Classification of analysis methods for characterization of

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XXI IMEKO World Congress Measurement in Research and Industry . August 30 September 4 2015 Prague Czech Republic, CLASSIFICATION OF ANALYSIS METHODS FOR. CHARACTERIZATION OF MAGNETIC NANOPARTICLE, PROPERTIES. O Posth 1 M F Hansen 2 U Steinhoff 1 L Bogart 3 P Southern 3 P Svedlindh 4 . C Gr ttner 5 L Fern ndez Barquin 6 W Szczerba 7 F Ludwig 8 . N Gehrke 9 O Kazakova 10 C Johansson 11, Physikalisch Technische Bundesanstalt Berlin Germany oliver posth ptb de . uwe steinhoff ptb de, Technical University of Denmark Kongens Lyngby Denmark mikkel hansen nanotech dtu dk. University College London London UK l bogart ucl ac uk p southern ucl ac uk. Uppsala Universitet Uppsala Sweden peter svedlindh angstrom uu se. Micromod Partikeltechnologie GmbH Rostock Germany gruettner micromod de. Universidad de Cantabria Santander Spain barquinl unican es. Bundesanstalt f r Materialforschung und pr fung Berlin Germany wojciech szczerba bam de. Technische Universit t Braunschweig Braunschweig Germany f ludwig tu bs de. NanoPET Pharma GmbH Berlin Germany nicole gehrke nanopet de. National Physical Laboratory Teddington Middlesex UK olga kazakova npl co uk. Acreo Swedish ICT AB G teborg Sweden christer johansson acreo se. Abstract The aim of this paper is to provide a roadmap for the that due to their magnetic moment they can be in situ. standardization of magnetic nanoparticle MNP manipulated by externally applied magnetic fields . characterization We have assessed common MNP analysis Moreover the particles can be located and imaged in tissue. techniques under various criteria in order to define the methods by noninvasive techniques without applying harmful. that can be used as either standard techniques for magnetic ionizing radiation . particle characterization or those that can be used to obtain a. comprehensive picture of a MNP system This classification is 2 DEMAND FOR STANDARDIZATION OF. the first step on the way to develop standards for nanoparticle MAGNETIC NANOPARTICLE. characterization CHARACTERIZATION, Keywords standardization metrology magnetic An open issue in the use of MNPs in biomedical.
nanoparticle iron oxide particles applications is the standardization of their physical. properties and conditions of application Regulatory work is. 1 INTRODUCTION required to guarantee a safe and effective implementation of. advanced techniques for application of magnetic, During the last years the number of applications where nanoparticles in the human body This comprises a. nanostructured objects are used has strongly increased reproducible production of nanoparticles with desired. Nanostructures are applied for instance in electronics physical and bio chemical properties as well as analysis. environment medicine or cosmetics In these applications it techniques to characterize the particle properties as. is utilized that nanoobjects show significantly altered accurately as needed in a metrologically traceable way For. physical properties compared to the properties of a practical application the characterization techniques have. macroobjects or bulk materials 1 Thus nanostructures to be cost effective easy to handle and they should provide. give access to novel techniques or they can be used to reproducible results on MNP properties Within the. improve existing applications framework of a European FP7 project Nanometrology. Magnetic nanoparticles MNPs are a significant class of Standardization Methods for Magnetic Nanoparticles. these novel nanoobjects and their application in biomedicine NanoMag 9 we have developed a roadmap for the. is under intensive investigation 2 MNPs are used for standardization of characterization of magnetic particles to. diagnostic applications as contrast agents in imaging 3 or be used in medical applications . tracers 4 for therapeutic applications such as magnetic A stakeholder committee was formed by interested. drug targeting 5 and magnetic hyperthermia 2 and for in members from industry and academia It is closely. vitro techniques like magnetic separation 6 7 or connected to the NanoMag project and provides valuable. magnetofection 8 The key benefit of the use of MNPs is guidance for the standardization process The committee. represents large companies and SMEs and researchers from descriptions of the MNP system properties and separate. different application fields MNP synthesis instrument approaches to standardization . developers and end users MNPs are complex physically chemically and even. It is known from the literature that the static and biologically active systems They require monitoring of a. dynamic magnetic behaviour of MNP systems vary large number of different physical properties in order to. significantly depending on the chemical composition and achieve a reproducible and safe application in a biomedical. physical structure of the actual MNP system and on the environment Their most important parameters are . interplay between the MNPs and the surrounding matrix hydrodynamic size distribution nanocrystal size. 10 13 Thus it is important first to identify classes of distribution aggregate size distribution particle shape and. MNPs that share common principal behaviours morphology crystal structure surface coating thickness . In a second step the physical measurement methods as chemical composition binding efficiency particle. well as the mathematical models and data analysis methods concentration in a suspension magnetic coercive field . exploring the properties of the respective MNP classes have magnetic saturation field total magnetic moment spin. to be described structure initial magnetic susceptibility critical. temperatures magnetic relaxation time effective anisotropy . particle surface charge and specific energy absorption rate . 3 METROLOGY OF MAGNETIC NANOPARTICLES Depending on the application of the MNPs further. parameters may be specified , During the process of standardization of MNP We apply a number of common analysis techniques to. characterization we first selected MNP systems suitable for investigate structural MNP properties as well as their static. the analysis methods Here we focused our investigations and dynamic magnetic behavior under influence of external. on a limited number of single or multi core magnetic fields and temperature changes We also. superparamagnetic iron oxide nanoparticles that are well investigate application oriented methods that are closely. established as contrast agents in magnetic resonance linked to existing biomedical applications e g magnetic. imaging MRI 14 or have been applied already in separation or magnetic hyperthermia In particular we. magnetic drug targeting magnetic hyperthermia 15 investigated whether different analysis techniques provide. magnetic separation techniques 16 and magnetic particle consistent physical parameters of the particles bearing in. spectroscopy 17 The MNPs are synthesized by the mind that the results of different techniques are interrelated. manufacturing partners of NanoMag or purchased from with each other . commercial suppliers Various synthesis processes and a A large number of methods exists that can be utilized for. variety of functional groups on the particle surface ensure nanoparticle characterization Every method varies in. that a wide range of existing MNP systems is covered 18 complexity and may determine directly or indirectly a. An example for particles which have been synthesized limited number of particle parameters To evaluate the. within the NanoMag project is shown in Fig 1 in suitability of a method to be chosen as a basic standard cha . Transmission Electron Microscopy TEM images The left racterization method the following aspects are important . image shows MNPs with a single magnetite core surrounded. by a silica shell In the right image multi core particles are Standardization of the measurement technique. shown where several crystallites are imbedded in the silica Are traceable standards and procedures available How. coating If the non magnetic shell layer of the single core sensitive is the method . particles ensures a sufficient distance between the magnetic Sample amount. cores the magnetic behavior of the single core nanoparticles What is the typical sample amount required for the. can be modeled as those of independent non interacting analysis . particles In contrast in the case of multi core particles the Throughput. dipolar interaction between them has to be considered due to What is the typical time required for sample. the small distance between the crystallites These are two preparation measurement and data analysis . main distinctive classes of particles that require separate Ease of use. What level of user expertise is required for sample. preparation measurement and data analysis , Availability. Is the method widely available What is the planning. effort before a measurement can be performed How is. the method regarded in the scientific community, standard method or basic research tool . Low cost, Is the technique commercially available What is the.
cost of an instrument What is the cost for a single. measurement , Fig 1 TEM images of single core left and multi core right . magnetic nanoparticles Partners of the NanoMag consortium being experts in the. field of nanoparticle research have answered these questions. for a number of analysis techniques Based on this a can be measured only with this method A low score means. comprehensive description of measurement methods has that the method is highly advanced and can be used to. been created to identify the methods to be used as standard determine additional rather than fundamental particle. methods for MNP characterization and those to be used to parameters . obtain a more detailed picture of an MNP system , Dynamic Light Scattering DLS . 3 1 Results 5, The measurement techniques for MNP have been. classified into methods for structural and magnetic. characterization as well as application oriented methods It 3. should be noted that some techniques provide information in. several categories marked by 2 Advanced, 1 Techniques for structure chemical composition and. particle size determination, Scanning Electron Microscopy SEM .
Transmission Electron Microscopy TEM , X Ray Diffraction XRD . Average score 4 3, Neutron Diffraction ND , Dynamic Light Scattering DLS Zeta potential Assessment. Asymmetrical Flow Field Flow Fractionation AF4 , Small Angle X ray Scattering SAXS Highly standard. Small Angle Neutron Scattering SANS Standard technique for hydrodynamic size determination Good for. Inductively Coupled Plasma Mass Spectrometry ICP quality monitoring of particle size and colloidal properties . Low cost method easy to perform high throughput requires only. small amount of sample highly available , M ssbauer Spectroscopy Should be performed as standard on all samples also during. X ray Absorption Fine Structure spectroscopy XAFS fabrication development . 2 Techniques for magnetic measurements, DC Magnetometry magnetization vs field and Neutron Diffraction ND .
temperature DCM 5, Cavity based Ferromagnetic Resonance FMR Standard. AC magnetic Susceptibility vs frequency ACS vs f 4. AC magnetic Susceptibility vs temperature ACS vs . Magnetorelaxometry MRX 2 Advanced, Magnetic Particle Spectroscopy MPS . Rotating Magnetic Field RMF phase lag vs f 1, 3 Application oriented techniques. Magnetic Separation MagSep , NMR Relaxivity R1R2 . Magnetic Hyperthermia treatment, Average score 1 8.
On chip AC Susceptometry Chip ACS , Assessment, Note that DLS and Zeta potential measurements provide. different MNP properties however some benchtop Highly advanced. instruments offer to measure both of them within the same Advanced technique for fundamental magnetic structure studies . device Requires large instrument facility a high amount of sample. Fig 2 shows as an example the detailed assessment of material prepared in a dry state is very time consuming . Dynamic Light Scattering DLS and Neutron Diffraction Should only be applied on a very limited set of samples selected. ND Here the rating of the method range 1 5 is plotted carefully after studies using other techniques . against different categories Equal weight was given to all. Fig 2 Scoring of DLS and ND as MNP analysis methods The. questions within a category A high score means that the. high score for DLS for MNP shows that the method is a candidate. method has potential to serve as a common technique for to be standardized On the other hand ND is a technique that can. particle characterization and therefore it should be be used to obtain a comprehensive picture of the particle. standardized A high number can result for example from properties . low measurement costs from a high throughput or from. possibilities to provide fundamental particle properties that. The high score for DLS is due to the fact that reference useful to combine these methods with high throughput. samples of monodisperse particles with certified sizes are methods like DCM and ACS that also provide information. available e g from NIST and that an ISO standard ISO on the particle core Advanced techniques such as ND or. 22412 2008 exists for the application of DLS to determine SANS are highly suited to characterize both structural and. the average particle size and the polydispersity index 19 magnetic properties of. macroobjects or bulk materials 1 Thus nanostructures give access to novel techniques or they can be used to improve existing applications Magnetic nanoparticles MNPs are a significant class of these novel nanoobjects and their application in biomedicine is under intensive investigation 2 MNPs are used for diagnostic applications as contrast agents in imaging 3 or tracers 4 for

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