Electrochemical and analytical performance of boron-doped diamond electrode for determination of ascorbic acid
At a Glance
Section titled âAt a Glanceâ| Metadata | Details |
|---|---|
| Publication Date | 2017-04-25 |
| Journal | Acta Chimica Slovaca |
| Authors | Ivana SĂĄlusovĂĄ, KristĂna CinkovĂĄ, Barbora BrtkovĂĄ, MariĂĄn Vojs, MariĂĄn Marton |
| Institutions | Czech Academy of Sciences, Institute of Analytical Chemistry, Slovak University of Technology in Bratislava |
| Citations | 8 |
| Analysis | Full AI Review Included |
Technical Documentation and Collateral: MPCVD Boron-Doped Diamond for Ascorbic Acid Sensing
Section titled âTechnical Documentation and Collateral: MPCVD Boron-Doped Diamond for Ascorbic Acid SensingâExecutive Summary
Section titled âExecutive SummaryâThe analyzed research paper validates Boron-Doped Diamond (BDD) electrodes as a superior, modification-free platform for highly sensitive and robust electroanalytical determination of Ascorbic Acid (AA) in complex media, specifically pharmaceuticals.
Core Value Proposition Highlights:
Section titled âCore Value Proposition Highlights:â- Superior Electrode Performance: BDD demonstrated a totally irreversible, diffusion-controlled oxidation peak for AA at +0.87 V, utilizing the materialâs excellent stability and low background current, surpassing conventional carbonaceous electrodes (GCE, CPE).
- Modification-Free Protocol: The method is simplified, rapid, and low-cost, eliminating the requirement for time-consuming electrode surface modification (a necessity for many competing chemically modified electrodes, CMEs).
- High Sensitivity and Precision: Achieved a low Limit of Detection (LOD) of 1.1 x 10-6 mol L-1 and excellent repeatability with a relative standard deviation (RSD) of 2.3%.
- Routine Analysis Capability: The BDD protocol proved suitable for direct quantification of AA in commercial pharmaceutical tablets using Differential Pulse Voltammetry (DPV) and the standard addition method.
- Optimal Material Specifications: The successful replication relies on highly doped BDD films (8000 ppm B/C ratio in the gas phase) fabricated via MPCVDâa core expertise of 6CCVD.
Technical Specifications
Section titled âTechnical Specificationsâ| Parameter | Value | Unit | Context |
|---|---|---|---|
| Electrode Material | Boron-Doped Diamond (BDD) | - | Highly doped, MPCVD film |
| BDD Doping Level | 8000 | ppm | B/C ratio in gaseous phase |
| BDD Film Diameter | 740 | ”m | Inner diameter used for working electrode |
| Optimal pH | 4.0 | - | Britton-Robinson (B-R) buffer |
| Oxidation Peak Potential (Ep) | +0.87 | V | CV, vs. Ag/AgCl, Irreversible reaction |
| Redox Process Control | Diffusion | - | Linear dependence of Ip vs. v1/2 (R2 = 0.954) |
| Linear Concentration Range (LCR) | 5 x 10-6 to 2 x 10-4 | mol L-1 | DPV Analytical Range |
| Limit of Detection (LOD) | 1.1 x 10-6 | mol L-1 | Calculated as 3x SD / Slope |
| Limit of Quantification (LOQ) | 3.5 x 10-6 | mol L-1 | Calculated as 10x SD / Slope |
| Repeatability (RSD) | 2.3 | % | For 6 replicate DPV measurements |
| Pharmaceutical Recovery | 122 | % | CelaskonÂź 250 tablet analysis |
Key Methodologies
Section titled âKey MethodologiesâThe study utilized advanced voltammetric techniques combined with specific material pretreatment to achieve stable and sensitive analytical results.
1. BDD Electrode Preparation and Pretreatment
Section titled â1. BDD Electrode Preparation and Pretreatmentâ- Electrode Type: Highly doped BDD working electrode (740 ”m inner diameter).
- Pretreatment Electrolyte: Simple cycling in 1.5 mol L-1 Sulphuric Acid (H2SO4).
- Cycling Range: -2.0 V to +2.0 V (vs. reference electrode).
- Objective: To achieve a stable signal, typically requiring 5 cycles, resulting in a hydrogen-terminated BDD surface, which exhibits low adsorption properties.
2. Electrochemical Setup and Conditions
Section titled â2. Electrochemical Setup and Conditionsâ- Instrumentation: Autolab PGSTAT 101, controlled by NOVA software.
- Reference Electrode: Ag/AgCl/3 mol L-1 KCl.
- Counter Electrode: Platinum (Pt) wire.
- Supporting Electrolyte: Britton-Robinson (B-R) buffer.
- Optimal Conditions: Selected at pH 4.0 due to highest peak current observed in DPV studies (ranging from pH 2.0-12.0).
3. Differential Pulse Voltammetry (DPV) Parameters
Section titled â3. Differential Pulse Voltammetry (DPV) Parametersâ- Modulation Amplitude: 50 mV.
- Modulation Time: 50 ms.
- Scan Rate: 10 mV s-1.
4. Quantification Protocol
Section titled â4. Quantification Protocolâ- Analytical Method: Standard Addition Method (SA) applied directly to filtered pharmaceutical samples.
- Calibration: Linear least-squares regression used for evaluation (R2 = 0.999).
6CCVD Solutions & Capabilities
Section titled â6CCVD Solutions & Capabilitiesâ6CCVD is uniquely positioned to support the replication and expansion of this research by supplying highly customized, high-quality MPCVD Boron-Doped Diamond (BDD) materials, ensuring reliable performance for advanced electroanalytical applications.
Applicable Materials
Section titled âApplicable MaterialsâThe successful results depend critically on the use of Heavy Boron-Doped Polycrystalline Diamond (BDD) films grown via Microwave Plasma Chemical Vapor Deposition (MPCVD).
| 6CCVD Material Recommendation | Material Specification Alignment | Advantage for Replicating Research |
|---|---|---|
| Heavy Boron-Doped PCD (BDD) | Achieves B/C doping levels well above the 8000 ppm threshold required for highly conductive, stable surfaces. | Ensures low resistivity and high electron transfer kinetics critical for sensitive DPV/CV applications. |
| PCD Substrates (Custom Thickness) | Available in thicknesses from 0.1 ”m up to 500 ”m on insulating or conductive substrates. | Allows engineers to optimize film thickness based on thermal load and sensor integration requirements. |
| Ultra-Polished BDD Films | Polishing capability down to Ra < 5 nm (inch-size PCD). | Provides superior surface morphology for applications where minimizing surface adsorption is essential, reducing background current and noise. |
Customization Potential
Section titled âCustomization PotentialâThe experimental setup utilized a BDD film with a precise 740 ”m diameter. 6CCVD offers complete material customization to meet specific sensor integration needs:
- Custom Dimensions and Geometry: We provide MPCVD BDD films on wafers up to 125mm. We utilize advanced laser cutting and patterning services to achieve custom electrode shapes, sizes (e.g., exact 740 ”m diameter disks), and arrays, facilitating miniaturization and scale-up.
- Advanced Metalization: While the paper used external contacts, 6CCVD provides in-house metalization services (Ti, Pt, Au, W, Cu, Pd) necessary for robust electrical contact pads, improving long-term stability and sensor integration for packaged devices.
- Substrate Choice: Supply BDD films on various substrates optimized for electrochemistry, including conductive (Si) or insulating (Quartz, Sapphire) carriers.
Engineering Support & Logistics
Section titled âEngineering Support & Logisticsâ- Expert Consulting: 6CCVDâs in-house PhD team provides specialized engineering consultation to assist customers in material selection, doping optimization, and surface termination protocols (e.g., hydrogen-termination vs. oxygen-termination) crucial for Electrochemical Sensors and Pharmaceutical Analysis projects.
- Global Supply Chain: We ensure reliable, worldwide delivery with flexible shipping terms (DDU default, DDP available), guaranteeing timely receipt of high-purity diamond materials wherever your research facility is located.
Call to Action
Section titled âCall to ActionâTo discuss heavy boron doping requirements, custom dimensions for miniaturized sensors, or integration of metal contact pads for sensitive electroanalytical devices, visit 6ccvd.com or contact our engineering team directly. We enable high-performance diamond applications.
View Original Abstract
Abstract The electrochemical behavior and determination of ascorbic acid (AA) was investigated at a bare boron-doped diamond (BDD) electrode using cyclic and differential pulse voltammetry. The influence of pH of supporting electrolyte and scan rate on the current response of analyte was examined to select the suitable experimental conditions. It was found that AA provided one well-shaped irreversible and diffusioncontrolled oxidation peak at +0.87 V vs. Ag/AgCl in Britton-Robinson buffer pH 4.0. Applying differential pulse voltammetry, the peak current of AA was linearly proportional to its concentration from 5 Ă 10 -6 to 2 Ă 10 -4 mol L -1 (R 2 = 0.999), with the limit of detection of 1.1 Ă 10 -6 mol L -1 and the good repeatability (relative standard deviation of 2.3 %). The developed electroanalytical protocol was successfully applied to determine the content of AA in commercial pharmaceutical preparations, based on the standard additions method, with the obtained recovery of 122 %. The accomplished analytical performance indicates that BDD electrodes are promising electrochemical sensors for pharmaceutical analysis.