NL2031837B1 - Method to combine optical imaging spectroscopy and analytical spectrometry - Google Patents

Method to combine optical imaging spectroscopy and analytical spectrometry Download PDF

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Publication number
NL2031837B1
NL2031837B1 NL2031837A NL2031837A NL2031837B1 NL 2031837 B1 NL2031837 B1 NL 2031837B1 NL 2031837 A NL2031837 A NL 2031837A NL 2031837 A NL2031837 A NL 2031837A NL 2031837 B1 NL2031837 B1 NL 2031837B1
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Netherlands
Prior art keywords
sample
sensor
property
chamber
measuring device
Prior art date
Application number
NL2031837A
Other languages
Dutch (nl)
Inventor
Van Gorsel Cornelis
Ahmed Hashmi Syed Sarfarazuddin
Original Assignee
Portolab B V
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Publication date
Application filed by Portolab B V filed Critical Portolab B V
Priority to NL2031837A priority Critical patent/NL2031837B1/en
Priority to PCT/EP2023/057943 priority patent/WO2023217455A1/en
Priority to PCT/EP2023/057950 priority patent/WO2023217456A1/en
Application granted granted Critical
Publication of NL2031837B1 publication Critical patent/NL2031837B1/en

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Classifications

    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/004—Combinations of spectrometers, tandem spectrometers, e.g. MS/MS, MSn
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/0022—Portable spectrometers, e.g. devices comprising independent power supply, constructional details relating to portability
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00—Particle spectrometers or separator tubes
    • H01J49/02—Details
    • H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
    • H01J49/0459—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for solid samples
    • H01J49/0463—Desorption by laser or particle beam, followed by ionisation as a separate step
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N2021/1734—Sequential different kinds of measurements; Combining two or more methods

Abstract

The invention relates to a measurement device for analysis of a sample contained in a sample holder having an opening, wherein the measurement device is configured to use at least two parallel measurements. The invention further relates to a method for parallel analysis of a sample contained in a sample holder having an opening using at least two measurements, wherein use is made of a measurement device according to the invention.

Description

NEXT22001NL/PO P35651NLO0/SBI
METHOD TO COMBINE OPTICAL IMAGING SPECTROSCOPY AND ANALYTICAL
SPECTROMETRY
The invention relates to a measurement device for analysis of a sample contained in a sample holder having an opening, wherein the measurement device is configured to use at least two parallel, e.g. simultaneous, measurements. The invention further relates to a method for parallel analysis of a sample contained in a sample holder having an opening using at least two measurements, wherein use is made of a measurement device according to the invention.
There is a demand for portable and rapid detection sensors in the security market for screening of risk related substances. With ever growing numbers of passengers the need for faster and better sensors is higher than ever. For example, airport security uses sensors to detect luggage of travellers for the presence of drugs. After a suspicious substance has been found the substance is tested using a first test. If this test returns a positive result, a suspect, e.g. the person whereon the substance is found, may be placed under arrest.
In many countries, a second test on the nature of the substance is required before a judge may give verdict, e.g. for drug trafficking. The first test is performed on site using a known sensor method and the second test is traditionally performed at a laboratory. Laboratory based methods, that are independent from the first test, may be reliable and performed by qualified personnel and are often seen as essential when dealing with a suspect substance.
Current detection methods used by security personnel that are laboratory based are time consuming, with between 1 to 3, sometimes even longer, before a laboratory produces a result, e.g. increasing the likelihood that the suspect is released on bail. Additionally, laboratory based methods are expensive, e.g. the second test performed at the laboratory is often much more expansive than the first test performed on site. A further downside of using a laboratory based method is that the sample of the suspicious substance has to be moved to the laboratory which may increase changes of contamination of the sample.
An object of the invention is to reduce the time between collecting a sample and providing two independent tests for determining a characteristic of the sample.
The object of the invention is achieved by a measurement device of claim 1.
The measurement device of claim 1 allows a single sample to be measured by two parallel, simultaneous and independent measurements. Each measurements relates to a respective test for testing a property of the substance. Each of the two measurements determines a property of the sample which is received by the processor determining a characteristic of the sample based on these properties. Thus removing the need to wait for the results of a second test after performing the first test and reducing the time between collecting the sample and providing the two independent tests for determining the characteristic of the sample.
The measurement device is configured to determine a characteristic of a sample that is contained in a sample holder having an opening. For example, the sample holder may be a vial or bottle having a top side opening. The opening of the sample holder may serve to allow sample, e.g. vaporized sample, to escape the sample holder and move to the second sensor through the separator. The sample holder may be provided with the measurement device as a kit so that the sample holder neatly fits into the sample chamber.
The measurement device is configured to be able to perform at least two parallel measurements. The measurements may be used parallel to each other, meaning that the two measurements, and thus the two tests, may be performed simultaneously on the same sample. In embodiments the device may also be operated such that only one of the tests is performed, or that the two tests are performed subsequently.
The measurement device comprises a sample chamber for placing the sample holder containing the sample. The sample chamber may be a cavity in the device comprising a openable wall for opening and closing the sample chamber allowing the sample holder to be placed in and removed from the sample chamber.
The measurement device further comprises a first sensor for performing a first measurement on the sample in the sample holder. The first sensor is configured for determining a first property of the sample using the first measurement. The first sensor is an optical sensor, i.e. a sensor relying on optical techniques to measure the first property, that is provided adjacent to the sample chamber. For example, the first sensor may be provided such that an opening or a window of the sample chamber allows the optical sensor, e.g. the light thereof, to measure the sample in the sample chamber.
The first sensor determines the first property of the sample based on optical properties of the sample. For example, the first sensor may be based on infrared measurement techniques whereby the sample is irradiated with infrared light. The first property may then be determined based on the reflection of the irradiated light, for example based on detected frequencies of infrared light that are absorbed by molecules of the sample. For example, the first sensor may be based on near infrared spectroscopy wherein compounds in the sample are detected based on detected frequencies of infrared light that are absorbed and emitted by molecules in the sample. The first property may be related to chemical structure of the sample, e.g. to determining the presence of a molecule in the sample based on the absorption of the light, e.g. the presence of a cocaine molecule in the sample.
The measurement device further comprises a sample ionizer for ionizing the sample. The sample ionizer may be provided such that the sample may be ionized in the sample chamber or in the vacuum chamber. The sample ionizer may ionize the sample by providing a large voltage to the sample.
The measurement device further comprises a vacuum chamber configured for comprising a vacuum. The vacuum chamber has an opening that is provided in a wall of the sample chamber. In embodiments, the opening is provided in an upper wall of the sample chamber.
The opening between the vacuum chamber and the sample chamber allows sample, e.g. vaporized or ionized sample, to drift from the sample chamber to the vacuum chamber.
The measurement device further comprises sample transfer means comprising a heatable separator provided between the vacuum chamber and the sample chamber, for separating the vacuum chamber from the sample chamber, wherein the heatable separator is porous to the sample, wherein the sample transfer means are configured for transferring a portion of the sample from the sample holder through the separator to the vacuum chamber. The sample transfer means are configured for transferring a portion of the sample from the sample holder through the separator to the vacuum chamber. The sample transfer means allow a portion of the sample, to be measured by the second sensor, to be transferred from the sample holder to the vacuum chamber for measurement. The sample transfer means may transfer the sample passively, e.g. by vaporizing, or actively, e.g. by using some pump mechanism.
The heatable separator allows the sample to go from the sample holder to the vacuum chamber by a controlled leak from the sample chamber to the vacuum chamber, e.g. without destroying the vacuum in the vacuum chamber. The separator is heated to prevent sample from forming on the separator, for example to prevent vaporized sample to reconversion from vapor to liquid or solid form. The separator may be provided at a distance of 0.5 mm to 10 cm, preferably at 2 cm, from the opening of the sample holder when the sample holder is placed in the sample chamber.
The separator may control a leak to the vacuum chamber from the sample chamber by a control leak valve or an opening. The separator may block moisture from entering the vacuum chamber to prevent damage to the vacuum chamber and/or the second sensor.
The measurement device further comprises a second sensor for performing a second measurement on ionized sample in the vacuum chamber and for determining a second property of the sample. The ionized sample is ionized by the sample ionizer. The second sensor is an analytical spectrometry sensor, such as a mass spectrometry sensor, provided in the vacuum chamber, which may detect the presence of compounds of interest, e.g. drugs or explosives, based on the molecular weight thereof. The second sensor allows a second, independent from the first, test to be performed on the sample. The sample may be measured by the first sensor while a portion of the sample is transferred to the vacuum chamber and measured by the second sensor. The second sensor may detect the second property based on mass-to-charge ratio of the ionized sample.
The measurement device further comprises a processor connected to the first sensor and the second sensor for receiving the first sample property and the second sample property. The processor is configured for determining a characteristic of the sample based on the first sample property and the second sample property. For example, if the first sample property and the second sample property are indicative of cocaine, the processor may determine that the sample is or contains cocaine. For example, if the first property and the second property are contradictory for determining a characteristic of the sample, the processor may determine that the characteristic of the sample may not be determined based on the first and second properties. The processor may show the determined characteristic on a display, e.g. on the request of an operator.
In embodiments of the measurement device, the measurement device comprises a heater for heating and vaporizing the sample contained in the sample holder located in the sample chamber, wherein the heatable separator is porous to the vaporized sample. In embodiments, the heater may be a metal or ceramic heater. Preferably, the heater is configured such that sample may not stick to the surface thereof. For example, the heater is provided outside of the sample chamber adjacent to a wall thereof. By vaporizing the sample, the sample may be transferred through the separator, e.g. under the effect of diffusion. In this embodiment, the sample ionizer may be provided to ionize the sample in the sample chamber or in the vacuum chamber.
In embodiments of the measurement device, the sample transfer means further comprises the sample ionizer, wherein the sample ionizer is configured to ionize the sample in the sample holder, and wherein the heatable separator comprises an ambient ionization probe for providing an electric potential to transfer the ionized sample from the sample chamber to the vacuum chamber. In this embodiment the sample is transferred to the vacuum chamber by ionizing the, portion of, sample and then transferring the sample under the influence of an electric potential, e.g. an electric field, through the separator which comprises an ambient ionization probe for providing the electric potential. For example, the ambient ionization probe may be a paperspray or an electrospray. For example, in this embodiment the separator may comprise a capillary with a diameter between 0.08mm and 0.13mm.
In embodiments, the separator may further comprise an intermediate vacuum region between the sample chamber and the vacuum chamber. For example, the vacuum chamber, intermediate vacuum chamber and the sample chamber are separated by orifice, for example having diameter of 1 mm. The vacuum in the intermediate vacuum chamber may be between 1mbar and 2mbar.
In an embodiment of the measurement device the heatable separator comprises a heatable membrane probe comprising a membrane and a porous metal mesh, preferably having openings with a size in the range of 10 micrometer to 100 micrometer. The heatable membrane probe allows for a controlled leak to the vacuum chamber, allowing sample to be transferred thereto while maintaining sufficient vacuum, e.g. under the influence of a vacuum pump. For example, the separator may comprise a membrane probe, e.g. a PDMS membrane in combination with a metal mesh, which is configured to control a flow of sample from the sample chamber to the vacuum chamber. For example, the control leak valve may be provided between the membrane probe and the vacuum chamber which has an opening having a diameter between 0.5mm and 1 mm. Instead of a control leak valve, it is possible that an opening is provided between the membrane probe and the vacuum chamber.
In an embodiment the heatable separator comprises a heatable capillary inlet. Similarly as for the membrane probe, the capillary inlet allows for a controlled leak to the vacuum chamber, allowing the sample to be transferred thereto. For example, the separator may comprise a heated capillary having a diameter between 10 micrometres and 100 micrometre for controlling a leak between the sample chamber and the vacuum chamber.
In embodiments of the measurement device, the heatable separator is heatable to at least 80 °C, preferably to at least 100 °C. It was found that for common samples, heating the heatable separator to at least 80 °C, preferably to at least 100 °C, prevents the sample from forming on the separator preventing the sample to be transferred to the vacuum chamber.
In embodiments of the measurement device, the first sensor is one of an infrared sensor, a
Raman spectroscopy sensor, an ultraviolet- visible spectroscopy sensor, and a hyperspectral spectroscopy sensor. The type of first sensor may be chosen based on the type of sample measurement requirements, which may depend on sample features such as: transmittance, interactance, transflectance, diffuse transmittance, and diffuse reflectance.
In embodiments of the measurement device, the second sensor is one of a mass spectroscopy sensor, a gas chromatogram sensor, and a gas chromatogram — mass spectrum sensor. These sensors allow to determine a second property of the ionized sample, independent from the first property. The type of second sensor may be chosen based on the sample.
In embodiments of the measurement device, the vacuum chamber is configured for having a pressure between 10% and 107 mbar. In embodiments of the measurement device, the measurement device comprises a vacuum pump, e.g. for maintaining the vacuum through the controlled leak of the separator. The pressure of the vacuum chamber may be controlled by the vacuum pump.
In embodiments of the measurement device, the first sensor and/or the heater are located adjacent a sidewall or a lower wall of the sample chamber. The first sensor and the heater may both be located below the lower wall.
In embodiments of the measurement device, the sample holder comprises a mirror having a mirroring surface, and wherein the first sensor is provided opposite the mirroring surface when the sample holder is placed in the sample chamber. For example, the sample may be too transparent for the optical sensor to accurately determine the first property. A solution is to provide a mirror that reflects light from the optical sensor that has travelled through the substance back to the sensor such that the first property may be determined based on this light that has travelled through the sample. For example, when the optical sensor is provided below a lower wall of the sample chamber, the mirroring surface may be parallel to the lower wall when the sample holder is placed in the sample chamber. The mirror may be provided in a cavity in the sample holder that contains the sample.
The sample holder may comprise a transparent vial of e.g. borosilicate glass, Quarts glass or plastic.
In embodiments of the sample holder, the heater is configured to heat the sample to at least 400 °C, preferably to at least 500 °C. Depending on the sample, by heating the sample first volatile compounds may be vaporized from the sample and measured by the second sensor.
By increasing the temperature less volatile compounds may be vaporized and measured by the second sensor. The sample may be heated to a temperature suitable for vaporizing interesting compounds therein. It was found that a temperature of at least 400 °C, preferably to at least 500 °C may allow for vaporizing samples sufficiently. For example, the heater may be controlled to selectively vaporize compounds from the sample. For example, the heating may be ramped up slowly such that volatile compounds are vaporized. After or during vaporizing the volatile compounds, the heater may be ramped up more to vaporize less volatile compounds. For example, the heating may be ramped up between 40 °C and 400 °C per minute.
The invention is further related to a method for parallel analysis of a sample contained in a sample holder having an opening using at least two parallel measurements, wherein use is made of a measurement device according to the invention.
In embodiments of the method, wherein use is made of a measurement device at least comprising a heater, the method comprising: - placing the sample holder containing the sample in the sample chamber; - vaporizing the sample by heating it with the heater; - ionizing the sample with the sample ionizer; - measuring, preferably simultaneously, the sample in the sample holder using the first sensor and the vaporized sample in the vacuum chamber using the second sensor; - sending a first sample property obtained by measuring the sample with the first sensor to the processor and sending a second sample property obtained by measuring the sample with the second sensor to the processor; - determining, by the processor, a characteristic of the sample based on the first sample property and the second sample property; and - outputting, by the processor, the determined characteristic
In further embodiments of the method the heater is operated based on the first sample property, e.g. wherein a temperature change of the heater, e.g. from a first temperature to a vaporizing temperature, is based on the first sample property.
In embodiments of the method, wherein use is made of a measurement device wherein the sample transfer means comprise the sample ionizer, the method comprising: - placing the sample holder containing the sample in the sample chamber; - ionizing the sample using the sample ionizer; - transferring ionized sample from the sample chamber to the vacuum chamber by applying the electric potential, - measuring, preferably simultaneously, the sample in the sample holder using the first sensor and the vaporized sample in the vacuum chamber using the second sensor; - sending a first sample property obtained by measuring the sample with the first sensor to the processor and sending a second sample property obtained by measuring the sample with the second sensor to the processor, - determining, by the processor, a characteristic of the sample based on the first sample property and the second sample property; and - outputting, by the processor, the determined characteristic
In embodiments of the method, the method further comprises cleaning the separator before placing the sample holder in the sample chamber. The separator may become contaminated with sample reducing the reliability of the device. By cleaning the separator before using the device, the reliability of the device is improved.
In embodiments of the method, the characteristic of the sample is characteristic of a chemical content of the sample, e.g. is indicative of a substance present in the sample.
The invention will be explained below with reference to the drawing in which:
Fig. 1 shows a measurement device according to a first embodiment; and
Fig. 2 shows a measurement device according to a second embodiment.
Figure 1 shows a measurement device 1 for analysis of a sample contained in a sample holder having an opening, wherein the measurement device 1 is configured to perform at least two parallel measurements on the sample. The measurements may be performed parallel and independent of each other due to the configuration of the measurement device 1.
This allows to combine two independent measurements and determine a characteristic of a sample with greater accuracy, e.g. in order to be allowed as proof in a court.
The measurement device comprises a sample chamber 3 for placing the sample holder containing the sample. The sample chamber 3 of the embodiment shown in figure 1 is shown as a protrusion in the measurement device 1. An outer wall, e.g. a closable and openable outer wall, may be provided such that the sample chamber 3 is separable from the outside once a sample holder is placed in the sample chamber 3.
The sample chamber 3 is provided adjacent to a heater 10 which is provided below a lower wall of the sample chamber 3, for heating and vaporizing the sample in the sample holder. By heating the sample in the sample holder a portion of the sample may vaporize and be transferred towards the second sensor 8 for measuring. The heater 10 may be configured to heat the sample to at least 400 °C, preferably to at least 500 °C.
The measurement device 1 further comprises a first sensor 4 for performing a measurement on the sample in the sample holder and determining a first property of the sample. The first sensor 4 is an optical sensor provided adjacent to a side wall of the sample chamber 3. The first sensor 4 may be a infrared sensor, a Raman spectroscopy sensor, an ultraviolet- visible spectroscopy sensor, or a hyperspectral spectroscopy sensor.
In the embodiment shown in figure 1, the sample ionizer 5 is provided in the vacuum chamber 6 for ionizing the vaporized sample that has been transferred to the vacuum chamber 6. The sample ionizer 5 may be embodied as an ion source provided in the vacuum chamber 6. The vacuum chamber 6 comprises a vacuum, preferably having a pressure between 10° and 107 mbar, which pressure may be monitored by a pressure gauge 11 and maintained or created by a vacuum pump 12. For example, the sample chamber 3 may be provided with an opening in a wall, e.g. an upper wall, to which the vacuum chamber 6 is connected, e.g. via the heatable separator 7.
The measurement device 1 comprises a heatable separator 7 for separating the vacuum chamber 6 from the sample chamber 3. The heatable separator is porous to the sample and may comprise a valve for controlling a leak between the sample chamber 3 and the vacuum chamber 8. The sample transfer means are configured for transferring a portion of the sample, e.g. a vaporized portion of the sample, from the sample chamber 3 to the vacuum chamber 6. For example, the heatable separator 7 may comprise a heatable membrane probe comprising a membrane and a porous metal mesh, preferably having openings with a size in the range of 10 micrometer to 100 micrometer. In another example, the heatable separator 7 may comprise comprises a heatable capillary inlet. The heatable separator 7 may be heatable to 80 °C, preferably to at least 100 °C.
In the embodiment of figure 1, the second sensor 8 of the measurement device 1 is provided in the vacuum chamber 6. The second sensor 8 is configured to perform a second measurement on the ionized, by the sample ionizer 5, and vaporized, by the heater 10, sample. The second sensor 8 is an analytical spectrometry sensor, for example a mass spectroscopy sensor, a gas chromatogram sensor, and a gas chromatogram — mass spectrum sensor.
The first sensor 4 and the second sensor 8 are connected to a processor 9 for receiving the first sample property and the second sample property. The processor 9 is configured to determine a characteristic of the sample, e.g. a chemical or molecular content of the sample, based on the first property and the second property. For example, if both the first property and the second property indicate a certain molecular content of the sample, the processor 9 may determine that the sample has this molecular content as its characteristic, whereas if either one of the first property and the second property do not indicate the molecular content, then the processor may determine that the sample does not have this molecular content as its characteristic.
The measurement device of figure 1 may be used use is in a method comprising: - placing a sample holder containing the sample in the sample chamber 3; - vaporizing the sample by heating it with the heater 10; - ionizing the vaporized sample with the sample ionizer 5; - measuring, preferably simultaneously, the sample in the sample holder using the first sensor 4 and the vaporized sample in the vacuum chamber 6 using the second sensor 8; - sending a first sample property obtained by measuring the sample with the first sensor 4 to the processor 9 and sending a second sample property obtained by measuring the sample with the second sensor 8 to the processor 9; - determining, by the processor 9, a characteristic of the sample based on the first sample property and the second sample property; and - outputting, by the processor 9, the determined characteristic.
The heater 10 may be operated based on the first sample property, e.g. wherein a temperature change of the heater 10, e.g. from a first temperature to a vaporizing temperature, is based on the first sample property.
Figure 2 shows a measurement device 1 according to a second embodiment, wherein the sample transfer means further comprises the sample ionizer 5 which is provided adjacent to the sample chamber 3. In other embodiments, the sample ionizer 5 may be provided inside the sample chamber 3. The sample ionizer 5 is configured to ionize the sample in the sample holder that is placed in the sample chamber 3. In this embodiment the heatable separator 7 comprises an ambient ionization probe for providing an electric potential to transfer the ionized sample from the sample chamber 3 to the vacuum chamber 6.
Inthe embodiment of figure 2 the sample is transferred to the vacuum chamber 6 by ionizing the, portion of, sample and then transferring the sample under the influence of an electric potential, e.g. an electric field, through the separator 7 which comprises an ambient ionization probe for providing the electric potential. For example, the ambient ionization probe may be a paperspray or an electrospray.
The measurement device 1 of figure 2 may be used in a method comprising: - placing the sample holder containing the sample in the sample chamber 3; - ionizing the sample using the sample ionizer 5; - transferring ionized sample from the sample chamber 3 to the vacuum chamber 6 by applying the electric potential, - measuring, preferably simultaneously, the sample in the sample holder using the first sensor 4 and the vaporized sample in the vacuum chamber 6 using the second sensor 8; - sending a first sample property obtained by measuring the sample with the first sensor 4 to the processor © and sending a second sample property obtained by measuring the sample with the second sensor 8 to the processor 9; - determining, by the processor 9, a characteristic of the sample based on the first sample property and the second sample property; and - outputting, by the processor, the determined characteristic.
The separator 7, or more generally the sample transfer means, may be cleaned before placing a new sample holder in the sample chamber 3 to prevent cross contamination between different samples, e.g. as a result of earlier sample sticking to the separator when a new sample is placed in the sample chamber.
EMBODIMENTS
1. Measurement device (1) for analysis of a sample contained in a sample holder having an opening, wherein the measurement device (1) is configured to perform at least two parallel, e.g. simultaneously, measurements on the sample, comprising: — a sample chamber (3) for placing the sample holder containing the sample; — a first sensor (4) for performing a first measurement on the sample in the sample holder and determining a first property of the sample, wherein the first sensor (4) is an optical sensor (4) provided adjacent to the sample chamber (3); — a sample ionizer (5) for ionizing the sample; — a vacuum chamber (8) configured for comprising a vacuum; — sample transfer means comprising a heatable separator (7) provided between the vacuum chamber (6) and the sample chamber (3), for separating the vacuum chamber (6) from the sample chamber (3), wherein the heatable separator (7) is porous to the sample, wherein the sample transfer means are configured for transferring a portion of the sample from the sample holder through the separator (7) to the vacuum chamber (6); — a second sensor (8) for performing a second measurement on ionized sample in the vacuum chamber (6) and determining a second property of the sample, wherein the second sensor (8) is an analytical spectrometry sensor (8) provided in the vacuum chamber (6); and — a processor (9) connected to the first sensor (4) and the second sensor (8) for receiving the first sample property and the second sample property and determining a characteristic of the sample based on the first sample property and the second sample property. 2. Measurement device according to claim 1, wherein the measurement device (1) comprises a heater (10) for heating and vaporizing the sample contained in the sample holder located in the sample chamber (3), wherein the heatable separator (7) is porous to the vaporized sample. 3. Measurement device according to claim 1, wherein the sample transfer means further comprises the sample ionizer (5), wherein the sample ionizer (5) is configured to ionize the sample in the sample holder, and wherein the heatable separator (7) comprises an ambient ionization probe for providing an electric potential to transfer the ionized sample from the sample chamber (3) to the vacuum chamber (6).
4. Measurement device according to one or more of the preceding claims, wherein the heatable separator (7) comprises a heatable membrane probe comprising a membrane and a porous metal mesh, preferably having openings with a size in the range of 10 micrometer to 100 micrometer.
5. Measurement device according to one or more of the preceding claims, wherein the heatable separator (7) comprises a heatable capillary inlet. 6. Measurement device according to one or more of the preceding claims, wherein the heatable separator (7) is heatable to at least 80 °C, preferably to at least 100 °C. 7. Measurement device according to one or more of the preceding claims, wherein the first sensor (4) is one of an infrared sensor, a Raman spectroscopy sensor, an ultraviolet- visible spectroscopy sensor, and a hyperspectral spectroscopy sensor.
8. Measurement device according to one or more of the preceding claims, wherein the second sensor (8) is one of a mass spectroscopy sensor, a gas chromatogram sensor, and a gas chromatogram — mass spectrum sensor. 9. Measurement device according to one or more of the preceding claims, wherein the vacuum chamber (6) is configured for having a pressure between 10° and 107 mbar. 10. Measurement device according to one or more of the preceding claims, wherein the first sensor (4) and/or the heater (10) are located adjacent a sidewall or a lower wall of the sample chamber (3). 11. Measurement device according to one or more of the preceding claims, wherein the sample holder comprises a mirror having a mirroring surface, and wherein the first sensor (4) is provided opposite the mirroring surface when the sample holder is placed in the sample chamber (3). 12. Measurement device according to at least claim 2, wherein the heater (10) is configured to heat the sample to at least 400 °C, preferably to at least 500 °C. 13. Method for parallel, e.g. simultaneous, analysis of a sample contained in a sample holder having an opening using at least two parallel measurements, wherein use is made of a measurement device (1) according to one or more of the claims 1 -12.
14. Method according to claim 13, wherein use is made of a measurement device at least according to claim 2, the method comprising: - placing the sample holder containing the sample in the sample chamber (3); - vaporizing the sample by heating it with the heater (10); - ionizing the sample with the sample ionizer (5); - measuring, preferably simultaneously, the sample in the sample holder using the first sensor (4) and the vaporized sample in the vacuum chamber (8) using the second sensor (8); - sending a first sample property obtained by measuring the sample with the first sensor (4) to the processor (8) and sending a second sample property obtained by measuring the sample with the second sensor (8) to the processor (9); - determining, by the processor (9), a characteristic of the sample based on the first sample property and the second sample property; and - outputting, by the processor (9), the determined characteristic.
15. Method according to claim 14, wherein the heater (10) is operated based on the first sample property, e.g. wherein a temperature change of the heater (10), e.g. from a first temperature to a vaporizing temperature, is based on the first sample property. 16. Method according to claim 13, wherein use is made of a measurement device at least according to claim 3, the method comprising: - placing the sample holder containing the sample in the sample chamber (3); - ionizing the sample using the sample ionizer (5); - transferring ionized sample from the sample chamber (3) to the vacuum chamber (6) by applying the electric potential; - measuring, preferably simultaneously, the sample in the sample holder using the first sensor (4) and the vaporized sample in the vacuum chamber (6) using the second sensor (8); - sending a first sample property obtained by measuring the sample with the first sensor (4) to the processor (9) and sending a second sample property obtained by measuring the sample with the second sensor (8) to the processor (9); - determining, by the processor (9), a characteristic of the sample based on the first sample property and the second sample property; and - outputting, by the processor (9), the determined characteristic.
17. Method according to one or more of claims 13 — 16, wherein the method further comprises cleaning the separator (7) before placing the sample holder in the sample chamber (3). 18. Method according to one or more of the claims 13 — 17, wherein the characteristic of the sample is characteristic of a chemical content of the sample, e.g. is indicative of a substance present in the sample.

Claims (18)

CONCLUSIESCONCLUSIONS 1. Meetinrichting (1) voor het analyseren van een monster dat in een monsterhouder met een opening is, waarbij de meetinrichting (1) is ingericht om ten minste twee parallelle, bijvoorbeeld tegelijkertijd, metingen op het monster te doen, omvattende: - een monsterkamer (3) voor het plaatsen van de monsterhouder met het monster; - een eerste sensor (4) voor het uitvoeren van een eerste meting op het monster in de monsterhouder en het vaststellen van een eerste eigenschap van het monster, waarbij de eerste sensor (4) een optische sensor (4) is die naburig aan de monsterkamer (3) is geplaatst; - een monsterioniseerder (5) voor het ioniseren van het monster; - een vacuümkamer (6) ingericht voor het omvatten van een vacuüm; - monsterverplaatsingsmiddelen omvattende een opwarmbare afscheiding (7) die tussen de vacuümkamer (8) en de monsterkamer (3) geplaatst is, waarbij de opwarmbare afscheiding (7) poreus is voor het monster, waarbij de monsterverplaatsingsmiddelen zijn ingericht om een gedeelte van het monster van de monsterhouder door de afscheiding (7) naar de vacuümkamer (6) te verplaatsen; - een tweede sensor (8) voor het uitvoeren van een tweede meting op geïoniseerd monster in de vacuümkamer (6) en het vaststellen vaneen tweede eigenschap van het monster, waarbij de tweede sensor (8) een analytische spectrometriesensor is die in de vacuümkamer verschaft is; en - een processor (9) die verbonden is met de eerste sensor (4) en de tweede sensor (8) voor het ontvangen van de eerste monstereigenschap en de tweede monstereigenschap en het vaststellen van een karakteristiek van het monster gebaseerd op de eerste monstereigenschap en de tweede monstereigenschap.1. Measuring device (1) for analyzing a sample that is in a sample holder with an opening, wherein the measuring device (1) is designed to make at least two parallel, for example simultaneously, measurements on the sample, comprising: - a sample chamber (3) for placing the sample holder with the sample; - a first sensor (4) for performing a first measurement on the sample in the sample holder and determining a first property of the sample, wherein the first sensor (4) is an optical sensor (4) adjacent to the sample chamber (3) has been posted; - a sample ionizer (5) for ionizing the sample; - a vacuum chamber (6) designed to contain a vacuum; - sample moving means comprising a heatable separation (7) placed between the vacuum chamber (8) and the sample chamber (3), wherein the heatable separation (7) is porous for the sample, wherein the sample moving means are designed to remove part of the sample from moving the sample holder through the partition (7) to the vacuum chamber (6); - a second sensor (8) for performing a second measurement on ionized sample in the vacuum chamber (6) and determining a second property of the sample, the second sensor (8) being an analytical spectrometry sensor provided in the vacuum chamber ; and - a processor (9) connected to the first sensor (4) and the second sensor (8) for receiving the first sample property and the second sample property and determining a characteristic of the sample based on the first sample property and the second monster property. 2. Meetinrichting volgens conclusie 1, waarbij de meetinrichting (1) een verwarmer (10) omvat voor het verwarmen en verdampen van het monster in de monsterhouder die in de monsterkamer (3) zit, waarbij de verwarmbare afscheiding (7) poreus is voor het verdampte monster.2. Measuring device according to claim 1, wherein the measuring device (1) comprises a heater (10) for heating and evaporating the sample in the sample holder located in the sample chamber (3), wherein the heatable partition (7) is porous for evaporated sample. 3. Meetinrichting volgens conclusie 1, waarbij de monsterverplaatsingsmiddelen verder de monsterioniseerder (5) omvatten, waarbij de monsterioniseerder (5) is ingericht voor het ioniseren van het monster in de monsterhouder, en waarbij de verwarmbare afscheiding (7) een ambient ionization probe omvat voor het verschaffen van een elektrische potentiaal om het geïoniseerde monster van de monsterkamer (3) naar de vacuümkamer (6) te verplaatsen.3. Measuring device according to claim 1, wherein the sample moving means further comprise the sample ionizer (5), wherein the sample ionizer (5) is designed for ionizing the sample in the sample holder, and wherein the heatable separation (7) comprises an ambient ionization probe for providing an electrical potential to move the ionized sample from the sample chamber (3) to the vacuum chamber (6). 4. Meetinrichting volgens een of meer van de voorgaande conclusies, waarbij de verwarmbare afscheiding (7) een verwarmbaar membraan probe met een membraan en een poreuze metalen maas omvat, bij voorkeur met openingen met een grote tussen de 10 micrometers en 100 micrometers.Measuring device according to one or more of the preceding claims, wherein the heatable separation (7) comprises a heatable membrane probe with a membrane and a porous metal mesh, preferably with openings with a size between 10 micrometers and 100 micrometers. 5. Meetinrichting volgens een of meer van de voorgaande conclusies, waarbij de verwarmbare afscheiding (7) een verwarmbare capillaire inlaat omvat.5. Measuring device according to one or more of the preceding claims, wherein the heatable separation (7) comprises a heatable capillary inlet. 6. Meetinrichting volgens een of meer van de voorgaande conclusies, waarbij de verwarmbare afscheiding (7) verwarmbaar is tot ten minste 80 °C, bij voorkeur tot ten minste 100 °C.Measuring device according to one or more of the preceding claims, wherein the heatable separation (7) can be heated to at least 80 °C, preferably to at least 100 °C. 7. Meetinrichting volgens een of meer van de voorgaande conclusies, waarbij de eerste sensor (4) een van een infrarood sensor, een Raman spectroscopiesensor, een ultraviolet- zichtbaar licht spectroscopiesensor, en een hyperspectrale spectroscopiesensor is.7. Measuring device according to one or more of the preceding claims, wherein the first sensor (4) is one of an infrared sensor, a Raman spectroscopy sensor, an ultraviolet-visible light spectroscopy sensor, and a hyperspectral spectroscopy sensor. 8. Meetinrichting volgens een of meer van de voorgaande conclusies, waarbij de tweede sensor (8) een van een massa spectroscopiesensor, een gas chromatogramsensor, en een gas chromatogram — massa spectroscopiesensor is.Measuring device according to one or more of the preceding claims, wherein the second sensor (8) is one of a mass spectroscopy sensor, a gas chromatogram sensor, and a gas chromatogram - mass spectroscopy sensor. 9. Meetinrichting volgens een of meer van de voorgaande conclusies, waarbij de vacuümkamer (6) is ingericht voor een druk tussen de 10% en 107 mbar.9. Measuring device according to one or more of the preceding claims, wherein the vacuum chamber (6) is designed for a pressure between 10% and 107 mbar. 10. Meetinrichting volgens een of meer van de voorgaande conclusies, waarbij de eerste sensor (4)en/of de verwarmer (10) naburig aan een zijwand of een onderwand van de monsterkamer (3) geplaatst zijn.Measuring device according to one or more of the preceding claims, wherein the first sensor (4) and/or the heater (10) are placed adjacent to a side wall or a bottom wall of the sample chamber (3). 11. Meetinrichting volgens een of meer van de voorgaande conclusies, waarbij de monsterhouder een spiegel met een spiegeloppervlak omvat, en waarbij de eerste sensor (4) tegenover het spiegeloppervlak geplaatst is wanneer de monsterhouder in de monsterkamer (3) geplaatst is.Measuring device according to one or more of the preceding claims, wherein the sample holder comprises a mirror with a mirror surface, and wherein the first sensor (4) is placed opposite the mirror surface when the sample holder is placed in the sample chamber (3). 12. Meetinrichting volgens ten minste conclusie 2, waarbij de verwarmer (10) is ingericht om het monster ten minste tot 400 °C, bij voorkeur tot ten minste 500 °C, te verwarmen.Measuring device according to at least claim 2, wherein the heater (10) is designed to heat the sample to at least 400 °C, preferably to at least 500 °C. 13. Werkwijze voor parallelle, e.g. gelijktijdige, analyse van een monster in een monsterhouder met een opening waarbij ten minste twee parallelle metingen worden gebruikt, waarbij gebruik wordt gemaakt van een meetinrichting (1) volgens een of meer van de conclusies 1 — 12.13. Method for parallel, e.g. simultaneous, analysis of a sample in a sample holder with an opening using at least two parallel measurements, using a measuring device (1) according to one or more of claims 1 - 12. 14. Werkwijze volgens conclusie 13, waarbij gebruik wordt gemaakt van een meetinrichting ten minste volgens conclusie 2, waarbij de werkwijze omvat: - het plaatsen van de monsterhouder met het monster in de monsterkamer (3); - het verdampen van het monster door het te verwarmen met de verwarmer (10); - het ioniseren van het monster met de monsterioniseerder (5); - het meten, bij voorkeur gelijktijdig, van het monster in de monsterhouder met de eerste sensor (4) en het verdampte monster in de vacuümkamer (6) met de tweede sensor (8); - het sturen van een eerste monstereigenschap die verkregen is door het meten van het monster met de eerste sensor (4) naar de processor (9) en het sturen van een tweede monstereigenschap die verkregen is door het meten van het monster met de tweede sensor (8) naar de processor (9); - het vaststellen, door de processor (9) van een karakteristiek van het monster gebaseerd op de eerste monstereigenschap en de tweede monstereigenschap; en - het outputten, door de processor (9) van de vastgestelde karakteristiek.Method according to claim 13, using a measuring device at least according to claim 2, wherein the method comprises: - placing the sample holder with the sample in the sample chamber (3); - evaporating the sample by heating it with the heater (10); - ionizing the sample with the sample ionizer (5); - measuring, preferably simultaneously, the sample in the sample holder with the first sensor (4) and the evaporated sample in the vacuum chamber (6) with the second sensor (8); - sending a first sample property obtained by measuring the sample with the first sensor (4) to the processor (9) and sending a second sample property obtained by measuring the sample with the second sensor ( 8) to the processor (9); - determining, by the processor (9), a characteristic of the sample based on the first sample property and the second sample property; and - outputting the determined characteristic by the processor (9). 15. Werkwijze volgens conclusie 14, waarbij de verwarmer (10) bestuurt wordt gebaseerd op de eerste monstereigenschap, bijvoorbeeld waarbij een temperatuurverandering van de verwarmer (10), bijvoorbeeld van een eerste temperatuur naar een verdampingstemperatuur, gebaseerd is op de eerste monstereigenschap.A method according to claim 14, wherein the heater (10) is controlled based on the first sample property, for example wherein a temperature change of the heater (10), for example from a first temperature to an evaporation temperature, is based on the first sample property. 16. Werkwijze volgens conclusie 13, waarbij gebruik wordt gemaakt van een meetinrichting ten minste volgens conclusie 3, waarbij de werkwijze omvat: - het plaatsen van de monsterhouder met het monster in de monsterkamer (3); - het ioniseren van het monster met de monsterioniseerder (5); - het verplaatsen van geïoniseerd monster van de monsterkamer (3) naar de vacuümkamer (6) door het toepassen van de elektrische potentiaal; - het meten, bij voorkeur gelijktijdig, van het monster in de monsterhouder met de eerste sensor (4) en het geïoniseerde monster in de vacuümkamer (6) met de tweede sensor (8); - het sturen van een eerste monstereigenschap die verkregen is door het meten van het monster met de eerste sensor (4) naar de processor (9) en het sturen van een tweede monstereigenschap die verkregen is door het meten van het monster met de tweede sensor (8) naar de processor (9);Method according to claim 13, using a measuring device at least according to claim 3, wherein the method comprises: - placing the sample holder with the sample in the sample chamber (3); - ionizing the sample with the sample ionizer (5); - moving ionized sample from the sample chamber (3) to the vacuum chamber (6) by applying the electric potential; - measuring, preferably simultaneously, the sample in the sample holder with the first sensor (4) and the ionized sample in the vacuum chamber (6) with the second sensor (8); - sending a first sample property obtained by measuring the sample with the first sensor (4) to the processor (9) and sending a second sample property obtained by measuring the sample with the second sensor ( 8) to the processor (9); - het vaststellen, door de processor (9) van een karakteristiek van het monster gebaseerd op de eerste monstereigenschap en de tweede monstereigenschap; en - het outputten, door de processor (9) van de vastgestelde karakteristiek.- determining, by the processor (9), a characteristic of the sample based on the first sample property and the second sample property; and - outputting the determined characteristic by the processor (9). 17. Werkwijze volgens een of meer van de conclusies 13 — 16, waarbij de werkwijze verder omvat het schoonmaken van de afscheiding (7) voordat de monsterhouder in de monsterkamer (3) geplaatst wordt.Method according to one or more of claims 13 - 16, wherein the method further comprises cleaning the separation (7) before the sample holder is placed in the sample chamber (3). 18. Werkwijze volgens een of meer van de conclusies 13 — 17, waarbij de karakteristiek van het monster karakteristiek is voor een chemische inhoud van het monster, bijvoorbeeld die indicatief is voor een substantie die aanwezig is in het monster.Method according to one or more of claims 13 - 17, wherein the characteristic of the sample is characteristic of a chemical content of the sample, for example indicative of a substance present in the sample.
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