WO2023217455A1 - Method to combine optical imaging spectroscopy and mass spectrometry - Google Patents

Method to combine optical imaging spectroscopy and mass spectrometry Download PDF

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Publication number
WO2023217455A1
WO2023217455A1 PCT/EP2023/057943 EP2023057943W WO2023217455A1 WO 2023217455 A1 WO2023217455 A1 WO 2023217455A1 EP 2023057943 W EP2023057943 W EP 2023057943W WO 2023217455 A1 WO2023217455 A1 WO 2023217455A1
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WO
WIPO (PCT)
Prior art keywords
sample
sensor
property
chamber
measurement device
Prior art date
Application number
PCT/EP2023/057943
Other languages
French (fr)
Inventor
Sarfarazuddin Ahmed Hashmi SYED
Cornelis GORSEL VAN
Original Assignee
Portolab B.V
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Portolab B.V filed Critical Portolab B.V
Publication of WO2023217455A1 publication Critical patent/WO2023217455A1/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

Definitions

  • the invention relates to a measurement device for determining a presence of a chemical substance in a sample contained in a sample holder having an opening, wherein the measurement device is configured to use at least two simultaneous measurements.
  • the invention further relates to a method for determining the presence of the chemical substance in the 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.
  • 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.
  • An object of the invention is to allow for faster and more reliable testing of a sample for a chemical substance.
  • 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 simultaneous and independent measurements. Each measurements relates to a respective test for testing a presence of the substance. Each of the two measurements determines a presence of the chemical substance in the sample which is received by the processor for determining the presence of the chemical substance in 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 presence of the chemical substance in the sample.
  • the measurement device is configured to determine a presence of a chemical substance in a sample that is contained in a sample holder having an opening.
  • the chemical substance may be a chemical substance provided on a list, e.g. a list provided to the measurement device.
  • 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 simultaneous measurements.
  • the measurements may be performed simultaneous to each other, meaning that the two measurements, and thus the two tests, may be performed simultaneously on the same sample.
  • 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 sample property 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.
  • 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 sample property based on optical properties of the sample.
  • the first sample property is indicative of the presence of the chemical substance.
  • 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.
  • 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 provided in the vacuum chamber for ionizing the sample.
  • 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.
  • Heating means are provided to heat the heatable separator.
  • 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 sample property.
  • the second sample property is indicative of the presence of the chemical substance.
  • 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 presence of the chemical substance 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 receiving the first sample property and the second sample property and determining the presence of a chemical substance in the sample based on the first sample property and the second sample property.
  • the presence of the chemical substance is determined when both the first sample property and the second sample property indicate the presence of the chemical substance
  • the processor may determine that the sample is or contains cocaine.
  • the processor determines that the presence of the substance inthe 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.
  • 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.
  • the heater may be a metal or ceramic heater.
  • the heater is configured such that sample may not stick to the surface thereof.
  • the heater is provided outside of the sample chamber adjacent to a wall thereof.
  • the sample ionizer may be provided to ionize the sample in the sample chamber or in the vacuum chamber.
  • the measurement device is configured to: receive the sample in the sample holder and receive the sample holder in the sample chamber; vaporize a portion of the sample with the heater and transfer the vaporized sample to the vacuum chamber with the sample transfer means; simultaneously measure the first sample property with the first sensor and the second sample property with the second sensor; and determine the presence of the chemical substance in the sample based on the first sample property and the second sample property, wherein the presence of the chemical substance is determined when both the first sample property and the second sample property indicate the presence of the chemical substance.
  • the sample transfer means further comprises a 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.
  • 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.
  • the ambient ionization probe may be a paperspray or an electrospray.
  • the separator may comprise a capillary with a diameter between 0.08mm and 0.13mm.
  • the separator may further comprise an intermediate vacuum region between the sample chamber and the vacuum chamber.
  • 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 1 mbar and 2mbar.
  • 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.
  • 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.
  • 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.
  • the heatable separator comprises a heatable capillary inlet.
  • the capillary inlet allows for a controlled leak to the vacuum chamber, allowing the sample to be transferred thereto.
  • 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.
  • 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.
  • 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.
  • 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.
  • the vacuum chamber is configured for having a pressure between 10' 5 and 10' 7 mbar.
  • 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.
  • 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.
  • 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.
  • 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.
  • 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.
  • the heater is configured to heat the sample to at least 400 °C, preferably to at least 500 °C.
  • 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.
  • 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.
  • the heater may be ramped up more to vaporize less volatile compounds.
  • the heating may be ramped up between 40 °C and 400 °C per minute.
  • the invention is further related to a method for determining a presence of a chemical substance in a sample using simultaneous measurements on the sample, wherein use is made of a measurement device according to the invention.
  • the method comprises: placing the sample holder containing the sample in the sample chamber; vaporizing a portion of the sample by heating it with the heater and transferring vaporized sample to the vacuum chamber; ionizing the vaporized sample with the sample ionizer; measuring 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 presence of a chemical substance in the sample based on the first sample property and the second sample property, wherein the presence of the chemical substance is determined when both the first sample property and the second sample property indicate the presence of the chemical substance; and outputting, by the processor, the determined presence of the chemical substance.
  • 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.
  • 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 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 presence of the chemical substance in the sample based on the first sample property and the second sample property; and outputting, by the processor, the determined characteristic
  • 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.
  • the invention further relates to a method for determining a presence of a chemical substance, e.g. a drug, at a customs, e.g. at an airport, in a sample, wherein use is made of a measurement system according to the invention and/or the method according the invention.
  • a chemical substance e.g. a drug
  • Fig. 1 shows a measurement device according to a first embodiment
  • Fig. 2 shows a measurement device according to a second embodiment.
  • Figure 1 shows a measurement device 1 for determining a presence of a chemical substance in a sample contained in a sample holder having an opening, wherein the measurement device 1 is configured to perform at least two simultaneous measurements on the sample. The measurements may be performed independent of each other due to the configuration of the measurement device 1.
  • 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 sample property.
  • 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 an infrared sensor, a Raman spectroscopy sensor, an ultraviolet- visible spectroscopy sensor, or a hyperspectral spectroscopy sensor.
  • 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' 5 and 10' 7 mbar, which pressure may be monitored by a pressure gauge 11 and maintained or created by a vacuum pump 12.
  • 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 6.
  • 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.
  • 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.
  • 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.
  • 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 presence of a chemical substance in 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, 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.
  • 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 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 presence of the chemical substance in the sample based on the first sample property and the second sample property; and outputting, by the processor 9, the determined presence.
  • 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, wherein the sample transfer means further comprises the sample ionizer 5 which is provided adjacent to the sample chamber 3.
  • 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.
  • 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.
  • 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.
  • an electric potential e.g. an electric field
  • 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 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
  • 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.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Sampling And Sample Adjustment (AREA)

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

METHOD TO COMBINE OPTICAL IMAGING SPECTROSCOPY AND MASS SPECTROMETRY
The invention relates to a measurement device for determining a presence of a chemical substance in a sample contained in a sample holder having an opening, wherein the measurement device is configured to use at least two simultaneous measurements. The invention further relates to a method for determining the presence of the chemical substance in the 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 allow for faster and more reliable testing of a sample for a chemical substance.
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 simultaneous and independent measurements. Each measurements relates to a respective test for testing a presence of the substance. Each of the two measurements determines a presence of the chemical substance in the sample which is received by the processor for determining the presence of the chemical substance in 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 presence of the chemical substance in the sample.
The measurement device is configured to determine a presence of a chemical substance in a sample that is contained in a sample holder having an opening. The chemical substance may be a chemical substance provided on a list, e.g. a list provided to the measurement device. 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 simultaneous measurements. The measurements may be performed simultaneous to each other, meaning that the two measurements, and thus the two tests, may be performed simultaneously on the same sample.
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 sample property 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 sample property based on optical properties of the sample. The first sample property is indicative of the presence of the chemical substance. 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 provided in the vacuum chamber for ionizing the sample. 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. Heating means are provided to heat the heatable separator.
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 sample property. The second sample property is indicative of the presence of the chemical substance. 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 presence of the chemical substance 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 receiving the first sample property and the second sample property and determining the presence of a chemical substance in the sample based on the first sample property and the second sample property. The presence of the chemical substance is determined when both the first sample property and the second sample property indicate the presence of the chemical substance 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 presence of the substance in the sample, the processor determines that the presence of the substance inthe 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. 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.
The measurement device is configured to: receive the sample in the sample holder and receive the sample holder in the sample chamber; vaporize a portion of the sample with the heater and transfer the vaporized sample to the vacuum chamber with the sample transfer means; simultaneously measure the first sample property with the first sensor and the second sample property with the second sensor; and determine the presence of the chemical substance in the sample based on the first sample property and the second sample property, wherein the presence of the chemical substance is determined when both the first sample property and the second sample property indicate the presence of the chemical substance.
In embodiments of the measurement device, the sample transfer means further comprises a 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 1 mbar 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 10'5 and 10'7 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 determining a presence of a chemical substance in a sample using simultaneous measurements on the sample, wherein use is made of a measurement device according to the invention.
In embodiments of the method, the method comprises: placing the sample holder containing the sample in the sample chamber; vaporizing a portion of the sample by heating it with the heater and transferring vaporized sample to the vacuum chamber; ionizing the vaporized sample with the sample ionizer; measuring 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 presence of a chemical substance in the sample based on the first sample property and the second sample property, wherein the presence of the chemical substance is determined when both the first sample property and the second sample property indicate the presence of the chemical substance; and outputting, by the processor, the determined presence of the chemical substance.
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 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 presence of the chemical substance in 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.
The invention further relates to a method for determining a presence of a chemical substance, e.g. a drug, at a customs, e.g. at an airport, in a sample, wherein use is made of a measurement system according to the invention and/or the method according the invention.
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 determining a presence of a chemical substance in a sample contained in a sample holder having an opening, wherein the measurement device 1 is configured to perform at least two simultaneous measurements on the sample. The measurements may be performed independent of each other due to the configuration of the measurement device 1.
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 sample property. 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 an infrared sensor, a Raman spectroscopy sensor, an ultraviolet- visible spectroscopy sensor, or a hyperspectral spectroscopy sensor.
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 10'5 and 10'7 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 6. 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 presence of a chemical substance in 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, 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.
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 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 presence of the chemical substance in the sample based on the first sample property and the second sample property; and outputting, by the processor 9, the determined presence.
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, 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.
In the 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 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 presence of a chemical substance in the sample based on the first sample property and the second sample property; and - outputting, by the processor, the determined presence.
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.

Claims

1. Measurement device (1) for determining a presence of a chemical substance in a sample contained in a sample holder having an opening, wherein the measurement device (1) is configured to perform at least two simultaneous measurements on the sample, wherein the measurement device comprises:
- 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 measuring a first sample property indicative of the presence of the chemical substance in the sample, wherein the first sensor (4) is an optical sensor (4) provided adjacent to the sample chamber (3);
- a vacuum chamber (6) configured for comprising a vacuum;
- a sample ionizer (5) for ionizing the sample provided in the vacuum chamber;
- 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), wherein heating means are provided for heating the separator;
- 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.
- a second sensor (8) for performing a second measurement on ionized sample in the vacuum chamber (6) and measuring a second sample property indicative of the presence of the chemical substance in 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 the presence of a chemical substance in the sample based on the first sample property and the second sample property, wherein the measurement device is configured to: receive the sample in the sample holder and receive the sample holder in the sample chamber; vaporize a portion of the sample with the heater and transfer the vaporized sample to the vacuum chamber with the sample transfer means; simultaneously measure the first sample property with the first sensor and the second sample property with the second sensor; and determine the presence of the chemical substance in the sample based on the first sample property and the second sample property, wherein the presence of the chemical substance is only determined when both the first sample property and the second sample property indicate the presence of the chemical substance.
2. Measurement device according to claim 1, 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.
3. Measurement device according to one or more of the preceding claims, wherein the heatable separator (7) comprises a heatable capillary inlet.
4. 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, by the heating means.
5. 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.
6. 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.
7. Measurement device according to one or more of the preceding claims, wherein the vacuum chamber (6) is configured for having a pressure between 10'5 and 10'7 mbar.
8. 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).
9. 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).
10. 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.
11. Method for determining a presence of a chemical substance in a sample using simultaneous measurements on the sample, wherein use is made of a measurement device (1) according to one or more of the claims 1 - 10.
12. Method according to claim 11, comprising: placing the sample holder containing the sample in the sample chamber (3); vaporizing a portion of the sample by heating it with the heater (10) and transferring vaporized sample to the vacuum chamber; ionizing the vaporized sample with the sample ionizer (5); measuring 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 the first sample property obtained by measuring the sample with the first sensor (4) to the processor (9) and sending the second sample property obtained by measuring the sample with the second sensor (8) to the processor (9); determining, by the processor (9), a the presence of the chemical substance in the sample based on the first sample property and the second sample property, wherein the presence of the chemical substance is determined when both the first sample property and the second sample property indicate the presence of the chemical substance; and outputting, by the processor (9), the determined presence.
13. Method according to claim 12, 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.
14. Method according to one or more of claims 11 - 13, wherein the method further comprises cleaning the separator (7) before placing the sample holder in the sample chamber (3).
15. Method for determining a presence of a chemical substance, e.g. a drug, at a customs, e.g. at an airport, in a sample, wherein use is made of a measurement system according to one or more of the claims 1 - 10 and/or the method according one or more of the claims 11 - 14.
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