Library · Materials, chemistry & fabrication
What Solvent Extraction & Crystallization got wrong, from 33 theses
Summary written by a model from the records below: The records document various operational failures and design challenges encountered during solvent extraction, precipitation, and crystallization experiments. Researchers encountered difficulties ranging from unfavorable solvent-solute interactions and impurity co-extraction to uncontrolled nucleation and predictive modeling errors. These records come from graduate theses, 2021 to 2025, each labeled with its degree where the repository states it, and each links to its thesis. They were extracted by language models reading the full text, so treat each as a lead to read, not a verdict.
Plus 8 problems the authors left open, listed at the end.
Failure modes, by theses reporting them
Select a mode to jump to its records.
Solvent incompatibility and low solubility hinder effective dissolution and crystallization
Precursors, polymers, and metal salts frequently failed to dissolve due to high lattice energies, extreme hydrophobicity, or insufficient solvent coordination. In other cases, low dielectric constants failed to induce phase separation, target compounds remained dissolved in reaction media, or excessive solvent volumes and heating duties made recovery impractical.
Tried and failed
dielectric constant-based solvent selection for phase separation applied to salt-induced liquid-liquid extraction mixtures. Outcome: no signal. Reason: low dielectric constant solvent failed to induce liquid-liquid phase equilibrium, disproving pure dielectric-based precipitation theories
Critical Material Recovery from Salt-Lakes and Spent Batteries with Membranes and Solvents · MIT · PhD
Tried and failed
high-concentration transition metal salt dissolution in ionic liquids applied to metal-containing ionic liquid stationary phases. Reason: exceeded solubility limit at room temperature, failing to form a homogeneous solution
Inverse gas chromatography for crucial separations using ionic liquids · UT Austin · PhD
Considered and rejected
Considered and rejected: Rejected solvent-based precipitation due to poor solubility requiring large, impractical amounts of organic solvents.
Phase 1 clinical trial evaluating safety, bioavailability, and gut microbiome with a combination of curcumin and ursolic acid in lipid enhanced capsules · UT Austin · PhD
Considered and rejected
Considered and rejected: Rejected Dextran (450k-650k) as a phase-separation additive due to low solubility and precipitation during extraction, causing poor repeatability.
Considered and rejected
Considered and rejected: Rejected DMSO and DMF for solution crystallization despite high theobromine solubility due to excessive solvent evaporation times.
Kokryształy alkaloidów purynowych – teobrominy, teofiliny oraz kofeiny Cocrystals of purine alkaloids – theobromine, theophylline and caffeine · Adam Mickiewicz University · PhD
Considered and rejected
Considered and rejected: Classical solution crystallization for F6PEN and PFT: rejected due to extremely low solubility, replaced by vacuum-based and ionic-liquid-mediated OMBD growth.
Untersuchung der strukturellen und optoelektronischen Eigenschaften fluorierter organischer Halbleiter Investigation of the Structural and Optoelectronic Properties of Fluorinated Organic Semiconductors · University of Marburg · PhD
Considered and rejected
Considered and rejected: Precipitation workup with light petroleum for thermal cyclization intermediates [16-19] was replaced with celite adsorption and flash column chromatography because intermediates [16-19] were soluble in diphenyl ether reaction media.
Considered and rejected
Considered and rejected: Direct recrystallization of [PtCo(SAc)4(4,4'-bipy)]inf from reaction powder was rejected due to minimal solubility; instead, crystals were grown directly from the reaction mixture using liquid-liquid layering of PC and toluene.
Chemical design of single molecule electronic components and quasi-1D chains · Boston University · PhD
Tried and failed
solution-phase purification and characterization applied to highly hydrophobic oligopeptoids. Reason: extreme hydrophobicity prevented dissolution required for liquid-phase purification and characterization
PRECISION ENGINEERING OF SMALL MOLECULES AND OLIGOMERS FOR ADVANCED TECHNOLOGIES · Cornell · PhD
Tried and failed
selective solvent dissolution of uncrosslinked polymer applied to polystyrene thin film removal. Outcome: worse than baseline. Reason: aliphatic and polar solvents yielded incomplete polymer dissolution compared to aromatic solvents like toluene
Vacuum ultraviolet enhanced atomic layer etching, and area selective atomic layer deposition for next generation nanofabrication · UT Austin · PhD
Considered and rejected
Considered and rejected: Rejected using diethyl ether for dissolution/purification of bis(diphenylphosphino)benzene diamine ligands due to sparse solubility; used acetonitrile recrystallization instead.
Catalysis and Coordination-Driven Self-Assembly: Exploring Reactivity of Multinuclear Architectures · University at Buffalo · PhD
Tried and failed
hydrocarbon solvating agent dissolution of ionic solid applied to alkali metal amide complexes. Reason: high crystal lattice energy prevented dissolution in weakly coordinating olefinic solvents
STRUCTURE-REACTIVITY PRINCIPLES OF SODIUM HEXAMETHYLDISILAZIDE · Cornell · PhD
Impurity co-extraction and byproduct entrapment impede product isolation and recovery
Precipitation and extraction procedures often co-extracted unwanted salts, lipids, or residual reagents that interfered with downstream analysis and degraded product properties. In several instances, target molecules remained trapped in polymeric byproducts or could not be separated cleanly from competing ionic species, leading to low yields or interfacial pellet loss.
Tried and failed
isopropanol acetonitrile protein precipitation extraction applied to lysophospholipid quantification in biological samples. Reason: low unnormalized extraction recovery percentage below fifty percent
A novel quantification method of lysophosphatidic acid and the role of autotaxin/Lysophosphatidic acid axis in acute-on-chronic liver failure · Imperial · PhD
Considered and rejected
Considered and rejected: Rejected salting-out extraction using 0.5 M NaCl due to salt crystallization and ion suppression matrix effects in LC-MS.
Chemical exposures in drinking water: contaminant analysis and physicochemical behavior · MIT · PhD
Considered and rejected
Considered and rejected: Rejected using solvent precipitation (SolvPrec) for broad HBM screening despite high chemical recovery, because it co-extracts salts and lipids that interfere with bioassays and mass spectrometry.
Effect-based human biomonitoring of complex chemical mixtures using high-throughput target screening and in vitro bioassays · Tübingen · PhD
Tried and failed
precipitation separation applied to radiosilver isolation from cesium interference. Reason: interfering cesium radionuclides could not be completely eliminated by precipitation alone
Environmental impact of noble metal radionuclides and their use in nuclear forensics Umwelteinwirkung von Edelmetallradionukliden und deren Verwendung in der nuklearen Forensik · Leibniz Universität Hannover · PhD
Lost to a baseline
Chemical thiosulfate leaching (0.2 mol/L) reached 88.4% gold extraction on refractory ore with Cu/NH3, while Bio-TS peaked at 34.7% due to copper precipitation and lower thiosulfate concentration.
Biogenic Thiosulfate Production for Gold Leaching · Queen's University · PhD
Tried and failed
sequential precipitation with reversed stage order applied to electrochemical mineral separation from brine. Outcome: worse than baseline. Reason: residual carbonic acid from initial carbonation consumed electrogenerated hydroxide, preventing subsequent alkaline hydroxide precipitation
ADVANCING ELECTROCHEMICAL PATHWAYS FOR UPCYCLING CARBON DIOXIDE EMISSIONS INTO SOLID CARBONATES AND SYNGAS · Cornell · PhD
Tried and failed
single-stage washing during precipitation extraction applied to biopolymer isolation from biomass. Outcome: worse than baseline. Reason: incomplete removal of extraction reagents caused poor physical and structural properties in the final product
In-Situ Resource Utilization of Pectin and Bosch Carbon for Energy Storage · Texas Tech · PhD
Tried and failed
chloroform-methanol precipitation applied to proteomic sample preparation with non-ionic detergents. Outcome: worse than baseline. Reason: interfacial pellet loss and inefficient detergent removal compared to bead-based clean-up
Prenylation dynamics of RAS oncogenes: a chemical biology investigation into alternative prenylation phenomena · Imperial · PhD
Lost to a baseline
Recrystallization of 2-amino-5-chlorobenzophenone yielded only 40–55% due to product trapping in polymeric PMHS byproducts, underperforming column chromatography (79–84%).
Stereoselective and Economical Methods for Chemical Synthesis of Essential Medicines · MIT · PhD
Solution crystallization fails to achieve desired crystal phase, stoichiometry, or stereochemical selectivity
Disparate precursor solubilities, moisture sensitivity, or reactant imbalances caused non-stoichiometric incorporation and the premature precipitation of stable competing phases. Attempts to achieve enantioselective separation or specific polymorphs failed when magnetic substrates lacked appropriate symmetry breaking or when additives and bulk crystallization induced twinning and isomerization.
Tried and failed
thermodynamic oversaturation modeling to induce metastable precipitation applied to iron sulfide mineral synthesis pathway simulation. Reason: the thermodynamically stable phase precipitated at lower threshold concentrations than the targeted metastable phases
Tried and failed
aqueous acid solution cooling-induced crystallization applied to hybrid metal halide perovskite synthesis. Reason: poor solubility of alkali precursor in concentrated acid caused premature precipitation and phase separation
Syntheses and Photophysical Studies of Two-Dimensional Hybrid Organic-Inorganic Semiconductors · MIT · PhD
Tried and failed
solution crystal growth using non-anhydrous solvents applied to moisture-sensitive halide perovskite single crystals. Outcome: unstable. Reason: residual water caused immediate precursor degradation and impurity phase precipitation
Investigation of Lead-free perovskites for Optoelectronic Application · EPFL · PhD
Tried and failed
surface-templated enantioselective crystallization on magnetic substrates applied to racemic small molecule crystallization. Outcome: unstable. Reason: stochastic domain twinning during crystal growth produced racemic polycrystalline clusters
A New Spin on the Origin of Biological Homochirality · Harvard · PhD
Tried and failed
external magnetic field during substrate crystallization applied to enantioselective crystallization of racemic precursors. Outcome: no signal. Reason: external magnetic field without surface spin polarization lacks the symmetry-breaking mechanism needed for chiral selection
A New Spin on the Origin of Biological Homochirality · Harvard · PhD
Tried and failed
crystallization on colloidal magnetic nanoparticles applied to chiral separation from racemic solution. Outcome: no signal. Reason: colloidal magnetic particles lacked the well-defined flat surface orientation required for spin-dependent enantioselectivity
A New Spin on the Origin of Biological Homochirality · Harvard · PhD
Lost to a baseline
ROY crystallization on U-CNC, O-CNC, and J-CNC drop-cast films showed poorer polymorph selectivity than aerogel confinement, yielding mixtures of polymorphs (Y, ON, and R) due to interference from unattached bulk crystallization.
Surface-Modified Cellulose Nanocrystal Gels for Applications in Pharmaceutical Crystallization · Georgia Tech · PhD
Considered and rejected
Considered and rejected: Rejected direct crystallization without prior purification because co-present xylo-aminooxazoline (XAO) acts as a crystal habit modifier, causing racemic rosette twinning
A New Spin on the Origin of Biological Homochirality · Harvard · PhD
Excessive nucleation and particle agglomeration cause slurry clogging and phase separation failure
High supersaturation and rapid primary nucleation led to particle collisions, crystal aggregation, column flooding, and transfer line clogging in continuous flow crystallizers. Similarly, unseeded precipitations or liquid-liquid demixing produced fine non-compact sludges or amorphous glasses that resisted solid-liquid separation.
Tried and failed
driving homogeneous nucleation via supersaturation rate control applied to solution crystallization. Reason: high primary nucleation rates caused particle collisions leading to crystal aggregation and cementation
Strategies for controlling nucleation and crystal growth in membrane distillation crystallisation. · Cranfield · PhD
Tried and failed
chemical precipitation without solid support matrix applied to hydrolysed urine nutrient recovery. Reason: formed a fine, non-compact sludge that resisted solid-liquid separation by gravity or centrifugation
Towards circular sanitation systems: Resource recovery via pyrolysis of human excreta · Imperial · PhD
Considered and rejected
Considered and rejected: PFR configurations for reactive crystallization were rejected due to severe slurry settling, transfer line clogging, and difficult solid-solid separation compared to MSMPR crystallizers.
Development of an Improved Amino Ester Hydrolase for Continuous Reactive Crystallization Of Beta-Lactam Antibiotics · Georgia Tech · PhD
Tried and failed
liquid-liquid demixing for crystallization applied to ternary polymer-solvent-antisolvent mixtures. Reason: polymer-rich phases kinetically arrested into amorphous glasses instead of nucleating crystalline phases
Designing nano- and micro-structured polymer materials: from solution thermodynamics to phase inversion · Imperial · PhD
Considered and rejected
Considered and rejected: Rejected using non-ethanol solvent mixtures (acetone, diethyl ether) for SPC recrystallization because they remained solutions or formed uncontrolled aggregates.
ENGINEERED FORMULATIONS FOR SUSTAINED OCULAR DRUG DELIVERY · Johns Hopkins · PhD
Thermodynamic equilibrium and bulk saturation models fail to predict real crystallization behavior
Calculations based on bulk saturation states missed localized surface supersaturation driven by rapid dissolution kinetics. Additionally, single-component stability failed to predict multi-component self-assembly, and equilibrium assumptions failed because non-equilibrium dissolution kinetics were neglected.
Tried and failed
predicting multi-component self-assembly from single-component stability applied to binary colloidal crystal phase behavior. Outcome: did not generalise. Reason: single-component assembly robustness did not translate to or predict binary mixture crystallization behavior
Binary Self-Assembly in Alloy- and Salt-Like Colloidal Compounds · Cornell · PhD
Tried and failed
equilibrium thermodynamic calculations applied to high-temperature phase fraction evolution. Outcome: did not generalise. Reason: neglect of non-equilibrium dissolution kinetics caused inaccurate phase volume predictions
Design and Development of Damage-Tolerant Active Materials · MIT · Doctorate
Left open by the authors
Problems the authors named and did not get to.
Left open
Perform life cycle assessment and techno-economic analysis comparing membrane distillation-crystallization lithium extraction against conventional methods. Blocker: None
AN INNOVATIVE MEMBRANE DISTILLATION-CRYSTALLIZATION PROCESS FOR BRINE TREATMENT · University of Nevada, Reno · PhD
Left open
Identify and test solvents for the direct dissolution of lead sulfate or raw sulfurized lead paste without prior desulfurization. Blocker: Requires a wet chemistry laboratory, chemical reagents, and physical battery paste samples for dissolution testing
Natural deep eutectic solvents (NADESs) for lead acid battery recycling · Imperial · PhD
Left open
Pair SLiC-SPEs with conversion-type cathode materials in lithium batteries to evaluate reduction of active material dissolution loss. Blocker: Requires wet lab chemical synthesis and battery fabrication/testing apparatus.
Polyphosphazene- and Acrylate-Based Polymer Electrolytes for Lithium Batteries · Georgia Tech · PhD
Left open
Optimize crystallization below 0 °C directly from crude effluent to increase paracetamol yield above 50% and reduce recrystallization steps to one. Blocker: Requires a wet-lab chemical synthesis and crystallization setup with crude reaction effluent
Green, Renewable, and Continuous Manufacturing of the Active Pharmaceutical Ingredient Paracetamol · Georgia Tech · PhD
Left open
Develop and optimize a recrystallization procedure using an NH4F/MeOH quenching method to remove PMHS byproducts. Blocker: Requires a wet chemistry laboratory and physical reagents to perform reaction quenching and recrystallization experiments
Stereoselective and Economical Methods for Chemical Synthesis of Essential Medicines · MIT · PhD
Left open
Experimentally measure pressure-dependent stable Cr isotope fractionation during clinopyroxene and mineral-melt crystallization. Blocker: Requires a high-pressure experimental petrology laboratory and mass spectrometry facilities
The Stable Chromium Isotope Signatures of Earth's Silicate Reservoirs: Probing the Deep Earth through Time · Tübingen · PhD
Left open
Investigate wastewater pretreatment strategies using adsorption, coprecipitation, and solvent extraction to mitigate catalyst deactivation in aqueous phase reforming. Blocker: Requires access to wet chemical laboratories, real wastewater streams, and experimental reactor setups.
Valorisation of biomass-derived wastewaters via aqueous phase reforming for energy recovery: a multi-level performance assessment · Politecnico di Torino · PhD
Left open
Model and optimize struvite crystallization kinetics and thermodynamics directly from real wastewater and hydrothermal liquefaction aqueous phase coproducts. Blocker: Requires real hydrothermal liquefaction aqueous phase samples, wet-lab experimental apparatus, and chemical characterization facilities
VALORIZATION OF AGRICULTURAL AND FOOD WASTES THROUGH SUSTAINABLE RESOURCE RECOVERY USING HYDROTHERMAL LIQUEFACTION AND STRUVITE CRYSTALLIZATION · Cornell · PhD
Who has worked on this
Authors of the public theses cited on this page, most-cited first.
- Sukru Furkan Ozturk · Harvard · PhD · 2024
A New Spin on the Origin of Biological Homochirality - Sarah Jane Mear · MIT · PhD · 2022
Stereoselective and Economical Methods for Chemical Synthesis of Essential Medicines - GIULIA FARNOCCHIA · Politecnico di Torino · PhD · 2026
Valorisation of biomass-derived wastewaters via aqueous phase reforming for energy recovery: a multi-level performance assessment - Nicolette A. Bugher · MIT · PhD · 2025
Chemical exposures in drinking water: contaminant analysis and physicochemical behavior - Peilong Lu · Cornell · PhD · 2025
ADVANCING ELECTROCHEMICAL PATHWAYS FOR UPCYCLING CARBON DIOXIDE EMISSIONS INTO SOLID CARBONATES AND SYNGAS - Jimin Park · Georgia Tech · PhD · 2025
Green, Renewable, and Continuous Manufacturing of the Active Pharmaceutical Ingredient Paracetamol - Nadja Eliane Kalinke · Tübingen · PhD · 2025
Introduction of a new two-phase extraction method covering a broad spectrum of analytes in food and environmental samples and its miniaturization to determine the pesticide body burden of individual i - Nathan Wilson · Texas Tech · PhD · 2025
In-Situ Resource Utilization of Pectin and Bosch Carbon for Energy Storage - Chaoqiuyu Wang · Cornell · PhD · 2024
PRECISION ENGINEERING OF SMALL MOLECULES AND OLIGOMERS FOR ADVANCED TECHNOLOGIES - Maria Eleni Koulouri · Imperial · PhD · 2024
Towards circular sanitation systems: Resource recovery via pyrolysis of human excreta - Zi Hao Foo · MIT · PhD · 2024
Critical Material Recovery from Salt-Lakes and Spent Batteries with Membranes and Solvents - Noora Kano · Imperial · PhD · 2024
A novel quantification method of lysophosphatidic acid and the role of autotaxin/Lysophosphatidic acid axis in acute-on-chronic liver failure
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