E H T microReport M ICRO M ERITICS I NSTRU M ENT C ORPORATION 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 accu- racy, 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 micro- pore 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 /g 3 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 dem- onstrates 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 impor- tant. Pore size measure- ment 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 pres- sures 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 2 VOL 23 NO 1 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 iso- therm collected at very low relative pressure. MicroActive for 3Flex software also includes a powerful 0.5 utility that allows the user to over- lay a mercury porosimetry pore size dV/dlog(w) Pore (cm Volume distribution with a pore size distri- bution calculated from gas adsorp- tion 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. 3 VOL 23 NO 1 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