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Gas Adsorption & Porosimetry Analyses at PTL

At PTL, our trained chemists perform routine as well as advanced material characterization analysis services.  They also conduct method developments, validations and execute transfer protocols all while solving complex problems for clients from a variety of industries.  These industries include pharmaceutical, environmental, petrochemical, manufacturing, cosmetics, dietary supplements, food and beverage and others.

Among the many types of particle sizing and characterization services offered at PTL, our expert chemists perform analyses using various gas physisorption techniques to determine BET surface area. Porosimetry can be measured using gas adsorption and mercury techniques depending on the material’s pore size. We follow standard methods from various organizations such as ISO, USP, and ASTM where applicable.

To determine the most appropriate techniques for your surface characterization needs, please contact us by clicking here.

Following is a brief description of PTL’s BET surface area analysis, micropore/mesopore measurement and mercury intrusion porosimitry testing.

BET SURFACE AREA ANALYSIS

 

Surface area analysis detects and measures the cracks or crevasses, surface roughness, or accessible pores of particles, all of which can greatly affect the performance and behavior of a material. Pharmaceuticals, catalysts, adsorbents, materials for separation technologies, pigments, cosmetics, geologic & construction materials are just some materials that exhibit varying physical properties and effectiveness depending on their surface area and porosity.

The BET (Brunauer, Emmett and Teller) Theory is commonly used to evaluate the gas adsorption data and generate a Specific Surface Area (SSA) result expressed in units of area per mass of sample (m2/g). Briefly, this method involves allowing a clean and dry sample to adsorb a select inert gas such as nitrogen or krypton at liquid nitrogen temperature.  The BET theory is subsequently applied to interpret the adsorption data into information on the surface area.

For more detailed information about BET surface area analysis, click here.

MICROPORE & MESOPORE MEASUREMENT

Nanoporous materials are found in many research and industrial applications, including controlled drug delivery, energy conversion and storage, etc. A comprehensive characterization of nanoporous materials with regard to pore size, surface area, and pore size distribution is required in order to select and optimize the performance of these materials.

To determine the porosity of a material, various techniques may be employed depending on the size of the pores present and the chemical characteristics of the material. Per the International Union of Pure and Applied Chemistry (IUPAC), porous materials can be categorized as containing micropores (< 2 nm in pore diameter), mesopores (2-50 nm in pore diameter), and/or macropores (> 50 nm in pore diameter).

MICROPORE MEASUREMENT

Micropores are defined as pores with internal diameters of less than 2 nm. Characterization of the micropores involves the use of physisorptive gases that can penetrate into the pores under investigation. Gases used are those which are physically bound at the solid surface, a process referred to as physisorption; for example, N2 at 77K, Ar at 87K, and CO2 at 273K. Micropores are filled at very low relative pressure (P/P0), therefore, specialized instrumentation is required to measure these low pressures.

For more detailed information about Micropore analysis click here.

 

MESOPORE MEASUREMENT   

The fundamental principles and procedures of mesopore measurement are similar to BET surface area analysis using the static volumetric method.  First, any excess adsorbed gases are removed from the sample surface using vacuum or inert gas flow, typically at elevated temperature.  Then the adsorbate gas, most commonly nitrogen, is allowed to adsorb onto and desorb from the surface at liquid nitrogen temperature at varying relative pressures.  The use of other gases such as argon at liquid argon temperature has also been proven beneficial, especially if investigation into the micropore range (pore diameter of < 2 nm) is of interest.

For more detailed information about Mesopore analysis click here.

 

MERCURY INTRUSION POROSIMETRY TESTING

Mercury porosimetry is widely used in the catalyst and petrochemical industries for determining the pore size and pore volume of catalyst substrates such as silica and alumina zeolites.  In the biomedical field mercury porosimetry has been used to characterize tricalcium phosphate granules or strips used in bone grafts.  The pharmaceutical industry has found porosimetry useful in evaluating tablets formed using varied compression forces, for example.

The Washburn Equation relates the applied pressure to pore diameter using physical properties of the non wetting liquid (mercury in this case).  The physical properties include the contact angle between the mercury and the material, as well as surface tension. Instruments utilized at PTL allow for pressures ranging from approximately 1 psi up to 60,000 psi which correlates to measurement of pores from about 250 µm to 0.003 µm (3 nm).  The contact angle of the mercury on the material under test is an important consideration for optimal results.  The contact angle can either be provided or measured; otherwise default values can be entered during the analysis.  The volume of mercury intruded into the sample is monitored by a capacitance change in a metal clad capillary analytical cell called a penetrometer.  The sample is held in a section of the penetrometer cell, which is available in a variety of volumes to accommodate powder or intact solid pieces.  Sample size is limited to dimensions of approximately 2.5 cm long by 1.5 cm wide.

For more detailed information about Mercury Intrusion Porosimetry analysis click here.

This brief description covers only a small portion of the particle characterization services offered by Particle Technology Labs. For questions, or to discuss your specific testing needs, please contact us by clicking here.

PTL is a proven cGMP (current Good Manufacturing Practices) compliant laboratory, in accordance with 21 CFR, Part 210 and 211. Our facility is FDA registered and inspected, and we host over 30 audits per year from the world’s largest pharmaceutical companies.  We are DEA licensed and approved to handle Schedule II through V Controlled Substances.

 

Particle Technology Labs Particle Characterization Contract Analysis Services

The Trend in Outsourced Scientific Research and Development

Outsourcing or contracting is a common practice used by companies to reduce costs and raise profits by cutting down on staff and equipment needs. Due to economic factors over the last few years, including high labor and equipment costs of in-house laboratories, outsourcing is becoming increasingly prevalent in the scientific community.

As more companies and institutions turn to outsourced science for research and development, more options are becoming available for contracted laboratory analysis services. With a wider range of choices, comes a wider range of quality and service. When given a choice, be sure to start with the experts.

PTL is Proud to be a Pioneer in the Contract Analysis Industry.

When new drugs are developed, or new technologies invented, laboratory analysis is a vital step to test or prove the end product. Making sure the end product is safe, effective and successful in the long run depends on the quality of its materials and structure. Detecting any inconsistencies or problems early on is key. Product recall, liability and poor sales due to product inconsistency or poor performance are just some examples of issues that can lead to unrecoverable loss of revenue. Not using an experienced laboratory for analysis services may lead to unimaginable costs.

Choosing a Proven and Reputable Contract Laboratory with Experience and Expertise Should be the Single Most Important Deciding Factor.

PTL has always been a particle characterization research and advisory contract lab. We are a trusted advisor to the world’s leading pharmaceutical, industrial, public sector, and scientific organizations. We have been an important part of the research and development of countless products in many industries including pharmaceutical, environmental, petroleum-chemical, manufacturing, cosmetics, dietary supplements, as well as food and beverage. During this time, we have worked with individuals up to industry giants as they bring their ideas and products to life. Our scope and expansive knowledge of particle technology allow us to provide our clients with precise, comprehensive results. We address problems that no one else can and provide the insight necessary for our clients to make the right decisions.

As the scientific industry changes and outsourced laboratories become more prevalent, choosing the right laboratory is vital. At PTL, this has been our only business for over 25 years. Our expertise, commitment to quality and the outstanding customer service we offer is why the world’s leading public and private organizations continue to choose Particle Technology Labs for their contract laboratory analysis needs.

PTL is a proven cGMP (current Good Manufacturing Practices) compliant laboratory, in accordance with 21 CFR, Parts 11, 210 and 211. Our facility is FDA registered and inspected, hosting over 30 audits per year from the world’s leading pharmaceutical companies. We are DEA licensed and approved to handle schedule II through V controlled substances. We also hold an ATF permit for analyzing pyrotechnic materials.

Start with the Experts

Dynamic Imaging at Particle Technology Labs Advanced Particle Sizing and Characterization

Particle Technology Labs is pleased to announce the recent installation of our newest dynamic image analyzer, Particulate System’s Particle Insight. Approved for cGMP analysis, the Particle Insight joins our other dynamic instrument, the Malvern Sysmex FPIA-3000.

Many times, particle size distribution analysis alone provides adequate information about a material’s physical characteristics. However, in cases where the shape of the particles can affect performance and quality of the end product, more detailed information may be needed. For these applications, dynamic image analysis provides thorough and accurate particle shape characteristic measurements.

With the ability to analyze thousands of particles in the same amount of time needed to measure just a small number by manual microscopy or static image analysis, this state-of-the-art dynamic imaging instrument not only measures particle size, but also defines and characterizes particle shape, reporting detailed variations between samples in a fraction of the time.

While instruments such as laser diffractors provide a “size” of particles, the theory for data processing assumes the particles are spherical and require the operator to enter known optical properties of the particle and carrier for best results. Dynamic imaging instrumentation has the ability to not only size particles, but also detect and enumerate agglomerates, over-sized particles and contaminant particles without the need for the spherical shape assumption nor knowledge of the suspension’s optical properties. It can accurately measure the size of non-spherical particles such as needle-shaped crystals by providing length and width data, and can detect differences in optical properties such as transparency. Values called “shape factors” are reported and can be used to quantify differences in particle shape amongst a set of samples. The Particle Insight dynamic image analysis instrument can also potentially differentiate between individual components within a mixture on the basis of morphological or optical characteristics.

Dynamic imaging works by using a high resolution digital camera to capture images of dispersed particulate in a liquid suspension.  This liquid suspension is circulated through an optical cell, during which the digital camera captures images of the particles. Using digital thresholding techniques, images of particles are automatically and objectively measured, analyzed and classified for inclusion/exclusion. In reporting, images are displayed together with particle size and shape data, providing a very effective visual verification of results. The analytical technique is summarized in ISO standard 13322-2:2006 Particle size analysis — Image analysis methods — Part 2: Dynamic image analysis methods.

The Particle Insight provides a robust statistical measurement of particles in a sample as a whole. Compared to manual microscopy or static image analysis, dynamic imaging analyzes a larger number of particles in a shorter amount of time, while also reducing operator subjectivity, leading to more reliable and accurate results. In addition, due to the shorter analysis time, these analyses can be offered as a more cost effective shape measurement option to our clients.  Limitations to the instrument’s capabilities exist of course, so please contact us to discuss if your sample is applicable.

Visit our Image Analysis page on our website for more information.

PTL Celebrates Earth Day 2018

Safe disposal practices, recycling, and green lighting are just a few of the ways PTL works to responsibly protect our environment.

Our newest initiative began at the beginning of this month when PTL made the switch to paperless reporting. PTL completes thousands of analyses each year, and for every analysis, a report is produced. Historically, these reports were printed on paper, put into folders and envelopes and made their way to clients via trucks and planes. To cut down on paper waste and the environmental cost of transporation, PTL final reports are now digitally delivered via a secure online portal. This environmentally friendly delivery system places final reports in our clients’ hands much sooner, with less waste and negative impact on our planet.

On earth day and every day, PTL is striving to help protect our environment while delivering outstanding service and particle characterization results to our clients.
This means when you do business with PTL, you’re greener too.

Learn More

To learn more about Earth Day, visit the links below.

PTLs’ Michael Vinakos to Give Presentation at AFS Filtcon 2018

Michael Vinakos, Particle Characterization Chemist IV and Team Leader at Particle Technology Labs, will be presenting a technical session titled Understanding Particle Size Distributions. Mr. Vinakos’ lecture is one of several offered under the Indoor Air Quality session of the Air/Gas Track.
The session will be offered at the American Filtration & Separations Society’s (AFS) FiltCon 2018 which takes place April 23rd through the 25th, 2018 at the Mystic Lake Conference Center in Prior Lake, Minnesota. The society is a technical, educational, nonprofit organization dedicated to the exchange of information among engineers, scientists, and technologists in all areas of the fluid/separation field.

Mr. Vinakos’ presentation will focus on the interpretation of particle size distribution data and how particle size analysis is performed on captured air emissions samples.

The AFS Filtcon conference will feature 6 plenary sessions, 24 technical sessions, an expo featuring exhibitors, a student poster session and networking opportunities. Filtcon will also feature a selection of short courses.
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Mr. Vinakos joined PTL as a Particle Characterization Chemist I before advancing to his current position as Particle Characterization Chemist IV and Team Leader. In his present supervisory role, Mr. Vinakos directs particle sizing & counting techniques as well as the microscopy & image analysis activities within PTL. His role involves leading complex projects and providing detailed technical review of analytical data. Mr. Vinakos received a Bachelor of Science degree in Biology from DePaul University and a Master of Science degree in Biotechnology and Chemical Science from Roosevelt University.

More information on AFS FiltCon 2018 can be found at: https://afsspring.societyconference.com.

PTL Announces Paperless Reporting

Particle Technology Labs is pleased to announce that starting in early April, all final reports will be delivered to our clients digitally using Sharefile®, a file sharing service that securely transfers encrypted documents through an easy to use online portal.
How paperless reporting works.
When your final report is complete, you will receive an email with a link to Sharefile®  where you can log in to view your report instantly. If it is your first time using Sharefile®, you will need to sign up for an account, which is very simple. Just enter your name, company name and email. Once you are signed in, you can download your final report as a PDF document.
Final reports will remain available for download on Sharefile® for thirty days.
Further instructions for using Sharefile® are available by clicking here.

Multiple benefits. 

PTL is excited to deliver reports faster with a more positive environmental impact, while at the same time continuing to provide outstanding service and particle characterization results to our clients.

Visit PTL at the 8th World Congress on Particle Technology April 23rd April 25, 2018

Particle Technology Labs invites you to join us April 23rd through the 25th, 2018 at the Orlando World Center Marriott in Orlando, Florida for the 8th World Congress on Particle Technology.

Held every 4 years since its inception in 1990, the WCPT8 is intended to stimulate discussions on the forefront of research in particle science and technology.

As experts in the field of fine particle technology, we welcome the opportunity to meet with you and discuss questions related to particle size and characterization. Feel free to contact us before the conference to schedule a time to meet during the conference. 630.969.2703.
For more info on the World Congress on Particle Technology itself, please visit

Not Attending?

 

If you are unable to attend WCPT8, please reach out to us to discuss your particle size and characterization needs.

New Chemisorption Instrument at Particle Technology Labs

New at PTL – 3Flex Surface and Catalyst Characterization

Particle Technology Labs is pleased to announce the installation of our newest advanced instrument, the Micromeritics 3Flex Surface Characterization Analyzer.

The 3Flex instrument is capable of high-performance chemisorption and physisorption (mesopore and micropore) analyses with superior accuracy, resolution, and data reduction.

PTL’s model, the Micromeritics 3Flex Chemi TCD, has wide-ranging capabilities for various chemisorption methods. This includes isothermal methods (static volumetric, and dynamic or pulse chemisorption) as well as temperature programmed methods (temperature-programmed reduction or TPR, temperature-programmed oxidation or TPO, and temperature-programmed desorption or TPD). Furthermore, our instrument can also utilize an organic vapor source as the probe molecules (e.g., pyridine, isopropyl amine, methanol, etc.) in addition to standard gases (e.g., ammonia, H2, CO, etc.) most commonly used in various chemisorption analyses.

Chemisorption measurements are important for surface characterization of catalysts used in several industries including oil and gas (e.g. petroleum refining, syngas conversions, biofuel production, fuel cells), petrochemicals, fine chemicals (e.g. hydrogen production, polymers and plastics production), environmental (e.g. automotive catalytic converters, green chemistry), and many others.

Chemisorption

Chemical adsorption, or chemisorption, is a process resulting from a chemical bond between adsorbate molecules and specific surface locations on a material, known as active sites. This interaction is much stronger than physical adsorption, or physisorption, which takes place on all surfaces if temperature and pressure conditions are favorable. Chemisorption only occurs on clean active sites and, unlike physisorption, ceases when the adsorbate can no longer make direct contact with the surface, making chemisorption a single layer process.

Chemisorption measurement techniques are useful for evaluating physical and chemical properties of materials that are critical for process / reaction performance. Primarily, chemisorption is used to evaluate the number of available active sites to increase the rate of, or catalyze, chemical reactions. Other properties can include the (reduction or oxidation) temperature at which catalysts become active, strength of specific types of active sites, or ability of materials to perform after reduction/oxidation cycles.

To read more about chemisorption, click here.
 
Methods
ASTM D4824, D3908
Analyses Offered


Chemisorption Tests:

  • Volumetric Chemisorption analysis
  • Dynamic or Pulse Chemisorption analysis
  • Pulse Chemisorption using liquid vapors

Temperature-Programmed Studies:

  • Temperature-Programmed Reduction (TPR)
  • Temperature-Programmed Desorption (TPD)
  • Temperature-Programmed Oxidation (TPO)

Other Chemisorption Experiments:

  • Heat of Desorption, first order Kinetics
  • Isosteric Heat of Adsorption

Particle Technology Labs’ Director of Analytical Services Gives Presentation in Amsterdam

Particle Technology Labs’ Executive Vice President and Director of Analytical Services William K. Kopesky just returned from the Netherlands where he was one of three presenters at The Center for Professional Advancement’s course entitled, Powders: Their Properties and Processing. The three-day event took place December 11th through December 13th, 2017, in Amsterdam.

The primary purpose of the course was to “review the various properties of powdered solids pertinent to the development and manufacture of the products of the pharmaceutical, cosmetic and allied industries.”  While the course was designed for those in product development, the event was attended by scientists, suppliers and technologists.

During the three day course, Mr. Kopesky presented on the following topics:

In his first session, Characterization of Powder Particle Size and Shape, Mr. Kopesky provided insight regarding particle size analysis, distributions and their presentation, and particle shape characterization.

In his second session, Characterization of Particle Surface and Pores, he covered surface area by BET and pore size distribution measurement by both gas physisorption and mercury porosimetry.

In his third and final session, Fine Particle Characterization, dynamic light scattering (photon correlation spectroscopy), zeta potential and flocculation/agglomeration were covered.

Joining PTL as a Particle Characterization Chemist in 2000, Mr. Kopesky became Laboratory Manager in 2002 before being named Managing Director in 2008 and Director of Analytical Services in 2012. His years at PTL have given him exposure to a tremendous variety of particle characterization topics, techniques, and projects spanning many industries including pharmaceutical, nutraceutical, environmental, industrial, and more. During his career with PTL, he has conducted presentations and training in the field of particle characterization, provided testimony for patent infringement cases, and has been involved with consulting services in addition to hands-on analytical work.

The Center for Professional Advancement – CfPA is the largest accredited technical training organization in the world offering technical training and continuing professional education courses to those in the Pharmaceutical, Biotechnology, Medical Device, Chemical Engineering and Cosmetics industries.

For further information about CfPA, click here

To learn more about Particle Technology Labs, click here