Microreport M I C R O M E R I T I C S I N S T R U M E N T C O R P O R a T I O N Volume 23 No

e h t microReport M i c r o m e r i t i c s I n s t r u m e n t C o r p o r a t i o n Volume 23 No. 1

Micromeritics’ New 3Flex - Versatile High- Throughput Surface Area, Mesopore, and Micropore Surface Characterization The 3FlexTM Surface Characterization Analyzer is a fully automated, three-station instrument capable of high-throughput surface area and pore size analyses In This Issue with superior accuracy, resolution, and MicroActiveTM Micromeritics’ New 3Flex ...... 1 data reduction. Each Particulate Systems NanoPlus analysis station is DLS Nano Particle Size and Zeta upgradeable from Potential Analyzer ...... 3 mesopore to micropore with its own Micromeritics to Showcase its transducers for cur- Extensive Line of Materials rent or future high- Characterization Instruments and throughput needs. A Services at Pittcon 2013 ...... 4 single 3Flex with its Guest Article “Carbon Dioxide minimal footprint and three configurable analysis stations eliminates Characterization of Carbons with the costly investment in multiple instruments and additional bench space. TriStar II 3020” ...... 6 The 3Flex provides a remarkable savings on analysis time compared to a single- or two-station instrument. Micropore ports include kryp- Particle Characterization Solutions ton capability for low surface area materials. Heated vapor analysis for Appearance and Structure capability is standard and an extended-range vapor option is also Assessment of Lyophilized available. Biopharmaceutical Compounds ... 8 Capturing the filling of micropores can be a challenge because, at Micromeritics Analytical Services cryogenic temperatures, micropores begin to fill at very low pressures Article: “Physical Characterization of (around 10-6 torr). A single dose of gas, such as nitrogen, could com- Shale,” News and Events ...... 9 pletely fill micropores such as those contained in zeolites. A detailed isotherm gives rise to a detailed pore size distribution. The instrument Micromeritics Pharmaceutical Services ...... 9 also delivers a reproducible isotherm collection from station to station.

Training Courses ...... 10 13x Isotherm log plot

Events ...... 11

)

STP

Quantity Adsorbed Quantity (cm

www.micromeritics.com Relative Pressure (P/Po) Figure 1. Logarithmic isotherm overlay of 13X zeolite isotherms continued on next page Vol 23 no 1

3Flex continued

the use of a greater ily selected. As a result, the sum- selection of adsorp- mary of values derived from the tives. The 3Flex calculations is instantly updated. boasts proven isother- Figure 3 demonstrates that either mal jacket technology some or the entire isotherm can be and a new dewar used for calculations. Within the design that provide calculation window(s), the range of the many hours of data used can be further refined. continuous tempera- New dosing options added to the ture control required pressure table give the user the when running micro- ability to change the pressure pore analyses. increment, volume dose increment, The 3Flex also and equilibration interval time includes enhanced between data points. Figure 4 demonstrates this feature. A detailed Figure 2. Pore size distribution of three 13X software capabilities, data reduc- zeolite samples analyzed simultaneously tion features, and instrument isotherm can be collected by speci- fying that a data point be recorded The 3Flex contains many design monitoring. An innovative dash- after a certain amount of gas is features that ensure superior board monitors and provides dosed, increasing the relative pres- performance and mark a major convenient access to real-time sure by a small amount, or both. advancement in surface charac- instrument performance indicators terization analyzers. Servo control and maintenance scheduling infor- for dosing and evacuation provides mation. The intuitive MicroActive a higher degree of gas manage- for 3Flex software gives the user ment and speeds the collection of the ability to interactively evalu- data points through reduction of ate isotherm data and reduce the dosing overshoot. Pneumatically time required to obtain surface actuated, hard seal valves provide area and porosity results. It is not ultra-clean instrument operation. necessary to generate reports to Stainless-steel construction, metal view results. seals, manifold, and gaskets elimi- Calculations, such as the BET nate interference from contami- surface area transform plot, can be nates and outgassing associated easily generated and adjusted. The Figure 4: The 3Flex pressure table allows with elastomer seals. These chemi- selection bars allow for a range of data points to be taken in small increments of cally resistive surfaces also allow data points to be quickly and eas- pressure, quantity dosed, or both Dosing small amounts of gas during a micropore analysis is very important. Pore size measurement is directly related to the relative pressure at which the pore is filled. Therefore, when lower relative pressures are achieved, smaller sizes of pores can be determined. The 3Flex is capable of collecting data at relative pressures as low as 10-9 with N2 at 77 K with its 0.1- torr pressure transducer coupled with a high- vacuum system.

Figure 3. Interactive selection of the BET surface area calculation range

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3Flex continued BJH Desorption dV/dlog(w) Pore Volume Alumina Additional software options include the ability to determine free space after analysis. As a result, the sample will not be exposed to 1.0 helium prior to analysis. In some

/g) cases, helium can be retained by 3 the presence of micropores and could mask a portion of the isotherm collected at very low relative pressure. MicroActive for 3Flex software also includes a powerful 0.5 utility that allows the user to overlay a mercury porosimetry pore size dV/dlog(w) Pore (cm Volume distribution with a pore size distribution calculated from gas adsorption isotherms (Figure 5). This new import function allows users to rapidly view micropore, mesopore, 0.0 10 100,000 and macropore distributions in one Pore Width (A) easy-to-use application.

Figure 5. Overlay of BJH desorption and mercury intrusion pore size distributions for alumina pellets

Particulate Systems’ NanoPlusTM DLS Nano Particle Size and Zeta Potential Analyzer

The NanoPlus is a unique electrode) method allows measure- instrument that utilizes photon ments to be carried out on concen- correlation spectroscopy and trated suspensions. electrophoretic light scatter- The NanoPlus is compact and easy ing techniques to determine to use with an extended analysis particle size and zeta potential. range, intuitive software, and mul- The instrument can measure tiple sample cells to fit the user’s the particle size of samples sus- application. The instrument is pended in liquids in the range available in three model configura- of 0.6 nm to 10 μm with sample tions: the NanoPlus-1 – nano par- NanoPlus solid sample cell allows suspension concentrations from ticle sizing instrument; NanoPlus- the determination of zeta potential 0.00001% to 40%. This instru- 2 – zeta potential instrument; and on flat surfaces and permits the ment also has the ability to mea- NanoPlus-3 – combination nano use of the NanoPlus AT for addi- sure the zeta potential of sample particle sizing and zeta potential tive/pH studies. suspensions in the -200 mV to instrument. +200 mV range with concentra- The optional NanoPlus AT is used tions from 0.001% to 40%. The The NanoPlus has an array of to titrate sample suspensions in a instrument makes use of Field compatible sample cells for both pH range from 1 to 13. The instru- Focus Technology, providing an zeta potential and nano particle ment automatically controls the excellent solution for measuring size measurements. Each sample pH of these suspensions and con- samples with high conductivi- cell provides additional measure- ducts titrations during zeta poten- ties. The patented FST (Forward ment capabilities of samples in liq- tial or nano particle size analysis Scattering through Transparent uid suspensions. For example, the measurements.

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Micromeritics to Showcase its Extensive Line of Materials Characterization Instruments and Services at Pittcon 2013

ittcon, a premier annual MicroActive Data Analysis Pconference devoted to labora- Software is also avail- tory science and instrumenta- able for Micromeritics’ tion, takes place from March 17 ASAP®, TriStar®, and through March 21, 2013, at the Gemini® gas adsorption Pennsylvania Convention Center instruments. Users can in Philadelphia, PA. Micromeritics easily include or exclude will be located in three locations at data, fitting models to the this year’s conference and will be desired range of experi- displaying a variety of instruments mentally acquired data including our new 3Flex Surface points. Interactive data Characterization Analyzer in booth manipulation minimizes 2024. Micromeritics Particulate the use of dialog boxes to Systems Division will highlight its specify calculation param- new NanoPlus DLS Nano Particle eters, allowing accurate Size and Zeta Potential Analyzer and efficient determination of The TriStar II 3020 Surface Area in booth 1224. Micromeritics surface area and porosity. It is not and Porosity System is an auto- Analytical Services (MAS) and necessary to generate reports to mated, three-station instrument Micromeritics Pharmaceutical view results. capable of increasing the speed of Services (MPS) will show- quality control analyses, with case their wide range of the accuracy, resolution, and contract materials charac- data reduction to meet most terization services in booth research requirements. The 2924. instrument includes a dedi- cated saturation pressure port Micromeritics (booth and three analysis ports that 2024) is highlighting operate simultaneously and its new 3Flex Surface independently of one another. Characterization Analyzer, Micromeritics is also showcasing A krypton option allows surface a fully automated, three-sta- the Saturn DigiSizer® II High- area measurements in a very low tion instrument capable of Definition Digital Particle Size surface area range (below 0.1 m2/g). high-throughput surface area, Analyzer, a highly advanced tool mesopore, and micropore analyses. for those faced with challenging The low-cost Gemini VII Series Each analysis station is upgrade- particle size distributions. If pro- Surface Area Analyzers utilize a able from mesopore to micropore cess variability is affecting the patented reference-sample tube with its own set of pressure trans- desired yield, performance, or qual- design to produce accurate and ducers. A single 3Flex with its ity of your product, take control repeatable surface area and poros- minimal footprint and three con- of your process with the Saturn ity results. Their low cost, small figurable analysis stations elimi- DigiSizer. Superior resolution footprint, speed, accuracy, simplic- nates costly investment in mul- and sensitivity allows the user to ity of use, reliability, and rugged- tiple instruments and additional characterize outlier particles not ness make the Gemini an ideal tool bench space. Micropore stations visible to other particle sizing sys- for teaching, research, and quality include krypton capability for low tems. With unique design and data control environments. The Gemini surface area materials. Vapor is reduction features, this instrument VII permits low to high surface standard and an extended-range measures particle size in a range of area measurements without vapor option is also available. 40 nanometers to 2.5 millimeters requiring the use of krypton. Three The 3Flex includes Micromeritics’ with an extremely high level of model options are available. intuitive MicroActive for 3Flex resolution, reproducibility, repeat- Micromertics’ AccuPyc® II 1340 software which gives the user the ability, and sensitivity from unit to Gas Displacement Pycnometry ability to interactively evaluate unit and site to site. System is a fast, fully automatic isotherm data and reduce the time analysis system that provides required to obtain surface area high-speed, high-precision volume and porosity results. measurements and density calculations. The AccuPyc determines absolute density of powders, solids,

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and slurries having volumes from 0.01 to 350 cm3 with superior sample suspension concentrations desorption isotherms of water and accuracy. For those who require from 0.00001% to 40% and zeta organic vapors on solid materials. high throughput, an integrated potential of sample suspensions Humidity can adversely affect a control and analysis module can in the -200 mV to +200 mV range range of materials to include food, operate up to five additional exter- with concentrations from 0.001% pharmaceuticals, fuel cells, pack- nal analysis modules. Custom- to 40%. The NanoPlus is avail- aging, high-energy materials, poly- sized modules can be configured to able in three model configurations: mers, building materials, filtration suit unique applications providing the NanoPlus-1 – nano particle materials, and personal care prod- even more versatility. sizing instrument; NanoPlus-2 ucts. Knowing how water vapor – zeta potential instrument; and interacts with these materials can Particulate Systems (booth NanoPlus-3 – combination nano yield vital information for their 1224) offers instruments that are particle sizing and zeta potential proper formulation, processing, complementary to Micromeritics’ instrument. and storage. The DVS-Intrinsic is core product line. Materials char- an entry level, water vapor instru- acterization analyses include: nano Particle Insight™ Dynamic Image ment for adsorption. It has a small particle size, zeta potential, par- Analyzer is ideal for applications footprint and operates in the 20 to ticle shape, high-pressure adsorp- where the shape, not just the 40 °C temperature range. tion isotherms, dynamic vapor diameter, of raw materials is criti- sorption, activity and selectivity of cal to the performance of the final Micromeritics Analytical catalysts, surface energy, segrega- product. The Particle Insight offers Services (MAS) (booth 2924) tion testing, and determination of up to 28 different shape parame- and Micromeritics Pharmaceutical low levels of iron content in a vari- ters analyzed in real-time in either Services (MPS) both provide con- ety of materials. aqueous or organic solvent sus- tract sample analyses and consult- pensions. Three size range model Micromeritics and Particulate ing services. Featuring products options are available: 1 - 150 µm, 3 Systems offer six instruments that manufactured by Micromeritics, - 300 µm, and 10 - 800 µm. use a different method of deter- they also offer services outside mining particle size distribution of The Elzone® II 5390 Particle Size Micromeritics’ current product powdered material, including one Analyzer determines the size, line. Materials characterization for characterizing particle shape. number, concentration, and mass services include: particle size dis- Methods include X-ray Monitored of a wide variety of organic and tribution, particle shape, particle Gravity Sedimentation, Static inorganic materials. Unlike other count, nano particle size, surface Laser Light Scattering, Dynamic measurement techniques, the area, micropore analysis, pore Laser Light Scattering, Electrical electrical sensing zone method volume distribution, total pore Sensing Zone, Air Permeability, (Coulter Principle) is capable of volume, density, surface energy, and Dynamic Image Analysis. accurately sizing samples of vary- dynamic water vapor sorption, Particulate Systems will exhibit ing optical properties, densities, TGA, DSC, active surface area, particle size models to include the colors, and shapes. The Elzone percent metal dispersion, crystal- new NanoPlus DLS. determines particle size in a range lite size, high-pressure adsorption suitable for a wide variety of isotherms, magnetic content, zeta industrial, biological, and geologi- potential, isosteric heat of adsorp- cal specimens down to 0.4 microm- tion, microscopy, method develop- eter. ment, method validation, and con- sulting services. Particulate Systems will also showcase the DVS-Intrinsic. Dynamic Micromeritics Pharmaceutical vapor sorption, commonly known Services (MPS) enables as DVS, is based on the gravimetric Micromeritics to expand its analyt- determination of the quantity of ical service capabilities and meet vapor adsorbed or desorbed from the growing demand for contract the sample material. By varying services from the pharmaceutical the vapor concentration surround- industry. MPS utilizes a DEA- ing a sample and measuring the licensed, FDA-registered, cGMP/ The NanoPlus Nano Particle change in mass it produces, the rate GLP-compliant contract analytical Size and Zeta Potential Analyzer and quantity of solvent adsorbed laboratory and provides a com- utilizes photon correlation spec- by a sample can be measured. prehensive service program to troscopy and electrophoretic light Surface Measurement Systems, provide additional services. These scattering techniques. Compact represented by Particulate Systems, services include API characteriza- and easy to use with an extended offers a wide range of Dynamic tion, excipient screening, powder analysis range, intuitive software, Vapor Sorption instruments that flow properties, batch variability, and multiple sample cells to fit utilize dynamic gas flow and the identification of critical quality the user’s application, the instru- gravimetric technique to produce attributes, and QbD/PAT imple- ment can measure particle size in high-resolution adsorption and mentation. the range of 0.6 nm to 10 μm with

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Carbon Dioxide Characterization of Carbons with the TriStar II 3020 Andrew D. D’Amico and Yundi Jiang Micromeritics Instrument Corporation

Introduction carbon dioxide, prepurified nitro- stroms, of the Carboxen 1012 carbon The use of carbon dioxide allows gen, and ultra-high purity helium are not shown for clarity. for rapid, high-resolution charac- were used during the analyses. terization of microporous materi- The resolution of the micropore als. The Micromeritics TriStar II Results and Discussion distributions is shown in Figure 2. When compared to nitrogen physi- 3020 can be used to characterize Figure 1 shows the nitrogen and micropores below 10 angstroms sorption, features of the pore size carbon dioxide isotherms of the distribution are captured in much within 8 hours using CO2 as the Carboxen 1012 and MAST synthet- adsorptive gas and an ice bath greater detail with DFT calcula- ic carbon. Nitrogen adsorption on tions from carbon dioxide sorp- (273 K) for the analysis bath. Carboxen 1012 displays type I iso- tion, and pore filling below 7 Å is Isotherms from CO2 adsorption therm behavior, while the MAST observed. were compared with N2 adsorp- carbon displays type IV isotherm Figure 3 shows the isotherms of tion isotherms at 77.3 K. Density behavior. The trend of enhanced carbon dioxide up to 760 torr com- functional theory (DFT) models gas uptake by the Carboxen 1012 pared with the measurements up for nitrogen and carbon dioxide on is observed with the carbon dioxide to 7600 torr—demonstrating the slit-pore carbon were used for the sorption as well. Mesopores of the agreement of high-pressure and pore-size-distribution calculations. MAST carbon and larger micro- “low-pressure” adsorption. Slow diffusion (equilibration) pores, between 10 and 20 ang- rates—on the order of hours to days—may be observed during 500 500 adsorption at cryogenic tem- N2 @ 77.35K CO2 @ 273K peratures on materials with small 450 450 400 400

) pores. Strong adsorption potentials )

-1

g in confined pores result in high g 350 350

3 uptake of adsorptives, such as 300 300 nitrogen, which corresponds to the 250 250 filling of micropores at very low 200 200 pressures that can challenge the 150 lower sensitivity limits of one-torr 150 100

Volume Adsorbed (cm Volume pressure transducers. Analysis Adsorbed (cm Volume 100 Carbonxen 1012 with carbon dioxide addresses 50 Carbonxen 1012 50 MAST MAST both of these issues by having 0 0 0.0 0.1 0.2 0.3 faster equilibration rates, due to 0.0 0.2 0.4 0.6 0.8 1.0 P/P P/Po increased temperature, and gas o uptake at much higher pressures. Figure 1. N2 and CO2 adsorption isotherms for the Carboxen 1012 and MAST synthetic carbon analyzed in this study. Experimental Two readily available carbon sam- ® ples, Carboxen 1012 from Supelco 2.0 4.5 1.4 N2 @ 77.3K and a sample of MAST synthetic N2 @ 77.35K )

) 4.0 1.8 -1 CO2@ 273K 1.2

-1 CO2@ 273K g

carbon, were used. A Micromeritics 3

g ) 1.6 3 3.5 TriStar II 3020 was the principle -1 g 1.0 3 1.4 3.0 instrument used for CO2 analyses 1.2 up to 760 torr (relative pressure 2.5 0.8 of 0.03). A Micromeritics ASAP 1.0 2.0 0.6 2050 high-pressure sorption ana- 0.8 1.5 lyzer was used to measure CO2 0.6 0.4 isotherms up to 7600 torr, and 0.4 1.0

Differemtial Pore (cm Volume

0.2 2 a Micromeritics ASAP 2020 was 0.2 Differemtial Pore (cm Volume 0.5

Differential Differential Pore (cm Volume

CO used to verify micropore sizes 0.0 0.0 0.0 using DFT calculations from nitro- 4 6 8 10 4 6 8 10 gen isotherms at 77 K. Bone-dry Pore width (A) Pore width (A)

Figure 2. Pore size distribution calculated by N2 adsorption at 77 K and CO2 adsorption at 273 K on MAST carbon (left) and Carboxen 1012 (right).

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350 TriStar 3020 (10 torr) ASAP 2050 300

) 250 Table 1. Surface areas for CO2 and N2 physisorption -1

3 200 Langmuir (CO2) BET (N2) Carboxen 1660 1692 100 150 MAST 945 940 75 50 100

Volume Adsorbed (cm Volume 25 Table 1 shows the surface area 0 calculations from carbon dioxide 50 0.00 0.01 0.02 0.03 sorption compared with calculations from nitrogen sorption. BET surface area calculations were 0.00 0.05 0.10 0.15 0.20 0.25 0.30 performed below 0.1 relative pres- P/Po sure in order to make the results physically meaningful, a common Figure 3. CO2 adsorption isotherm at 273 K at 760 torr and 7600 torr for Carboxen 1012. procedure for microporous materi- Conclusions als. The Langmuir surface areas 273 K can be extended to high pres- from CO2 adsorption were calcu- From the data presented, it can be lated over an absolute pressure concluded that the TriStar II 3020, sure, allowing for Langmuir and BET range of 600-3000 torr. Langmuir as well as other Micromeritics surface areas to be calculated. For the two materials analyzed in this work, surface areas (not shown) from N2 physisorption instruments, can be adsorption, calculated using pres- used to obtain rapid, high-resolu- the Langmuir surface areas calculated sures up to an absolute pressure tion characterization of micro- from CO2 adsorption at 273 K are of 50 torr, agreed within 6% with pores in carbons. The technique comparable to BET surface areas calcu- the nitrogen BET surface areas. of carbon dioxide physisorption at lated from N2 adsorption at 77.3 K.

Recently Introduced

New Product Family Brochures for both Micromeritics and Particulate Systems Link to both by clicking on the images

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Particle Characterization Solutions for Appearance and Structure Assessment of Lyophilized Biopharmaceutical Compounds

here is an expanding empha- The inner cake Tsis in the area of lyophilized morphology of products in the pharmaceutical freeze-dried prod- and biopharmaceutical industries. ucts can act as a Pharmaceutical companies are gauge for process increasingly using lyophiliza- conditions such tion technologies and produc- as freezing rate tion processes to produce a final or shelf tempera- dosage form that has a longer ture/pressure shelf life, enhanced stability, and settings during fewer restrictions on transporta- the primary and tion and storage. It has recently secondary drying been reported that 40% or more phases. It is well of pharmaceutical industry R&D documented that and revenue now involves bio- physio-chemi- pharmaceuticals. Close to 60% cal activity as of biopharmaceuticals (such as well as long- enzymes, proteins, and monoclonal term stability antibodies) must be lyophilized of protein-based as they are insufficiently stable pharmaceuti- for ready-to-use solution dosage cals are directly forms. Micromeritics’ TriStar II influenced by ice Surface Area Analyzer, AutoPore® crystal formation IV Mercury Porosimeter, and and their contri- AccuPyc II 1340 Gas Displacement bution to surface Pycnometer are essential tools for area. Surface determining the integrity of bio- area data provide pharmaceutical lyophilized cake. important infor- The structure of the cake, includ- mation on structure and reconsti- that can help predict the effect ing density, total pore volume, tution of the cake by presenting a of freeze-drying variations and pore size, and surface area needs picture of the morphology of the enhance process control steps to to be tightly controlled in produc- solid phase. prevent cake collapse. tion. Any variability in the produc- Mercury intrusion porosimetry Micromeritics’ AutoPore IV mer- tion process, such as the freeze can provide information on the cury porosimeter uses mercury temperature, primary drying internal cake structure. Total pore intrusion and extrusion to deter- temperature, or secondary drying volume and pore size distribution mine total pore volume, pore size temperature can impact the physi- are directly related to the integrity distribution, percent porosity, den- cal and chemical properties of the of the cake and its reconstitution sity, and compaction/compression. lyophilized cake. The three most properties. The correlation of pore The instrument collects extremely commonly used characteristics size to surface area data can quan- high-resolution data. It can either to release or approve a batch are tify the degree of cake shrinkage be equipped with two low-pressure appearance, thermal properties, during freeze-drying and deter- stations and one high-pressure sta- and surface area. BET surface mine the final pore size of the tion or four low-pressure stations area, mercury intrusion porosim- dried cake. and two high-pressure stations for etry, and gas pycnometry provide Micromeritics’ TriStar II is based increased sample throughput. a more quantitative solution to on the well-established static gas The AccuPyc II is a gas displace- visual inspection of the lyophilized adsorption technique. It is a fully ment pycnometer that produces cakes. automated, three-station analyzer high-speed, high-precision volume BET surface area generated by capable of increasing the speed measurements and density deter- the gas adsorption analytical tech- and efficiency of quality control minations of powders, solids, and nique can be used to determine analyses with the accuracy, resolu- slurries. Helium pycnometry is shrinkage, collapse, and optimal tion, and data reduction features recognized as one of the most reli- cooling/drying rates as indicators to meet most production and R&D able techniques for obtaining true for product performance and man- requirements. The TriStar II can density. ufacturing process optimization. provide BET surface area data

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Application Highlight www.particletesting.com

Physical Characterization of Shale Recent economic conditions have solved gas on the surface or in gy, dynamic water vapor sorption, led researchers and companies pores, and kinetics for rate of gas TGA, DSC, active surface area, to investigate the possibility of production. percent metal dispersion, crystal- extracting gas and oil from shale lite size, high-pressure adsorption Gas displacement pycnometers isotherms, magnetic content, zeta reserves in the U.S. and around measure the skeletal volume of the world. Shale samples are potential, isosteric heat of adsorp- shale. When combined with other tion, microscopy, method develop- unique because of the complexity density measurements, skeletal of their porosity and the potential ment, method validation, and con- volume can be used to determine sulting services. problems associated with cleaning porosity of both crushed and intact the samples prior to analysis. As shale samples. is always the case with any sam- News High pressure gas adsorption ple, the key to properly character- Greg Thiele, General Manager isotherms using methane, carbon izing shale is thorough cleaning of MAS, recently presented dioxide, or nitrogen can be used to of the material prior to any mea- a technical paper at the US model kinetic data and determine surement. This is typically accom- Biochar Conference, titled volume adsorbed at simulated plished using a soxhlet extraction “Analytical Options for shale depth conditions. procedure prior to testing. Characterizing Biochar.” A copy Mercury intrusion porosimetry is Micromeritics Analytical Services of this paper is available for commonly used to provide pore (MAS) offers these sample analyses download at the link below. size information as well as total to the shale gas industry on a con- http://www.micromeritics.com/ pore volume, porosity, and density tract basis with fast turn-around Repository/Files/Analytical_ measurements of shale. The data times and outstanding customer Options_for_Biochar_full_ are used to calculate pore tortu- service. Featuring products manu- paper_2012.pdf osity, diffusion parameters, and factured by Micromeritics, MAS other geological parameters. also provides additional services Events outside of Micromeritics’ current MAS will be exhibiting at BET surface area using the gas product line. A full list of materials the upcoming Pittcon, booth adsorption technique is another characterization services includes: number 2924. Please stop by common test used to character- particle size distribution, particle our booth to learn how we can ize shale samples. Surface area shape, particle count, nano particle help you solve your challeng- is used to predict the amount of size, surface area, micropore analy- ing material characterization free gas stored within pores, the sis, pore volume distribution, total problems. amount of adsorbed gas or dis- pore volume, density, surface ener-

www.micrx.com

Our areas of expertise include • Method transfer documenta- • Porosity (Gas Adsorption, particle size distribution analysis tion Mercury Porosimetry) (micrometer and nano particles), • Secure Method and • Thermal Analysis (DSC/TGA) particle shape and morphology, Validation storage for future • Dynamic Vapor Sorption surface area, surface energy, vapor projects (DVS) sorption, porosity, density, thermal analysis, and material flow Analytical Services • Volumetric Vapor Sorption properties. • Particle Size, Particle Shape • Surface Energy (IGC) (Light Scattering, Dynamic • Surface Energy (Volumetric Method Development / Light Scattering, Electrical Gas Adsorption-Density Validation Sensing Zone, Dynamic Functional Theory) Image Analysis, Microscopy) • Method Development • Zeta Potential Services for all analytical • Surface Area (Gas adsorp- tests tion, BET) MPS is a DEA-licensed, FDA- • Method Validation Services • Density (True, Apparent, registered, cGMP/GLP-compli- for all analytical tests Bulk, TAP, Carr index) ant contract lab service orga- nization

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Learning Center

Micromeritics’ representatives Report Optimization provide basic start-up training for Learn to configure reports and most instruments during instal- obtain the most useful informa- lation. However, when operators tion, as well as improve report wish to maximize their proficiency comprehension. and broaden their capability with Troubleshooting Students attending their Micromeritics instrument, Learn techniques to quickly locate a recent Training Course more advanced training is needed. and resolve instrument related To achieve this goal, Micromeritics problems. offers, for most instruments, targeted classes in which cus- User Maintenance Training Courses tomers may expand their ability Under the guidance of a April - August and improve their understand- Micromeritics Maintenance 2013 ing by learning from the experts. Specialist, attendees learn routine These classes, periodically held at maintenance and troubleshoot- Micromeritics’ headquarters near ing techniques which improve ASAP 2020 Atlanta, Georgia, include: operation, reduce downtime, and increase data accuracy. Physi and Chemi Theory Overview April 8 - 11 Learn about the science upon Course Enrollment which each instrument is based Training courses last from two to four days and are designed to pro- Advanced Course: and how this science applies to Textural Characteriza- successful sample preparation, vide hands-on, performance-based instrument skills and knowledge. tion of Porous Materi- analysis, and results interpreta- als using NLDFT tion. Small classes allow individual instruction and peer interac- April 12 Detailed Operations tion. Course materials include a Effective sample file creation, use Study Guide, a complimentary Saturn DigiSizer II of analysis parameters, and man- copy of Analytical Methods in June 4 - 6 ual sample entry are all covered. Fine Particle Technology, relevant Increase efficiency and learn to use application notes, and a wealth the full power and flexibility of the Advanced Course: of other educational material. A Using Shape and Size operating software. Certificate of Completion is award- to Characterize Par- Automatic Analyses ed to each trainee. ticle Morphology Develop correct analysis proce- Advanced Training June 7 dures to optimize collection of Offered as one-to-two day sessions accurate, reproducible data. Much that can be taken as a stand-alone 3Flex class time is spent performing course or in conjunction with a rel- July 16 - 18 analyses in a hands-on, interactive evant instrument training course, environment. these courses are excellent options AutoChem II System Utilities for those looking to achieve a August 5 - 7 Learn instrument software utili- greater depth of understanding in ties which help manage sample the analytical capability of their files and directories, protect data, Micromeritics instrument and the- Advanced Course: and select system options. ory of materials characterization. Characterization of Sup- Advanced courses are conducted ported Heterogeneous by a member of Micromeritics’ Catalysts by Temp- perature-Programmed For additional information or Scientific Services staff and con- Surface Reactions to register for the class of your tain a thorough examination of August 8 - 9 choice, visit www. each topic in a classroom environ- micromeritics.com. ment. While there are no prerequi- Early registration is sites, attendees should either have TriStar II recommended since class space a basic understanding of their August 20 - 22 is limited. instrument and its daily operation, or take the standard instrument training course prior to the advanced course.

10 Vol 23 No 1

Upcoming Events

Pittcon 2013 Analytica Vietnam POWTECH 2013 3/17/2013 - 3/21/2013 4/17/2013 - 4/19/2013 4/23/2013 - 4/25/2013 Pennsylvania Convention Center Saigon Exhibition Center Exhibition Centre Nuremberg Philadelphia, PA Ho Chi Minh City, Vietnam Nuremberg, Germany ACS 2013 Advanced Porous Materials IMMS 2013 4/07/2013 - 4/11/2013 Workshop 2013 5/20/2013 - 5/24/2013 Morial Convention Center 4/18/2013 - 4/19/2013 Awaji Yumebutai International New Orleans, LA National Institute of Chemistry, Convention Center Ljubliana, Slovenia Awaji Island, Hyogo, Japan MIC / KIT Workshop 4/16/2013 - 4/17/2013 Interphex 2013 Forum Labo Biotech Stadthalle Frickenhausen 4/23/2013 - 4/25/2013 6/04/2013 - 6/07/2013 Hotel Meintzinger Javits Center Porte de Versailles Frickenhausen, Germany New York, NY Paris, France

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