As October ends and Diwali excitement fills the air, there’s a fun and colorful use of powders: the vibrant tradition of rangoli! This art form uses colorful powders to create intricate designs, symbolizing prosperity and welcoming the goddess of wealth and good luck. To achieve those beautiful, detailed designs, the powders need specific rheological properties—and that’s where powder rheology comes in.

Rangoli colors are as vibrant as Diwali itself, each adding joy to the festivities. Creating rangoli designs is a fun experience, especially with a variety of powders. When creating rangoli, you’ve probably noticed that sometimes, even when you get powders from the same factory, some colors flow smoothly while others can be a bit stubborn. This could be due to differences in additives and pigment properties. Differences in flow behavior due to things like additives and pigments are part of what powder rheology can help us understand.

As Diwali approached, we got our hands on five vibrant powders – red, blue, green, yellow, and white – all from the same factory. We thought, “Why not study their powder rheology and see how they behave?” Cool, right? So, we set up a little experiment in our backyard rheology lab using our powder rheology accessory.

When it comes to selecting materials for your next innovative product, the material specification sheet is likely the first place that you will turn. This document provides core properties measured by the manufacturer and serves as an essential tool for supplier verification and new product development. However, while these sheets are reliable and provide a standard method for comparison, they often fail to tell the whole story.

For successful material selection, product performance, failure prevention, it is important to go beyond the spec sheet and conduct in-house testing. This proactive approach will save you both time and money by facilitating informed material choices and enhancing product design.

A material specification sheet provides a snapshot of a material’s key properties as measured by the manufacturer. These properties are typically measured using standardized methods such as ASTM or ISO standards, offering some consistency and comparability across different materials. The spec sheet can be used for various purposes:

• Supplier Verification: Ensuring that the material provided by a supplier meets the necessary criteria for production.
• New Product Development: Aiding in the selection of new materials during the design phase of a product.

While spec sheets provide a foundational understanding, relying solely on them can be risky; they often provide incomplete information to know the material’s performance or predict lifetime of a product, especially in real-world application conditions.

Spec sheets are foundational for understanding general material properties, but they often lack detailed information about how a material will behave under specific conditions, such as the effects of different temperatures, prolonged stress or stress cycles, or exposure to harsh environments. Uncovering these blind spots is necessary for improving processing conditions, understanding material lifespan, and ultimately selecting the right material at the start of your development process.

To fully understand a material’s properties and ensure it meets your specific requirements, additional testing is required. Here are some critical aspects to consider:

Environmental Impacts

Materials can perform differently under various environmental conditions, such as UV exposure, or humidity. Due to the impracticality of inspecting materials in active use, such as polymer coatings on wires embedded in walls, a quick test lasting only a few minutes to hours is conducted to estimate the long-term stability of these materials over decades.¹

Differential scanning calorimetry (DSC) with oxidative induction time (OIT) analysis helps predict the aging and degradation of polymers, guiding material selection for longevity and reliability. For instance, polymers exposed to heat, oxygen, or light degrade faster, and OIT provides insights into their lifespan.

A variation of the OIT test, known as high-pressure OIT (HPOIT), is becoming increasingly popular. Proponents argue that oxidative data obtained under high pressure and temperature conditions align more closely with results from traditional, accelerated aging tests. The HPOIT test offers two primary advantages: high pressure raises the boiling points of additives, reducing their volatility, and it increases the concentration of the reacting oxidizing gas. This enables the use of lower test temperatures or significantly reduces test durations at comparable temperatures.²

Alternatively, high-pressure thermogravimetric analysis (HP-TGA) simulates extended exposure to harsh environments by using a combination of heat and elevated pressure. It is particularly useful for materials used in industrial applications, such as cabling for electrical or fiber optic systems. Safeguarding polymers against catastrophic degradation when exposed to direct sunlight or buried underground is crucial for these applications.³

Mechanical Behavior

Understanding the mechanical properties of materials beyond the scope of the datasheet is essential for nearly every application. For example, the following should be considered:

• Temperature Effects: Materials can exhibit drastically different properties at varying temperatures. Datasheets typically only list tensile properties at room temperature, but materials are frequently expected to perform under higher or lower temperatures.
• Long-Term Loading: What happens if a material is subjected to a load for weeks, months, or even years? Will it deform over time, i.e., creep? Will it crack under prolonged stress, i.e., creep rupture? For example, a clothing hanger may perform well under normal use, but storing a heavy coat over winter could cause the neck to elongate and eventually break. In this example, the clothing hanger began failing to perform its function (holding up clothes) due to creep and fell off the rod. Had it not fallen due to deformation, it would have eventually cracked due to creep rupture.

• Repeated Loading: In a process known as fatigue, repeated loading can cause accumulating damage, leading to fracture. It is important to know the stress levels and number of loading cycles a material can withstand before failure. Polymers exhibit fatigue in a very different way than metals and fatigue life estimates cannot be extrapolated from tensile strength as easily. Additionally, the usage temperature can have a significant impact on fatigue life at much lower temperatures than metals.

Mechanical test instruments evaluate durability and mechanical characteristics under various stresses (forces), frequencies, and environmental conditions. Specifically, Electroforce load frame instruments measure a sample’s response to force, whether it is a single push or pull (tensile test), repetitive load (fatigue), or creep/stress-relaxation test. Mechanical testing also accounts for environmental effects by testing in temperature-controlled air, gas, or fluid submersion.

Material testing is crucial in manufacturing and product development because it minimizes the risk of product failure, which can have costly and even dangerous consequences. Unexpected material behavior can lead to malfunctions, product recalls, and reputational damage.

For example, a woven fiberglass composite had a manufacturer’s recommended operating temperature up to 130°C. However, Dynamic Mechanical Analysis (DMA) testing revealed that the material’s storage modulus and loss modulus began to change around 100°C.⁴ Further fatigue testing data revealed that the material had a 90% reduction in its fatigue life at 100°C.⁵ Manufacturers could have mistakenly put this material into products used at high temperatures, such as baking, without realizing that it was highly likely to break.

Conducting thorough testing upfront provides higher confidence in material choices, ultimately saving time, money, and resources. Moreover, comprehensive material testing contributes to better long-term product reliability and performance. By thoroughly examining how a material responds to factors like fatigue, creep, and environmental degradation, manufacturers can design products that not only meet initial requirements but also maintain integrity throughout their life cycle. This proactive approach fosters innovation in product design, as engineers gain a deeper understanding of the material’s limits and capabilities, allowing for the creation of more efficient, safer, and longer-lasting products.

Going beyond the spec sheet is not just a recommendation; it is a necessity. By investing in additional testing, such as OIT using DSC and HP-TGA, you can uncover profound insights about material performance. By adding DMA and Electroforce fatigue testing to your testing suite, you can better predict material properties at various temperature conditions and repeat loading. These insights will ensure you make informed decisions that save time, money, and valuable resources by selecting the proper material for your application conditions. TA Instruments is here to support you with precision instruments and technical expertise, ensuring you have the tools needed to expertly evaluate materials and make the best decisions for your projects.

Biologic therapies derived from living organisms have revolutionized the treatment of complex diseases, yet their high development costs are often passed onto patients. Biosimilar drugs offer a promising solution to reduce costs while maintaining therapeutic efficacy. Unlike generic drugs, biosimilars cannot be exact replicas of their reference biologics due to their complex structures, necessitating rigorous testing and regulatory approval. Microcalorimetry, specifically Differential Scanning Calorimetry (DSC), plays a crucial role in this process by assessing the thermal stability of biosimilars to ensure they are structurally similar and perform equally to their reference drugs. In this blog, we examine why testing is crucial in the regulatory process and how instruments like the DSC are helping usher an influx of biosimilars to patients who need them.

Biologic treatments–those sourced from living things like proteins, stem cells, or genetic material–have saved and improved billions of lives. You, or someone you care about, has benefited from their unique ability to tackle some of our trickiest and deadliest diseases, be it insulin to control and treat diabetes, the mRNA vaccines that curbed and reversed the global COVID-19 pandemic, or immunotherapies helping to slow and reverse deadly cancers.

These pharmaceutical breakthroughs have, no doubt, made the world a healthier place, but not without requiring billions of investment dollars in research, development, and commercialization. That cost is ultimately passed on to insurance companies, healthcare providers, and patients themselves. Fortunately, there is a burgeoning solution to curb cost and increase access: Biosimilar drugs.

In this blog, we examine why biosimilars–despite offering comparable benefits to their “generic” small-molecule drug counterparts–undergo a more stringent regulatory process and how testing for thermal stability using Differential Scanning Calorimetry (DSC) is a critical step in ensuring these therapies function safely and effectively when they reach the patients who rely on them to stay alive.

Like generic drugs, biosimilars can be developed and prescribed once their breakthrough name-brand counterparts’ patent expires. Yet there’s one fundamental difference.

• Generic drugs have a small-molecule structure that is an exact copy of the original name-brand version. Think of Advil (the name-brand) and ibuprofen (the generic) or Lipitor and atorvastatin. The ability to reproduce a structurally perfect copy means a far more straightforward approval process. It also allows pharmacies to fill name-brand prescriptions with generic versions without additional testing or regulation.
• Biosimilars are precisely as the name suggests–similar versions to their name-brand biologic. Because they are sourced from living components, their structures are enormously complex. A perfect copy is impossible. That means, even if their treatment efficacy is the same, they require far more stringent testing and regulation before reaching the market. In particular, if the developer wants to create a therapy that will safely replace or interchange with the original treatment under the same prescription.

Both biosimilars and generics provide similar benefits to patients. More options mean easier access and lower cost. Yet a biosimilar’s journey from lab to patient is more complicated, which is why there are far fewer in the market.

Global regulatory agencies require a biosimilar to meet a specific set of criteria before entering the market. Despite not being molecularly identical to their name brand, a biosimilar must:

1. Use the same “mechanism of action:” The way in which the biosimilar interacts with, controls, or fights the illness must be identical to the original drug.
2. Use the same “route of administration:” If the original is administered through an injection, a patch, or a pill, the biosimilar needs to be delivered through identical means.
3. Be manufactured with a similar potency, purity, and dosage: The biologic’s efficacy can’t rely on more or less treatments or volume.
4. Undergo clinical trials to approve efficacy: However, this process is faster and less strenuous because the original biologic has already endured rigorous study. Which, of course, is why biosimilars are more affordable.

The goal, ultimately, is to ensure the biosimilar performs as well as its counterpart so that, even though it is slightly different at the micro level, it still provides the same effective treatment. But getting there doesn’t just require human trials; testing the formulation’s structure and stability in the lab is a critical early step.

In the past 15 years, countries worldwide have adopted similar regulatory processes to develop, test, and approve biosimilar drugs. Each includes an “Analytical Similarity Assessment“: a series of independent lab tests to prove that the structural properties of the biosimilar closely match the name brand.

‘Conformational Stability” is a fundamental component of the assessment. This tests how the drug’s structure changes through varying temperatures, time, or both. Researchers commonly use a specialized instrument called a Differential Scanning Calorimeter (DSC) to capture the necessary data for the assessment. The tool allows researchers to examine how multiple samples of a given compound transform or react to minute, precisely controlled temperature changes. To be considered a biosimilar, a new therapy must react to heat in the same way as the original biologic. Tools like the Nano DSC offer automated throughput and the highest level of measuring sensitivity to extract vital data during the regulatory process for low dose antibody drug products. Which means it is highly likely, and increasingly necessary, that the biosimilar drugs used in treatment today underwent some form of DSC testing.

The one disadvantage of traditional DSC instruments is that high concentration drug products require dilution to avoid damaging a fixed cell. The new TA Instruments RS-DSC solves this by using disposable micro fluidic chips, allowing for formulations with concentrations >20 mg/mL to be tested in their natural state, quickly and at scale. Ultimately, this provides the most accurate thermal stability data possible while mimicking real-world conditions.

Even if a biosimilar is approved, one additional regulatory hurdle must be surmounted for ubiquitous accessibility. In an ideal scenario, a biosimilar could be swapped for the original biologic at any time during the treatment (if, say, there is a shortage of the name-brand option or the cost becomes prohibitive).

When this option is available, the biosimilar has been approved for “interchangeability.” The drug has undergone human clinical trials and significant lab testing to ensure it behaves precisely the same way as its peer. This additional process differs from generic small-molecule drugs. Because they are functionally identical to their originals, this extra approval isn’t necessary.

But a biosimilar drug’s stability and efficacy can sometimes change, even when stored in the exact same conditions. Which is why testing, at the micro level, how and why the formulation changes compared to the name brand is critical. That can only be done prior to the human trial in a lab using a bevy of instruments, including DSC.

When more biosimilars reach commercialization, global healthcare becomes more accessible and equitable. It’s great news, then, that expiring patents and development innovations will ensure an influx of biosimilars in the near future. But the stringent, regulated process required before reaching patients is vital. Testing, whether done during human trials or earlier in the lab using DSCs along with other instrumentation, ensures that no matter where the treatment comes from, it’s as safe and effective as the blockbuster drug that inspired it.

The composites market is evolving fast. Global market projections indicate a 10.8 % growth by 2028, driven by the demand for composites across industries looking for materials with superior performance at reduced weight and cost.¹ This blog explores how advanced material analysis can enhance R&D and manufacturing processes in the composites market, ultimately leading to financial savings and increased efficiency.

While traditionally associated with the aerospace sector, composite materials have been adopted by several industries. Sectors actively utilizing composites include:

• Aerospace: Valued for their high strength-to-weight ratio, composites like carbon fiber reinforced polymer and aramid reinforced polymer enable the production of lighter, more fuel-efficient aircraft and satellites, contributing to reduced operational costs and increased payload capacities.²
• Automotive: A variety of automotive components, such as chassis and suspension systems, rely on composites for improved safety, fuel efficiency, and performance. Stringent emission regulations are driving this shift, including lightweighting automotive materials for enhanced fuel economy.³
• Renewable Energy: Composites are integral to the renewable energy sector, particularly in the construction of wind turbine blades and solar panel components. Companies are leveraging the dimensional stability, durability, and strength of these materials for operation under harsh environmental conditions, enhancing the longevity and efficiency of renewable energy systems.³
• Construction: Advanced composite materials, such as high-performance concrete mixes and fiber-reinforced polymers, can create structures more resistant to environmental degradation while offering excellent design flexibility. This improves construction longevity, reducing maintenance costs over time.⁴

While composites offer numerous advantages, manufacturers and material scientists face several challenges during their development and manufacturing including:

Designing and Selecting the Right Material

One of the main challenges in composites R&D is the selection of appropriate materials for specific applications. Researchers must consider criteria such as mechanical strength, thermal stability, and environmental resistance, which will entail the careful balancing of trade-offs between different performance characteristics.

Increased Complexity of Material Design

In achieving the desired balance of characteristics, scientists need to precisely control parameters such as filler orientation and distribution. Research has shown that the incorporation of nanofillers into a polymer matrix can bolster its mechanical properties and reduce water absorption in fiber-reinforced composites. As a result, strong interfacial adhesion is established between the matrix and nanofillers, allowing for efficient stress transfer during loading.

However, if not properly managed, the orientation and distribution of fillers within a composite can lead to variations in strength and other properties. The subsequent effect on the interfacial interactions can induce premature failure in the material.⁵

Sustainability

Reinforced polymer composites present several benefits, including the conservation of depleting resources such as metals and alloys. However, their disposal poses significant environmental challenges due to the non-biodegradable nature of petroleum-based polymers and synthetic fibers.

Consequently, research has increasingly focused on developing fully biodegradable and eco-friendly materials known as green composites. The use of green composites has significantly expanded across various engineering disciplines, yet the limited solubility of lignin-based materials for analytical purposes restricts the complete understanding and development of lignin-based green composites.⁶

New Manufacturing Techniques

Techniques like lightweighting and additive manufacturing deliver benefits but also introduce new challenges. Lightweighting replaces heavy materials with lighter-weight composites without compromising strength-to-weight ratios or structures’ fundamental design, while additive manufacturing increases throughput and design complexity. However, researchers must tackle the expensive nature of lightweighting processes, which can also risk impairing the ductility and formability of the materials, as well as concerns regarding the fabrication of composites with long fibers and complex cavities that surround additive manufacturing.^7,8

High Manufacturing Costs

Producing complex composite parts can require costly raw materials, specialized equipment, and skilled labor, leading to high costs. Effective quality control measures are essential to ensure that the final products meet the required standards without excessive waste or rework.⁹

To overcome these challenges, precise material analysis is essential. Key material properties to measure include:

• Glass Transition and Crystallinity: Differential Scanning Calorimetry (DSC) is a powerful technique for measuring the glass transition temperature and crystallinity of composites. These parameters are critical for understanding the thermal and mechanical properties of the material. For example, NASA uses a TA Instruments DSC to determine the quality of thermoplastic composite panels, which is vital for ensuring their performance in space applications.¹⁰ Further examples of real-world composites research using DSC can be found in our blog.
• Cure Kinetics, Cross-Linking, Gelation, and Cure Conversion: DSC paired with LED-PCA accessory can measure cure kinetics and the extent of cross-linking, gelation, and cure conversion in composite materials. These measurements help optimize processing conditions to achieve the desired mechanical properties and durability.^11,12
• Structural Relaxation, Time-Temperature Superposition, and Aging: Dynamic Mechanical Analysis (DMA) provides insights into the viscoelastic behavior of composites, including structural relaxation, time-temperature superposition, and aging effects. This information is key for predicting the long-term performance and stability of composite materials under various, sometime harsh, environmental conditions.¹³ Learn more about DMA testing of composites in this blog.
• Coefficient of Thermal Expansion: Thermomechanical Analysis (TMA) measures the coefficient of thermal expansion, which is important for understanding how composite materials will behave under thermal cycling. This is particularly relevant for applications where materials are exposed to varying temperatures, such as in aerospace and automotive industries.¹⁴

In response to the rising demand for materials that combine superior performance with low weight and cost, the composites market is rapidly expanding. This growth trajectory underscores the importance of addressing inherent challenges in the development and manufacturing of composites, such as selecting and designing appropriate materials, ensuring sustainability, implementing new manufacturing techniques, and managing high production costs.

Advanced material analysis techniques, including DSC, DMA, and TMA, are crucial in overcoming these challenges. These techniques provide critical insights into the thermal and mechanical properties of composites, enabling researchers and manufacturers to optimize processes and achieve the desired performance and durability.

TA Instruments supports composite R&D with cutting-edge material analysis instruments, helping you to overcome the complexities of composite design and manufacturing. By investing in advanced material analysis, companies can lower costs, increase efficiency, and stay competitive in the rapidly evolving composites market.

For more information on how TA Instruments can support the R&D of your composites, visit our composites page or contact us to speak with an expert.

The stability of high-concentration drugs can change under storage conditions, but until now, thermal testing in the lab using traditional calorimetry methods has been time-consuming and challenging. The new TA Instruments RS-DSC fills a critical antibody formulation development gap by allowing for high-throughput short-term thermal stability testing at formulation strength concentrations. In this blog, we explore why that’s essential.

Subcutaneous injection has revolutionized how billions of patients receive the crucial treatments that keep them alive. From a regular dose of insulin to treat diabetes to the monoclonal antibody adalimumab that regulates rheumatoid arthritis, the ability to self-administer these life-saving therapies provides enormous benefits for both patients and healthcare providers, saving time, money, and resources.

To be effective, though, these treatments require a higher drug concentration within each dose. Researchers already use various testing methods to evaluate drug product stability, from differential scanning calorimetry (DSC) to dynamic light scattering (DLS). While both these methods provide accuracy in the lab using diluted samples, they can’t quickly or effectively measure the stability of real-world concentration levels. Even slight adjustments to the solution environment, including increasing concentration, can introduce unknown and unpredictable changes in high-concentration biologics. Until now, though, analyzing the thermal stability of drugs under high concentration conditions has been time-consuming and challenging.

TA Instruments’ newest innovation, the RS-DSC (Rapid Screening-Differential Scanning Calorimeter), fills a critical testing gap, allowing labs to quickly understand thermal stability of their formulation strength drug products. In this blog, we explore the importance of thermal stability testing and how the RS-DSC drastically improves the process.

Until recently, most biologics have been administered through intravenous injection. For patients, that meant a trip to the doctor’s office and oversight from a professional to receive their life-saving therapies. A simple shot into the skin via needle and syringe is far cheaper and more convenient, which explains the wide adoption of subcutaneous (the innermost layer of skin tissue) injections. From 2017 to 2021, roughly half of all FDA-approved treatments were developed to be administered subcutaneously.

While the method has lowered costs and expanded global access to essential drugs, it makes research and development more complex. Unlike the steady drip of an IV, a shot through the skin requires far less volume, meaning the concentration of the biologic must be significantly higher. That ratio can change the biopharmaceutical stability — and effects the entire development pipeline.

Understanding how a biopharmaceutical responds to thermal stress is an important predictor of shelf-life and efficacy. Short-term thermal stability lends insight into biopharmaceutical structure and understanding how functional variations arise. It is a key metric employed in candidate selection and provides critical information in selecting buffer composition in the development of clinical formulations. Lower thermal stability can be an indicator of aggregation, poor shelf-life, and ultimately drug efficacy. Thermal stability testing ensures researchers know the way a drug will change under stress, letting them predict how that drug will behave in a patient’s home or on a pharmacy shelf.

Aggregation and structural stability are commonly evaluated using light scattering and calorimetry:

Dynamic Light Scattering (DLS): In this method, a laser is passed through a liquid sample, causing light to scatter between individual particles. This lets researchers determine the size distribution and aggregation of drug particles over time. Understanding these changes can help determine if a drug remains safe and effective in varying concentrations and while stored in differing temperatures.

Differential Scanning Calorimetry (DSC): This method uses the controlled application of heat to examine how and when the substance transforms. Researchers can then precisely understand the formula’s stability at different concentrations and under different conditions. Evaluating the thermal stability of a given solution gives insight into the folding and function of the protein and informs understanding of the impact of the solution environment on the protein structure as a whole.

In biologics development, DSC is the gold standard for short-term stability testing. But the process has one major flaw: high-concentration samples must be diluted. That’s because DSC requires a fixed sample cell that must be cleaned between samples. High-concentration solutions can clog the cell when heated, either making it useless or forcing researchers to employ harsh, lengthy cleaning protocols between trials. For intravenous treatments, this isn’t an issue. The low concentration means most tests never reach the instrument’s upper limit. Not so with subcutaneous injections. As the treatment delivery option becomes increasingly popular, the industry needs a scalable, cost-effective, and fast solution that outputs reproducible and accurate results.

The RS-DSC is revolutionary because it can rapidly test a high number of samples at high concentrations and low volume– while still employing calorimetry to provide the most accurate thermodynamic data possible. The key innovation comes from disposable microfluidic chips rather than relying on a fixed measurement cell as seen in traditional DSC instruments. This offers three key benefits:

1. The instrument can test 24 samples simultaneously, significantly increasing throughput while reducing sample consumption.
2. The low volume microfluidic cells only require 11 µL of sample, maximizing material use and minimizing cost.
3. Disposable chips eliminate cleaning and remove the need for dilution. Thus, the effects of formulation strength antibody treatments can be predicted far more quickly and accurately.

All this means the RS-DSC doesn’t only test higher-concentration samples with greater accuracy. It saves time and material, and therefore money. That means breakthrough therapies can reach more patients–faster and cheaper.

Advances in therapeutic biologics mean more and more people will receive life-saving treatment via a shot through their skin. But this convenient, cheap, and easily administered treatment option is only possible if pharmaceutical researchers are completely confident their high-concentration drugs can tolerate real-world conditions. That’s why, in a drug’s journey from lab development to blockbuster adoption, the RS-DSC is now a critical link to better treatments and healthier patients.

High-performance polymers are a critical material for manufacturers due to their combination of mechanical, thermal, and chemical properties, but especially their cost. Without adequate testing, manufacturers could run into a slew of issues, from immediate product failure to poor performance or failure after some time in usage. In this post, we review the three most important types of mechanical testing to better predict and ensure performance, safety and reliability.

As high-performance and technical industries innovate, so do the materials they use to build their products. A car company might have to design a specialized part to handle increased torque from an EV. An engineer might need to develop a novel storage solution for critical scientific cargo in a rocket headed to the International Space Station. No matter the goal, each component must perform safely, reliably, and predictably. Success requires a multi-faceted testing approach in the development stage, because the stakes could not be higher when a product reaches the real world (or leaves it).

Whether a new supplier is necessary because of lingering supply chain complexities after the COVID-19 pandemic, weight and cost reduction are required to innovate, or sustainability is mission critical, more and more industries around the globe–from aerospace to automotive to life sciences and beyond–have shifted toward one common materials solution: High-performance, synthetic polymers.

High-performance polymers are a category of chemically-produced substances such as polyamides, polyethylene, Teflon, and synthetic rubber. They offer numerous benefits, including reduced production costs and lower weight than historical engineering materials like steel and aluminum.

However, implementing any new material into your production process takes extensive lab time to answer two key questions: How does this material change over time? And how does this material respond to specific types of stress? Proactively answering these questions before launching your product isn’t just essential to your P&L. It’s also crucial to establish parameters for safe and reliable use.

Here are three types of mechanical testing that measure polymer behavior–whether that polymer is headed through the grocery store parking lot or into low earth orbit.

Fatigue Testing

Polymers usually fail in one of two ways:

1. Over time from repeated use.
2. All at once under extreme stress.

Manufacturers almost always test number two, yet they frequently overlook number one. But plastics are actually more sensitive to failure over time. Which is why fatigue testing is critical in any high-performance product–it reproduces the conditions in which a material behaves tomorrow, next week, or in 10 years.

Fatigue testing ensures you know precisely how many “pulls” it takes to break a product or material. Specialized equipment, like Load Frame Instruments, replicates real-world conditions, using predetermined levels of force over and over until a failure occurs. This information can predict product endurance, optimize structural design, inform safety limits, or help determine durability.

Observing a material after its first or even 10th use might be relatively simple. But what about its 40,000th? Fatigue testing is the most accurate and timely way to answer that question before your product leaves R&D into the real world.

Tensile (Monotonic) Testing

What happens to a polymer under a single, powerful blow? How much force is required to break it? Tensile–or monotonic–testing gets the answer.

Data like this is necessary in its own right, but tensile testing provides even more valuable insight when combined with fatigue testing. An initial tensile test provides thresholds that can then repeat over thousands of cycles. An instrument like the ElectroForce 3200 can perform both by applying precise levels of force and then duplicating those levels – thousands or even millions of times.

That testing rigor provides a fuller understanding of a material’s weakness – from catastrophic failure to normal wear and tear. This means you will gain the insight needed to save both money and time during the pre- and post-production cycles. More importantly, you’ll also get information that can save lives.

Dynamic Mechanical Analysis (DMA)

Time and force are crucial variables in polymer research. But so is temperature. Dynamic Mechanical Analysis combines all three to measure three fundamental material properties:

• Storage modulus: The stored energy (stiffness) of a material, and how that energy returns when it’s stretched and returns back into shape.
• Loss modulus: The energy lost to heat from the materials’ viscous properties, also known as damping.
• Glass transition: The temperature range in which a material changes from its rigid “glassy” state into a more rubbery, viscous state.

From testing the modulus difference between multiple samples of one polymer, understanding how a modulus changes across a temperature range, or finding the precise temperature ranges where a material loses its structural rigidity, DMA provides robust data with a wide range of applications. Quality control, product development, and product performance just to name a few.

A complete understanding of a polymer’s behavior is not possible through any single form of mechanical testing. You might know how much force it takes to break a single sample. But what about when 50% of that force is applied 10,000 times? Or if that force is applied next to a running engine at midday?

Any one mechanical test–be it fatigue, tensile, or DMA–provides an incomplete picture. As more and more industries need to navigate the polymer development journey, only combining all three ensures they’re fully equipped to ensure they do it successfully. But with the proper tools and a rigorous testing process, polymers will continue to fuel innovation in industries worldwide.

The method of drug delivery significantly influences the final stages of the manufacturing process. Currently, lyophilization—a widely adopted technique—enables drug developers to stabilize formulations and therapeutic molecules using a validated commercial approach. In this process, precise control of pressure and temperature within a lyophilizer facilitates the removal of liquids from formulations containing thermally sensitive or hydrolytically unstable active pharmaceutical ingredients or formulation components.¹ The resulting solid product exhibits enhanced stability, an extended storage life, suitability for higher-temperature storage, and ease of packaging compared to aqueous solutions. Remarkably, over 60% of biologics available in today’s market owe their existence to lyophilization, rendering this technique exceptionally attractive for integration into the manufacturing process.

Currently, many lyophilization strategies can be used to develop high-concentration monoclonal antibodies. To begin, the development of successful antibody therapies requires administration at high dose levels. However, it is challenging for high-concentration monoclonal antibodies to be delivered effectively due to their limited intrinsic stability. By introducing an optimal lyophilization process, developers would be able to increase stability, limit storage requirements, and ease the shipping issues. There are three distinct stages in the lyophilization process: freezing, primary drying, and secondary drying. The first stage, freezing, is carried out at temperatures below Tg (glass transition temperature) for an amorphous, or below Teu (eutectic temperature) for a crystalline state, for a sufficient period to allow for full transformation into a solid.² To achieve high crystallization rate and complete crystallization, the annealing temperature is usually held between the Tg of the amorphous phase and the Teu of the bulking agent.² Additionally, it is important to start off by using a moderate cooling point to prevent any degradation.

The subsequent phase, known as primary drying, eliminates frozen water by raising the shelf temperature and reducing chamber pressure. Optimizing primary drying can significantly reduce cycle time and depends on factors such as formulation, shelf temperature, container type, and chamber pressure.2 Overall, achieving a high sublimation rate with uniform heat transfer is the goal during this step. Following primary drying, we encounter the secondary drying phase. Here, water is extracted from the solute phase through desorption. The effectiveness of secondary drying hinges on the ramp rate, which varies based on the product type (whether amorphous or crystalline).² Additionally, various stability-affecting factors—such as antibody concentration, excipients, and container properties—should prompt a case-by-case approach to secondary drying for optimal efficiency. A comprehensive grasp of these three pivotal stages contributes to successful lyophilized product development and streamlines the manufacturing process in drug development.

While lyophilization offers advantages such as increased stability, solid-state drug delivery, and other benefits, it remains a highly specific process demanding meticulous control. Deviations from proper procedures can result in inadequate freezing, equipment overload, or sample damage, ultimately compromising drug efficacy and potency.³ Therefore, comprehensive characterization is essential to optimize sample preparation, lyophilization, and product delivery. Researchers must conduct thermal analysis throughout the entire process to assess how temperature variations impact material properties.

The Tg is the point at which there is increased mobility of a lyophilized sample as it transitions from its frozen, brittle state to a more viscous state.³ It is critical for researchers to identify the glass transition temperature to optimize the temperatures used at each step of the lyophilization process. TA Instruments offers, the Discovery DSC and the Multi-Sample X3 DSC to measure Tg directly. Both instruments utilize TA Instruments’ patented Fusion Cell design to provide the highest level of performance for the most accurate and robust thermal analysis measurements.³ The Multi-Sample X3 DSC offers a distinctive advantage: the capability to simultaneously run three samples, providing a wealth of data in a shorter timeframe.

After freeze drying a sample, researchers can use Thermogravimetric Analyzers (TGAs) to reliably detect even the smallest amount of residual moisture. This analysis can be used to evaluate the quality of the lyophilization process, predict how stable a product is likely to remain, and determine optimal parameters for lyophilization.⁴ In addition, TGA can also measure weight loss due to thermal decomposition, which can reveal insights into how the properties of the product might have changed during lyophilization. TA Instruments offers a range of TGAs for every lab’s needs. The TGA 55 is a rugged, reliable, and cost-effective option with proprietary Tru-Mass balance for the most accurate measurements across competitive models. The TGA 550 offers enhanced performance and flexibility with add-on features and optional expansion. Lastly, the TGA 5500 provides ultimate performance with less drift than any competitive TGA, plus the fastest heating and cooling rates available. Therefore, for any lab attempting to optimize their lyophilization process, TA Instruments offers a TGA to suit their needs.

Finally, it is important to make sure the in-solution properties of the protein have remained unchanged after lyophilization and reconstitution. The Nano DSC allows one to evaluate any alterations in the product’s stability or efficacy by measuring shifts in melting temperature and enthalpy. Using these parameters, the Nano DSC provides insights into whether the lyophilization process impacted molecular stability.

In the world of biologics, stability is crucial. Lyophilization, our trusted ally, preserves delicate formulations and therapeutic molecules. Yet, success hinges on precise temperature control. In this blog, we’ve highlighted the pivotal role of thermal analysis &ndash a compass guiding us toward optimal lyophilization conditions. By using this tool, we optimize the process and protect protein integrity during lyophilization.

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