Vice President of Surface Measurement Systems and renowned sorption scientist, Dr. Daniel J. Burnett, and Dr. Rajesh N. Davé of the CIMSEPP, NJIT, will welcome delegates to the event and highlight just what is possible when the sorption community comes together to enable innovation and pioneer new materials to address the issues facing industries and societies across the world.

Crystal Pharmatech is a leading CRO/CDMO specializing in API solid state research, pre-formulation, formulation development and cGMP manufacturing services. We help our clients with polymorph screening, thermodynamic stability assessment, solubility enhancement by salt and co-crystal screening , phase selection and crystallization, crystal structure elucidation, as well as vehicle screening for PK and Tox studies. Our solid state lab is full of variety of equipment that we use to understand the chemical composition and physical properties of each crystalline phase that we discover when the crystals are not big enough to collect single crystal structure data. 

Our strength lies in our extensive experience in solid state characterization, which helps us to categorize the crystalline phases and predict their eventual instability in the drug product or during drug product manufacturing. The information from XRPD, DSC, TGA, and DVS is combined and used as pieces of a puzzle to build a comprehensive picture of the chemical and physical properties of the crystalline phases. The data generated by DVS analysis of salts and co-crystals produced during screening are critical for the solid phase selection. The sorption isotherms as defined by IUPAC can be used in conjunction with the DSC and TGA data to categorize the crystalline phase (per example channel hydrate, desolvated phase).we frequently use DVS Resolution to study the formation of solvates or mixed solvate/hydrates.

Assessing stability and assigning shelf life is a critical part of pharmaceutical product development that must be repeated at multiple points of the development cycle. Since the majority of solid drug products have at least some sensitivity to moisture, the primary packaging plays an important role in stabilizing drug products by controlling the relative humidity inside the packaging. The internal relative humidity can be calculated by incorporating moisture sorption isotherms with moisture vapor transmission rates (MVTR) into packaging models. Accelerated predictive stability models are an efficient way to assess the packaging requirements needed to achieve a target shelf life. This talk will demonstrate how shelf life-limiting attributes can be modeled in packaging based on short term experimental studies, with a case study using the ASAPprime® software. Packaging modeling can also evaluate sudden impacts on stability, such as phase transitions. The role of moisture sorption isotherms in choosing packaging and setting water specifications to avoid sudden impacts will be detailed. The applicability of using moisture sorption isotherms generated at room temperature (25°C) for accelerated (40°C) conditions will be discussed.

Take a quick break to grab some complimentary refreshments, converse with your peers, and take in some of the poster presentations.

The session explores the use of moisture sorption kinetics data to predict the critical water activity of encapsulation materials, providing physical basis using diffusion principles, and validating the prediction using conventional method of glass transition vs. water activity correlation.

Samuel L. Zelinka Samuel V. Glass Natalia Farkas Emil E. Thybring

Over the past eight years, we have shown that commonly used protocols for using automated sorption balances (often called dynamic vapor sorption or DVS analyzers) for collecting water vapor sorption isotherms in wood lead to unacceptably high errors and uncertainties in the data. These commonly used protocols stop the absorption prior to equilibrium resulting in an under prediction of up to 1% moisture content in the equilibrium moisture content (10% relative error). However, our suggested protocols for acquiring high quality DVS data are still often not used because they require a long hold time at each relative humidity step. Previous work has shown that a systematic correction factor can be applied to data collected with the commonly used short hold times, although this was only tested on a small amount of data from one laboratory. In 2021 we began a worldwide interlaboratory investigation in automated sorption measurements. The goal of this study was to gather data on matched wood samples from many different types of sorption balances and many different laboratories to develop a systematic correction factor that could be applied to sorption data collected with short hold times. However, along the way, we have learned many lessons about the temperature, mass, and relative humidity stability of these instruments. This paper shares lessons learned on how to identify potential problems with DVS instruments and how to obtain high quality sorption data. 

Enjoy lunch with your peers and view the poster presentations around the auditorium

The moisture sorption isotherm (MSI) has been traditionally associated with the association of different water binding association with the food matrix, generally grouped in to three major section, the free moisture, multilayer moisture and the monolayer moisture. Various models have been associated for describing the MSI, but in general they indicate a sigmoid type of behavior when the water activity is plotted against the moisture content, the the stable region normally situated around the middle when the slope of MSI curves changes the sign. The MSI curves can be converted to stability plots by plotting the first derivative of the curve vs water activity which generally indicates the stable zone as a flat section on the derivative curve with both ends showing steeper changes. The same concept can also be extended to compute the equilibrium water activity in packaged multi-component dry snack foods such as raisin bran etc., which are highlighted in this presentaion

It is estimated that that, globally, we spend around $100 billion on hair care per annum. Clearly, this attracts many companies to play in this space and develop products to meet the needs of a diverse marketplace.

From a scientific perspective, hair is a highly complex bio-composite material whose properties vary greatly with water content. Such differing properties can be both advantageous and detrimental. For example, providing the ability to create temporary styles, impacting tactile properties, influencing the tendency for breakage, etc. 

Yet the cosmetic industry is about pandering to the consumer – who generally cares little for the fundamental science. Consumers frequently misdiagnose issues and use nebulous phrases and terminology – making guidance difficult. Accordingly, an important part of working in this industry involves traversing the minefield between “consumer language” and “scientific language”. 

This presentation will show how DVS sheds light on some of these issues and therefore helps better provide guidance for mitigation. 

Take a quick break to grab some complimentary refreshments, converse with your peers, and take in some of the poster presentations.

Soft contact lenses (hydrogels) are materials with an inherent water content in the range of 30 – 80%. The rate of water loss from these materials is a factor likely related to contact lens comfort. Dynamic vapor sorption is a versatile tool that provides a controlled environment for measuring the evaporation rate of water from these materials. Using a specially designed pervaporation cell intended to mimic on-eye conditions, evaporation rates have been measured for a series of commercially available contact lenses, including both traditional and silicone hydrogels. The evaporation rates were found to be dependent on both the identity of the material and the relative humidity of the environment. To better assess the significance of this evaporative water loss on lens comfort, a model was developed that considers water loss from the surface of a lens as a function of evaporation rate, exposure time, and area of exposure. This presentation will discuss the important aspects of the DVS experiment, material dependence of the evaporation rates, and implications for contact lens comfort.

Transmission rates of solvents and moisture through polymer films are often measured to evaluate the barrier properties of polymers and to evaluate the extent of protection they offer relative to a chemical or physical environment. For example, nitrile gloves are used to safeguard hands from exposure to chemicals, while silicone potting material is commonly employed to shield electronic components from exposure to moisture.

There are several key parameters that can be used to understand the response of a material to chemical exposure. These include the permeation, diffusion, and solubility coefficients. The seminar will highlight the differences between permeation and diffusion rates and will discuss experimental techniques (using both breakthrough and gravimetric techniques) to evaluate both. Several examples of applying sorption data to model molecular transport in industrial processes, e.g., modified atmospheric packaging, membrane separations, and polymer devolatilization, will also be discussed.

Details Pending

Leading sorption scientists will be here to address some key questions facing the sorption community, and take queries from the audience. A great opportunity to take advantage of the panels technical expertise, raise a query of your own, or get their views on something raised in the course of the days program.

The use of solid sorbents such as zeolites, MOFs, and finely divided metal oxides is one of the most promising avenues for the implementation of low cost and effective carbon capture (CC). Depending on the technology, sorbents can be tuned either for direct air or point source capture, and have the potential to facilitate CO₂ up-conversion and storage. Identifying, characterizing and scaling-up solid adsorption-based carbon capture systems has become highly desirable, as they show potential for high recovery, low energy solutions. Nevertheless, bringing a promising material from the lab to an industrially relevant technology readiness level requires a comprehensive screening of a number of material properties in process conditions.

In this talk, several topics will be discussed related to advanced characterization of the performance of CO₂ capture materials. In a first instance we will discuss the suitability of common key performance indicators (KPI) used for screening solid sorbents, such as CO₂ uptake, working capacity, selectivity, kinetics, regeneration potential, thermal properties etc. Special focus will be placed on measurement techniques that asses these KPI with sufficient accuracy, and in realistic conditions. In particular, measuring the interference of other contaminants like water, which can compete with CO₂ for sorption sites in many materials (zeolites and most MOFs), while in others the presence of a certain amount of humidity can increase total amount adsorbed, or speed up the sorption kinetics (amine-based materials and alkali or alkaline earth metal carbonation processes). We will finally discuss the challenge of achieving sufficient experimental throughput to screen and optimize large numbers of samples, often hundreds at a time.

S. McIntyre1*, A. Foster2, P. Budd2, D. R. Williams3, P. Iacomi1

1Surface Measurement Systems, London, UK,
2The University of Manchester, Manchester, UK,
3Imperial College London, London, UK
*smcintyre@surfacemeasurementsystems.com

An attractive type of membrane material for CCS applications are polymers with intrinsic microporosity (PIMs) – forming flexible and easy-to-manufacture single-component membranes with high gas permeabilities and selectivity for CO2 over N2 and O2 – primary components of flue gas. In this work, a novel membrane analyzer was developed to observe the multi-component permeation of flue gas constituents through membranes of PIM-1 and its more hydrophilic carboxylate functionalized version, cPIM-1, to reveal the impact of contaminants and industrial process conditions on the membrane separation efficiency.

Humidity was first introduced to the membranes for 3 hours, followed by 10% CO2 in N2 whilst maintaining the selected humidity. The permeation curves were measured using CO2 and humidity probes at the inlet and outlet, with nitrogen measured using a TCD.

The caroxylated PIM-1, cPIM-1, was studied under the same conditions as PIM-1. The carboxylation is known to make the cPIM-1 membrane more hydrophilic and thus the effect of increasing relative humidity was found to be more pronounced, with a 40% decrease in CO2 permeation observed in cPIM-1 compared to the 20% decrease observed for PIM-1. The CO2/N2 selectivity of cPIM-1 was found to decrease by 20% over the same humidity range. Separate water permeation studies found that the behavior of the cPIM-1 membrane when exposed to water was opposite to that behavior of PIM-1 owing to the hydrophilicity of cPIM-1, with the water permeation and diffusion constant increasing with relative humidity.

Further studies were undertaken using Dynamic Vapor Sorption (DVS) to confirm the membrane uptake behavior, most importantly that of water in the Langmuir voids [1,2] of the polymers and the subsequent impact of this water build-up on CO2 uptake.

Take a quick break to grab some complimentary refreshments, converse with your peers, and take in some of the poster presentations.

Abstract pending

Specific surface area (SSA) is an important parameter in drug development that affects other downstream pharmaceutical properties of interest such as stability, powder flow, and dissolution. Traditionally, the Brunauer–Emmett–Teller (BET) SSA of pharmaceutical powders are measured using gas adsorption (nitrogen or krypton) that is preceded by a prolonged degassing step under low pressure. This degassing step may not be suitable for certain pharmaceutical hydrates that are susceptible to dehydration and phase transformation under reduced pressure and humidity conditions. Inverse gas chromatography (iGC) was explored as a reliable alternate technique for determining the SSA of model anhydrate–hydrate systems (trehalose and thiamine hydrochloride) that are prone to such phase transformation during SSA measurement. Both trehalose dihydrate and thiamine HCl non-stoichiometric hydrate were found to undergo partial phase transformation to anhydrous forms after krypton gas adsorption measurements. In contrast, these hydrates remained stable during surface area analysis using iGC owing to measurements under controlled relative humidity. Thus, iGC proved to be a viable technique for SSA measurement of pharmaceutical hydrates without compromising their physical stability

Enjoy lunch with your peers and discuss the morning's sessions.

Vincent Abeyta*, Fredrik L. Nordstrom*

*Solid state & API Engineering, Material & Analytical Sciences, Boehringer-Ingelheim,
900 Ridgebury Road, Ridgefield, Connecticut 06877, United States

Control of API purity in early development is a common challenge as the chemical synthesis is not fully developed and tested at scale. Higher levels of impurities are typically produced and carried all the way to the API step. Crystallization is the key unit operation that is relied upon to effectively remove these impurities and control the purity of the API used for non-clinical studies. While the main focus of the crystallization at this stage is to remove impurities, reciprocal effects are often encountered where the impurities tend to affect the performance of the crystallization itself.

In the past, crystallization inhibition has been thought to be a kinetic phenomenon due to crystallization inhibition at the surface by impurities inhibiting attachment of additional molecules to existing crystals in solution. Recent work in our labs has shown that the underlying mechanism responsible for these adverse effects was found to be formation of thermodynamic solid solutions between the API and impurities. 

This previous work has demonstrated that relatively low levels of impurities exerted a dramatic impact on the success and robustness of the crystallization by affecting the API solubility, seed step, yield and apparent crystallization kinetics. In addition, the extent and severity of encrustation during the crystallization was directly linked to the presence of impurities. However, none of the techniques employed probed the surface of the final crystals. 

Here we present the surface energy evaluation of final products both pure and with known amounts of impurities present to determine effects of impurities on crystal surface energy. The surface energy information in conjunction with other results will improve holistic understanding of how impurities inhibit crystallization.

• Measurement of Henry’s Law Constant using the SEA for functionalized MOF materials
• Comparison of the Henry’s Law Constant measurements with the functionalization design strategy
• Comparison of the Henry’s Law Constant measurements using the SEA with measurements obtained using Quartz Crystal Microbalance
• Addressing challenges posed by high surface area materials
• Addressing challenges posed by low vapor pressure materials  
  

Take a quick break to grab some complimentary refreshments, converse with your peers, and take in some of the poster presentations.

Guohui Wang*, Elizabeth H. Denis*, Nicholas L. Huggett, Anjelica Bautista, and April J. Carman
Pacific Northwest National Laboratory, Washington, USA
*Emails: guohui.wang@pnnl.gov and elizabeth.denis@pnnl.gov

Noble gas and other vapor transport through geologic materials has important applications in the verification and characterization of underground nuclear explosions. However, transport of those gases to the surface is a complex process relying on the adsorption and diffusive processes in the subsurface at different temperatures and pressures. Our recent work demonstrated that inverse gas chromatography (iGC) is effective in analyzing key physicochemical parameters (e.g., adsorption, partition coefficient, and diffusion coefficient) used for modeling subsurface gas transport [1,2]. In this study, a method was developed to measure trace noble gas element adsorption to geologic materials in the presence of a background gas that could potentially compete for surface adsorption sites. Adsorption of four noble gas elements (Ne, Ar, Kr, and Xe) at variable concentrations in helium and nitrogen were measured on a sample of crushed tuff (a volcanic zeolitic material) at 0 – 45 °C. Another study was conducted to better understand the diffusion process in relevant porous geologic materials, especially noble gas diffusion from rock fractures to the surrounding rock matrix. A modified time-lag method by using a chromatographic column based on Fick’s law was developed and used to measure krypton and xenon diffusion through crushed tuff in the presence of a background gas (N2) under different temperatures (0 – 60°C) and pressures (10 – 50 psi). For higher temperatures, in collaboration with Surface Measurement Systems (SMS) using their new high-temperature iGC, the partition coefficient for zeolite samples were measured with organic vapors at 100 – 500 °C. The results indicate that the iGC method is a useful tool for better understanding vapor transport in the subsurface.

References:
[1] Denis et al. 2021. Physicochemical gas-solid sorption properties of geologic materials using inverse gas chromatography. Langmuir 37, 6887-6897.
[2] Cantrell et al. 2022. Noble gas adsorption to tuff. J. Environ. Radioact. 243: 106809.

Acknowledgements:
This Low Yield Nuclear Monitoring (LYNM) research was funded by the National Nuclear Security Administration, Defense Nuclear Nonproliferation Research and Development (NNSA DNN R&D). The authors acknowledge important interdisciplinary collaboration with scientists and engineers from Los Alamos National Laboratory (LANL), Lawrence Livermore National Laboratory (LLNL), Nevada National Security Site (NNSS), Pacific Northwest National Laboratory (PNNL), and Sandia National Laboratories (SNL).

Details pending

Leading sorption scientists will be here to address some key questions facing the sorption community, and take queries from the audience. A great opportunity to take advantage of the panels technical expertise, raise a query of your own, or get their views on something raised in the course of the days program.

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