WO2016146512A1

WO2016146512A1 - Conditioning a sample container by means of conditioning fluid for promoting thermal coupling and for suppressing steam build-up

Info

Publication number: WO2016146512A1
Application number: PCT/EP2016/055265
Authority: WO
Inventors: Gernot Leuprecht
Original assignee: Anton Paar Gmbh
Priority date: 2015-03-13
Filing date: 2016-03-11
Publication date: 2016-09-22
Also published as: AT516382B1; AT516382A4

Abstract

The invention relates to a conditioning device (20) for conditioning a sample container (1) designed to accommodate a sample (2) for a sample measuring device (50), wherein the conditioning device (20) has a thermal coupling body (6) that can be thermally conductively coupled to the sample container (1) in order to promote a thermal energy exchange between the sample container (1) and an environment, and has a supply device (22) that is designed to supply a conditioning fluid in such a way that a first portion of the conditioning fluid can be supplied to the sample container (1) to suppress a steam build-up in the sample container (1), and a second portion of the conditioning fluid can be supplied to the thermal coupling body (6) to promote a thermal energy exchange between the thermal coupling body (6) and the environment.

Description

Conditioning a sample container by means of conditioning fluid to promote heat coupling and to suppress fogging

The invention relates to a conditioning device and a method for conditioning a sample container and a sample measuring device.

For the examination of samples, it is advantageous to temper them.

For this purpose, in many cases arrangements are used with Peltier elements that can transport heat with the help of electric current and a thermal countermass. Measurements at sample temperatures below the

Room temperature, require in optical measuring devices additionally one

Device that reliably prevents fogging of a sample cuvette due to indoor humidity. This is achieved in many cases by the metered influx of the cuvette with dry air.

The state of the art is described in US Pat. Nos. 4,975,237, WO 2007/019704 and US Pat

US 6,103,081.

In conventional devices Peltierelemente for temperature control of

Samples are used, wherein the waste heat in massive base plates, which simultaneously form the base plate of the optical bench, is passed. By using a solid base plate on which the entire optics assembly (with

Interferometer) can be a rapid heat dissipation in the cooling of

Samples are allowed.

Disadvantageously, the desired cooling temperature of the sample can only be maintained until the heat absorption capacity of the massive

Base plate is exhausted. This can be in the range of only about one hour, depending on the ambient conditions. Keeping the cooling temperature permanently is not possible with such arrangements.

Another limitation is that the heated base plate, due to its low surface area, can not quickly release the heat stored in it. Driving temperature cycles, ie. alternating heating and cooling for a long time, as may be desired in sample testing, then brings a considerable amount of time for temperature stabilization or does not succeed in the case of low sample temperatures.

Furthermore, the heat generated during cooling of the sample is distributed and stored virtually entirely in the device or the optical bench. This can lead to thermal expansions and voltages in the interferometer arrangement and influence the measurement signal quality.

It is an object of the present invention to provide a way to condition a sample container for a sample meter in a compact and efficient manner for sample metering.

This object is solved by the objects with the features according to the independent claims. Further embodiments are shown in the dependent claims.

According to one embodiment of the present invention is a

Conditioner for conditioning (i.e., for setting

Operating conditions) of a sample container designed to receive a sample (which may, for example, comprise a liquid and solid and / or liquid particles contained therein), the conditioning device comprising a (in particular of a thermally conductive material, more particularly highly thermally conductive material, For example, from a material having a thermal conductivity of at least 1 W / m K or at least 20 W / m K or at least 100 W / m K) thermal coupling body with the sample container (and in particular with a

Container holder with a receiving volume in which the sample container can be accommodated or held) can be coupled thermally conductive in order to thermal between the sample container and an environment

To promote energy exchange, and having a supply device, which is for supplying a conditioning fluid (i.e., a fluid for conditioning of the

Sample container, wherein a fluid having a gas and / or a liquid can) such that a first part of the conditioning fluid for suppressing fogging of the sample container (in particular with condensing moisture from the environment) can be supplied to the sample container and a second part of the conditioning fluid for promoting a thermal energy exchange (in particular for promoting heat exchange by convection ) between the thermal coupling body and the environment of the thermal coupling body can be fed.

According to a further embodiment of the present invention, a (in particular optical) sample measuring device for measuring a sample is provided, wherein the sample measuring device a sample container, the

Receiving the sample is formed, and having a conditioning device with the features described above for conditioning the sample container.

According to another exemplary embodiment is a

A method for conditioning a sample receiving sample container of a sample measuring device is provided, wherein in the method, a thermal coupling body is thermally conductively coupled to the sample container in order to heat between the sample container and an environment

To promote energy exchange, and a conditioning fluid by means of a

Feeding device is supplied such that a first part of the

Conditioning fluid for suppressing a fogging of the sample container is supplied to the sample container and a second part of the conditioning fluid for promoting a thermal energy exchange between the thermal coupling body and the environment is supplied to the thermal coupling body.

According to one embodiment of the invention, an arrangement for

Tempering of samples are created, with the anyway in the

Conditioner fluid (eg, dry air) to be introduced to a sample gauge to avoid fogging of a sample container simultaneously to improve the thermal energy exchange, in particular for improved

Heat dissipation, can be used. This is a thermal Coupling body (in particular a heat sink, ie, a thermal countermass) acted upon synergistically with conditioning fluid from the same or a common Konditionierfluidquelle, which also for suppressing

Condensation of liquid from ambient moisture to one

Sample container can be passed. Because of passing through

Conditioning fluid to the convection thermal coupling body forced convection can be obtained a thermally very powerful and flexible temperature control, which in a compact sample measuring device (for example, a DLS (Dynamic Light Scattering) measuring device) can be installed and advantageous to carry out relatively fast and reproducible

Temperature measuring cycles of samples allowed.

This has advantages: On the one hand, a compact and maintenance-free realization of a temperature control system due to the use of the already necessary air supply to the sample container (for example, to a cuvette) also allows thermal regulation of the thermal coupling body. Furthermore, the measures mentioned allow the achievement of very low sample temperatures (for example, up to 0 ° C and below) even at very high

Ambient temperatures (for example up to 35 ° C and above) in continuous operation. In this case, it can be ensured that the thermal coupling body remains below a maximum temperature (of, for example, 65 ° C.) which is permissible for surfaces which can be touched during normal operation. Another advantage is the relatively short time required for temperature stabilization of the sample by rapid

Heat release by forced convection by means of air. The sample can be exposed to rapidly changing temperature cycles. In this way, even long series of samples (by means of, for example, a flow cell and an autosampler) can be measured sequentially. Another advantage is that, as the sample cools, the resulting heat may be released to the environment virtually entirely and not distributed and stored in the sample meter or sensitive components thereof (eg, an optical bench which may include a sensitive interferometer) , Advantageously, a simply designed feeder (for example in the form of simply designed air supply elements) can be implemented, which has a small footprint. In addition, it can be achieved that in the

Essentially no vibrations, no noise, no

Staubverschleppung or no deposition and no power consumption, as in an electric fan or other mechanically and / or electrically driven feeders are generated. In addition, can be greatly reduced over the targeted supply of Konditionierfluids its amount compared to a fan. Compared to the amount of air to be carried by a fan, according to an exemplary embodiment of the invention, it is possible to carry much less air, which also produces less noise or vibration.

In the following, additional exemplary embodiments of the conditioning device, the sample measuring device and the method will be described.

According to one embodiment of the invention, the

Feeding device be adapted to remove the first part and the second part of the conditioning of a common conditioning fluid source. Such a conditioning fluid source may be a reservoir of conditioning fluid.

By feeding the first part and the second part of the conditioning fluid from the same source, a compact arrangement is made possible. The

For example, conditioning fluid source may be fluidly coupled to components of the delivery device by means of, for example, a branched, hose connection (or pipe connection or capillary connection) employing the first part and the second part of the conditioning fluid to suppress fogging and promote thermal exchange.

According to one embodiment of the invention, the

Conditioning fluid source be designed as Druckgascontainer. The pressure with which the conditioning fluid is stored in the compressed gas container advantageously provides the drive energy for the conditioning fluid, with which the first part of the conditioning fluid is flowed onto the sample container and the second part of the conditioning fluid is brought into heat exchange operative connection with the thermal coupling body. The pressure of the conditioning fluid can also be set and controlled via a respective valve / throttle for the first part and the second part (not shown). In other words, according to an exemplary embodiment of the invention, it is possible to quantitatively adjust the supply pressure with respect to the first part and the second part. For example, it is possible to temporarily shut off the dry air supply during heating with a Peltier element. More generally, therefore, the conditioning device may include a controller that may be configured to control or adjust a respective amount of the first portion of the conditioning fluid and an amount of the second portion of the conditioning fluid (and optionally temporarily supply the first portion and / or the second portion Can interrupt partially). Advantageously, no vibrating source (for

Example, the motor of a fan), which for example for an optical bench (which may have an optical interferometer) of an optical sampler would have highly disturbing influences on the measurement.

According to one embodiment of the invention, the

Conditioning fluid is a conditioning gas, in particular a low-moisture (that is less moisture than the ambient air), at least partially dehumidified (i.e., resulting from a process, with the

Inlet fluid is deprived of moisture) or moisture-free

Be conditioning gas. Especially suitable for the conditioning gas

Dry air, nitrogen or oxygen. But also helium -, etc. can be used.

According to one embodiment of the invention, the

Feeding device be set up for supplying a conditioning fluid such that the first part of the conditioning fluid can be directed to the sample container and / or the second part of the conditioning fluid to the thermal coupling body is correctable. In other words, the supply device can be designed to split the conditioning gas into the first part and the second part and then direct the respective parts in a targeted manner to the respective target areas. As a result, the inlet window and / or outlet window of the sample container can be effectively and reliably kept moisture-free, and the additional cooling effect can be specifically focused on the areas where the effects are particularly positive (for example for promoting convection and enhancing a cooling effect) the venturi effect).

According to one embodiment of the invention, the

Feeder be free of (in particular motor) movable components, in particular be vibration-free operable, further in particular

be fan-free. As a result, unwanted disturbances of the actual measurement procedure, for example, an optical bench with interferometer, can be avoided and thus a high accuracy of measurement can be achieved.

According to an embodiment of the invention, the second part of the

Conditioner be greater than the first part of the conditioning fluid. To the

Preventing fogging of the sample container may already be sufficient with a small amount of conditioning fluid generating a breath of air. In contrast, the supply of a considerable amount of conditioning fluid can particularly effectively increase the heat exchange at the thermal coupling body, advantageously by an additional reinforcement using the venturi effect.

According to one embodiment of the invention, the

Supply means comprise a common fluid drive (i.e., means for effecting the flow or flow of the conditioning fluid) for supplying the first part and the second part of the conditioning fluid. This allows the device to be made very compact. The fluid drive may be integrated into a conditioning fluid source and may, for example, be implemented in the form of a pressurized gas cylinder from which the pressurized conditioning gas flows from itself. The conditioning fluid source may be used for

Example by means of a hose connection or any other Fluid line the first part or the second part of the conditioning fluid purposefully lead to sample container or the thermal coupling body.

According to one embodiment of the invention, the

Feeding means a feed body having at least one fluid inlet opening for admitting the second part of the conditioning fluid and a plurality

Fluid outlet for discharging parts of the second part of the

Have conditioning to different areas of the thermal coupling body. The supply body may be fluidly coupled to a conditioning fluid source by means of the above-mentioned hose connections. Of the

Feeding body can be arranged relative to the thermal coupling body in such a way that the heat exchange (in particular a

Dissipation of energy from the thermal coupling body to the environment) by the targeted flow of individual areas of the thermal

Coupling body with the divided into partial flows second part of the

Conditioning fluids can be particularly effective.

According to an exemplary embodiment of the invention, the at least one fluid inlet opening and the plurality of fluid outlet openings can be fluidically coupled to one another by means of a branched network of fluidic channels in the feed body. The conditioning fluid can therefore start from one, two or more fluid inlet openings into a larger number

Fluid outlet openings flow and thereby be vividly spatially fanned out. In this way, the flow of the thermal coupling body can be done in a deterministic and highly effective manner. The more

Fluid outlet are provided, the more spatial areas of the thermal coupling body can be flown and so included in the gain of the cooling effect. For example, a series of parallel fluid outlet openings may be provided, all of which are flowed through in parallel direction by partial flows of the second part of the conditioning fluid (see, for example, FIG. 2). Another improvement of thermal energy exchange can be achieved by two (or more) such rows (see, for example, Figure 4).

According to one embodiment of the invention, the thermal coupling body can be thermally coupled to the sample container

Base portion and a plurality of starting from the base portion extending thermal coupling structures for thermal coupling with the environment, wherein between the thermal coupling structures

Intermediate spaces can be provided along which conditioning fluid and / or medium can flow out of the environment. The base portion may be a plate, for example. The individual coupling structures can for

Example, fins or ribs that may extend, for example, perpendicular to the plate. The material of the thermal coupling body may be thermally conductive, in particular be highly thermally conductive.

According to one embodiment of the invention, the

Feed device be adapted to supply parts of the second part of the conditioning fluid associated with the thermal coupling structures. This allows the ability of each individual of the thermal coupling structures, the

To increase heat dissipation, further increased.

According to one embodiment of the invention, the

Fluid outlet and the thermal coupling structures are arranged relative to each other such that the fluid outlet openings supply conditioning fluid between each adjacent the thermal coupling structures. In other words, each partial flow of the conditioning fluid can be replaced by a

Passage between two adjacent coupling structures (in particular fins or ribs) are passed and flow through this passage in the environment. This may be due to the Venturi effect to a by

Convection triggered further increase in the thermal exchange. This can be demonstrated experimentally by placing a candle under the coupling structures and passing the second part of the conditioning fluid through the fluid outlet openings. Due to the venturi effect comes it causes the flame of the candle is deflected by the resulting draft or the like.

According to one embodiment of the invention, the thermal coupling body may have a substantially L-shaped configuration. Such

Embodiment is shown in FIG. It has been found that this geometry leads to an efficient thermal energy exchange.

According to one embodiment of the invention, the

Conditioner have a tempering, in particular a cooling and / or heating device, which is arranged between the sample container and the thermal coupling body and for tempering the

Sample container is set up. The tempering device may preferably have a Peltier element. If such, for example, thermoelectric tempering between a sample container (or a

Container holder for holding the sample container) on the one hand and the

On the other hand sandwiched thermal coupling body, it is possible by appropriate control of the tempering an efficient and rapid heating or cooling of the sample and yet ensures a rapid and effective heat dissipation through the thermal coupling body.

According to one embodiment of the invention, the

Tempering device be designed to pressurize a sample located in the sample container with time-varying temperature cycles. A control device (for example a processor) can, according to a predeterminable profile of desired temperature cycles, control the tempering device for providing or removing thermal energy in accordance with a current temperature cycle, wherein the sample in the sample container changes temperature due to the spatial proximity and high thermal conductivity of the material disposed therebetween the tempering can follow quickly. If a rapid heat dissipation is desired in the event of a temperature change, this can be done on the side facing away from the sample the tempering carried out by means of the local conditionierfluidbeaufschlagten thermal coupling body.

According to one embodiment of the invention, the

Conditioner having a container holder, the one

Recording volume for holding the sample container has. The

Container holder may have a receiving space in which the

Sample container can be held. The container holder itself can be thermally highly conductive in order to achieve good thermal coupling between the sample in the sample container and the thermal coupling body. Laterally, a thermally insulating enveloping body can at least partially surround the container holder and the sample and largely thermally decouple from the environment laterally. The container holder and the enveloping body may be jointly penetrated by at least one passage opening of the feed device for feeding the first part of the conditioning fluid.

According to one embodiment of the invention, the

Conditioning device may be formed as a module which is operable and connectable with different sample measuring devices and is wiederabtrennbar of a respective sample measuring device. Such a compact module can be combined in a modular manner with different sample measuring devices, so that the provision and provision of a universal conditioning device is sufficient for different sample measuring devices.

According to one embodiment of the invention, the

Sampling device, an electromagnetic radiation source (for example, a laser) for providing electromagnetic primary radiation (for example, a preferably coherent and / or monochromatic beam

electromagnetic radiation, in particular visible light, infrared light and / or UV light) for irradiating a sample arranged in the sample container and an electromagnetic radiation detector (for example a photocell or a CCD detector, etc.) for detecting

Have electromagnetic secondary radiation by interaction is generated between the electromagnetic primary radiation and the sample. It is possible to use a single electromagnetic radiation detector

provide that detects, for example, in a predetermined direction of scattering. Alternatively or additionally, the use of several

electromagnetic radiation detectors possible, for example, in

Forward direction, under a certain scatter angle and / or in

Backward direction Measure scattered radiation. Such a detection method, which is based in particular on the scattering of light, often requires optical benches which are negatively influenced in terms of thermal expansion and / or the presence of vibrations in their functionality or at least accuracy. This is especially true for a high sensitivity optical interferometer of such an optical bench. In accordance with a

Exemplary embodiment, a vibration-free achievable improvement of the heat coupling is possible, the measurement accuracy of corresponding sample measuring devices is improved.

According to one embodiment of the invention, the

Supply means are adapted to direct the first part of the conditioner for suppressing the fogging of the sample container to an inlet window of the sample container for admitting the electromagnetic primary radiation and / or to an outlet window of the sample container for discharging the electromagnetic secondary radiation. This will be a

Influence of primary and / or secondary radiation due to moisture, which can be reflected on the respective windows, reliably avoided and thereby improves the measurement accuracy.

According to one embodiment of the invention, the

Sampling device as Electrophoretic Light Scattering (ELS) measuring device and / or Dynamic Light Scattering (DLS) measuring device. This is

Particle characterization devices using the method of dynamic and / or electrophoretic light scattering. This can cause particles in the Sample are characterized in terms of size (in particular size distribution) or a Zetapotential the sample can be determined.

Electrophoretic light scattering (ELS) is a technique for measuring the electrophoretic mobility of particles in dispersion or solution, where the mobility can be converted to values of zeta potential. ELS is based on electrophoresis: A dispersion is introduced into a measuring cell with two electrodes. An electrical voltage is applied to the electrodes. Particles with a net electrical charge move at a speed towards the oppositely charged electrode, which is referred to as mobility and is dependent on the zeta potential.

Dynamic light scattering (DLS) is a technique for measuring the size and size distribution of particles. Applications for the dynamic

Light scattering is the characterization of particles that are dispersed or dissolved in a liquid. The Brownian motion of particles in suspension causes the scattering of laser light with different

Intensities. The analysis of these intensity fluctuations gives the

Speed of Brownian motion. From this, the particle size is calculated using the Stokes-Einstein equation. In the following, exemplary embodiments of the

Present invention described in detail with reference to the following figures.

FIG. 1 and FIG. 2 show different views of one

Conditioning device according to an exemplary embodiment of the invention.

FIG. 3 and FIG. 4 show different views of one

Conditioning device according to another exemplary

Embodiment of the invention. FIG. 5 shows a diagram which shows temperature profiles on a sample container and a thermal coupling body without exposure to air.

FIG. 6 shows a diagram showing the temperature profiles on a

Sample container and a thermal coupling body with air admission according to an exemplary embodiment of the invention.

FIG. 7 shows a diagram, the temporal temperature profiles

correspondingly predetermined temperature cycles on a sample container and a thermal coupling body with air admission according to an exemplary embodiment of the invention.

FIG. 8 is a schematic representation of an optical one

Sample measuring device according to an exemplary embodiment of the invention. The same or similar components in different figures are provided with the same reference numerals.

Before describing exemplary embodiments of the invention with reference to the figures, a few general aspects of the invention and the underlying technologies will be explained:

Dynamic Light Scattering (DLS) is a method to study the dynamics of light-scattering samples and determine the Brownian motion of particles in the sample by diffusion coefficients. In particular, for the analysis of polymeric and colloidal systems DLS can be used advantageously. In concentrated systems DLS offers the possibility to study the dynamic properties and to study the different relaxation processes. The scattering centers in the sample move, and thus the distance between the scattering centers changes. Thus, the scattered light intensity fluctuates. That way you can

Particle sizes and distributions are determined. In order to be able to exploit the Brownian motion of particles in a sample and to determine their size or size distribution sufficiently accurately via the intensity fluctuations from the DLS technique, it is advantageous to prevent external disturbances on the particle movement or parasitic intensity fluctuations at the detector.

In most DLS experiments, only light interferes with the detector, which was scattered by different particles (so-called soap beating). Due to temporal changes in the relative position of the particles arise

Intensity fluctuations. Such experiments are relatively insensitive to vibration since all scattered light sources are within a very small volume and because the liquid between the particles is virtually incompressible.

Measurements in which, however, consciously or unconsciously a proportion of light that was not scattered by the particles (so-called local oscillator) arrives at the detector are sensitive to relative movements of the optical components and thus also to vibrations.

So-called homodyne DLS experiments become conscious

Derived reference beam from the primary laser and superimposed on the scattered light at the detector. In order to be able to describe the results analytically, the reference beam should be much stronger than the scattered light of the particles. Vibrations strongly disturb such measurements.

Often "seif beating" appliances are also used

unconscious homodynen component by reflections at the input or

Exit window of the sample cuvette or by reflections on other optical elements in the light path.

There are measuring geometries in which a small proportion of a homodyne component can hardly be completely avoided. This is the case, for example, if at very large scattering angles, near the

Backward scattering is worked. Frequently, the detector and the laser beam are focused by the same lens. Due to internal reflections within the condenser lens enters a small amount of laser light in the detector and acts there as a "local oscillator". In addition, it is very difficult for very large scattering angles, reflections from the entrance or exit window of the cuvette completely hide from the detector.

At the same time, however, backscatter geometry offers important advantages when it comes to measuring turbid samples where multiple scattering can occur. By moving the collecting lens or the sample cuvette, the scattering volume (ie, the overlap volume of detector and laser beam) can be placed close to the cuvette wall. This achieves very short path lengths of light within the sample, and the probability of multiple scattering can be reduced. Due to the virtually unavoidable homodyne component in this scattering geometry, however, such instruments are

typically significantly more susceptible to vibrations than instruments that operate at a 90 ° angle of spread.

A quantitative description of the effects of vibrations is difficult. Qualitative statements are possible.

The analysis of the measured correlation function is usually carried out using the so-called cumulant method (ISO 13321 and ISO 22412). This provides not only the average hydrodynamic diameter but also one

Polydispersity. This describes the width of the

Size distribution function. The influence of vibrations on the mean hydrodynamic diameter is typically small compared to the influence on the polydispersity index. The latter becomes too small under the influence of vibrations and under certain circumstances even negative.

Basically, vibrations at low frequencies (especially below 150 Hz) are critical. Measurements with large particles (especially above 500 nm) are more strongly influenced than measurements with small ones

Particles. When measured just below the surface of the liquid sample (i.e., low level in the cuvette), the effects of

Vibration stronger than at high sample levels in the cuvette. A stiff one Construction of the optical bench and all optical components and a good anti-reflection coating of the optical components help to reduce the influence of vibrations. External vibration can cause the

Affect measurement accuracy in a DLS device. Furthermore, it may be advantageous to suppress vibrations per se when massive

Materials used in the construction.

For temperature-dependent DLS measurements on samples, it is now also necessary to cool the sample sufficiently quickly and to release the resulting heat as quickly as possible to the environment. For this Peltier elements can be used with heat sinks. To ensure a high level of operational safety

To get laboratory gauge, the heatsink used should not reach a predetermined maximum temperature (of for example 65 ° C) or should shut down the laboratory device in this case.

Conventional DLS devices use cooling systems with fans or other mobile cooling units, which, however, can greatly affect a DLS measurement. This is especially the case when the mobile cooling units no longer function vibration-free over time, for example due to dust deposits. For example, moving / rotating parts of a cooling system would have to be maintained regularly to avoid disturbing vibrations and thus to obtain a reliable measurement result.

A cooling system for a DLS measuring device according to an exemplary embodiment of the invention, however, can prevent these disturbing vibrations, as can be dispensed with any moving parts and still allows effective cooling of a sample in a sample container.

FIG. 1 and FIG. 2 show different views of one

Conditioning device 20 according to an exemplary embodiment of the invention. Figure 1 and Figure 2 thus show a basic structure of a sample tempering arrangement with air admission. The conditioning device 20 is for conditioning (i.e., for

Setting the operating conditions) of a sample container 1 for an optical sampler 50 formed to receive a sample 2 shown in FIG. Sample 2 is a liquid matrix containing solid and / or liquid particles. The sample container 1 is shown in FIG

Embodiment of a cuvette. The sample measuring device 50 is used to determine an information indicative of the size of the particles of the sample 2 by means of dynamic light scattering and is thus designed as a DLS / ELS measuring device.

The conditioning device 20 includes a designed as a thermally conductive heat sink thermal coupling body 6, with the

Sample container 1 and the sample 2 contained therein, spaced by a thermally conductive container holder 3 and a temperature control device 5, is thermally conductively coupled. As a result, the thermal coupling body 6 can promote a thermal energy exchange between the sample container 1 and a surrounding air atmosphere.

A feeding device 22 of the conditioning device 20 is configured to supply drying gas as a conditioning fluid to the sample container 2 and to the thermal coupling body 6. This is done in such a way that a comparatively small first part of the conditioning fluid for suppressing fogging of the sample container 1 can be fed to an optical inlet window 10 and an optical outlet window 10 ^{λ of} the sample container 1. One

remaining and therefore relatively large second part of the

Conditioning fluids are supplied directed to promote thermal energy exchange between the thermal coupling body 6 and the environment of the thermal coupling body 6. In this case, the feed device 22 removes the first part and the second part of the conditioning fluid of a common conditioning fluid source 30 (for reasons of simple illustration shown only in Figure 1, but also in Figure 2 to Figure 4) in the form of a Druckgaskontainers, in which the conditioning fluid stored under pressure. The conditioning fluid source 30 is also shown by way of example only in FIG branched fluid lines 40 (realized, for example, by hoses and / or tubes and / or capillaries) fluidly with a feed body 7 and by means of the container holder 3 and a surrounding thermally insulating

Covering body 4 coupled to an outer wall of the sample container 1.

More precisely, partial fluid lines of the fluid line 40 run between a conditioning fluid outlet 42 of the conditioning fluid source 30 on the one hand and

respective fluid inlet openings 32 of the feed body 7 or openings 8, 8 ', 8 "and 8"' in the container holder 3 and the enveloping body 4 towards the

Light entrance or light exit surfaces (see reference numeral 10, 10 ^λ ) of the sample container 2 on the other. Conditioning fluid thus flows in part through the openings 8, 8 ', 8 "and 8'" and through a gap 44 to the optical inlet window 10 and the optical outlet windows 10 ^λ, and flows to another part in the feeder body 7. The pressure of the Pressurized container also serves as a common fluid drive for conveying the conditioning fluid from the pressurized gas container to the respective target positions, as will be described in more detail below. Therefore, the feeder 22 free of motor-movable components, in particular without a fan, and thus

be formed vibration-free. This ensures fault-tolerant operation of a sensitive optical bench of the sample measuring device 50, see FIG. 8.

Advantageously, the feed body 7, the two fluid inlet openings 32 to

Admitting the second part of the conditioning fluid and a larger number of fluid outlet openings 9 for discharging partial flows of the second part of the conditioning fluid to different areas of the thermal coupling body 6 towards. The two fluid inlet ports 32 and one or more

Fluid outlet openings 9 are fluidly coupled to each other by means of a branched network of fluidic channels in the interior of the feed body 7.

The formed as a heat sink thermal coupling body 6 has a thermally coupled to the sample container 1 plate-shaped base portion 34 and a plurality of extending from the base portion 34 perpendicular thereto fin-shaped or rib-shaped thermal coupling structures 36 for thermal coupling with the environment. The tempering device 5 is mounted on the plate-shaped base portion 34. Between

Thermal coupling structures 36 are gaps 38

provided along which conditioning fluid and ambient air can flow. The feeder 22 is shaped and relative to the thermal

Coupling body 6 arranged so that mutually parallel partial flows of the second part of the conditioning fluid associated with the thermal

Coupling structures 36 are supplied. More specifically, the serially provided fluid outlet openings 9 and the thermal coupling structures 36 are arranged parallel relative to one another such that the fluid outlet openings 9 feed conditioning fluid between respectively adjacent ones of the thermal coupling structures 36. The fluid outlet opening 9 can also have a gap or consist of a gap extending along the feed body 7 (for example milled in as a groove in the feed body 7).

The conditioning device 20 further comprises the optional cooling or heating operable and formed as a Peltier element tempering device 5, which is mounted between the container holder 3 and the thermal coupling body 6 and is set up for tempering the sample container 1. Controlled by a control device not shown in the figure is the

Tempering device 5 (for example, by alternating heating and cooling) able to apply a sample 2 located in the sample container 1 with time-varying temperature cycles.

According to FIG. 1 and FIG. 2, the conditioning device 20 is realized as a module that can be operated universally with different sample measuring devices 50.

In Figure 1 and Figure 2 is thus a possible inventive

Embodiment of an arrangement for sample temperature shown. The transparent cuvette as a sample container 1, which includes the sample 2, sitting in the shaft of a cuvette holder as a container holder 3, the good

thermally conductive metal. Outside of the cuvette holder are with a surrounded thermal insulating part as enveloping body 4, which causes the necessary thermal insulation to the environment. On at least one side of the cuvette holder - in the illustrated case the underside - is at least one Peltier element as tempering 5, which in turn rests on a ribbed heat sink as a thermal coupling body 6, which also consists of good heat conducting metal. The sample temperature is measured via a

Temperature sensor 11, which is mounted in the sample holder 3 and allows the control of the sample temperature. The monitoring of the coupling body temperature is carried out with the aid of a further temperature sensor 12. The optical access to the sample 2 is made possible by light passage openings (see reference numerals 10, 10 ', 10 "and 10"'). On the one hand, the laser light enters the sample tempering unit through these openings, which are arranged in different directions in the cuvette holder, and on the other hand, the scattered light leaves the sample space through these openings in the direction of the detector units of the instrument (see FIG. 8).

With this arrangement, it is now by applying an electrical

Voltage to the Peltier elements or the possible, the cuvette holder and thus the sample 2 at temperatures above ("heating") or below

("Cooling") to bring the ambient temperature. In the case of "heating" flows due to the Peltier electric heating and heat from the thermal coupling body 6 in the sample holder 1 and thus in the sample 2. The thermal coupling body 6 cools down because it is deprived of heat. The thermal coupling body 6 absorbs heat from the environment. In the case of "cooling", the current direction is reversed and the one or more Peltier elements withdraw / withdraw heat from the sample holder 1. This heat flows under

Temperature increase of the thermal coupling body 6 in the same and is released to the environment.

If the sample 2 is now cooled below the ambient temperature, it may, depending on the selected sample temperature and humidity of the ambient air to condensation phenomena especially on the outer sides of the cuvette come. This interferes with the passage of light into and out of the sample 2 and is undesirable for the measurement by means of optical methods. To avoid this fogging, dry air is passed through the openings 8, 8 ', 8 "and 8"' to the small areas of the outside of the cuvette which are transparent for optical measurement. This dry air displaces the humid room air. In the case of fogging already occurred, the cuvette outside are dried in the optically relevant areas. Alternatively or in addition to the dry air, other fluids / gases (for example nitrogen) can also perform this task.

Up to which absolute temperature the sample 2 now with a

Peltier arrangement can be cooled, hanging next to the

Ambient temperature and other influences (such as the effect of the insulating enveloping body 4) strongly on the heat-emitting capacity of the thermal coupling body 6 from. The more heat the thermal coupling body 6 can deliver to the environment, the lower the achievable temperature of the sample holder 1. Restrictive effect on the one hand, the performance of the Peltier elements and on the other usually the most for the thermal

Coupling body 6 available space in the sample measuring device 50, since thus the heat-exchanging surface is determined.

An installation of an electric fan to increase the convection and thus the increase in heat dissipation through the thermal coupling body 6 in addition to the additional space required the main disadvantage of

Vibrations near the sample 2 and thus the influence of the measurement result. However, a DLS or ELS meter should be substantially free of vibration during the measurement.

From the user's point of view, it is desirable, too

Ambient temperatures of up to 35 ° C reliably and permanently

To be able to reach sample temperatures of 0 ° C.

According to the described embodiment of the invention will now be initiated by the already be initiated dry air through a suitable air distributor in the form of the Zuführkörpers 7 diverted a part and in each

Cooling rib space between the thermal coupling body 6 passed. This air supply element in the form of the feed body 7 has a corresponding number of air outlet openings or fluid outlet openings 9, through which the air flows into the intermediate spaces. To increase the effect, the design of the arrangement can be made so that as a result of from the

Fluid outlet 9 flowing air due to the Venturi effect

Ambient air flows into the intermediate spaces 38 and thus the

Total air flow and the forced convection can be significantly increased.

The heat-releasability of the thermal coupling body 6 is thereby increased, and the achievable and durable sample temperatures in the case of "cooling" significantly reduced. In addition, the

Surface temperature of the thermal coupling body 6 settle at a lower level than without exposure to air, and it can therefore be arranged in a region on the outer skin of the sample measuring device 50, which is a touchable surface in normal operation and its

Maximum temperature therefore for safety reasons to a given

Temperature of, for example, 65 ° C can be limited.

The effluent from the sample 2 and the sample holder 1 heat is thus released directly over the thermal coupling body 6 virtually entirely to the environment and not stored in the sample measuring device 50 or an optical bench of the same and distributed. Thermal strains and

Tensions thus primarily affect the thermal at best

Coupling body 6 and not the interferometer assembly, which is used in the DLS / ELS sampler 50 to determine the Zetapotentail the sample 2. In addition, by a decoupled suspension of the thermal coupling body 6 any heat input into the optics can be practically eliminated. In addition, disturbing vibrations are produced for a DLS measurement

prevented, for example, which would cause a fan or other motorized parts of a cooling unit. Special biological samples, which are measured alternately at high and at low temperatures, should advantageously be heated very quickly. In a DLS sample analyzer 50 with a

Temperature control unit according to an exemplary embodiment of the

Invention, it is possible via a reserve or a Autosampier introduced into a flow cell sample 2 with different fast

To measure temperature cycles.

Advantageous features of a conditioning device 20 according to an exemplary embodiment of the invention are on the one hand the

Use existing dry air (or other conditioning fluid) to improve the effectiveness of the temperature and on the other hand, the simple elements of the air supply to the thermal coupling body 6, in particular the air supply element in the form of the feed 7 with the

Air outlet openings or fluid outlet 9 for each individual

Fin spacing. One according to an exemplary

Embodiment of the invention possible decoupled suspension of

Conditioning device 20 eliminates thermal strains and stresses in the optical bench.

FIG. 3 and FIG. 4 show different views of one

Conditioning device 20 according to another exemplary

Embodiment of the invention. Many features of the conditioning device 20 according to FIG. 3 and FIG. 4 correspond to those of the conditioning device 20 according to FIG. 1 and FIG. 2 and will not be described again below. Furthermore, in FIG. 3 and FIG. 4, the fluid connection between the

Conditioning fluid source 30 and the respective fluid inlets not shown, so reference is also made in this regard to Figure 1 and Figure 2 and the associated description. FIG. 3 and FIG. 4 show a construction of a sample temperature control arrangement with a double-row air feed element as feed body 7. Moreover, in this exemplary embodiment, FIG formed thermal coupling body 6 with an L-shaped configuration, as can be seen in Figure 4.

FIG. 3 and FIG. 4 show a further advantageous embodiment of an arrangement for sample temperature control. Here is the

Heat sink surface by the L-shape of the thermal coupling body 6 further increased. In addition, the air supply element is provided as a feed body 7 with two rows of air outlet openings or fluid outlet openings 9, so that also in this case vertical cooling rib intermediate spaces are exposed to air. Again, the Venturi effect causes the

Afterflow of ambient air and thus an increase in the

Total air flow and the heat output.

FIG. 5 shows a diagram 500 which shows temperature profiles on a

Sample container 1 and a thermal coupling body 6 without

Air exposure shows. Figure 5 includes an abscissa 502 along which time is plotted. Along an ordinate 504 of Figure 5, the temperature is plotted. A first curve 506 represents the temperature profile at

A second curve 508 represents the temperature profile at the heat sink (that is, more generally at the thermal coupling body 6). FIG. 6 shows a corresponding diagram 600 which shows temperature profiles on a sample container 1 and a thermal coupling body 6 Air application according to an exemplary

Embodiment of the invention shows. Figure 5 thus illustrates temporal temperature curves on cuvette holder and heat sink without exposure to air Figure 6, however, shows temporal temperature characteristics of cuvette holder and

Heat sink with Luftbeaufschlagung.

To illustrate the effect of the air flow are in Figure 5 and Figure 6, the results of experiments with an arrangement that the targeted

Applying the rib gaps of the heat sink allowed with air, shown. As curves are entered in each case of the two

Temperature sensors measured temperatures of the cuvette holder (see Curve 506, corresponds to the sample temperature) and the heat sink (see curve 508) as a function of time. FIG. 5 shows the progressions without exposure to air. In FIG. 6, the heat sink has been described

Exposed to dry air flow. Starting from room temperature, it is possible in both cases to achieve a sample temperature of 0 ° C within a few minutes. It turns out, however, that in the case of non-exposure to air after initial rise and short fall after the sample temperature reaches 0 ° C, the heatsink temperature progressively increases to reach the critical value of 65 ° C after about 90 minutes. The sample measuring device 50 would have to switch off the power supply to the Peltier elements for safety reasons when reaching the 65 ° C at the thermal coupling body 6. Thus, it does not set a stable temperature state of the heat sink, and a continuous operation is therefore not possible. In the case of forced air flow on the heat sink, on the other hand, its temperature stabilizes after 15 minutes, after an initial increase or short-term overshoot at a level of approximately 38 ° C. Even after more than five hours of operation, sample and heat sink temperatures remain constant in this case. Both experiments were at a

Ambient temperature of about 26 ° C performed. It is thus apparent that even at an ambient temperature of 35 ° C, the heat sink in the case of air exposure can maintain a stable temperature level well below 65 ° C.

FIG. 7 shows a diagram 700, which illustrates temporal temperature profiles according to predeterminable temperature cycles on a sample container 1 and a thermal coupling body 6 with air admission according to an exemplary starting example of the invention. FIG. 7 thus represents temperature cycles, with temporal temperature profiles on the cuvette holder (or more generally sample container 1) and cooling body (or more generally the thermal coupling body 6) with air admission being shown.

In Figure 7, the behavior of the conditioning device 20 in the

Execution of temperature cycles with cooling air at ambient temperature represented by about 25 ° C. The curve 506 shows the temperature profile of

Starting from room temperature, the sample 2 is first cooled to 0 ° C and subsequently heated several times to 90 ° C and cooled again to 0 °. The cooling of sample 2 takes about twice as long as the heating, but both periods remain over the five cycles shown here

unchanged. Already after the first cycle, a relatively stable temperature oscillation of the thermal coupling body 6 sets, i. after the respective heating phase, the thermal coupling body 6 has a

Temperature level of about 28 ° C-30 ° C, and after the cooling phase, its temperature is slightly below 50 ° C. From this it can be deduced that even after further cycles over a longer period of time and even higher

Ambient temperature, the coupling body temperature will hardly reach the allowable limit of 65 ° C. However, it can be seen that the temperature of the sample 2 between 90 ° C and 0 ° C stable and very fast with the

Peltier heating / cooling can be achieved without the thermal

Coupling body 6 which reaches 65 ° C. Without active cooling, the

Sample temperature of 0 ° C can be achieved only after a much longer time and measuring times with frequency sample supply in a flow cell very time consuming or impossible.

Figure 8 is a schematic representation of a Dynamic Light

Scattering (DLS) meter formed sample measuring device 50 for measuring a sample 2 according to an exemplary embodiment of the invention.

The sample measuring device 50 has the sample container 1, the

Recording the sample 2 is formed. Furthermore, the sample measuring device 50 contains a conditioning device 20 with the features described with reference to FIGS. 1 to 4 for conditioning the sample container 1.

In addition, is designed as a laser electromagnetic

Radiation source 52 for providing electromagnetic primary radiation (for example, a light beam) for irradiating a in the sample container 1 arranged sample 2 is provided. For example, as a photocell or CCD detector formed electromagnetic radiation detectors 56, 57, the

Forward scattering or backward scattering are for detecting electromagnetic secondary radiation (for example stray light)

provided by interaction between the electromagnetic

Primary radiation and the sample 2 is generated. It is also possible to provide only a single electromagnetic radiation detector in a sample measuring device 50 according to the invention.

The feeding device 22 may be advantageously arranged to supply the first part of the conditioning fluid for suppressing the fogging of the sample container 1 onto an inlet window 10 of the sample container 1 for admitting the

To direct electromagnetic primary radiation and an outlet window 10 ^{λ of} the sample container 1 for discharging the electromagnetic

To direct secondary radiation.

FIG. 8 thus shows the sample measuring device designed as a DLS / ELS device

50, further comprising a primary optic 53 and a secondary optic 55, a control unit 59 (for example, for setting a desired

Temperature by means of appropriate control or Regge the at least one Peltier device), an evaluation unit 58 and a Autosampier 61.

In addition, it should be noted that "having" does not exclude other elements or steps, and "one" or "one" does not exclude a plurality

excludes. It should also be appreciated that features or steps described with reference to any of the above embodiments may also be used in combination with other features or steps of other embodiments described above. Reference signs in the claims are not to be considered as limiting.

Claims

Patent claims

A conditioning apparatus (20) for conditioning a sample container (1) formed to receive a sample (2) for a sample meter (50), the conditioning apparatus (20) comprising:

a thermal coupling body (6) which is thermally conductive coupled to the sample container (1) to promote a thermal energy exchange between the sample container (1) and an environment;

a feeder (22) adapted to supply a conditioning fluid such that a first portion of the conditioning fluid for

Suppressing a fogging of the sample container (1) the sample container (1) can be supplied and a second part of the conditioning fluid for promoting a thermal energy exchange between the thermal coupling body (6) and the environment of the thermal coupling body (6) can be fed.

2. conditioning device (20) according to claim 1, wherein the

Feeding device (22) is adapted to remove the first part and the second part of the conditioning fluid of a common conditioning fluid source (30), in particular a by means of a fluid line (40) fluidly with the rest of the feed device (22) coupled conditioning fluid source (30).

3. conditioning device (20) according to claim 2, wherein the

Conditioning fluid source (30) is designed as Druckgascontainer.

4. conditioning device (20) according to any one of claims 1 to 3, wherein the conditioning fluid is a conditioning gas, in particular a

low-moisture, at least partially dehumidified or moisture-free conditioning gas is, in particular dry air, nitrogen, helium or oxygen.

5. conditioning device (20) according to one of claims 1 to 4, wherein the feed device (22) is adapted for supplying a conditioning fluid, that the first part of the conditioning fluid on the sample container (1) can be directed and / or the second part of the conditioning fluid on the

thermal coupling body (6) is directable.

6. conditioning device (20) according to one of claims 1 to 5, wherein the feed device (22) is free from moving, in particular motor-movable, components, in particular vibration-free operable, further in particular is fan-free.

7. conditioning device (20) according to any one of claims 1 to 6, wherein the feed device (22) is formed so that the supplied second part of the conditioning fluid is greater than the supplied first part of the conditioning fluid.

8. conditioning device (20) according to one of claims 1 to 7, wherein the feed device (22) has a common fluid drive, in particular integrated in a Konditionierfluidquelle (30) for providing the

Conditioning fluid for driving the conditioning fluid to supply the first part and the second part of the conditioning fluid.

9. conditioning device (20) according to any one of claims 1 to 8, wherein the feed device (22) has a feed body (7) with at least one

Fluid inlet opening (32) for admitting the second part of the conditioning fluid and one or more fluid outlet openings (9), in particular single-row or multi-row fluid outlet openings (9), in particular for discharging partial flows of the second part of the conditioning fluid to different areas of the thermal coupling body (6) having.

10. The conditioning device (20) of claim 9, wherein the at least one fluid inlet port (32) and the one or more

Fluid outlet openings (9) are fluidically coupled to each other by means of a branched network of fluidic channels in the interior of the feed body (7).

11. conditioning device (20) according to one of claims 1 to 10, wherein the thermal coupling body (6) with the sample container (1) thermally coupled base portion (34) and a plurality of starting from the base portion (34) extending thermal coupling structures ( 36) for thermal coupling with the environment, wherein between the thermal coupling structures (36) intermediate spaces (38) are formed, along which the second part of the conditioning fluid and / or medium from the

Environment can flow.

12. conditioning device (20) according to claim 11, wherein the

Feeding device (22) is arranged, partial flows of the second part of the

Supplying conditioning fluids associated with the thermal coupling structures (36).

13. conditioning device (20) according to claims 9 and 11, wherein the fluid outlet openings (9) and the thermal coupling structures (36) are arranged relative to each other such that at least a part of the

Fluid outlet ports (9) supplying conditioning fluid between adjacent ones of at least a portion of the thermal coupling structures (36).

14. conditioning device (20) according to one of claims 1 to 13, wherein the thermal coupling body (6) has a substantially L-shaped configuration.

15. conditioning device (20) according to one of claims 1 to 14, comprising a tempering device (5), in particular a cooling and / or Heating device which is arranged between the sample container (1) and the thermal coupling body (6) and adapted for tempering the sample container (1).

16. conditioning device (20) according to claim 15, wherein the

Tempering device (5) has a Peltier element.

17. conditioning device (20) according to claim 15 or 16, wherein the tempering device (5) is formed, in the sample container (1) located sample (2) with time-varying temperature cycles

apply.

18. conditioning device (20) according to one of claims 1 to 17, comprising a container holder (3) having a receiving volume for holding the sample container (1) and in particular of at least one passage opening (8, 8 \ 8 ", 8" ^λ ) of the supply means (22) for supplying the first part of the conditioning fluid is traversed.

19. conditioning device (20) according to one of claims 1 to 18, designed as a module which is operable with different sample measuring devices (50).

20. A sample measuring device (50) for measuring a sample (2), wherein the

Sample measuring device (50) has:

a sample container (1) adapted to receive the sample (2); and

a conditioning device (20) according to any one of claims 1 to 19 for conditioning the sample container (1).

21. A sample measuring device (50) according to claim 20, designed as an optical sample measuring device (50).

22. A sample measuring device (50) according to claim 20 or 21, comprising:

an electromagnetic radiation source (52) for providing

electromagnetic primary radiation for irradiating a in the

Sample container (1) arranged sample (2); and

at least one electromagnetic radiation detector (56, 57) for detecting secondary electromagnetic radiation generated by

Interaction between the electromagnetic primary radiation and the sample (2) is generated.

The sample measuring apparatus (50) according to claim 22, wherein the supply means (22) is arranged to supply the first part of the conditioning fluid for suppressing the fogging of the sample container (1) to an inlet window (10) of the

A sample container (1) for the admission of the electromagnetic primary radiation to judge and / or on an outlet window (10 ^λ ) of the sample container (1) for

Omission of secondary electromagnetic radiation to judge.

24. A sample measuring device (50) according to any one of claims 20 to 23, designed as one of the group consisting of an Electrophoretic Light Scattering (ELS) meter and a Dynamic Light Scattering (DLS) meter.

25. A method of conditioning a sample (2) receiving

Sample container (1) of a sample measuring device (50), the method comprising: thermally conductive coupling of a thermal coupling body (6) with the sample container (1) to between the sample container (1) and a

Environment to promote a thermal energy exchange;

Supplying a conditioning fluid such that a first portion of the

Conditioning fluids for suppressing fogging of the sample container (1) the sample container (1) is supplied and a second part of the conditioning fluid for promoting a thermal energy exchange between the thermal coupling body (6) and the environment of the thermal coupling body (6) is supplied.