WO2017130218A1 - Fabrication d'une cartouche d'électrodes de puce en plastique comprenant une membrane de liquide ionique contenant du chlorure d'argent - Google Patents

Fabrication d'une cartouche d'électrodes de puce en plastique comprenant une membrane de liquide ionique contenant du chlorure d'argent Download PDF

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Publication number
WO2017130218A1
WO2017130218A1 PCT/IN2017/050028 IN2017050028W WO2017130218A1 WO 2017130218 A1 WO2017130218 A1 WO 2017130218A1 IN 2017050028 W IN2017050028 W IN 2017050028W WO 2017130218 A1 WO2017130218 A1 WO 2017130218A1
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WIPO (PCT)
Prior art keywords
pcc
pcre
mixture
ionic liquid
polymer
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PCT/IN2017/050028
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English (en)
Inventor
Divesh Narayan SRIVASTAVA
Mosarrat Perween
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Council Of Scientific & Industrial Research
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Publication of WO2017130218A1 publication Critical patent/WO2017130218A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28—Electrolytic cell components
    • G01N27/401—Salt-bridge leaks; Liquid junctions
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
    • G01N27/28—Electrolytic cell components
    • G01N27/30—Electrodes, e.g. test electrodes; Half-cells
    • G01N27/301—Reference electrodes

Definitions

  • the gadgets based on electrochemical techniques are not unusual in contemporary market. Still the potential of electrochemical techniques are not adequately utilized in the service of civilization. A major obstacle in this direction is scarcity of suitable off- laboratory electrodes and their limited choice. Therefore various tailored and unconventional electrodes are developed and utilized; still they are not so cost- effective.
  • the present invention relates to the production of cost-effective, full-bodied electrode cartridge [hereafter called Plastic Chip Cartridge (PCC)] for on-site use-and- throw applications. More specifically, the invention relates to development of cartridge electrode consist all the three electrodes (working, counter and reference) in a single structural unit. This invention also deals with development of solid state reference electrode [hereafter called Plastic Chip Reference Electrode (PCRE)] .
  • PCCE Plastic Chip Reference Electrode
  • Plastic Chip Electrode has been used as platform for the development of PCRE and PCC.
  • the performance of PCRE has been tested in various electrochemical techniques, which includes potentiometry (pH sensing) and cyclic voltammetry
  • the performance of the PCC has been tested in cyclic voltammetry of different redox couple and anodic stripping voltammetry (ASV) for the separate as well as simultaneous detection of Pb 2+ , Hg 2+ and Cd 2+ at ppb.
  • PCC has also been tested for the analysis of field sample by ASV.
  • the prime object of the present investigation is to develop cost effective, portable and bulk conducting electrode assembly (PCC) using PCE platform.
  • PCE PCE platform
  • Yet another object of this study is to develop silver chloride saturated ionic liquid- polymer salt bridge with appropriate ratio of IL-polymer.
  • Yet another object of the present investigation is to test PCRE in various potentiometric and voltametric applications. Yet another object of this investigation is to test PCC in various electrochemical applications such as stripping voltammetry for the detection of heavy metals in synthetic as well as in natural water.
  • the present invention provides a complete three electrode system in single unit (PCC) and a solid state reference electrode (PCRE) made on the platform of plastic chip electrode (PCE).
  • the PCRE comprises coating of silver paint and silver chloride mixture at one end of PCE and a ionic liquid- polymer salt bridge, wherein the ionic liquid (IL) used is either l-butyl-3-methylimidazolium hexafluorophosphate ⁇ [C 4 mim][PF6] ⁇ or l-butyl-3-methylimidazolium bis(trifluoromethylsulfonyl) imide ⁇ [C 4 mim][NTF2] ⁇ while polymer is polyvinylidene fluoride ⁇ PVDF ⁇ .
  • the IL- polymer weight ratio in salt bridge ranges betweenl.5:l to 4: 1.
  • present invention provides a product (PCC) and process for its fabrication.
  • shelf-life of the PCRE is tested and found at least up to 8 months or more.
  • the PCRE is tested in pH sensing using polyaniline indicator electrode and found active in pH range 2 to 7.
  • Another embodiment of the present invention provides a full bodied cartridge electrode (PCC) for use in electrochemistry and electroanalysis in aqueous media.
  • the PCC is tested in techniques like cyclic voltammetry of various redox couples in aqueous medium and anodic stripping voltammetry for the discrete as well as simultaneous detection of heavy metals in synthetic as well as in natural water system.
  • Figure 1 represents preparative step for PCRE.
  • Figure 2 represents pH sensing in Britton-Robinson buffer using PCRE-2 (black symbol) and std. Ag/AgCl reference electrode (red symbol).
  • Indicator electrode Polyaniline coated PCE. Details are given in example 9.
  • Figure 3A represents cyclic voltammogram of [Ru(bpy) 3 ] /[Ru(bpy) 3 ] redox couple (lmM) recorded at 50 mVs "1 using PCRE-2 (sold line) (soaked for about 1 hour) and std. Ag/AgCl (sat. KCl) (dashed line) as reference electrode. Details are given in example 10.
  • Figure 3B represents change in peak potentials (cathodic and anodic) for soaked and unsoaked PCRE-2 for [Ru(bpy) 3 ] +2 /[Ru(bpy) 3 ] +3 redox couple with time.
  • Working electrode glassy carbon
  • counter electrode platinum foil. Details are given in example 10.
  • Figure 4A shows cyclic voltammogram of the Fe (CN)6 3 ⁇ /4 ⁇ redox couple recorded at different scan rate (10 mV/s to 500 mV/s) on PCC having PCRE-2. [In-set - Corresponding peak current vs. square root of scan-rate plot for cathodic as well as anodic scans]. Details are given in example 11.
  • Figure 4B shows cyclic voltammogram of (Ru(bpy) 3 +2/+3 redox couple recorded at different scan rate (10 mV/s to 500 mV/s) on PCC having PCRE-2. [In-set - Corresponding peak current vs. square root of scan-rate plot for cathodic as well as anodic scans]. Details are given in example 11.
  • Figure 5A represents stripping step of square wave anodic stripping voltammetry for Pb +2 on PCC having PCRE-2 at various concentrations of the analyte. Details are given in example 12.
  • Figure 5B represents calibration plot for lead (solid line) in synthetic sample and corresponding concentration of lead in different real water samples (dotted lines). Details are given in example 12.
  • Figure 6 shows stripping step of square wave anodic stripping voltammetry for simultaneous detection of Pb +2 , Cd +2 and Hg +2 ions on PCC having PCRE-2 at various concentrations of the analytes (equal quantity). [In-set- corresponding calibration curve for all three elements]. Details are given in example 13.
  • the present invention relates to the fabrication of a full bodied cartridge electrode incorporating standards three electrode electrochemical system. This invention also relates to the design and development of a solid state reference electrode.
  • the invention recognized that plastic chip electrode (PCE) previously invented by our group, is a cost effective, self-standing and bulk conducting electrode material capable of functioning as a platform for the development of cartridge.
  • a cost-effective electrode cartridge having a working, counter and a solid state reference electrode with ionic liquid salt bridge is designed and fabricated.
  • step (e) Drying the mixture as obtained in sub step (e) at room temperature to get a thin film by ensuring the slow evaporation; iv. Coating mixture of silver paint (about 50 ⁇ ) and silver chloride (20 mg) around one end of PCE in 1.5 cm length with a small brush; v. Cutting of IL-polymer film as obtained in step (iii) in 1.6 x 1.6 cm dimension with a small scissor; vi. Wrapping of IL-polymer film as obtained in step (v) around Ag paint/ AgCl coated PCE as obtained in step (iv) [ Figure- 1]; vii. Lamination of system by heat pressing as obtained in step (vi), and maintaining provision for electrical and solution contact, to obtained PCRE. viii. Lamination of system by heat pressing as obtained in step (vi), with two PCE as obtained in step (i), and maintaining provision for electrical and solution contact, to obtained PCC.
  • a cartridge electrode PCC is therefore designed and fabricated.
  • PCC complementary metal-oxide-semiconductor
  • hydrophobic ionic liquid is excellent candidate for salt bridge owing to its restricted solubility in aqueous phase.
  • a composite of a hydrophobic ionic liquid in combination with a polymer is employed as salt bridge in PCRE. 5.
  • IL-polymer film was made in various ratios viz. 1.5: 1, 2: 1, 3: 1 and 4:1 denoted as IL-1.5, IL-2, IL-3, and IL-4 respectively and corresponding plastic chip reference electrode (PCRE) as PCRE- 1.5, PCRE-2, PCRE-3, and PCRE-4 respectively.
  • PCE plastic chip reference electrode
  • the thickness of IL-1.5, IL-2, IL-3, and IL-4 film for a total mass 0.8 gm for casting area 38.5 cm 2 and equilibrium open circuit potential (OCP) of the PCRE made using these film measured at 23 °C in 0.1 M KC1 solution are furnished in table 1.
  • the thickness of IL-2 film made in different total mass for casting area 38.5 cm 2 and the OCP of the PCRE made using these film as salt bridge is given in table 2 measured under similar conditions as mentioned above.
  • Total mass includes mass of IL and polymer only (excluding mass of AgCl).
  • Thickness of IL- polymer film made in various ratios for a total mass 0.8 gm and casting area 38.5 cm 2 and the equilibrium open circuit potential (OCP) of the PCRE made using these film at 23 °C and in 0.1 M KC1 solution.
  • the equilibrium potential was said to achieve when potential drift was less than 0.1 mV/min.
  • PCRE PCRE
  • PCRE-2 PCRE
  • OCP OCP was measured in similar way as mentioned in example 1.
  • the OCP of PCRE was 79 mV, which is same to the PCRE formed in example- 1-4, within the limits of experimental errors.
  • the PCRE-2 was used as reference electrode in pH sensing using Britton-Robinson buffer of pH 2 to 10 and polyaniline coated PCE as indicator electrode.
  • Polyaniline was coated on PCE by potentiodynamic method in -0.2 V to 0.8 V potential range for 100 cycles using potentiostat.
  • the monomer having 0.1 M aniline in 0.5 M sulfuric acid was used for this purpose.
  • Platinum foil was used as counter and standard Ag/AgCl (sat KCl) as reference electrode.
  • the potential vs. pH plot for two set of experiments having PCRE-2 and conventional Ag/AgCl (Sat KCl) reference electrode is given in Figure 2.
  • the PCRE-2 was used as reference electrode for cyclic voltammetry measurements using three electrode electrochemical system in 1 mM solution of [Ru(bpy) 3 ]Cl 2 in 10 " 1 M KN0 3 . Glassy carbon electrode was employed as working while platinum foil and PCRE-2 as counter and reference electrode respectively. The result of CV was compared with that of using standard Ag/AgCl (sat KCl) reference electrode whereas working and counter electrodes were same. Both the cyclic voltammograms (CVs) are given in Figure 3A. The CV of same redox couple during the equilibration of PCRE-2 was also recorded.
  • E formal potential calculated by taking the mean of the cathodic and anodic peak potentials
  • DE difference between anodic and cathodic peak potential
  • I pa anodic peak current
  • I pc cathodic peak current.
  • the PCC having PCRE-2 was used for the detection of Pb +2 via stripping voltammetry in natural water.
  • a standard calibration plot was plotted by recording square wave stripping voltammograms in synthetic solution (Figure 5 A) of pH 4 for different concentration of lead (100 ppb to 1000 ppb) under step potential 5 mV, amplitude 50 mV and frequency 100 Hz. Preconcentration was done by applying -1.2 V for 10 minutes. The peak current obtained at different lead concentration was normalized with base current and were used to prepare calibration plot. Three concentrations viz 400 ppb, 600 ppb and 800 ppb were chosen for the testing of lead in natural water system. The behavior (in term of peak current) of PCC in all mentioned natural water at given concentration of lead (dotted lines) was compared with the calibration plot made in synthetic acid solution (solid line) and shown in Figure 5B.
  • the PCC having PCRE-2 was used for the simultaneous detection of Pb +2 , Cd +2 and Hg +2 ions via stripping voltammetry.
  • Acetate buffer of pH 4.5 was used as electrolyte.
  • Equal concentration of all the three metals ranging from 50 ppb to 500 ppb were used for the recording square voltammogram ( Figure 6).
  • the electrode was cleaned by applying +1.0 V for 10 minutes after each measurement and checked for any peak in blank electrolyte.
  • Other experimental conditions were same as mentioned in example 11.
  • a full bodied electrode comprises all the three electrodes (working, counter and reference) in single unit.
  • a solid state reference electrode with an ionic liquid salt bridge having a stable junction potential • A solid state reference electrode with an ionic liquid salt bridge having a stable junction potential.

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Molecular Biology (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
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  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

La présente invention concerne la conception et la fabrication d'une électrode de référence pratique solide (PCRE) et d'une cartouche d'électrodes (PCC) comprenant trois électrodes électrochimiques (électrode de travail, contre-électrode et électrode de référence) dans une unité structurale. La PCRE est recouverte par un pont salin de liquide ionique polymérisé contenant AgCl présentant un potentiel stable.
PCT/IN2017/050028 2016-01-29 2017-01-18 Fabrication d'une cartouche d'électrodes de puce en plastique comprenant une membrane de liquide ionique contenant du chlorure d'argent WO2017130218A1 (fr)

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Cited By (2)

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Publication number Priority date Publication date Assignee Title
CN109946362A (zh) * 2017-12-19 2019-06-28 恩德莱斯和豪瑟尔分析仪表两合公司 参比电极以及参比电极的制造方法
CN115151814A (zh) * 2020-03-03 2022-10-04 株式会社堀场先进技术 含有离子性液体的聚合物

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109946362A (zh) * 2017-12-19 2019-06-28 恩德莱斯和豪瑟尔分析仪表两合公司 参比电极以及参比电极的制造方法
US11125711B2 (en) 2017-12-19 2021-09-21 Endress+Hauser Conducta GbmH+Co. KG Reference electrode and method for manufacturing a reference electrode
CN115151814A (zh) * 2020-03-03 2022-10-04 株式会社堀场先进技术 含有离子性液体的聚合物
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