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WO2016150910A1 - Procédé pour mesurer une propriété magnétique de nanoparticules magnétiques - Google Patents

Procédé pour mesurer une propriété magnétique de nanoparticules magnétiques Download PDF

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Publication number
WO2016150910A1
WO2016150910A1 PCT/EP2016/056142 EP2016056142W WO2016150910A1 WO 2016150910 A1 WO2016150910 A1 WO 2016150910A1 EP 2016056142 W EP2016056142 W EP 2016056142W WO 2016150910 A1 WO2016150910 A1 WO 2016150910A1
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WIPO (PCT)
Prior art keywords
liquid
nanoparticles
capillary
measuring
magnetic
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Ceased
Application number
PCT/EP2016/056142
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German (de)
English (en)
Inventor
Norbert LOEWA
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Bundesministerium fuer Wirtschaft und Energie
Physikalisch-Technische Bundesanstalt
Original Assignee
Bundesministerium fuer Wirtschaft und Energie
Physikalisch-Technische Bundesanstalt
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Filing date
Publication date
Application filed by Bundesministerium fuer Wirtschaft und Energie, Physikalisch-Technische Bundesanstalt filed Critical Bundesministerium fuer Wirtschaft und Energie
Publication of WO2016150910A1 publication Critical patent/WO2016150910A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
    • G01N2015/0038—Investigating nanoparticles

Definitions

  • the invention relates to a method for measuring a magnetic property of magnetic nanoparticles having the features of claim 1. According to a second aspect, the invention relates to a nanomagnetic particle analysis device for determining a magnetic property of magnetic nanoparticles having the features of claim 7.
  • Nanoscale particles are used, for example, in medicine and pharmacy. They usually consist of a magnetic core with a magnetic moment, which has a preferred direction and a shell. Depending on the material and size of the nanoparticle, the magnetic moment is stationary or can change direction due to thermal fluctuation.
  • the shell serves to stabilize the magnetic properties of the core material. For example, the shell protects against oxidation and / or agglomeration of the nanoparticles.
  • the nanoparticles must have predetermined magnetic properties.
  • specifications exist on their size, shape, chemical composition and / or crystallographic structure. Since both physiological and physical nanoparticle properties show a significant dependence on the size of the nanoparticles, the precise determination of the size distribution and the distribution of the magnetic properties of the nanoparticles is an important metrological task.
  • DLS dynamic light scattering
  • US 2010/0 033 1 58 A1 discloses a method for measuring agglutination parameters, in which the magnetic particles are processed in an assay.
  • the disadvantage of this is the comparatively long measurement time.
  • the invention has for its object to improve the measurement of magnetic properties of magnetic nanoparticles.
  • the invention solves the problem by a method having the features of claim 1.
  • the invention also solves the problem by a nanomagnet particle analysis apparatus having the features of claim 7.
  • An advantage of the invention is that a sample containing magnetic nanoparticles can be characterized with high accuracy.
  • the fractionated liquid stream is first prepared, which can be done by field-flow fractionation.
  • the nanoparticles are fractionated by a property, for example by their size.
  • the resulting liquid stream is then passed through the tortuous capillary. Due to the small Kapillarinnen tomessers it comes in the capillary to a laminar liquid flow, but not to turbulence. This ensures that the magnetization parameter is always determined only by the particles belonging to the fraction that is going through the capillary flows. Measurement errors due to sedimented or in a dead zone trapped magnetic particles can be at least largely excluded.
  • the method according to the invention thus makes possible a time-saving and precise characterization of dispersed magnetic nanoparticles.
  • the magnetic property of this fraction can be correlated with the property after which it was fractionated.
  • the invention allows characterization of the magnetic particles simultaneously, simultaneously, by means of two independent parameters.
  • the measurement can be carried out quickly.
  • measurement times of less than one minute, in particular less than 10 seconds can be achieved for characterizing a sample.
  • the liquid containing the nanoparticles is understood in particular to mean elution.
  • the elution is preferably designed so that the nanoparticles do not agglomerate during the performance of the method according to the invention or agglomerate only in a negligible amount.
  • the magnetization parameter is understood to be a number, a variable, a vector of numbers and / or variables, or another set of individual parameters, by means of which the magnetic properties of the nanoparticles can be characterized.
  • the magnetization parameters around the spectrum of the signal picked up by a receiver coil or magnetic field sensors.
  • the receiving coil detects the magnetic field in the immediate vicinity of the nanoparticles in the sample receptacle under the action of the alternating magnetic field.
  • the spectrum contains not only the first harmonic, but also the excitation frequency, ie the frequency of the alternating magnetic field, pronounced odd harmonics from which the magnetization of the nanoparticles can be deduced.
  • a coiled capillary is understood in particular to mean a liquid channel whose clear cross-section is at most 4 mm, in particular at most 2 mm.
  • the tortuous capillary is spirally wound.
  • Such a capillary can be produced in a particularly simple and reliable manner.
  • nanoparticles is meant, in particular, particles whose equivalent diameter is smaller than 1000 nanometers, smaller than 500 nanometers and especially at most 300 nanometers. Preferably, the equivalent diameter is greater than 1 nanometer, in particular greater than 10 nanometers. It should be noted that a magnetic nanoparticle always has magnetic material but does not have to be made entirely of it.
  • the capillary is preferably formed of quartz glass or plastic.
  • a plastic hose has the advantage of being disposable after use, ensuring that no contamination between two samples is possible.
  • the use of a glass capillary also offers the advantage of repeated use by resistance to chemical cleaners such as hydrochloric acid.
  • Fractionation is understood to mean, in particular, that a liquid stream is produced from the sample containing nanoparticles, with one, in particular exactly, property of the nanoparticles changing monotonously over time, in particular strictly monotonously.
  • the equivalent diameter is fractionated, which is a preferred embodiment, then the equivalent diameter at a given location where the fractionated liquid stream bypasses decreases or decreases monotonically with time.
  • it is a continuous fractionation, that is, the individual fractions flow smoothly into each other.
  • fractionation is by field-flow fractionation, in particular by asymmetric flow-field-flow fractionation.
  • the property to be fractionated may be, for example, size, shape, anisotropy, density and / or electrical conductivity.
  • the liquid is passed at a flow rate through the capillary, which is chosen so that there is a laminar flow in the capillary. It is advantageous that sedimentation effects and separation processes that could lead to changes in the properties of the fractionated liquid stream be avoided.
  • additional connecting points between the supply line and the liquid sample carrier in the measuring range can be dispensed with, since the supply line itself is also the liquid sample carrier in the measuring range.
  • One of the main causes of band broadening and hence loss of temporal resolution are junctions between tubing and flow cells, as well as flow cells themselves, as they often cause mixing of fluid flow due to their geometry (sharp-edged transitions).
  • the liquid is passed through the capillary such that the Reynolds number, calculated as the quotient of the product of the density of the liquid with the nanoparticles, a flow rate and capillary diameter of the capillary as a numerator and the dynamic viscosity of the liquid with the Nanoparticles is not more than 3000. If one or more of these variables change over time, this condition must always be met.
  • the measurement of the magnetization parameter takes place in an alternating magnetic field which is chosen so strongly that the non-linear region of the magnetization of the nanoparticles is achieved.
  • the field strength is preferably above 1 millitesla, for example in the range between 1 millitesla and 50 millitesla. It is favorable if the flow rate in the capillary is between 0.05, in particular 0.1 milliliter per minute and 3, in particular 1, milliliter per minute. At these flow velocities, the magnetophoretic force is insufficient to enrich the nanoparticles in the measuring chamber.
  • the measurement of the magnetization parameter takes place in a homogeneous alternating magnetic field (B).
  • B homogeneous alternating magnetic field
  • the volume can be increased in the sensitive, homogeneous measuring range of the coil. The influence of the volume in the inhomogeneous measuring range of the coil the measured signal is thereby reduced. Only then can a continuous measurement take place.
  • a nanoparticle measuring device preferably comprises a size distribution measuring device for measuring the size distribution of the nanoparticles in the fractionated liquid stream.
  • the size distribution measuring device is a device for performing a dynamic light scattering and / or for multi-angle light scattering.
  • the magnetization parameter is preferably measured by DC and / or AC susceptometry, by magnetic particle spectroscopy, magnetorelaxometry, nuclear magnetic resonance, electron spin resonance and magneto-optical relaxation measurement.
  • the effective magnetic moment of the particles can be determined from the measured curves which are obtained by means of the abovementioned methods by means of known physical relationships.
  • the effective magnetic and hydrodynamic size and size distribution of the particles, the saturation magnetization and the directional dependence of the magnetization can be derived.
  • the quantities mentioned are magnetization parameters according to the present description.
  • the measurement of the magnetization parameter takes place at least also by nonlinear AC susceptibility measurement, which is described, for example, in B. Gleich, J. Weizenecker, Nature 435 (2005) 1214-1217 or in N. Loewa, F. Wiekhorst, et al., IEEE Trans Magn. 49 (2013) 275-278.
  • the non-linear magnetization response MNP is measured with periodic - preferably sinusoidally oscillating - excitation.
  • the time-dependent measurement signal is recorded in broadband via a receiver coil and usually represented by Fourier transformation in the frequency domain. It contains not only the first harmonic (excitation frequency) but also pronounced odd harmonics (spectral moments).
  • a fixed excitation frequency of, for example, f -25 kHz and variable excitation amplitudes of 0-30 ⁇ s.
  • the measured signal spectrum allows the reconstruction of the size distribution of the magnetic nanoparticles contained in the sample.
  • the nonlinear magnetic particle signal is specifically measured without the influence of the linear diamagnetic background. Depending on the particle property, detection limits for nanoparticulate iron up to the picogram range are possible.
  • the detection limit using a capillary is significantly reduced again (factor of 2), as it does not have to be changed.
  • the moderate excitation amplitude ⁇ 50 mT compared to NMR, ESR, DC susceptometry
  • the dipolar interaction is not dominant for conventional particle sizes, which is why a significant sample change by the measurement is not to be feared.
  • a nanomagnetic particle analyzing apparatus preferably has a liquid supplying device configured to supply the liquid to be laminar in the capillary.
  • the nanomagnetic particle analysis device preferably comprises a size distribution measuring device for measuring the size distribution of the nanoparticles in the fractionated liquid flow and / or a measuring device for determining the concentration in the form of a UV or refractive index (RI) detector.
  • the size distribution measuring device is preferably a DLS or multi-angle light scattering (MALLS) measuring device.
  • the particle fractionating device is preferably arranged upstream of a fraction characterizing device in the flow direction of the liquid, the term fraction characterizing device being the general term for the size distribution measuring device, the MALLS detector and the DLS or multi-angle light scattering device. (MALLS) measuring device and magnetic property measuring device.
  • the magnetic property measuring device comprises the measuring coil and the device for evaluating the measuring signals of the measuring coil.
  • the nanomagnet particle analyzer device comprises a fraction collector for volume-resolved enrichment of the eluting liquid stream.
  • FIG. 2 shows a capillary of the analysis device according to FIG. 1 and FIG.
  • FIG. 3 shows a measurement curve which was obtained in the context of a method according to the invention.
  • FIG. 1 shows a nanomagnetic particle analysis device 10 according to the invention which has a liquid sample carrier 12 and an alternating field generator 14.
  • the alternating field generator 14 comprises a coil 16, which can be acted upon by a schematically drawn control unit 20 with an alternating current I.
  • the nanomagnet particle analysis device 10 has a liquid supply device 24, which is schematically drawn.
  • the sample 26 When the sample 26 is supplied to the liquid supply device, it generates a liquid flow of liquid 29 (see FIG. 2) by means of a particle fractionating device 28, which is passed into the liquid sample carrier 12.
  • the nanomagnet particle analysis apparatus 10 additionally comprises a measuring coil 18, by means of which the magnetic field B is measured, which is set up by the alternating field generator 14 and the magnetization of the material in the sample receiver 22 becomes .
  • a measuring coil 18 by means of which the magnetic field B is measured, which is set up by the alternating field generator 14 and the magnetization of the material in the sample receiver 22 becomes .
  • the construction of the measuring coil 18 and its position relative to the capillaries 30 are shown in detail.
  • the liquid keitsprobenarme 1 2 has a capillary 30, ie in the present case consists of quartz glass and is spirally wound.
  • the liquid feed device 24 comprises a schematically drawn pump 32 which is designed to supply a liquid containing the sample 26 at a flow rate v which is at least substantially constant over time.
  • d is the capillary internal diameter of the capillary (see FIG.
  • a size distribution measuring device 34 is arranged, which in the present case comprises a MALLS detector 42 and a DLS detector 43 and by means of which a measurement by means of light scattering can be carried out.
  • an additional concentration measuring device 40 in the form of a UV detector and / or a Rl detector is arranged in front of the alternating field generator.
  • the size distribution measuring device 34 provides the distribution function F indicating, for each equivalent diameter of the nanoparticles, what proportion of nanoparticles that can be given, for example, in mass percent or volume percent, at most equals this equivalent diameter.
  • the equivalent diameter is understood in particular to mean the hydrodynamic equivalent diameter.
  • FIG. 2 shows a partial view of the capillary 30. It can be seen that it has a measuring section 36. In this measuring section 36, the capillary 30 is spirally wound, as can be seen in the lower part of the image. In the operating state, the measuring section 36 is located in the measuring coil 18.
  • the measuring section 36 is formed in the preceding case so that an envelope cuboid has a side length of less than 1 2 mm, in particular less than 1 0 mm.
  • the Hüllquader has a side length of 8 mm.
  • the envelope cuboid is the imaginary cuboid minimum page length that completely surrounds the measuring section.
  • the choice of the corresponding measurement volume depends on the required resolution for a given volume flow. The smaller the volume at the same volume flow, the higher the temporal resolution. In addition, the corresponding measurement volume is determined by the required detection limit (minimum particle concentration to be detected). The larger the volume, the lower concentrations can be detected.
  • a capillary diameter D of the capillary 30 in the present case is 0.5 + 0.15 millimeters.
  • the outer diameter D out is approximately 2 + 0.5 millimeters.
  • first of all liquid is dispensed from the liquid feed device 24 (FIG. 1) into the liquid sample carrier.
  • the discharged liquid amount V (t) is determined and stored as a function of time.
  • the control unit 20 energizes the outer coil 16 so that it generates the alternating magnetic field B.
  • the measuring coil 18 comprises a receiving coil 17, in which the measuring section 36 of the liquid sample carrier 12 is arranged, and a reference coil 19, which form a gradiometer arrangement. This suppresses the excitation frequency and increases the measurement accuracy. It is possible, and represents a preferred embodiment, that the measuring coil 18 is arranged spatially within the coil 16.
  • an induced voltage Uind (t) is measured as a function of the time t.
  • the liquid Before passing through the sample holder 22, the liquid flows into the size measuring device 34, which also distributes the size as a function of the time t measures. Since the time offset for each liquid fraction of the fractionated liquid flow between two meters is known, it can be determined at which time this liquid fraction has flowed through the sample holder 22 and when through the size distribution measuring apparatus 34. This time offset is determined, for example, in a preliminary experiment by bolus injection.
  • the aforementioned measurement results are fed to an evaluation unit 38, which may be part of the control unit 20 and liquid supply means 24, but this is not necessary.
  • FIG. 3 shows a measurement result that was determined with the nanomagnetic particle analysis device 10 according to the invention.
  • the abscissa shows the elution volume virus in milliliters.
  • the curve DLS indicates the particle diameter d of the particles as measured by DLS. It can be seen that the particle diameter increases approximately linearly with the elution volume, since in this case the asymmetric flow-field-flow fractionation was used, which causes a separation of the applied sample according to hydrodynamic size.
  • the curve marked MPS shows the amplitude of the third harmonic ⁇ 3 in the square of the ammeter normalized to the iron content CFe in moles of iron. It can be seen that this curve passes through a maximum for particles with a diameter between 50 and 60 nanometers and does not correlate linearly with the hydrodynamic size of the particles, whereby the added value of the magnetic measuring device is detected.
  • the magnetic particle analysis device 10 may have a concentration measuring device 40 which is designed to measure a concentration CF 2 of nanoparticles in the fractionated liquid flow. Such a measurement result is shown in the curve marked CFeuv. It can be seen that the measured sample has a large proportion of very small nanoparticles, but they have a very small magnetic moment.
  • the particle fractionating device 28 is in the flow direction of the liquid 29 upstream of the fraction characterizing devices, namely, the size distribution measuring device 34, the MALLS detector 42, and the DLS or multi-angle light scattering (MALLS) measuring device 43.
  • the fraction characterizing devices namely, the size distribution measuring device 34, the MALLS detector 42, and the DLS or multi-angle light scattering (MALLS) measuring device 43.

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  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Materials By The Use Of Magnetic Means (AREA)

Abstract

L'invention concerne un procédé pour mesurer une propriété magnétique de nanoparticules magnétiques dont les étapes consistent à : faire passer un liquide (29) contenant les nanoparticules (31) à travers un champ magnétique alternatif (B), mesurer un paramètre de magnétisation décrivant une relation entre la magnétisation des nanoparticules (31) et le champ alternatif (B), et faire passer le liquide (29) à travers le champ alternatif (B) à l'intérieur d'un capillaire enroulé (30) . Selon l'invention, un fractionnement des particules magnétiques (31) dans le liquide (29) est effectué avant leur passage à travers les capillaires enroulés, ce qui donne un courant de liquide fractionné, la mesure du paramètre de magnétisation comprenant une mesure résolue dans le temps du paramètre de magnétisation au niveau du courant de liquide fractionné.
PCT/EP2016/056142 2015-03-23 2016-03-21 Procédé pour mesurer une propriété magnétique de nanoparticules magnétiques Ceased WO2016150910A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102015205202.8 2015-03-23
DE102015205202.8A DE102015205202A1 (de) 2015-03-23 2015-03-23 Verfahren zum Messen einer magnetischen Eigenschaft von magnetischen Nanopartikeln

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107473597A (zh) * 2017-08-24 2017-12-15 东莞市龙博自动化设备有限公司 一种玻璃蚀刻机的供液系统
CN108663295A (zh) * 2018-08-06 2018-10-16 上海景瑞阳实业有限公司 一种纳米粒子粒径分布测试仪及测试方法

Citations (4)

* Cited by examiner, † Cited by third party
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US20080095705A1 (en) * 2004-11-09 2008-04-24 Virtanen Jorma A Methods and Devices for Facile Fabrication of Nanoparticles and Their Applications
US20090085557A1 (en) * 2006-04-19 2009-04-02 Anatol Krozer Detection device and method
US20100243574A1 (en) * 2007-10-29 2010-09-30 Koninklijke Philips Electronics N.V. Separator column, separator system, method of fractionating magnetic particles, method of manufacturing a separator column and use of a separator column
US20110135061A1 (en) * 2008-05-21 2011-06-09 Thuenemann Andreas Device and method for analyzing nanoparticles by combination of field-flow fractionation and x-ray small angle scattering

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US8217647B2 (en) * 2006-12-19 2012-07-10 Koninklijke Philips Electronics N.V. Measuring agglutination parameters

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20080095705A1 (en) * 2004-11-09 2008-04-24 Virtanen Jorma A Methods and Devices for Facile Fabrication of Nanoparticles and Their Applications
US20090085557A1 (en) * 2006-04-19 2009-04-02 Anatol Krozer Detection device and method
US20100243574A1 (en) * 2007-10-29 2010-09-30 Koninklijke Philips Electronics N.V. Separator column, separator system, method of fractionating magnetic particles, method of manufacturing a separator column and use of a separator column
US20110135061A1 (en) * 2008-05-21 2011-06-09 Thuenemann Andreas Device and method for analyzing nanoparticles by combination of field-flow fractionation and x-ray small angle scattering

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107473597A (zh) * 2017-08-24 2017-12-15 东莞市龙博自动化设备有限公司 一种玻璃蚀刻机的供液系统
CN107473597B (zh) * 2017-08-24 2023-03-24 东莞市龙博自动化设备有限公司 一种玻璃蚀刻机的供液系统
CN108663295A (zh) * 2018-08-06 2018-10-16 上海景瑞阳实业有限公司 一种纳米粒子粒径分布测试仪及测试方法
CN108663295B (zh) * 2018-08-06 2024-01-23 上海景瑞阳实业有限公司 一种纳米粒子粒径分布测试仪及测试方法

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