Bench Boost by Inorganic Ventures

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This week Mike & Ashley review the standardized methods for elemental impurity analysis in pharmaceuticals: ICH Q3D, USP <232>, and USP <233>. ICH Q3D provides guidelines for testing up to 24 elements and emphasizes risk assessment but not detailed testing calculations; USP <232> sets elemental impurity limits; and USP <233> addresses sample preparation and analysis and relies on ICH Q3D concepts such as “J” concentrations (to be covered next week). They explain risk assessment factors (element, route of administration, intentional addition, and screened materials) and outline element classes. They also discuss sample types (APIs, drug products, excipients) and how early screening can reduce final testing needs.

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The Inorganic Ventures team members answer more listener questions relevant to trace analysis. They address low mercury recovery at 2 ppb, noting mercury instability in nitric acid, adsorption to plastic, options such as preparing in HCl or stabilizing with ~1 ppm gold. They explain detection limit calculations using calibration data and blank replicates & distinguish instrument vs method detection limits, with suggestions to improve precision and sensitivity via conditions and sample introduction components. For heavy metals in blood studies, they warn of vacutainer/polypropylene contamination and recommend vessel leaching or vessel blank studies. Finally, they describe pH product certification against NIST standards, potential meter entry limitations, and temperature effects on calibration.

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The Inorganic Ventures team answers listener questions focused on pharmaceutical elemental impurity analysis by ICP-MS. They explain why an indium internal standard becomes unstable in high-pH matrices due to insoluble hydroxide formation and how EDTA complexation can stabilize indium when used for iodine analysis. They discuss mercury washout problems caused by volatility, adsorption to sample introduction surfaces, memory effects, and redox/speciation, and emphasize proper rinse sequencing and the roles of chloride-based rinses and specialty solutions like ICP True Rinse to prevent carryover and failed QC checks. They address poor gold recovery during heated prep due to adsorption, reduction, and volatility. Finally, they advise diluting working standards in matrices that match samples while considering element stability and compatibility in stock matrices.

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This week on Bench Boost Mike, Autumn, Micah, and Josh discuss common ICP-OES/ICP-MS issues in mining analyses and how to troubleshoot them by separating sample-prep from instrument root causes. Key sample-prep problems include incomplete digestion of refractory minerals, loss of volatile analytes, spitting, and adsorption/instability during transfers. They review contamination before jumping into issues borne from instrument assays; covering the topics of matrix effects from high TDS & mitigation via dilution, internal standards, matrix matching, and more. They also note how physical effects will impact nebulization or transport efficiency. QC pitfalls with non-matrix-matched standards, internal-standard limitations, and the importance of representative CRMs are discussed before the team provides a structured troubleshooting checklist including blanks, duplicate agreement, spike recovery, dilution linearity, and multi-wavelength/isotope agreement.

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This week on Bench Boost Mike, Autumn, and Thomas dive deep into validation procedures for ICP-OES and ICP-MS methods. They discuss the importance of planning validation parameters early, understanding sample matrices & analyte levels, and achieving complete dissolution via appropriate digestions. They review the seven key validation parameters of accuracy, precision, detection limits, linearity, selectivity, robustness, and stability. They also outline best quality control practices including analyzing blanks, CCVs, duplicates, spikes, and implementing control charts.

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This week on Bench Boost the team from Inorganic Ventures discusses avoiding precipitation during sample preparation. They review mining sample challenges including high concentrations of Ca, Fe, Al, & silicates, sulfate-rich matrices forming insoluble sulfates, and rare earth elements requiring a more acidic matrix. Thomas explains how hydrolysis leads to insoluble metal hydroxides and reviews prevention strategies. Liv outlines how to use Ksp and how temperature effects compound solubility. Lastly, Autumn covers alternative ligands, such as EDTA, for higher pH stability.

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This week on Bench Boost on team spotlights mining analysis challenges on ICP-MS due to high total dissolved solids, aggressive digestions, and low-ppb targets requiring interference control. They review ICP-MS interference types, giving examples such as ArO on Fe, and ArCl on As. The team explains how collision cell (helium KED) is used to reduce polyatomics and how reaction cell gases are used for mass-shifting analytes or interferences. Finally, they discuss triple-quad ICP-MS principles for stronger mitigation and share method-planning tips: isotope tables, chloride/oxide checks, survey scans, dilution/argon dilution for TDS, matrix matching (including HCl), calibration choices, and internal standards.

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This week on Bench Boost our team reviews special considerations for measuring lithium by ICP-OES and ICP-MS. They discuss common lithium sample types and preparation guidance. Autumn emphasizes the impact of high total dissolved solids (TDS) and easily ionizable elements (EIEs) causing plasma ionization-balance shifts and signal suppression for some sample types. Additional tips include selecting appropriate internal standards, choosing suitable emission lines, and avoiding error propagation during large dilutions. 

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In this episode of Bench Boost our team revisits method detection limits (MDLs) with a focus on why mining applications often produce higher MDLs than expected. Autumn contrasts instrument detection limits with method detection limits, which reflect real sample matrices, interferences, and method variability. Liv explains mining-specific drivers of elevated MDLs, including aggressive sample preparation and impacts from dilution and high total dissolved solids. Mike closes the episode this week by discussing practical ways to improve MDLs.

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In this episode of Bench Boost, Mike, Autumn, and Thomas discuss the differences between axial and radial views when using ICP-OES instruments. The focus is on how each view will impact precision, sensitivity, detection limits, and more. Our team compares which view is more prone to background interferences and which better handles complex samples with high concentrations of total dissolved solids. The episode also covers the challenges of analyzing mining samples including common matrix effects and spectral interferences, and provides guidance on when to use each view for optimal accuracy.