Process Safety and Scale-Up Systems

Application of Smart Overpressure Protection Devices to batch and semi-batch processes: The zero-emission mode

Thermal hazard assessment of cyclohexane-type liquid crystal monomer from the Grignard cross-coupling reaction by different calorimeters

Kinetics and safety analysis of peracetic acid

Thermal hazards evaluation for sym-TCB nitration reaction using thermal screening unit (TSU)

Research on Thermal Decomposition Kinetics and Thermal Safety for a New Epoxiconazole Crystal

Thermal decomposition characteristics of octyl(phenyl)-N,N-diisobutylcarbamoylmethylphosphine oxide-tri n-butyl phosphate–nitric acid systems

Thermal hazard assessment of tris(2-methyl butyl) phosphate: A comparison with tri-n-butyl phosphate and tri-n-amyl phosphate

Studies on thermal decomposition behaviour of N,N-dialkyl octanamides

Determination of SADT and TMRad of 3-bromo-1-(3,5-dichloropyridin-2-yl)-4,5-dihydro-1H-pyrazole-5-carboxylic acid: Applying thermal decomposition kinetics

The multiple runaway-reaction behavior prediction of MEK–oxidation reactions

Thermal decomposition behaviour of diglycolamide – Nitric acid system

A kinetic-based approach in accelerating rate calorimetry with the varying thermal inertia consideration

Thermodynamics and kinetics of thermal decomposition of dibutylalkyl and dipentylalkyl phosphonate-nitric acid systems

Effect of gamma irradiation on thermal decomposition of tri-iso-amyl phosphate–nitric acid biphasic systems

Venting of a runaway organic peroxide decomposition in viscous solvents on pilot scale

Thermodynamics and kinetics of thermal decomposition of diamylamyl phosphonate-nitric acid systems

Runaway decomposition of dicumyl peroxide by open cell adiabatic testing at different initial conditions

Studies on the flame propagation characteristic and thermal hazard of the premixed N2O/fuel mixtures

The Effects of Acid and Hydrogen Peroxide Stabilizer on the Thermal Hazard of Adipic Acid Green Synthesis

Novel validation on pressure as a determination of onset point for exothermic decomposition of DTBP

The modified Stoessel criticality diagram for process safety assessment

Thermal decomposition behaviour of irradiated tri n-butyl phosphate and mixture of di and mono n-butyl phosphate-nitric acid systems

Calorimetric studies on the thermal decomposition of tri n-butyl phosphate-nitric acid systems

New Thermal Runaway Risk Assessment Methods for Two Step Synthesis Reactions

Hazard evaluation for chlorination and amination reactions of fluorocytosine production process

Advanced kinetics-based simulation of time to maximum rate under adiabatic conditions

Calorimetric studies on thermal decomposition of tri isoamyl phosphate–nitric acid systems

Effect of reaction type on TMRad, TD24 and other data obtained by adiabatic calorimetry

Kinetic-parameters-free method of determining autocatalytic decomposition from experimental adiabatic data

Process hazard evaluation for catalytic oxidation of 2-octanol with hydrogen peroxide using calorimetry techniques

Systematic thermal and flammability hazard analysis of a DMPAT explosion accident in Taiwan

Thermal hazard analysis of 1-((cyano-1-methylethyl) azo) formamide and effect of incompatible substances on its thermal decomposition

Thermal hazard and reaction mechanism of the preparation of adipic acid through the oxidation with hydrogen peroxide

Mathematical methods for application of experimental adiabatic data – An update and extension

Safety Concerns for MOF Syntheses—Understanding the Behavior of DMF Mixtures at Elevated Temperature and Pressure

Thermal characterization of the polymerization of methyl methacrylate

Process safety evaluation of the synthesis of tert-butyl peracetate

Evaluation of the thermal runaway decomposition of cumene hydroperoxide by adiabatic calorimetry

Preparation and thermal hazard evaluation of 1,3,3,5-tetra(1H-tetrazol-5-yl)-pentane

Thermal hazard assessment using closed-cell adiabatic calorimetry

Reaction hazard and mechanism study of H2O2 oxidation of 2-butanol to methyl ethyl ketone using DSC, Phi-TEC II and GC-MS

Use of isoperibolic reaction calorimeter for the study of reaction kinetics of acetic anhydride hydrolysis reaction: Effect of acetic anhydride and water ratio

Analysis of thermal hazards of tert-butylperoxy-2-ethylhexyl carbonate by calorimetric technique

Effects of typical additives on the thermal stability of ammonium peroxydisulfate

Effects of metal ions on thermal hazard of tert-butyl peroxy-3, 5, 5-trimethylhexanoate

Thermal stability evaluation of tert-butyl peroxybenzoate mixed with impurities

Towards Improved Reaction Runaway Studies: Kinetics of the N-Oxidation of 2-Methylpyridine Using Heat-flow Calorimetry

Scale-Up of a Vilsmeier Formylation Reaction: Use of HEL Auto-MATE and Simulation Techniques for Rapid and Safe Transfer to Pilot Plant from Laboratory

On-Line Monitoring of a Crystallization Process

Use of reaction calorimetry in thermal risk assessment studies and safe design of batch reactions that can lead to a runaway: application on hydrogen peroxide

Modeling the Precipitation of l-Glutamic Acid via Acidification of Monosodium Glutamate

Towards an Information-Rich Process Development. Part I: Interfacing Experimentation with Qualitative/Semiquantitative Modelling

Thermal Behavior of Aqueous Solutions of Hydroxylamine During Isothermal and Isoperibolic Decomposition in a Closed System

The influence of oscillations on product selectivity during the palladiumcatalysed phenylacetylene oxidative carbonylation reaction

Fuzzy logic and rigid control of a seeded semi-batch, anti-solvent, isothermal crystallizer

Adaptive MIMO neuro-fuzzy logic control of a seeded and an unseeded anti-solvent semi-batch crystallizer

A Practical Method For Stabilizing Lithiated Halogenated Aromatic Compounds

Isothermal decomposition of hydroxylamine and hydroxylamine nitrate in aqueous solutions in the temperature range 80–160 ◦C

Utilising high throughput technologies for the determination of the reaction network of the L-proline catalysed aldol reaction

A New Autocatalytic Thioacetate-Enal Addition Reaction: A Michael Addition or Not?

Reaction calorimetric analysis of batch cooling crystallization processes: studies of urea in supersaturated water–methanol solutions

Toward an inherently safer design and operation of batch and semi-batch processes: The N-oxidation of alkylpyridines

Inherently safer reactors: Improved efficiency of 3-picoline N-oxidation in the temperature range 110–125 °C

Oscillatory carbonylation of phenylacetylene in the absence of externally supplied oxidant

The effect of using a methanol–water solvent mixture on pH oscillations in the palladium-catalyzed phenylacetylene oxidative carbonylation reaction

A study on the scale-up of acyl azide synthesis in various continuous flow reactors in homogeneous and biphasic systems

On the Breakage of High Aspect Ratio Crystals in Filter Beds under Continuous Percolation

Thermal hazards evaluation of the synthesis of N-methylmorpholine-N-oxide

Polymorph and Particle Size Control of PPAR Compounds PF00287586 and AG035029

Scale-Up of a Vilsmeier Formylation Reaction:  Use of HEL Auto-MATE and Simulation Techniques for Rapid and Safe Transfer to Pilot Plant from Laboratory

Synopsis: The journal describes the application of reaction calorimetry and process modelling to allow for rapid and safe scale-up of a Vilsmeier formylation reaction, wh

Isothermal reaction calorimetry as a tool for kinetic analysis

Synopsis: This paper reviews the most important reaction calorimetric principles and their application in commercial or scientific devices, giving examples of various rea

Thermal Hazards of the Vilsmeier−Haack Reaction on N,N-Dimethylaniline

Achieving pH and Qr oscillations in a palladium-catalysed phenylacetylene oxidative carbonylation reaction using an automated reactor system

Synopsis: This experimental shows evidence for oscillations in both pH and heat output (Qr) during a palladium-catalysed phenylacetylene oxidative carbonylation reaction

Control of Supersaturation in a Semibatch Antisolvent Crystallization Process Using a Fuzzy Logic Controller

Kinetics Estimation and Single and Multi-Objective Optimization of a Seeded, Anti-Solvent, Isothermal Batch Crystallizer

Synopsis: This journal estimates the nucleation and growth kinetic parameters of paracetamol in an isopropanol-water antisolvent batch crystalliser, by nonlinear regressi

The influence of reaction temperature on the oscillatory behaviour in the palladium-catalysed phenylacetylene oxidative carbonylation reaction

Autonomous reorganization of the oscillatory phase in the PdI2 catalyzed phenylacetylene carbonylation reaction

Synopsis: The PdI2 catalyzed oxidative carbonylation of phenylacetylene has been shown to produce pH oscillations over the temperature range 0-40 °C under semi-batch con

Thermal Hazards of Synthesizing a Grignard Reagent under Different Dosing Rates

Some Reaction Safety Aspects of Ruthenium-Catalyzed Allylic Oxidations of Δ-5-Steroids in the Pilot Plant

Synopsis: This journal discusses the identification of thermal runaway in the ruthenium-catalysed allylic oxidation of ∆-5-steroids with tert-butyl hydroperoxide into u

The Use of Adiabatic Calorimetry for the Process Analysis and Safety Evaluation in Free Radical Polymerization

Synopsis: This paper studies the free radical polymerisation of methyl methacrylate (MMA), which is exothermic and auto-accelerating, and so can lead to a runaway reactio

Thermal Stability: A Review of Methods and Interpretation of Data

Synopsis: This review discusses the strengths and weaknesses of individual thermal testing methods, and how the data obtained from them can be applied. The assessment and

Calorimetric Approach and Simulation for Scale-Up of a Friedel−Crafts Reaction

Synopsis: This journal studies the use of combined calorimetric and simulation techniques for the optimisation of the scale-up of a Friedel-Crafts acylation of toluene wi

Different scale experimental techniques to approach the problem of substances generated in the loss of control of chemical systems: a study on ethyl diazoacetate decomposition

Synopsis: This journal discusses 4 scales of experimental techniques used to analyse substances generated in the exothermic decomposition of ethyl diaxoacetate (EDA). One

Safe and Productive Operation of Homogeneous Semibatch Reactors. II. The Nitration of N-(2-Phenoxyphenyl) Methane Sulfonamide

Synopsis: This journal discusses an analysis of the nitration of N-(2-phenoxyphenyl) methane sulfonamide (FAM) to N-(4-nitro, 2-phenoxyphenyl) methane sulfonamide (NIM),

Calorimetric studies on the thermal stability of methyl ethyl ketone peroxide (MEKP) formulations

Synopsis: This journal studies the energetic decomposition of methyl ethyl ketone (MEKP) and its formulations, which has a high number of reported dangerous incidents. Th

Simple Procedure for Optimally Scaling-up Fine Chemical Processes. I. Practical Tools

Synopsis: A simple and general scale-up procedure, based on boundary and temperature diagram safety criteria for exothermic semibatch reactors (SBRs), has been developed.

Zero-Order Versus Intrinsic Kinetics for the Determination of the Time to Maximum Rate under Adiabatic Conditions (TMRad): Application to the Decomposition of Hydrogen Peroxide

Synopsis: This journal compares the use of zero-order approximation to intrinsic kinetics, for easing the determination of maximum rate under adiabatic conditions (TMRad)

Analysis of thermal hazards of tertbutylperoxy2ethylhexyl carbonate by calorimetric technique

An integrated calorimetric approach for the scale-up of polymerization reactors

Synopsis: This journal uses an integrated calorimetric approach to study the suspension polymerisation of methylmethacrylate (MMA). The Phi-TEC I was used to carry out ad

Applications of reaction calorimetry in reaction kinetics and thermal hazard evaluation

Synopsis: This paper addresses a systematic approach to the determination of the kinetics of the exothermic esterification of methanol and acetic anhydride by reaction ca

Polymerization Hazard

Synopsis: In this communication to the editor, an unexpected and violent polymerisation is discussed, which occurred during an attempt to prepare the condensation product

Development of a Scalable and Safe Procedure for the Production of (3R)-3-(2,3-Dihydro-1-benzofuran-5-yl)-1,2,3,4-tetrahydro-9H-pyrrolo[3,4-b]- quinolin-9-one, an Intermediate in the Synthesis of PDE-V Inhibitors RWJ387273 (R301249) & RWJ444772 (R290629)

Synopsis: This journal discusses the development of a new process for the oxidative arrangement of 𝛽-carboline to quinoline derivatives, intermediates in the synthesis

Critical Assessment of Pharmaceutical Processes A Rationale for Changing the Synthetic Route

Synopsis: This review was written as an analysis of the issues in creating a synthetic route for the pharmaceutical industry. It groups these issues into 6 categories: Sa

Safety Aspects of a Cyanamide Reaction: Inherent Safe Design through Kinetic Modelling and Adiabatic Testing

Synopsis: This journal discusses cyanamide, a highly unstable compound, which begins to decompose at temperatures above ambient. It is used in the synthesis of Active Pha

Experimental sensitivity analysis of the runaway severity of Dicumyl peroxide decomposition using adiabatic calorimetry

Synopsis: This journal investigates the behaviour of dicumyl peroxide (DCP) under runaway conditions using low and high 𝜑 factor calorimeters. Closed cell runaway expe

An Alternative Scalable Process for the Synthesis of 4,6-Dichloropyrimidine-5-carbonitrile

Synopsis: This journal discusses an alternative synthesis of 4,6-dichloropyrimidine-5-carbonitrile, a key intermediate in active pharmaceutical ingredients (API) and pest

A Comparison of Reaction Hazard Screening Techniques

Synopsis: The purpose of this journal was to compare the accuracy of different pieces of commercially available equipment used in chemical reaction screening. It compares

Nitrilase-Catalysed Desymmetrisation of 3-Hydroxyglutaronitrile:  Preparation of a Statin Side-Chain Intermediate

Synopsis: This journal describes an alternative, efficient route for the synthesis of (R)-4-chloro-3-hydroxybutyrate, a useful intermediate in statin side chain synthesis

Safety Concerns Regarding the Transportation of Organic Powders on Dry Ice: How CO 2 Adsorption Can Lead to Powder Spills

Synopsis: In this letter, the transfer of active pharmaceutical ingredients (API) and intermediates between international laboratories in discussed. The stability of API

A Convenient and Stable Synthon for Ethyl Azide and Its Evaluation in a [3 + 2]-Cycloaddition Reaction under Continuous-Flow Conditions

Synopsis: This research aims to create a safe, selective and high yielding process for the synthesis of N1-alkylated-1,2,3-triazole carboxamides. This requires a regiosel

2-Bromo-3-(cyclohexyloxy)acrylaldehyde: An Isolable Enol Ether of Bromomalonaldehyde Suitable for Use in the Manufacture of Imidazolecarboxaldehydes

Synopsis: The purpose of this experimental was to find an enol ether which can be mass produced for use in the synthesis of imidazolecarboxaldehydes, which are used in ma

Aminodifluorosulfinium Salts: Selective Fluorination Reagents with Enhanced Thermal Stability and Ease of Handling

Synopsis: This journal investigates the physiochemical properties of various dialkylaminodifluorosulfinium salts. These salts include: diethylaminodifluorosulfinium tetra

Thermal Decomposition Analysis and Safety Study on Di-tert-butyl Peroxide

Synopsis: This safety study discusses a thermal decomposition analysis on di-tert-butyl peroxide (DTBP), which can be used as a modifier and polymerisation initiator in i

Safety Parameters and Preliminary Decomposition Kinetic of Organo-Peroxy Acids in Aqueous Phase

Thermal behaviour of Peracetic Acid for the epoxydation of vegetable oils in the presence of catalyst

Explosion Hazards of Sodium Hydride in Dimethyl Sulfoxide, N,N-Dimethylformamide, and N,N-Dimethylacetamide

Synopsis: NaH/solvent matrices are used frequently in synthetic chemistry, despite their very high hazard levels, their dangers are under communicated and underappreciate

Continuous Safety Improvements to Avoid Runaway Reactions: The Case of a Chloro-Thiadiazole Intermediate Synthesis toward Timolol

Synopsis: The purpose of this research was to assess in detail, using thermal analysis, the synthesis of a morpholine-adduct used to produce the 𝛽-blocker timolol. The

A detailed kinetic model for the thermal decomposition of hydroxylamine