of phosphate, which is an electro-inactive species, is done without using enzymes, that is. It is made non-enzymatically. According to the applications of the invention to various samples molybdenum blue modified carbon-based electrode or molybdenum blue modified inert Simultaneous, fast and expert personnel in measurements made by immersing metal electrodes Phosphate can be determined without the need for

Ayrica bulus ile bir uygulamada elde edilen molibden mavisi modifiye karbon temelli elektrot kullanilarak modifiye edilmis bir sensör elde edilmistir. Bir diger uygulamada elde edilen molibden mavisi modifiye inert metal elektrot kullanilarak modifiye edilmis bir sensör elde edilmistir. Karbon temelli elektrodun kullanilmasi ile bu elektrodun daha düsük inaliyette ve daha kolay bulunmasi ve ayrica tek kullanimlik olmasi gibi avantajlari bulunmaktadir. Tek kullanimlik karbon temelli elektrot kullanilarak bulusta, fosfatin ve diger maddelerin yükseltgenmesinden kaynaklanan elektrot kirliliginin temizlenmesi de mümkün olmaktadir. In addition, molybdenum blue obtained in an application with the invention is based on modified carbon. A modified sensor was obtained using an electrode. In another application The obtained molybdenum blue was modified using a modified inert metal electrode. a sensor is obtained. With the use of a carbon-based electrode, this electrode is more It has advantages such as low cost and easier to find and also single use. are available. In the invention, using a disposable carbon-based electrode, phosphate and Cleaning of electrode pollution caused by oxidation of other substances is also is possible.

Bulusun Ayrintili Açiklamasi: Sekillerin Açiklanmasi Sekil-1: Yöntemde kullamlan üç elektrotlu düzenegin seinatik görünüsüdür. Detailed Description of the Invention: Explanation of Figures Figure-1: The seinatic view of the three-electrode device used in the method.

Sekil-2: Bulus konusu molibden mavisi modifiye elektrodun üretim yönteminin akis diyagramidir. Figure-2: The reflection of the production method of the molybdenum blue modified electrode, which is the subject of the invention is the diagram.

Sekillerdeki referanslarin açiklamasi: Bulusun anlasilabilir olmasina yönelik olarak ekli sekillerdeki parçalara tek tek referans numaralari verilmis olup bu numaralarin karsiligi asagida verilmistir. 1. Düzenek . Çalisma elektrodu 1 l. Destek Elektrolit 12. Karsi elektrot 13. Referans elektrot 14. Voltaj veya Akim Kaynagi/Ölçüm Cihazi Bulus konusu inolibden mavisi elektrot, bir çalisma elektrodundan (10) bulus konusu yöntein (500) ile elde edilmektedir. Explanation of references in the figures: Individual reference to the parts in the accompanying figures for clarity of the invention numbers are given and the corresponding numbers are given below. 1. Assembly . working electrode 1 liter Support Electrolyte 12. Counter electrode 13. Reference electrode 14. Voltage or Current Source/Meter The subject of the invention is the inolybdenum blue electrode, the subject of the invention from a working electrode (10). It is obtained with the method (500).

Fosfat tayininde kullanilmak üzere bir çalisnia elektrodunun(10) molibden mavisi ile kaplanmasi ile modifiye bir elektrot elde edilmistir. To be used in the determination of phosphate, a working electrode (10) was mixed with molybdenum blue. A modified electrode was obtained by coating it.

Bulus konusu yöntem(500) 'üç elektrotlu bir düzenekte(l) uygulanmaktadir. Uç elektrotlu düzenek(l), bir referans elektrodu (13) bir karsi elektrot(12) (ve bir çalisma elektrodu(10) içermektedir. Çalisma elektrodu(10) bulusun bir uygulamasinda inert inetal elektrottur. The method (500) of the invention is applied in a three-electrode device (1). with end electrode assembly (1), a reference electrode (13), a counter electrode (12) (and a working electrode (10) contains. The working electrode (10) is an inert inert electrode in one embodiment of the invention.

Bulusun bir diger uygulamasinda çalisina elektrodu(10) karbon temelli elektrottur. Söz konusu çalisma elektrodundan(10) inolibden mavisi modifiye elektrot üretildikten sonra inolibden mavisi modifiye elektrot fosfat tayini yapmak için bir sensör olarak kullanilabilinektedir. Sözü geçen sensör kolaylikla analiz yapilinasi istenen yerlere tasiiiabilmektedir. Çalisma elektrodu(10) olarak karbon temelli elektrotlarin kullanilmasi ve bu elektrotlariii ucuz olmasi, tek kullanimlik olniasi ve modifiye edilebilmesi büyük avantajdir. Elektrodun modifiye edilmesi, baslangiçtaki çalisma elektroduna inolibden mavisinin kaplanmasi ile son elektrot yani molibden mavisi elektroduii elde edilmesidir. In another embodiment of the invention, the working electrode (10) is a carbon-based electrode. Promise After producing the inolybdenum blue modified electrode from the working electrode (10), as a sensor for the determination of inolybdenum blue modified electrode phosphate can be used. The aforementioned sensor is placed in the desired places where analysis can be done easily. can be carried. Using carbon-based electrodes as working electrode(10) And these electrodes are cheap, disposable, and modifiable. is an advantage. Modifying the electrode adds inolybdenum to the initial working electrode. The last electrode, that is, molybdenum blue electrode, is obtained by coating the blue.

Elde edilen molibdeii mavisi modifiye elektrot ile fosfat tayini yapilmaktadir. Inert inetal elektrotlar ile de modifikasyon isleini kolaylikla gerçeklesebilmektedir. Phosphate determination is made with the obtained molybdeii blue modified electrode. inert Modification can be easily performed with electrodes.

Bulus konusu yöntemde(500) kullanilan çözeltilerin hiç birinde enzim kullanilmamistir. No enzyme was used in any of the solutions used in the method (500) of the invention.

Fosfatin analizinin yapilabilmesi için (örnegin toprakta) topragin ön islemlerden geçip kati halden sivi hale getirilmesi yani analize hazirlanmasi gerekmektedir. Bu hazirlik sonucu elde edilen son ortam diger bir ifadeyle analizin yapildigi ortam çözelti (numune) ortamidir. In order to be able to analyze the phosphate (for example, in the soil), the soil must be pre-treated and solid. It must be made liquid from state, that is, it must be prepared for analysis. As a result of this preparation the final medium obtained, in other words, the medium in which the analysis was carried out, the solution (sample) environment.

Bulus konusu molibden mavisi modifiye elektrot asagidaki yöntem(500) adimlarina göre üretilmektedir. The molybdenum blue modified electrode of the invention is according to the following method (500) steps. is produced.

- Onceden belirleninis bir oranda molibden mavisi ve bunu tamamlayan oranda asit çözeltisinden olusan destek elektrolitin (1 l) hazirlanmasi (501) - Hazirlanaii destek elektrolit (1 l) ortamina daldirilaii çalisina elektroduna(lO) önceden belirlenen bir potansiyel araliginda ve önceden belirlenmis bir tarama hizinda bir potansiyel uygulanmasi (502) - Uygulanan potansiyelin etkisi ile destek elektrolit(11) ortaininda çalisma elektroduna(10) inorganik bir tür olan molibden mavisiiiiii kaplanmasi (503) - Molibden mavisi modifiye elektrodun üretilmesi(504) - Molibdeii mavisi modifiye elektrodun destek elektrolit(l l) ortamindan çikarilmasi (505) - Molibden mavisi modifiye elektrodun önceden belirlenmis bir oranda polimer ve bu orani tainamlayan oranda organik çözücü içeren bir polimer ve organik çözücülü karisima daldirilmasi ve böylece molibden inavisi modifiye elektrodun yüzeyinde molibden mavisinin kaliciliginin saglanmasi (506) Yöntemin(500) 501. Adiiniiida sözü geçen molibden inavisinin oraiii %5 ila % 50 araligindadir. - a predetermined proportion of molybdenum blue and a complementary proportion Preparation of supporting electrolyte (1 l) consisting of acid solution (501) - The working electrode(10) that can be immersed in the prepared supporting electrolyte (1 l) environment in a predetermined potential range and a predetermined sweep applying a potential at speed (502) - Working in the middle of the supporting electrolyte (11) with the effect of the applied potential coating the electrode(10) with molybdenum blueiiiiii, an inorganic species (503) - Production of molybdenum blue modified electrode(504) - Molybdeii blue modified electrode from the supporting electrolyte(l l) medium removal (505) - A predetermined ratio of the molybdenum blue modified electrode to the polymer and a polymer and organic solvent containing a proportion of organic solvents exceeding this ratio. immersion in the solvent mixture, thereby modifying the molybdenum ensuring the persistence of molybdenum blue on the surface of the electrode (506) 5% to 50% of said molybdenum inavidin in Method (500) 501. is in the range.

Bulus konusu yöntemin (500) 501. Adiniinda sözü geçen tainainlayan oran, optimum asit miktaridir. Bu miktarin altinda ve üstünde elektrot modifikasyonu olmamaktadir. The carrying ratio mentioned in the 501. Name of the method (500) of the invention is the optimum acidity. is the amount. There is no electrode modification above or below this amount.

Yöntemin(500) 502. adimda çalisma elektroduna(10) uygulanan potansiyel araligi - 2 V ila +2 V dir. The potential range applied to the working electrode (10) in step 502 of the method (500) - 2 V to +2 V.

Yöntemin(500) 502. Adiminda sözü geçen çalisma elektrodu(lO) bulusun bir uygulamasinda karbon temelli elektrot(100), bir diger uygulamasinda inert metal elektrottur. The working electrode (10) mentioned in step 502 of the method (500) is a part of the invention. In one application, carbon-based electrode (100), in another application, inert metal is the electrode.

Yöntemin (500) 506. Adiminda sözü geçen tainainlayan oran Önceden belirlenmis bir polimer oranina karsilik organik çözücünün bu orani tamamlayan oranda olmasidir. Örnegin polimer orani % 5 ise organik çözücü % 95 tir. The retaining ratio mentioned in Step 506 of the method (500) is a predetermined It is the ratio of organic solvent to polymer ratio that completes this ratio. For example, if the polymer ratio is 5%, the organic solvent is 95%.

Bulusun bir uygulamasinda çalisma elektrodu(lO) olarak karbon temelli elektrot (100) kullanilmissa yöntemle (500) üretilen elektrot molibden mavisi karbon temelli elektrottur. In an embodiment of the invention, carbon-based electrode (100) as the working electrode (10) If used, the electrode produced by the method (500) is a molybdenum blue carbon-based electrode.

Bulusun bir diger uygulamasinda çalisma elektrodu(lO) olarak inert inetal elektrot kullanilmissa yöntemle (500) üretilen elektrot inolibden mavisi inert metal elektrottur. In another application of the invention, inert inetal electrode as the working electrode (10) If used, the electrode produced by the method (500) is an inolybdenum blue inert metal electrode.

Bulusun uygulamalarina göre üretiini tamamlanan molibden mavisi modifiye karbon temelli veya molibden mavisi inert inetal elektrodun sensör olarak kullanilmasi ile fosfat tayini yapilmaktadir. Fosfat tayini söz konusu elektrotlardaii birinin içerisinde fosfat oldugundan süphelenilen çözeltilere daldirilmasi ve sonrasinda diferansiyel puls voltametri yöntemi kullanilarak gerçeklestirmektedir. Molybdenum blue modified carbon manufactured according to the applications of the invention phosphate-based or molybdenum blue inert inert electrode as a sensor. appointment is made. Phosphate determination in one of the mentioned electrodes immersion in suspected solutions and then differential pulse performed using the voltammetry method.

Fosfat tayini, hazirlanan çalisma elektotlar1(10) araciligi ile ve diferansiyel puls voltainetri yönteini ile yapilmaktadir. Diferansiyel puls voltametri eser miktardaki organik, inorganik ve metalik iyon türlerin tayini için son derece kullanisli bir yöntemdir. Bu yönteinde lineer olarak artmakta olan gerilim üzerine sabit siddette bindirileii pulslar, istenilen zaman araliklarinda çalisma elektroduna(10) uygulaiimaktadir. Bu yöntemde akim, puls uygulainasindan heinen önce ve puls uygulamasinin sonuna dogru yani yükleine akiminin yaklasik sifir oldugu durumda olinak üzere iki kez ölçülmektedir. Akimlar arasindaki fark gerilime karsi grafige geçirildiginde pik seklinde bir voltainogram elde edilmektedir. Phosphate determination through the prepared study electrodes1(10) and differential pulse voltainetry is done with the method. Differential pulse voltammetry traces organic, inorganic and it is an extremely useful method for the determination of metallic ion species. In this method, linear The pulses superimposed on the increasing voltage at a constant intensity, at the desired time It is applied to the working electrode (10) at intervals. In this method, current, pulse before the application of the pulse and towards the end of the pulse application, that is, the load current It is measured twice, in the case of approximately zero. difference between currents When graphed against tension, a peak-shaped voltainogram is obtained.

Bulusun uygulamalarina göre çalisma elektrodu(10) olarak kullanilan inert metal elektrot veya karbon temelli elektrot yüzeyine kaplanan molibden mavisinin elektrot yüzeyinde kalici olarak kalabilinesi için molibden mavisi inodifiye elektrot, %5 ila % 50 oraninda polimer ve bunu tamamlayan oranda organik çözücü içeren karisima daldirilmaktadir. Çalisma elektrotlari(10) bu islemden sonra kalici olarak inolibden mavisi ile kaplanarak fosfat. tayininde kullanilabilir hale getirilmistir. Inert metal electrode used as the working electrode (10) according to the applications of the invention or on the electrode surface of molybdenum blue coated on the carbon-based electrode surface. molybdenum blue inodified electrode, 5% to 50% It is dipped into the mixture containing the polymer and the organic solvent in the complementary ratio. After this process, the working electrodes (10) are permanently coated with inolybdenum blue. phosphate. made available for assignment.

Bulus konusu yöntem(500) ile üretilen molibden mavisi modifiye elektrodun fosfat tayini yapilirken hazirlanan molibden mavisi modifiye elektrotlarm polimer ve organik çözücü ortamina daldirilarak ve kurutularak kullanima hazir hale getirilmesi saglanmaktadir. Phosphate determination of the molybdenum blue modified electrode produced by the method of the invention (500) polymer and organic solvent of the molybdenum blue modified electrodes prepared while It is provided to be ready for use by immersing in the environment and drying.

Sonrasinda içeriginde fosfat bulunan analitin çözeltisi hazirlanarak ve 3 elektrotlu sistein kurularak diferansiyel puls voltametri yöntemi ile fosfat tayini yapilmaktadir. Afterwards, a solution of the analyte containing phosphate was prepared and a 3-electrode cysteine solution was prepared. Phosphate is determined by differential pulse voltammetry method.

Bulus konusu yöntemle(500) üretilen molibden mavisi modifiye elektrot ile fosfat tayini enzim ihtiyaci duyulmadan kolaylikla yapilabilmektedir. Ayrica bulus konusu yöntemle (500) elde edilen molibden mavisi modifiye elektrot fosfat tayini yapilinasi için bir sensör olarak kullanilabilecektir. Determination of phosphate with molybdenum blue modified electrode produced by the method of the invention (500) It can be easily made without the need for enzymes. In addition, with the method of the invention, (500) a sensor for the determination of molybdenum blue modified electrode phosphate obtained can be used as

Bulus konusu yöntemde(500) kullanilan destek elektrolit(l l), molibden mavisinin çalisma elektrot yüzeyine iyi bir sekilde kaplaiiinasi için çok önemlidir. Destek elektrolit(11) olarak %5 ila %50 molibden mavisi ve bunu tamamlayan oranda asit çözeltisi ortami kullanilmistir. The supporting electrolyte (11 l) used in the method (500) subject of the invention, is the study of molybdenum blue. It is very important for a good coating on the electrode surface. Support electrolyte(11) 5% to 50% molybdenum blue as an acid solution medium used.

Bulus ile gelistirilen elektrot üretme yönteminin(500), literatürde yer alan diger elektrot üretme yöntemlere göre pek çok avantaji vardir. Bunlar arasinda en önemlisi; bulus kapsaminda bahsi geçen molibden mavisi modifiye elektrot hazirlanmasinda enzim temelli maddelerin kullanilmamasidir. Bulusta bir kimyasal tür olan molibden mavisi, elektrot yüzeyine modifiye ediliyor. Enzim ile kaplanan elektrotlar ile çalismak zor olmakla beraber sicaklik gibi ortam sartlardan dolayi yapilari bozulmakta ve denatüre olabilinektedirler Böylece bulusta enzim kullanilmadigi için üretilen molibden mavisi modifiye elektrodun stabilitesinde ve yapisinda deformasyon meydana gelme süresi enzim temelli molibden mavisi modifiye elektrotlara göre çok daha uzundur. Bulus ile üretilen molibden mavisi modifiye elektrot sensör olarak kullanilabilecektir. Böylece bulus kapsaminda elde edilen fosfat sensörü tayin siniri iyi olan, enzim içermeyen ve oda kosullarinda yapisi bozulmadan kolaylikla muhafaza edilebilen voltametrik yöntem ile hazirlanmis sensörlerdir. The electrode production method (500) developed with the invention is the other electrode production method in the literature. It has many advantages over production methods. The most important among them; meet In the preparation of the molybdenum blue modified electrode mentioned in the scope of substances are not used. Molybdenum blue, a chemical species of the invention, surface is modified. Although it is difficult to work with electrodes coated with enzyme, However, their structure is deteriorated and denatured due to environmental conditions such as temperature. they can be Thus, since no enzyme is used in the invention, the molybdenum blue modified electrode produced Deformation time in stability and structure enzyme based molybdenum much longer than the blue modified electrodes. molybdenum blue produced by the invention The modified electrode can be used as a sensor. Thus, the results obtained within the scope of the invention It has a good phosphate sensor detection limit, does not contain enzymes and has a structure in room conditions. prepared by the voltammetric method, which can be easily preserved without spoiling are sensors.

Bulusun sanayiye uygulanabilirligi Bulus konusu yöntem (500) non-enzimatik yani enzim içermeyen elektrot düzenegiyle fosfatin analizinin yapildigi bir yöntemdir. Bu yöntem ile çok kisa süre içerisinde pek çok numunenin analizi gerçeklestirilebilecek, sanayi alaniiida fosfat tayini için kolaylik saglayacaktir. Ayrica, bulus konusu yöntem(500) ile diger tayin yöntemlerinde kullanilan cihazlara uygulanan ön islem basamaklari uygulanmadan fosfatm analizi gerçeklestirilebilecektir. Mali olarak degerlendirecek olursa hazirlanan fosfat sensörlerinden birinin temel malzemesi olan grafit, ticari elektrotlardan çok daha düsük maliyetlidir. Industrial applicability of the invention The method (500) of the invention is non-enzymatic, that is, enzyme-free electrode arrangement. It is a method of analysis of phosphate. With this method, many Convenience for phosphate determination in industrial area where sample analysis can be performed it will provide. In addition, the method (500) which is the subject of the invention and the other determination methods used Phosphate analysis without applying the pretreatment steps applied to the devices can be realized. Phosphate prepared if financially evaluated Graphite, the base material for one of its sensors, is much lower than commercial electrodes. is costly.

Bulus konusu yöntem(500) ile gelistirilen inolibden mavisi modifiye elektrot ve bu elektrottan elde edilen kolay tasinabilir sensör sayesinde fosfat aiializine ihtiyaç duyulan tarim, ilaç ve gida endüstrisi ile diger sektörlerde hizli, yüksek maliyet gerektirmeyen ve yerinde yani istenilen her yerde analizler yapilabilecektir. The inolybdenum blue modified electrode developed by the method (500) of the invention and this Thanks to the easily portable sensor obtained from the electrode, phosphate aallysis is needed. in agriculture, pharmaceutical and food industry and other sectors, fast, low-cost and analyzes can be made on-site, that is, anywhere desired.

Bulus ile fosfatin tayininde siklikla karsilasilan problemlere çözümler getirilebilecektir. With the invention, solutions to the problems frequently encountered in the determination of phosphate can be found.

Toprak numunelerinde, gübreleme için önemli olan fosfat miktarinin belirlenmesinde yerinde, hizli, düsük maliyetli ve kolay bir analiz gerçeklestirilebilecektir. In determining the amount of phosphate in soil samples, which is important for fertilization. an on-site, fast, low-cost and easy analysis will be possible.

Ayrica, ilaç endüstrisinde, gida sanayisinde, fosfat grubu içeren birçok molekülün kalitatif ve kantitatif analizinde rahatlikla kullanilabilecektir. In addition, in the pharmaceutical industry, in the food industry, many molecules containing phosphate groups are qualitatively and can be easily used in quantitative analysis.

Bulus konusu molibden mavisi modifiye elektrot ve bu elektrottan elde edilen sensör, ticari olarak kullanilan glikometreler gibi portatif bir sensöre dönüstürülebilecektir. The subject of the invention is the molybdenum blue modified electrode and the sensor obtained from this electrode, It can be converted into a portable sensor like commercially used glucometers.

Bulus, yukarida açiklanan uygulamalar ile sinirli olmayip, teknikte uzman kisi kolaylikla bulusun farkli uygulamalarini ortaya koyabilir, Bunlar, bulusun istemler ile talep edilen korumasi kapsaminda degerlendirilmelidir. Önceden belirlenmis bir oranda molibden mavisi ve bunu (11) hazirlanmasi Hazirlanan destek elektrolit (11) ortamina daldirilan çalisma önceden belirlenmis bir tarama hizinda bir potansiyel uygulanmasi tamamlayan oranda asit çözeltisinden olusan destek elektrolitin f' 501 elektrodunallo) önceden belirlenen bir potansiyel araliginda ve f› 502 Uygulanan potansiyelin etkisi ile destek elektrolit(11) ortaminda çalisma elektroduna(10) inorganik birtür olan molibden mavisinin kaplanmasi Molibden mavisi modifiye elektrotun üretilmesi f› 504 Molibden mavisi modifiye elektrotun destek elektrolit(11) ortamindan çikarilmasi f› 505 Molibden mavisi modifiye elektrodun önceden belirlenmis bir oranda polimer ve bu orani tamamlayan oranda organik çözücü içeren bir polimer ve organik çözücülü karisima daldirilmasi ve böylece molibden mavisi modifiye elektrodun yüzeyinde molibden mavisinin kaliciliginin saglanmasi The invention is not limited to the above-described embodiments, but is readily available to the skilled person. may reveal different embodiments of the invention, these are the claims of the invention should be considered under its protection. a predetermined ratio of molybdenum blue and (11) preparation The study immersed in the prepared supporting electrolyte (11) medium. potential at a predetermined scan rate. implementation f' 501 of the supporting electrolyte consisting of acid solution in a complementary ratio Elektrodunallo) in a predetermined potential range and fi 502 Working in support electrolyte (11) environment with the effect of applied potential coating of molybdenum blue, an inorganic species, on the electrode (10) Fabrication of molybdenum blue modified electrode f› 504 Molybdenum blue modified electrode from the supporting electrolyte(11) environment. removal f› 505 a predetermined ratio of molybdenum blue modified electrode. polymer and a polymer containing organic solvents at a complementary ratio and immersion in a mixture with organic solvents and thus molybdenum blue Ensuring the persistence of molybdenum blue on the surface of the modified electrode

Claims (1)

ISTEMLER Istenilen her yerde, hizli, düsük maliyetli ve kolay fosfat tayini gerçeklestirmek üzere, - Onoeden belirlenmis bir oranda molibden mavisi ve bunu tamamlayan oranda asit çözeltisinden olusan destek elektrolitin (1 l) hazirlanmasi (501) - Hazirlanan destek elektrolit (l 1) ortamina daldirilan çalisma elektroduna(10) hizinda bir potansiyel uygulanmasi (502) - Uygulanan potansiyelin etkisi ile destek elektrolit(l l) ortaminda çalisma elektroduna(10) inorganik bir tür olan molibden mavisinin kaplanmasi (503) - Molibden inavisi niodifiye elektrodun üretilmesi(504) - Molibden mavisi modifiye elektrodun destek elektrolit( 1 1) ortamindan çikarilmasi (505) - Molibden mavisi modifiye elektrodun 'Önceden belirlenmis bir oranda polimer ve bu orani tamamlayan oranda organik çözücü içeren bir polimer ve organik çözücülü karisima daldirilmasi ve böylece molibden mavisi modifiye elektrodun yüzeyinde molibden mavisinin kaliciliginin saglanmasi (506) adimlari ile karakterize edilen bir molibden mavisi elektrot üretme yöntemi (500). 501. Adiminda sözü geçen molibden mavisinin oraninin %5 ila % 50 araliktaki bir oran olmasi ile karakterize edilen istem l”deki gibi inolibden mavisi modifiye 502. Adimda sözü geçen çalisma elektrodu(10) olarak karbon temelli bir elektrot(100) kullanilmasi ile karakterize edilen istem 1°deki gibi molibden mavisi modifiye 502. Adimda sözü geçen çalisma elektrodu(10) olarak inert metal bir elektrot kullanilmasi ile karakterize edilen istein lideki gibi molibden mavisi modifiye 502. adimda çalisma elektroduna(10) uygulanan potansiyel araliginin - 2 V ila +2 V olmasi ile karakterize edilen istem l'deki gibi molibden mavisi modifiye elektrot üretme yöntemi (500). 506. Adiminda sözü geçen tamamlayan oran, Önceden belirlenmis bir polimer oranina karsilik organik çözücünün bu orani tamamlayan oranda olmasi ile karakterize edilen istem 1 !deki gibi molibden mavisi modifiye elektrot üretme yöntemi (500). Kullanilan tüm çözeltilerde enzimin kullanilmamasi ile karakterize edilen yukaridaki istemlerden herhangi birindeki gibi bir yöntem(500). Yukaridaki istemlerden herhangi birindeki bir yönteme göre üretilen bir elektrot. Fosfat tayininde kullanilmak üzere bir çalisma elektrodunun(10) molibden mavisi ile kaplanarak elde edildigi bir elektrot. Çalisma elektrodunun(10) inert metal oldugu istem 9°deki gibi bir elektrot. Çalisma elektrodunun(10) karbon temelli oldugu istem 9”deki gibi bir elektrot. Fosfat tayininde kullanilmak üzere istem 8 ila 1 l =den herhangi birindeki gibi bir inolibden mavisi elektrottan elde edilen tasinabilir bir sensör.REQUESTS In order to carry out fast, low-cost and easy phosphate determination wherever desired, - Preparation of supporting electrolyte (1 l) consisting of a predetermined ratio of molybdenum blue and complementary acid solution (501) - Immersed in the prepared supporting electrolyte (l 1) medium Application of a potential to the working electrode(10) at speed (502) - Coating of molybdenum blue, an inorganic species, to the working electrode(10) in the supporting electrolyte(ll) environment with the effect of the applied potential (503) - Production of molybdenum inavi niodified electrode(504) - Molybdenum blue removing the modified electrode from the supporting electrolyte( 11) environment (505) - Immersion of the molybdenum blue modified electrode in a mixture with a polymer and organic solvent containing a predetermined ratio of polymer and organic solvent in a complementary ratio, thus ensuring the permanence of molybdenum blue on the surface of the molybdenum blue modified electrode A molybdenum characterized by the steps (506) Method for producing n-blue electrodes (500). 501. Inolybdenum blue modified as in claim 1, characterized by the ratio of molybdenum blue mentioned in step 502 being between 5% and 50%. As in claim 1, modified molybdenum blue 502. It is characterized by the use of an inert metal electrode as the working electrode (10) mentioned in the step 502. It is characterized by the use of an inert metal electrode as in the above step 502. The potential range applied to the working electrode (10) is -2 V to +2 The method of producing molybdenum blue modified electrode (500) as in claim 1, characterized in that it is V. 506. Molybdenum blue modified electrode production method (500) as in claim 1, characterized in that the said complementary ratio in step 1 is a predetermined polymer ratio versus organic solvent in a ratio that complements this ratio. A method (500) as in any one of the above claims, characterized in that the enzyme is not used in all the solutions used. An electrode produced according to a method in any of the preceding claims. An electrode in which a working electrode (10) is coated with molybdenum blue for use in phosphate determination. An electrode as in claim 9, where the working electrode (10) is an inert metal. An electrode as in claim 9, where the working electrode (10) is carbon-based. A portable sensor obtained from an inolybdenum blue electrode as in any one of claims 8 to 11, for use in phosphate determination.
TR2016/13170A 2016-09-21 2016-09-21 AN ELECTRODE FOR USING PHOSPHATE DETERMINATION AND A METHOD FOR ELECTRODE PRODUCTION TR201613170A1 (en)

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