EC‐MS Technical Notes
EC-MS Technical Note #5: step-by-step QMS peak and EM voltage tuning in PV MassSpec, with signal examples from a well-tuned system.
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EC-MS Technical Note #17 outlines best practices for studying the hydrogen evolution reaction (HER) with a Spectro Inlets EC-MS system: choosing aqueous vs. non-aqueous chips, calibrating for accurate faradaic efficiency and TOF quantification, consulting Pourbaix diagrams for catalyst stability, proper cleaning procedures, matching scan rate to bandwidth filter, and using potentiostatic measurements with H₂ calibration to characterize HER activity.
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EC-MS Technical Note #16 covers best practices for oxygen evolution reaction (OER) experiments: choosing standard vs. non-aqueous chips, cleaning protocols, Pourbaix diagram considerations for catalyst stability, avoiding CO2/bicarbonate detection pitfalls in alkaline electrolyte, CV-based redox characterization, and potentiostatic methods (including SPEIS stepping) for accurate faradaic efficiency quantification.
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Standardized EC-MS benchmark measurements for Pt-Poly and glassy carbon electrodes — CV and chronopotentiometry procedures covering HER, OER, and CO2 oxidation, with M2 signal decay half-lives (~3.8 s for Pt-Poly) for validating system cleanliness and performance.
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EC-MS Technical Note #3: how capacitive EC-cells cause potentiostat instability in CV measurements, and how to fix it with a series resistor and post-measurement iR compensation.
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EC-MS Technical Note #2: standardized cyclic voltammetry and chronopotentiometry benchmark measurements on Pt-Poly and GC electrodes, with expected M2 decay half-lives.
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Learn how to send Ar and He gas pulses through the EC-MS gas exchange system with minimal switching time. Covers the step-by-step MFC and valve sequence, plus expected switching times — roughly 20 seconds from He to Ar, and 50 seconds from Ar to He.
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A detailed troubleshooting guide for identifying and preventing MS signal fluctuations caused by bubbles — covering electrolyte injection defects, cell (re)mounting steps, pressure set-point tuning, and how to distinguish bubble-related M28/M32/M40 spikes from normal signals.
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EC-MS Technical Note #4: how non-aqueous chips perform in IPA, THF, and KOH — CV and chronopotentiometry comparisons against standard chips.
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This technical note explains soft ionization in EC-MS — operating at low electron energies (15–22 eV) to minimize fragmentation — and shows how it separates the NH₃ signal from water's overlapping OH⁺ fragment at m/z=17, plus step-by-step guidance for safely adjusting ionization parameters in PV MassSpec.
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A step-by-step guide to checking and configuring the external ion gauge interlock in PV MassSpec — recognizing the HPT200 gauge, setting the trip-high action at 5E-5 mbar, and calibrating the internal ion plate as part of standard maintenance.
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Application Notes
EC-MS Application Note #3: how measuring the H2 produced, rather than using the electrochemical current as a proxy, improves HER analysis. Examples cover polycrystalline Pt in HClO4, H2SO4 and KOH, Pt/C, Pd/C and MoS2, including identification of parasitic currents and faradaic efficiencies.
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EC-MS Application Note #4: how detecting O2 directly separates true OER current from carbon oxidation and other parasitic processes. Examples cover polycrystalline Pt in HClO4, H2SO4 and KOH and glassy carbon in HClO4, with notes on turn-over frequencies, isotope labeling and support and electrolyte stability.
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EC-MS Application Note #2: how to calibrate EC-MS signals for quantification, using electrochemical (HER/OER) calibration on a polycrystalline Pt disk and partial pressure calibration with gas mixtures, including ixdat code examples. Across 13 O2 and 15 H2 calibration measurements, the standard deviation of the calibration factor was 4.5% and 3.5% of the mean, respectively.
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A step-by-step guide to the CO-stripping technique with EC-MS — using adsorbed CO oxidation to determine electrochemically active surface area (ECSA) and calibrate the CO2 mass spectrometer signal, illustrated with a Pt disk in H2SO4.
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