flow regulation system to maintain a stable gas flow, groupings of flow regulation system method to

专利摘要:
FLOW REGULATION SYSTEM TO MAINTAIN A STABLE GAS FLOW, GROUPING FLOW REGULATION SYSTEMS, METHOD FOR MEASURING A FLOW WITH THE USE OF A FLOW REGULATION SYSTEM, DEVICE FOR MONITORING COMPOUNDS TRANSPORTED BY AIR IN THE AIR IN THE AIR IN THE AIR. A GASEOUS PHASE AS A PARTICLE PHASE, AND METHOD FOR THE DETECTION OF ANALYTES TRANSPORTED BY AIR IN AN AIR FLOW THROUGH THE USE OF THE MONITORING DEVICEIt is a flow regulation system to maintain a stable air flow comprising at least one pump, a mass flow sensor, an ambient temperature sensor, an ambient pressure sensor, a temperature compensation sensor that measures the temperature of said mass flow sensor and a control system, as well as a method to measure a flow using said flow regulation system, a device for monitoring airborne components present in the air both in a gas phase as well as in a particle phase, in which it comprises a sampling device, an enrichment collector 1, a calibration and tuning module, a raw block module, said flow regulation system, a chromatography unit and a detection unit and a method for detecting airborne compounds in an air flow using said monitoring device.
公开号:BR112012021866A2
申请号:R112012021866-2
申请日:2011-03-01
公开日:2020-07-07
发明作者:Gunnar Skarping；Marianne Dalene
申请人:Provtagaren；
IPC主号:

专利说明:

FLOW REGULATION SYSTEM TO MAINTAIN A STABLE GAS FLOW, GROUPING FLOW REGULATION SYSTEMS, METHOD FOR MEASURING A FLOW USING A FLOW REGULATION SYSTEM, COMPOUND MONITORING DEVICE TRANSPORTED BY AIR PRESENT IN THE AIR BOTH IN A GASEOUS PHASE AS IN A PARTICULAR PHASE, AND, METHOD FOR THE DETECTION OF ANALYTES CARRIED BY AIR IN AN AIR FLOW BY USING THE MONITORING DEVICE
FIELD OF THE INVENTION The present invention relates to a flow regulation system to maintain a stable air flow comprising at least one pump, a mass flow sensor, an ambient temperature sensor, an ambient pressure sensor, an temperature compensation sensor that measures the temperature of said mass flow sensor and a control system and a method for measuring an air flow using said flow regulation system. The present invention also relates to a monitoring device for monitoring airborne compounds present in both the gas phase and the particle phase, in which it comprises a sampling device, an enrichment collector, a tuning and calibration module , a raw block module, said flow regulation system, a chromatography unit and a detection unit and a method for said detection.
BACKGROUND OF THE INVENTION There is a clear demand for monitoring airborne compounds that can have health effects on exposed individuals. There is great interest for compounds that have occupational exposure limit values, defined by government bodies, to ensure that the levels of such compounds are satisfactorily low. In many cases, it is not known what air contaminants consist of and, for that reason, it is of interest to learn more details about the nature of these “unknown” compounds and to reveal the identity of the most prevalent compounds. Another field of interest is to study and verify the effect of measures to reduce these levels in the air, for example, to verify the effectiveness of “true” ventilation or other measures to control air levels. Devices for this purpose can also be used for monitoring the quality of compressed air and air in respiratory protection devices. Other fields of application for such devices are, for example, the control of different volatile compounds present in the food. Such compounds can be used as markers for the degradation of certain food components or to monitor raw materials to ensure satisfactory quality. Such devices can also be used to ensure that other compounds have not contaminated the food. In hospitals, such devices can be used to check air levels of, for example, narcosis gases and to ensure that staff, patients or others are not exposed to toxic levels. Chemical fighting agents are compounds that need to be checked in order to reveal their presence and to ensure that individuals are not exposed.
In environmental analysis, there is a need to monitor air quality in cities, public places and in nature. One purpose is to obtain background data for statistical studies and to verify that the levels are below the levels defined by international and national bodies. They can also be used to check whether the emission of industrial pollutants results in exposure to nature or populated areas. The data obtained can have an impact on the decisions and interpretation of a certain situation. There is, therefore, a demand for satisfactorily high data quality.
There are many examples of air pollutants that occur in both the particle and gas phases. Of particular interest are fractions of size that have the ability to reach the lower respiratory tract. There are reasons to believe that toxicology is different depending not only on chemistry as such, but also on the distribution in different target organs in the human body. There is a need to know more about exposure to the fraction of respirable particle present in the air.
Numerous devices exist for monitoring airborne compounds and there is a wide variety of technology used. In principle, devices can be grouped into selective and non-selective devices. Non-selective devices provide a response to several compounds and do not differentiate between two or several compounds and can also result in false positive results. Such devices are still used today, possibly due to the low cost. In many applications, false-positive results can result in a high cost for the user, if costly measures are taken from invalid data.
Selective devices provide an answer for a selected compound or group of compounds. Other compounds present do not interfere with the result. The frequency of false-positive results will be much less compared to non-selective monitoring. The quality of the data obtained is essential. The typical factors that describe the quality of the data are: repeatability, reproducibility, linearity (characteristics of calibration graph with intercept and background), limit of detection and limit of quantification. Additionally, knowledge of the interference of other compounds is necessary. It needs to be mentioned that a particular compound can influence the result even if the compound itself does not give rise to a response.
Similar techniques for the detection of airborne compounds involve the use of, for example, photoionization detectors (PID, Thermo Scientific, Franklin, MA, USA), flame ionization detectors (FID, Thermo Scientific, Franklin, MA, USA ), infrared (IR) detectors, portable gas chromatography (GC) -PID (PID Analyzers, Pembroke MA, USA), portable GC mass spectrometers (MS, Inficon Inc., New York, USA), GC-DMS ((Differential Mobility Spectrometry), Sionex Inc., Bedford, MA, USA). All techniques provide an answer for a certain analyte, but in order to know the concentration the answer needs to be translated into concentration using information from a more or less sophisticated calibration curve. For many of the above techniques, the response varies with time due to aging, detector contamination (reduces the signal) and other variables.
The GC-DMS technique mentioned above is used in the MicroAnalyser instrument (Sionex Inc., Bedford, MA, USA). The GC-DMS technique is based on the separation of GC, in relation to the volatility of the compound, in combination with the separation in a DMS sensor, in relation to other molecular properties such as shape, size, charge, etc.
There are several disadvantages with the present types of instruments. For PID and FID, the identification of individual chemicals is not possible. The PID and FID detectors measure the sum of VOCs (Volatile Organic Compounds). Infrared detectors have problems with inferences. IR detectors cannot be used when monitoring VOCs at a low concentration when other interfering compounds are present.
For direct monitoring using GC-PID (eg VOC71M from Environment sa; www.environnementsa.com) and the GC-DMS instrument (eg Sionex Inc., Bedford, MA, USA) there are limitations that lead to imprecise identification and quantification of analytes and the pre or post complementary external calibration has to be done. For existing products, it is not possible to carry out calibration automatically in the field. In addition, there are problems with the occurrence of a non-linear relationship between the sampling time and determined concentrations, which thereby disables long-time sampling if the quantity exceeds the calibration range. Furthermore, when a volume is collected it needs to be calibrated to a volume and volumetric and possibly corrected for the ambient temperature and air pressure. Sampling a volume in a certain sample volume container or in a sorbent followed by thermal desorption (in the case of a sorbent) and subsequently injecting the compounds collected in the GC the chromatography peaks will be enlarged so that the resolution of the chromatography will be affected.
Another problem in known techniques is to analyze different analytes with a large difference in concentration. The compounds that were introduced to the sampling system cause transport problems and memory effects to samples that are analyzed. In fact, there is no practical way to guarantee that the estimated concentration is true, if not a sample that represents the baseline or the bottom or the raw block that is analyzed before and after the actual sample of the environment is collected.
Another important parameter in this area is the gas flow containing the compound to be detected, that is, the analyte, in the apparatus used for the detection. During the sampling of compounds in the air it is important to have the ability to control and record the flow and volume of the acquired amount of air through the sampling device as there is a direct correlation between the levels in a sample and the volume of air collected. Taking several samples simultaneously is also important for three reasons, more precisely to increase the accuracy of a certain sample, to detect erroneous samples and to acquire different compounds simultaneously. When manipulating the sampling results, it is also important to be able to track how the sample was collected, time, flow, temperature, pressure and humidity.
Existing solutions to maintain a steady flow during sampling do not show to maintain a steady flow over time and require filter calibration. The flow rate needs to be calibrated before and after sampling to ensure that the sample rate is correct and has not changed over time. A registration feature is also often missing.
An existing solution tried is the SKC AirChek pump (see www.skcinc.com), where a differential pressure sensor indicates whether a change in flow system back pressure has occurred and adjusts the pump control signal to compensate for this. However, this solution has been shown to provide deviation errors over time and a calibration with an external flow meter is required in order to set a certain flow rate for your pump.
Another existing solution is the Casella Apex pump system (see www.casellameasurement.com). It has a registration function, an ability to transfer recorded data to a PC and the ability to control the flow through a display and buttons. The inventors behind the present invention conducted tests on these pumps in 2006 and the results did not agree with their specifications, as the pumps were unable to maintain a steady flow as a sampler inducing a particular back pressure was connected to them. For samplers with high back pressure, Casella Apex did not work at all.
A problem with existing pump systems is that the flow sensors incorporated in them can fluctuate with the temperature of the flow sensor electronics. Most flow sensors, using different techniques for the actual measurement of gas flow, have an output voltage signal that corresponds to the measured flow. The output signal is, however, easily affected by the temperature of the electronic components in the flow sensor.
An additional problem with the existing devices for the detection of airborne compounds is the occurrence of a memory effect in the system in view of different analyte compounds and also other compounds of no interest to detect which have passed through the system. This phenomenon gives rise to inaccurate and erroneous detection results. The instrumentation is, in most cases, completely flexible and a pipe needs to be connected from the measurement site to the instrumentation. The piping can in many cases be long and contain a certain volume. To obtain representative samples that are introduced into the instrument and the sampling device, the volume needs to be rinsed with several more volumes compared to the volume of the pipes.
In view of this, there is a great demand for an improved direct monitoring device for the detection of airborne compounds or analytes and for an improved method for the detection of such compounds or analytes.
There is also a high demand for an improved pump for the monitoring device for the aforementioned detection of airborne compounds, a pump that has the ability to deliver the proper pumping performance required for accurate measurements.
SUMMARY OF THE INVENTION An objective of the invention is to eliminate the problems mentioned above and to provide a device and a method for the improved detection of airborne analytes in different locations of interest.
According to the present invention, this objective is achieved by means of a monitoring device including a flow regulation system, a method for the detection of airborne analytes as defined in the independent claims and a method for measuring a flow with the use of said flow regulation system. Useful modalities are defined in the dependent claims.
According to one aspect, the present invention relates to a flow regulation system to maintain a stable air flow comprising at least one pump, a mass flow sensor, an ambient temperature sensor, a pressure sensor environment, a temperature compensation sensor that measures the temperature of said mass flow sensor and a control system. The input of the sensors mentioned above to the control system is adapted to regulate said at least one pump to maintain a stable mass flow.
According to another aspect, the present invention relates to a monitoring device for the detection of airborne compounds present in an air flow in both a gas phase and a particle phase, in which it comprises a sampling device , an enrichment collector, a tuning and calibration module, a raw block module, said flow regulation system,
a chromatography unit and a detection unit.
According to a further aspect, the present invention relates to a method for detecting airborne analytes using the monitoring device according to the present invention, comprising the following consecutive steps; a) one or more different calibration and tuning modules containing different analyte references are inserted into the monitoring device, b) the air flow containing the airborne analytes and a reagent are introduced into the sampling device to be reacted with each other the other in the same, Cc) the sampling device that contains the sampling tube, the filter and the sorbent or the first sorbent, the filter and the second sorbent, is heated in order to release the analytes absorbed in the sampling device, d) the analytes released from said sampling device are collected in one or more enrichment collectors, e) the analytes are subjected to a chromatography step, f) the analytes are detected quantitatively and qualitatively.
According to a still further aspect, the present invention relates to a method for measuring a flow using said flow regulation system according to the previous one. The method comprises the steps of: measuring the mass flow with the mass flow sensor, measuring the temperature of the mass flow sensor using the said temperature compensation sensor, adjusting the mass flow measurement value of according to a predetermined calibration of the temperature-related error and the measurement signal of said temperature compensation sensor, calculate a volumetric flow of said mass flow measurement using the measured mass flow and the ambient temperature, the ambient pressure . The calculation of the volumetric flow is performed using the said measured values of mass flow, ambient temperature and ambient pressure and the law of ideal gases.
The back pressure sensor allows real-time monitoring of how the air sampling is proceeding and is recorded to present sampling quality information. In addition, the back pressure sensor and / or the mass flow sensor allow the monitoring of the flow pulsation characteristics. Thereafter, the flow pulse can be reduced by introducing a device that induces a cancellation pulse.
The flow regulation system can be stacked or be part of a group of flow regulation systems to validate the collection of air samples. With several stacked flow regulation systems, simultaneous sample collection can be performed. When two of said flow regulation systems are used simultaneously, where one of said systems has, for example, half the flow rate of the other, the rupture or overload of the samples can be assessed.
BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 shows a flow chart of an embodiment of the method according to the present invention.
Figures 2 to 5 show four different modalities of the sampling tube connected to one or more enrichment collectors in the monitoring device according to the present invention.
Figure 6A shows an embodiment of a particle size selective sampling device according to the present invention.
Figure 6B shows in detail the impactor 13 of the sampling device shown in Figure 6A.
Figure 7 shows an embodiment of the calibration and tuning device in the monitoring device according to the present invention.
Figures 8A and 8B show in detail a modality of the gas flow regulation system and the computer-controlled pump in the monitoring device according to the present invention.
Figure 9 shows an example of a sampling sequence used in the method according to the present invention.
Figure 10 shows GC-DMS chromatograms of a sampling sequence.
Figure 11 shows the GC-DMS responses of repeated benzene measurements.
Figure 12 shows the temperature response of a thermal differential flow sensor. DETAILED DESCRIPTION OF THE DIFFERENT MODALITIES OF THE
INVENTION The present inventors have eliminated or reduced the problems mentioned above in connection with known techniques in the area of detection of airborne compounds in different environments by the provision of the monitoring device and the method for the detection of airborne analytes according to present invention.
the analytes of interest to detect are generally: Solvents: 1,2,3-trimethylbenzene, 1,2,4-trimethylbenzene, 1,3,5-trimethylbenzene, l-butanol, l-butanone, 27 methylnaphthalene, 4- methylbenzaldehyde, acetone, acetonitrile,
Acetophenone, Acetaldehyde, Acetylene, Benzaldehyde, Benzene, Bromomethane, COS (Carbonyl Sulphide), Cyanuric Acid, Cyanogen Chloride, Cyclohexane, Decane, Dichloromethane, Dimethyl Ether, DIMP, DMMP, DPM, Ethanol, Ethyl Acetate , Fluroetano 1112 / Freon l134a, Freon 22 CFFM, Freonl52a, Hexadecane, Hexanal, Hexane, Hydrochloric Acid, Isobutylene, Isopropanol, m-xylene, Methanol, Methyl Acetate, Methylcyclohexane, MES (Methyl Ethyl Sulfide), Salicylate , Nitric Dioxide, Nonanal, o-xylene, Octamethylcyclotetrasiloxane, Octane, Pp-xylene, Pentamethyldiethylenetriamine, Pentane, Styrene, Sulfur Dioxide, TBM (tert-Butyl Mercaptano), Tetraline, tetrahydro thiophene, toluene, tridecane.
Tris (l-chloro-2-propyl) phosphate, Urea and compounds containing functional groups such as: isocyanates, isothiocyanates, amines, aldehydes, ketones, ethers, esters, phenolics, etc.
Explosives: AN, DNT, EGDN, TATP, oOo-MNT, DMNB, p-MNT, NG, HMTD, RDX / C4, TNT, PETN, Tetril Chemical fighting agents: VX, GA (Tabun), GB (Sarina), GD (Soman), GF (Ciclosarina), HD (Sulfur Mustard), L (Levisite), HN3 (Nitrogen Mustard), AC (Hydrogen Cyanide), CK (Cyanogen Chloride), but, in principle, any compound present in an air flow is possible to be detected by the use of the present invention, as long as it can be captured in the sampler.
The term "analyte" used throughout the order text must mean the specific compound or group of compounds to be detected in the air flow analyzed.
The term "sample compound" or "analyte compound" could also be used as a synonym.
The present invention is useful within the military, petroleum industry, chemical industry, oil industry, plastics industry, aviation industry, food industry, cosmetics industry, respiratory protection device industry, related to environmental analysis, environmental work analysis, quality control and as an alarm instrument, particularly within environmental and environmental work applications, but is in principle useful within any area where airborne compounds are harmful to health or disadvantageous for any other reason they are suspected of being present.
Figure 1 shows schematically an embodiment of the method according to the present invention. An air sample is introduced through the sample inlet into a sampling device. A raw block is also introduced into the sampling device via a raw block input. The analytes are collected in the sampling device and are then subjected to thermal desorption, in which they emit the sampling device and are transported to an enrichment collector. After an additional thermal desorption step, the analytes emitted from the enrichment collector and are then separated - “chromatographically. Then, the analytes are ionized and passed through an ion filter, followed by a quantitative and qualitative detection step.
An inlet must be present that delivers air or atmosphere to the sampling device. The delivery must deliver a defined air flow from the sampling atmosphere through the sampling device. The entrance can be a heated capillary vessel that minimizes the surface interaction between the capillary walls and the analyte during the transport of the air to be analyzed for the sampling device. Optionally, the inlet can be provided with a tubular device attached to the inlet opening in order to facilitate sampling in areas where it is difficult to arrange the monitoring device in a location where a reliable air flow measurement is obtained, for example example, when the air flow is at a distance from the monitoring device. One or several transfer lines or piping can be attached to the instrument or the sampling device. The monitoring device according to the present invention comprises a sampling device for sampling the analytes in the air flow introduced into the monitoring device. An effective and controlled sampling of both the gas and the particles in the air flow is required. The sampling device according to the present invention has the ability to differentiate between the analyte present in the gas phase and / or in the particle phase of the air flow. A similar sampling device (EasySampler) that has this differentiation capability is disclosed in WO 00/75622 and US-2006-0239857 (Gunnar Skarping & Marianne Dalene). With reference to Figures 2 to 5, four different modalities involving the sampling device will be revealed below.
In a first embodiment, a sampling tube 8, also called a denudator, is used to collect analytes in the gas phase of an air flow 2 introduced at the entrance of the monitoring device and a filter 5 is used to collect analytes in the particle phase of said air flow 2. As seen from Figure 2, the filter 5 is arranged below and connected to the sampling tube 8 in such a way that the air flow 2 passes through the sampling tube 8 first and then continue through the filter 5. Simultaneously with the introduction of the air flow 2 to analyze a flow a reagent 3 is pressed through a separate inlet to and through the sampling device. During the sampling step, the analytes in the gas phase of the air stream 2 are absorbed into the wall of the sampling tube 8 and are reacted there with the introduced reagent. The sampling device may also contain a carrier 4 for the collection of gas phase analytes. Said reagent is a volatile compound that reacts with the reactive analyte and protects it from further degradation. The reaction product will then be analyzed and thermally desorbed. For example, if the analytes are isocyanates, the reagent is DBA (di-n-butylamine) or another type of secondary amine. The particles that carry analytes are not collected in the sampling tube 8. Instead, the analytes in the particles that passed through the sampling tube 8 and reached the filter 5 react with its present reagent and are collected in said filter 5. The said particles are then captured in filter 5. An absorbent 6 is disposed below and is connected to filter 5 to collect the gas phase analytes that were emitted from the particles captured in filter 5. After the sampling step (10 seconds to several hours) a thermal desorption step of the different parts of the sampling device (sampling tube 8, filter 5, absorbent 6) is carried out (50 to 400 ºC, 10 seconds to hours, heated with an electric resistance heater or peltier element or microwave heating), in which the analytes are released from each of said parts of the sampling device. In order to determine the analyte concentration or gas and particle concentration separately, thermal desorption according to a first modality is performed for the sampling tube 8, the filter 5 and the sorbent 6 separately, as shown in Figure
2. The analytes emitted from the different parts of the sampling devices during the thermal desorption step are transported through exits from each of the said patches of the sampling device through a pipe / duct / tube 9 and are then , captured in a focusing collector 1, respectively, as shown in Figure 2.
In order to determine the total analyte concentration, thermal desorption is, according to a second modality, performed for the entire sampling device and the analytes released from the different parts of the sampling device are transported via an outlet 7 at the bottom of the sorbent 6 for an enrichment collector 1 by means of a conduit 9, as shown in Figure 3. According to a third embodiment shown in Figure 4, a tubular sorbent 10 is used instead of the sampling device 8 for the collection of analytes in the gas phase of air flow 2. Thus, the sampling device in this third modality comprises both a first sorbent 10 and a second sorbent 6. Otherwise, the action of the sampling device according to said third modality corresponds to that according to the first modality. In addition, according to a fourth embodiment shown in Figure 5, the total analyte concentration in the entire sampling device can be determined in a manner corresponding to that revealed in the second embodiment.
Figures 2 and 3 show the sampling of reactive compounds (for example, isocyanates) that are derivatized into stable derivatives. After sampling, the analytes are thermally desorbed and transferred to the enrichment collector. After capture in the enrichment collector, the compounds are thermally desorbed and injected into the chromatographic column. In Figure 3, the analytes in the different sampler parts 8, 5 and 6 are analyzed together and the sum of all analytes is analyzed in a chromatographic run. In Figure 2, the analytes in the different sampler parts 8, 5 and 6 are analyzed separately. The information is obtained in relation to the analyte in the gas phase and in the particle phase. In addition, data are obtained for the analytes that escaped the samples in filter 5 by analyzing the sorbent 6. In Figures 4 and 5 sampling is shown for non-reactive compounds such as benzene, toluene, etc. After sampling, the analytes are thermally desorbed and transferred to the enrichment collector. After capture in the enrichment collector, the compounds are thermally desorbed and injected into the chromatographic column. In Figure 5 the analytes in the different parts of sampler 8, 5 and 6 are analyzed together and the sum of all analytes is analyzed in a chromatographic run. In Figure 5 the analytes in the different parts of sampler 8, 5 and 6 are analyzed separately. The information is obtained in relation to the analyte in the gas phase and in the particle phase. Additionally, the data are obtained in relation to the analytes that escaped the samples in the filter 5 by analyzing the sorbent 6.
In Figure 6A, an example of a particle size selective sampling device according to the present invention for airborne compounds is presented. A pre-selector 11 is arranged at the entrance of the sampling device in order to remove large particles, typically having a diameter greater than 100 nm. The pre-selector 11 has the purpose of removing the large particles preventing them from entering the denudator 8 (sampling tube) of the sampling device. The direction of flow in the preselector 11 is changed and the large particles will settle in the preselector 11. A carrier 4 in denudator 8 collects the gas phase compounds.
For example, isocyanates, denudator 8 is covered on the inside with a glass filter coated with a mixture of acetic acid and di-n-butylamine (DBA). isocyanates are reacted effectively with DBA to establish urea derivatives and are collected in denudator 8. An impact plate 13 is arranged in series with the purpose of separating (cutting) particles larger than inhalable (<100 nm) or breathable (< 4 a). The separated particles that pass through the 13: 4 tube are collected in a filter 12. As shown in Figure 6B, the flow passes through a 13: 1 cone with a small nozzle 13.2 to accelerate the linear flow.
The flow current is directed to a 13: 3 impact plate to capture said particles.
The 13: 3 impact plate can be a small plate in which the particles collide and are deposited and retained.
Alternatively, the 13: 3 impact plate is connected to a 13: 4 tube that has a small flow, about 1/5 to 1 / 1,000 or typically 1/10 of the main flow, to separate particles larger than the cut size main flow current.
In addition, in series, there is a filter 5 arranged to collect inhalable or breathable particles.
Such inhalable or breathable particles are effectively collected in said filter 5 (for example, 0.4 µm). In one embodiment, said filter 5 is impregnated with DBA-acetic acid.
During sampling, filter 5 is rinsed with DBA which is evaporated from denudator 8. Effective derivation of isocyanates is made possible by this.
Impactor 13 is described here for isocyanates.
It can also be used for airborne organic and inorganic compounds that are transported by particle.
In addition, it can be modified to separate other fractions of size <100 µm.
The particle size selective sampling device is described here as an independent sampler, but it can also be an integrated part of direct reading instrumentation.
The present particle size selective sampling device is useful as the sampling device in the monitoring device according to the present invention. Furthermore, as the particle size selective sampling device alone is not known before, the present invention also relates to the device itself.
The monitoring device according to the present invention also comprises a calibration and tuning module, which is attachable and detachable from the monitoring device. Said calibration and tuning module can be present in a cassette that contains one or more different reference compounds in view of the analytes to be detected. When desired, this module can be replaced by a new module with the same or other reference compounds.
It is well known that all electronic monitoring devices need to be calibrated at the factory and in the field the calibration needs to be validated. The monitoring devices in the known techniques are devoid of a calibration function or require complicated and costly calibration measures, for example, the GC-DMS instrument mentioned above from Sionex. Calibration is performed by analyzing the raw blocks and reference standards at different levels of concentration.
The calibration and tuning device according to the present invention requires little user intervention. During calibration mode, the computer connected to the calibration and tuning device manages flow values, timings and data analysis automatically. In the few steps where user interaction is required, the user will be guided through an easy-to-use graphical interface, explaining each step. An advanced calibration mode in which the user has full control over the calibration parameters is also available. Together with the factory calibration, calibrations and continuous tuning will ensure that the calibration data will be available to convert non-linear data into a linear result as long as the relationship between the non-linear data and the result is strictly monotonic within the relevant range. This conversion will take place in the software of the computer involved.
During the calibration step, a defined concentration and a defined volume mass of a relevant calibration compound are delivered from the calibration and tuning module to the sampling device and this is done several times in order to check for any deviations.
Referring to Figure 7, which shows a part of a modality of the calibration and tuning module, said module contains a closed unit, preferably a cylindrical or tubular unit, for example, a permeation tube that is typically made of silicone, teflon or another type of inert permeable polymer, which contains one or more reference compounds in gaseous form or in the form of a liquid or a solution. Said unit has an entrance and an exit and is surrounded, preferably concentrically, by a heating device and during the heating of said unit, said one or more reference compounds are released at a defined rate and penetrate through the walls of the unit closed.
There are several solutions for electronically identifying the closed unit of the calibration and tuning module. One solution is to have an integrated circuit that contains logic that can provide a unique ID for the container. There can also be several electrical resistances, through which a voltage is measured when connected to the main controller.
A series of voltages provides the module with a unique identification.
For quantitative calibration, the module is characterized by its ability to deliver a certain amount of the compound per unit of time.
By varying the temperature, the amount per unit of time released is affected.
When introduced to the enrichment collector the amount that is captured is dependent on the time and temperature of the calibration device.
The expression “calibration and tuning module” used throughout this application means that said module has the ability to calibrate, for quantitative measurements, the monitoring device with reference compounds and to tune the monitoring device against specific analytes in a measurement location, where the monitoring device recognizes the specific analyte and focuses and adjusts the detection parameters in such a way that the measurement of said specific analyte becomes more accurate and reliable than otherwise.
Said tuning is regulated by a computer.
More precisely, the detector parameters, for example, for DMS equipment, such as the RF voltage and the compensation voltage, need to be optimized.
Also, the retention time in a GC column needs to be optimized.
The tuning is carried out by introducing reference standards to the sampling device or direct to the detection unit, for example, DMS sensor. the software that controls tuning on the computer can predict the result for the specific compound in question.
The forecast can be made from the factory calibration or from previous tunings.
When sampling the tuning module, the forecast will be tuned to a new calibration by the sampling result.
The present invention relates to a flow regulation system as defined in claim 1 as well as a monitoring device comprising said flow regulation system.
Said air flow regulation system comprises, among others, a computer that regulates the pump, a mass flow sensor for the gas to be analyzed, a temperature sensor and a pressure sensor, in which said inputs sensors for said computer regulates said at least one pump to maintain a steady mass flow.
This until now had not been possible with the known instruments and devices used in the art.
A defined and stable volumetric gas flow reduces errors derived from the flow rate.
This could also, according to the present invention, be accomplished by a conventional flow regulation system that is different from the flow regulation system defined in claim 1, as long as an acceptable flow is maintained in the monitoring device during the analysis.
According to one aspect of the present invention, a defined and stable volumetric gas flow is, however, achieved by said computer controlled flow regulation system.
The computer acquires signals from several sensors, for example, a mass flow sensor, an ambient temperature sensor, an ambient pressure sensor, a flow system back pressure sensor and a temperature sensor that measures the temperature of the temperature sensor. flow and compensates for its nonlinear behavior by temperature.
With the data from these sensors, the computer regulates the pump to maintain a steady flow as close as possible to the desired flow.
Flows, temperatures, pressures, humidity for the flow system are all logged.
The present inventors have created a solution to the problems mentioned above in connection with unstable air and gas flows.
The inventors' goal was to find a solution in which a gas flow through a sampling device can be adjusted to a desired flow rate, while a control system measures and controls the flow to keep it stable at the desired rate and records log the flow to ensure proper sampling and track how sampling was done.
The solution must also include a way to conduct several samplings simultaneously.
Flow measurements must be robust with respect to varying degrees of freedom: temperature and pressure range within the relevant atmospheric conditions (to produce an appropriate volumetric flow conversion) and back pressure levels for existing “heavy” samples (up to 15 kPa) . The solution should also make it possible to transfer log data of flow, time, temperature and pressure to a PC and adjust a device to make an appropriate sampling acquisition.
Through a wireless connection, a pump serves as a master, other pumps as slaves and a network of pumps can be controlled from the master pump or from a PC that serves as a master.
A schematic flow chart of the components within the gas flow regulation system according to an aspect of the present invention is shown in Figure 8A.
The gas flow regulation system in Figure 8A is located after the sampling device in Figure 1. The pump (PMPl) is controlled to maintain a steady flow at a user-defined setpoint, which is compared to a measurement of correct flow.
This measurement is made using a mass flow sensor and several compensation steps described in the “Flow measurement system” section below.
The gas flow is induced by a rotary vane pump with four dampers (PMP1). The gas flow could be induced by any electric gas pump or any device that is capable of being controlled electronically and that is capable of inducing a flow. The flow is measured by a mass flow sensor (PMP2) whose signal is compensated for the non-ideal properties of mass flow sensors with respect to temperature and pressure. The flow measurement procedure is described in more detail in the “Flow measurement system” section below. Dust and other particles can contaminate the sensitive flow sensor. A particle filter (PMP9) prevents contamination of the flow system. For considerations of IECEx (International Electrotechnical Commission, explosive atmospheres) and ATEX (EU directive 94/9 / EC: Appareils desté à être utilisés en ATmosphêres “EXplosibles) (spark mitigation), sintered filters (PMP8) will also be included in the system flow.
The flow system is capable of maintaining a stable flow that does not deviate more than 2% from the desired flow which can be adjusted in the range of 1 ml / min to 4000 ml / min.
Flow regulation system The control system depends on whether the flow can be precisely measured. In order to acquire a correct flow measurement, the steps shown in Figure 8B are taken.
Each step is crucial to acquire a correct flow measurement. The solution for each step and the alternatives are described below.
The main sensor for controlling the flow is a differential mass flow sensor (PMP2). The principle of this sensor is that the gas flows through a passage in that sensor, in which a heating element is located. Before and after the heating element, a differential temperature sensor is located. The gas is heated when it passes through the heating element. The temperature difference before and after the heating element corresponds to a certain flow rate. The output signal of the mass flow sensor is a voltage between 1V and 5V. Other mass flow sensors that can be miniaturized could also be used, for example, a Coriolis mass flow sensor.
The output signal from the mass flow sensor contains noise, mainly derived from non-laminar flow inducing pumps. The output signal is filtered by an electronic active low-pass filter (PMP7) with a cut-off frequency of 5Hz.
The low-pass filter could also be implemented as a) a passive low-pass filter, with resistors, inductors and capacitors, b) a software algorithm, either by averaging or using a fast Fourier transformation, or c) a flow pulse, which reduces pulses in the flow, making the initial flow sensor signal less noisy.
The voltage is converted into a digital value using a 14-bit ADC (Analog to Digital Converter (PMP12)). The ADC uses successive approximation. It could have any resolution greater than 10 bits and it could be a ZA type or an integrated type. The mass flow sensor is not ideal for all conditions and can be deflected with increased back pressure. Therefore, a back pressure sensor (PMPl3) is introduced to make it usable for relevant back pressure (0 to 15 kPa). The back pressure sensor is a differential pressure sensor that measures the difference between atmospheric pressure and pressure within the flow system. This value is used in a software compensation algorithm. The back pressure measurement could be measured by: a) having an absolute pressure sensor inside the flow system and comparing the reading with the absolute atmospheric pressure sensor, or b) having an absolute pressure sensor inside the flow system and using a differential pressure sensor to read atmospheric pressure.
The mass flow sensor signal deviates with its temperature. Therefore, the temperature of the mass flow sensor must be measured in order to acquire a correct flow for different ambient temperatures. Attaching a temperature compensation sensor (PMPlI4) to the mass flow sensor body makes it possible to compensate for the temperature deviation of the mass flow sensor. The relationship between the mass flow sensor voltage signal and the actual flow is not linear and differs between individual flow sensors. Therefore, a factory calibration data table (PMP6) is established to convert the mass flow signal into a mass flow. The calibration data table contains a variety of posts with signal values and corresponding mass flow. When converting a value to a flow, an interpolation is made between the closest values in the calibration table.
The calibration data table could be replaced by a polynomial function that describes the relationship between the mass flow and the sensor signal.
In order to convert the mass flow figure into a volume flow, the ideal gas law is applied, in which atmospheric pressure and temperature are measured by an atmospheric compensation sensor (PMP4). This measurement could be done by separate sensors for temperature and pressure. The pressure measurement could be made using an absolute pressure sensor inside the flow system and a differential pressure sensor between the flow system and the atmosphere.
Flow control is implemented as an application that works on a microcontroller computer module.
It could also work on an embedded PC. The control system needs a correct flow measurement, as described in the “Flow measurement section” section above. The flow measurement is compared to the desired flow set by the user. This comparison is made on a software PID controller. The PID controller controls the output signal to the pump.
A diffuse logic part in the software evaluates the control signals necessary for the pump to maintain a certain flow given a certain back pressure. From this data, the fuzzy logic part can override the PID controller when a condition in the flow system is drastically changed (back pressure, desired flow) in order to achieve a faster response. The flow-inducing pump is controlled by a Pulse Width Modulated signal. It could also be controlled by the output voltage of a D / A converter.
The mechanical parts in the flow system will wear out over time. Diagnostics for the flow system will be implemented by comparing the following three properties: flow system back pressure, pump control signal and flow measured by the mass flow sensor. By comparing data from the internal pressure sensor (PMP3), the mass flow sensor (PMP2, and the signal level to the pump (PMPl), flow system diagnostics can be achieved.The diagnostics software has several assumptions , for example, "if the pump needs a high control signal even though neither the back pressure nor the measured flow is high, the pump is in a bad condition".
The measured flow is recorded in a digital memory (flash) (PMP7). Additional parameters logged are temperature, pressure, humidity, GPS position and time. Log files can be managed on a computer with USB. The pump can be connected to a PC via USB. In order to control several pumps simultaneously, they must be connected to each other. The pump can be connected to a PC or other pumps via Bluetooth. Other wireless connections can be deployed (ie, ZigBee, WiFi).
The pump contains one or more Li-ion batteries. The batteries can either be charged via a USB connection to a computer or via a USB wall adapter. A battery indicator will be available to display the battery level to the user. The battery indicator can be deployed as one or several LED (s) or integrated into a graphical user interface. The pump's operating time is estimated at 12 hours for standard sampling conditions. The device is equipped with an OLED display that displays the current flow.
The display can be omitted or replaced with a 7-segment display, graphic LCD, matrix character LCD (for example, HD4470), LEDs, indicating the appropriate flow and paper display E. The user controls the pump by means of several buttons, which have different purposes depending on what menu state the user interface is in. An example is two buttons, where one walks through the graphic menu alternatives and the other modifies the selected menu.
The monitoring device according to the present invention also comprises a raw block module.
During the sampling cycle, a raw block sample is collected. An additional input, only used for raw block sampling, is present in the monitoring device. The inlet is connected to said raw block module, which contains a filter and an absorbent to capture compounds to ensure clean reference air.
The device gives a certain response to a certain concentration of the analyte.
To translate the response into concentration, information about the calibration curve needs to be present.
The calibration curve can be linear or more complex.
The intersection can pass through the origin or not.
To find out about the intersection, a raw block sample needs to be analyzed in order to have a valid calibration curve for translating the electrical response into concentration.
The monitoring device according to the present invention must be enclosed in a housing.
Said device can be used as a handheld device, but it can also be placed in a location with a certain retainer or attached to, for example, a tripod.
It can also be transported with a belt clip or harness.
The pump (s) will be certified by IECEX and approved by ATEX for use in explosive environments.
The pump will have an exposed connector, that is, a USB connector.
The USB connector is for wired communication and charging.
When using the device in explosive areas, this connector will be covered by a rigid seal against dust, air and water.
The pump display will be covered from behind by a transparent surface that meets the requirements of IECEx and ATEX.
Thus, a direct reading device for improved qualitative and quantitative monitoring of airborne compounds in both the gas and particle phases is provided.
The monitoring device can also be used for compounds on the surface or in a matrix that can be made volatile by, for example, heating. the use of the pump during sampling typically includes five scenarios: 1) manual sampling:
The device is turned on. Through a graphical user interface, the desired flow is adjusted to a certain amount of ml / min.
The pump is programmed through the user interface to stop after a certain time. The pump is then started using a graphical user interface. The pump control system maintains a flow as close as possible to the desired flow. The pump is stopped (manually if not pre-programmed) after a certain time.
2) Preset sampling: The device is pre-programmed into a computer via USB. At device startup, the user can select “perform pre-defined sampling”, while the pump runs at a certain flow for a certain time, then stops.
3) Slave mode: The pump is placed in one location and can be controlled remotely through a computer application or another pump device configured to control other pumps remotely. This mode can also be used in laboratory environments where an arbitrary number of pumps can be controlled simultaneously and in which sequential sampling schedules can be configured in the computer application.
4) Transfer of logged data: The pump is turned on and connected to a computer via USB. The pump is administered through a computer application. Through the application, one or more of the pump device's log files can be transferred to the computer and / or deleted from the pump device's memory.
5) As a component in other devices: This assembly is a solution to acquire a stable volumetric flow and can be used as a module or component in any device where the generation of a stable flow is necessary.
In accordance with an embodiment of the present invention, the detection unit contains an ion filter (DMS). The separation of the different analytes in the fluxo flow is based on their volatility before the ion filter, that is, in the chromatography unit.
A focusing collector is added before a chromatographic column.
When the analytes have been thermally desorbed from the sampling device, or by separate or total analysis and then have been collected from one or more enrichment collectors 1, the analytes are then thermally desorbed from each enrichment collector 1. These will then be in a gas value less than the sampling device and a focusing effect is achieved before entering the chromatography unit, such as a GC column.
The use of enrichment collectors reduces peak width and increases peak symmetry in GC chromatography, resulting in lower detection limits and improved repeatability.
In the ion filter modality of the detection unit system according to the present modality, the ionization of the analytes separated by chromatography is carried out before entering the ion filter (DMS). More precisely, the analytes eluted from the chromatographic column are ionized.
A stable and reproducible ionization is required for accurate monitoring.
An ionization technique based on, for example, photoionization, Ni ”ionization etc. is used.
For sufficient selectivity, an additional separation of the ionized analytes needs to be carried out in order to separate and detect the ionized compounds based on their differential mobilities in the lower parts per trillion region. For that purpose, a microDMx "" sensor chip (Sionex Inc., Bedford, MA, USA) can be used. As explained above, problems with memory effects, that is, analyte transport, can occur during peak concentration sampling. The present inventors solved this problem by introducing an air cleaning step, in which the sampling device, the enrichment collector and all necessary connections and piping are cleaned between the sampling cycles. Cleaning is performed to ensure that no relevant transport takes place. If the analysis of a raw block sample indicates that there is a transport, the cleaning parameters (flow speed, duration, etc.) are adjusted until no transport is observed.
As can be seen, the flow regulation system and the monitoring device according to the present invention have several advantages and differences in comparison with the techniques currently known. An important difference compared to the known methods is that the introduction of sample in the mass separator and / or mass filter (the sampling device) and / or ion filter and / or mass spectrometer and / or gas chromatography and / or detector and / or analyzer is made in such a way that both carrier compounds by gas or particles are collected, desorbed and determined in a quantitative and qualitative way. In addition, automatic volumetric sampling is made possible by the sampling device. Reactive compounds, that is, analytes, for example, isocyanates, isothiocyanates, aldehydes, amine anhydrides, etc. and compounds containing functional groups that can be derived into volatile compounds that can be analyzed and determined are collected and derived in stable and desorbed derivatives and analyzed by the active reactive sampling device.
Valid results are obtained by automatic field calibration and sampling is checked for breakage.
Transport compounds and memory effects are verified by automatic analysis of raw blocks.
Linearity defects are compensated by adjusting the sampling time to achieve sample concentrations in the linear range.
Example 1 Figure 9 shows an example of a measurement cycle for a volatile analyte compound.
The GC-DMS system used in this modality monitors the analyte concentration and alternates between monitoring the concentration of the analytes, the crude block and a reference.
Example 2 Figure 10 shows an example of GC-DMS chromatographies of a sampling sequence of 4 samples containing different concentrations of benzene and a reference containing 5 ppb of benzene.
The samples are taken from four different pipes located at different positions in a system.
After each collection of a sample for the sampling system, a raw block sample is taken.
The figure shows that no memory or transport effect of a sample or a reference sample is observed in the raw block samples.
At the reference of 5 ppb, it can be seen that an additional chromatographic peak is observed.
This peak is not benzene, but it is an unknown compound.
Chromatographic resolution is necessary to distinguish the analyte (benzene) from other components that may be present.
Example 3 Figure 11 shows the GC-DMS response to benzene (5 ppb) for 59 measurements over a two week period.
The variation (RSD) was <6%. The figure shows that the response varies over time and there is a tendency for the response to decrease over time. This demonstrates that the instrument needs to be calibrated in order to generate a valid concentration estimate. The deviation in response is due to the deviation in the parameters adjusted for the ion source, mass separator (DMS) and the detector. It may be due to electronic deviation and contamination of electrodes and / or differences in conditions due to a variation in conditions for gas flow (humidity, flow rate, etc.). The figure shows the need for field calibration and tuning and that the factory-set parameters are insufficient to obtain valid results.
Example 4 Figure 12 shows the temperature response of a thermal differential flow sensor. To investigate the temperature deviation of a thermal differential flow sensor, the thermal differential flow sensor was placed in a temperature controlled environment and fed with a well-known constant mass flow. The actual flow was kept constant and was measured using another flow meter, unaffected by temperature. In Figure 12, the voltage output of the mass flow sensor has been converted to a volumetric flow according to the mass flow meter calibration data. As can be seen in Figure 12, the flow measured is greatly affected by temperature. An increase in the measured flow from 818 ml / min to 866 ml / min, that is, an increase of approximately 6%, can be noticed when the temperature of the sensor is raised from 3ºC to 28ºC. Therefore, it is important to compensate for the sensor temperature in order to produce accurate and precise measurement results. A variety of measurement results as shown in Figure 12, that is, when changing the temperature of the sensor while measuring the actual flow through the flow meter can be used as a calibration curve to compensate for the sensor temperature in actual measurements using the flow regulation system. This calibration procedure is also repeated for different flows to compensate for different temperature dependence on mass flow sensor electronics at different flow levels. References Schneider BB, Covey TR, Coy SL, et al, Control of chemical effects in the separation process of a differential mobility mass spectrometer system, EUROPEAN JOURNAL OF MASS SPECTROMETRY, 2010, 16 (1), 57 to 71 Krylov EV, Nazarov EG , Electric field dependence of the ion mobility, 2009, INTERNATIONAL JOURNAL OF MASS SPECTROMETRY, 285 (3), 149 to 156 Krylov EV, Coy SL, Nazarov EG, Temperature effects in differential mobility spectrometry, INTERNATIONAL JOURNAL OF MASS SPECTROMETRY, 2009, 279 (2-3), 119 to 125 Krylov EV, Nazarov EG, Miller RA, Differential mobility spectrometer: Model of operation, INTERNATIONAL JOURNAL OF MASS SPECTROMETRY, 2007, 266 (1-3), 76 to 85 Kendler & S, Lambertus GR, Dunietz BD, et al., Fragmentation pathways and mechanisms of aromatic compounds in atmospheric pressure studied by GC-DMS and DMS-MS, INTERNATIONAL JOURNAL OF MASS SPECTROMETRY, 2007, 263 (2-3), 137 to 147 Marand À, Karlsson D ., Dalene M., Skarping G., Solvent-free sampling with di-n-butylamine for mo nitoring of isocyanates in air, J. Environ. Monit., (2005), DOI:
10.1039 / B414761H.

权利要求:
Claims (37)
[1]
1. FLOW REGULATION SYSTEM TO MAINTAIN A STABLE GAS FLOW, characterized by comprising at least one pump, at least one mass flow sensor, an ambient temperature sensor, an ambient pressure sensor, and a control system, wherein the input of said sensors to said control system is adapted to regulate at least one pump to maintain a stable mass flow.
[2]
2. FLOW REGULATION SYSTEM, according to claim 1, characterized in that it further comprises: a temperature compensation sensor that measures the temperature of said mass flow sensor.
[3]
3. FLOW REGULATION SYSTEM, according to either of claims 1 or 2, characterized in that said control system is an electronic device, preferably a computer.
[4]
4, FLOW REGULATION SYSTEM, according to any one of claims 1, 2 or 3, characterized in that said at least one pump is a rotary vane pump.
[5]
5. FLOW REGULATION SYSTEM, according to any one of claims 1, 2, 3 or 4, characterized in that it comprises two or more mass flow sensors.
[6]
6. FLOW REGULATION SYSTEM, according to any one of claims 1, 2, 3, 4 or 5, characterized in that said mass flow sensor is a thermal differential flow sensor.
[7]
7. FLOW REGULATION SYSTEM, according to any one of claims 1, 2, 3, 4, 5 or 6,
characterized in that it also comprises a back pressure sensor, in which the output of said back pressure sensor is connected to said control system.
[8]
8. FLOW REGULATION SYSTEM, according to any one of claims 1, 2, 3, 4, 5, 6 or 7, characterized in that it also comprises an ambient humidity sensor, in which the outlet of said humidity sensor ambient humidity is connected to the said control system.
[9]
9. FLOW REGULATION SYSTEM, according to any one of claims 1, 2, 3, 4, 5, 6, 7 or 8, characterized in that it also comprises logging means for logging one or a combination of the values contained in the group: mass flow, back pressure, ambient temperature, ambient pressure, ambient humidity, mass flow sensor temperature, GPS position, power consumption, battery level, and time.
[10]
10. FLOW REGULATION SYSTEM, according to any one of claims 1, 2, 3, 4, 5, 6, 7, 8 or 9, characterized in that it also comprises a graphical display and a user interface displayed on the said graphic display.
[11]
11. FLOW REGULATION SYSTEM, according to any one of claims 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10, characterized in that it also comprises means of user navigation to adjust the flow regulation system configurations.
[12]
12. FLOW REGULATION SYSTEM, according to any one of claims 1, 2, 3, 4, 5, 6, 7, 8, 9, 10 or 11, characterized in that it also comprises connection means for connecting the said flow regulation system to an external electronic device.
[13]
13. FLOW REGULATION SYSTEM, according to claim 12, characterized in that said electronic device is one of the electronic devices contained in the group consisting of: a personal computer, a handheld computer, a smartphone, a memory device digital.
[14]
14. FLOW REGULATION SYSTEM, according to any one of claims 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12 or 13, characterized in that it also comprises a system diagnostics that uses input signals from said back pressure sensor, from said mass flow sensor and the signal level for said at least one pump.
[15]
15. GROUPING OF FLOW REGULATION SYSTEMS, characterized in that at least two flow regulation systems, as defined in any one of claims 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11 , 12, 13 or 14 above, are connected in series or in parallel.
[16]
16. METHOD FOR MEASURING A FLOW WITH THE USE OF A FLOW REGULATION SYSTEM as defined in any one of claims 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14 or 15, characterized in that the method comprises the steps of: measuring the mass flow with the mass flow sensor, adjusting the mass flow measurement value in accordance with a predetermined temperature-related error calibration, calculating a volumetric flow from the said mass flow measurement using the measured mass flow, the ambient temperature and the ambient pressure.
[17]
17. METHOD FOR MEASURING A FLOW, according to claim 16, characterized in that the method further comprises the step of: measuring the temperature of the mass flow sensor using the said temperature compensation sensor adjusting the value of mass flow measurement in accordance with a predetermined temperature calibration error and the measurement signal of said temperature compensation sensor.
[18]
18. METHOD FOR MEASURING A FLOW, according to claim 16 or 17, characterized in that it further comprises the step of converting the analog output signal of the mass flow regulation system into a digital signal.
[19]
19. METHOD FOR MEASURING A FLOW, according to any one of claims 16, 17 or 18, characterized in that it also comprises the step of monitoring and / or logging the flow pulsation using the flow sensor pasta.
[20]
20. METHOD according to any one of claims 16, 17, 18 or 19, characterized in that the flow regulation system further comprises a back pressure sensor, and in which the method further comprises the compensation step of errors in said mass flow measurement due to current back pressure, by adjusting the mass flow measurement value by a predetermined increment depending on said measured back pressure.
[21]
21. METHOD, according to any of claims 16, 17, 18, 19 or 20, characterized in that it also comprises the step of monitoring and / or logging the flow pulsation using the back pressure sensor.
[22]
22. METHOD according to any one of claims 16, 17, 18, 19, 20 or 21, characterized in that it further comprises the step of introducing a cancellation pulse to reduce or cancel said flow pulse.
[23]
23. COMPOUND MONITORING DEVICE
TRANSPORTED BY THE AIR PRESENT IN THE AIR BOTH IN A GASEOUS PHASE AS IN A PARTICLE PHASE, characterized by comprising a sampling device, an enrichment collector 1, a calibration and tuning module, a raw block module, said regulation system flow rate as defined in any one of claims 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13 or 14, a chromatography unit and a detection unit.
[24]
24, MONITORING DEVICE, according to claim 23, characterized in that the sampling device comprises a sampling tube 8 which has an inlet 2 for the air flow and which has the capacity to absorb the analyte in the gas phase of said air flow, a filter 5 connected to the sampling tube and which has the capacity to absorb the analyte in said air flow, and a sorbent 6 connected to the filter 5 and which has the capacity to absorb any analytes that pass through the filter 5 .
[25]
25. MONITORING DEVICE, according to claim 24, characterized in that an enrichment collector 1 is connected to each one of the sampling tube 8, the filter 5 and the sorbent 6 to separate the detection of analyte released from said tube sampling 8, filter 5 and sorbent 6, respectively, or connected to only sorbent 6 for total detection of analyte released from the sampling device.
[26]
26. MONITORING DEVICE, according to claim 23, characterized in that the sampling device comprises a first sorbent 10 which has an inlet 2 for the air flow and which has the capacity to absorb the analyte in the gas phase of said flow of air, a filter 5 connected to the first sorbent 10 and which has the capacity to absorb the analyte in the particle phase of said air flow and a second sorbent 6 connected to the filter 5 and which has the capacity to absorb any analyte that passes through filter 5.
[27]
27. MONITORING DEVICE, according to claim 26, characterized in that an enrichment collector 1 is connected to each one of the first sorbent 10, the filter 5 and the second sorbent 6 to separate the detection of released analyte from said first sorbent 10, filter 5 and second sorbent 6, respectively, or connected to only the second sorbent 6 for total detection of analyte released from the sampling device.
[28]
28. MONITORING DEVICE, according to any one of claims 23, 24, 25, 26 or 27, characterized in that the sampling device is a particle size selective sampling device comprising a pre-selector 11 for removing particles large, the denudator 8 to collect gas phase analytes, an impactor 13 to separate large particles of inhalable or breathable sizes and a filter 5 to collect inhalable or breathable particles.
[29]
29. MONITORING DEVICE, according to any of claims 23, 24, 25, 26 or 27, characterized in that the calibration and tuning module is insertable and separable from the monitoring device, is connected to the sampling device and is regulated by a computer in order to calibrate and tune the monitoring device in view of analyte references.
[30]
30. MONITORING DEVICE, according to claim 29, characterized in that said calibration and tuning device comprises a closed tube that contains the analyte reference and is surrounded by a heating device.
[31]
31. MONITORING DEVICE, according to any one of claims 23, 24, 25, 26, 27, 28, 29 or
30, characterized in that the raw block module is connected to the sampling device, has a separate entrance for the monitoring device and comprises a filter and a sorbent.
[32]
32. MONITORING DEVICE, according to any one of claims 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19 , 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30 or 31, characterized in that said at least one pump in said flow regulation system is present between the enrichment collector 1 and the chromatograph, optionally also between the sampling device and the enrichment collector.
[33]
33. MONITORING DEVICE, according to any one of claims 23, 24, 25, 26, 27, 28, 29, 30, 31 or 32, characterized in that the chromatography unit comprises a gas chromatography.
[34]
34. MONITORING DEVICE, according to any one of claims 23, 24, 25, 26, 27, 28, 29, 30, 31, 32 or 33, characterized in that said detection unit is based on DMS (spectrometry of differential mobility) or is a gas chromatography detector or a direct reading detector.
[35]
35. METHOD FOR THE DETECTION OF ANALYTES
TRANSPORTED BY AIR IN A FLOW OF AIR THROUGH THE USE OF THE MONITORING DEVICE as defined in any of claims 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33 or 34 in accordance with this invention, characterized in that it comprises the consecutive steps to follow; a) one or more different calibration and tuning modules containing different analyte references are inserted into the monitoring device, b) the airflow containing the airborne analytes and a reagent is introduced into the sampling device to be reacted between itself, Cc) the sampling device containing the sampling tube 8, the filter 5 and the sorbent 6, or the first sorbent 10, the filter 5 and the second sorbent 6, is heated in order to release analytes adsorbed in the sampling device, d) the analytes released from said sampling device are collected in one or more enrichment collectors 1, e) the analytes are subjected to a chromatography step, f) the analytes are detected quantitatively and qualitatively.
[36]
36. METHOD, according to claim 35, characterized in that after the detection of each analyte a crude block is subjected to steps a) to £).
[37]
37. METHOD, according to claims 35 or 36, characterized in that the monitoring device is occasionally cleaned with air in order to eliminate any memory effects of the analytes and other compounds that have passed through said monitoring device.
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类似技术:

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公开号 | 公开日 | 专利标题

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2020-07-21| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]|

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2020-09-08| B06U| Preliminary requirement: requests with searches performed by other patent offices: procedure suspended [chapter 6.21 patent gazette]|

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优先权:

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申请号 | 申请日 | 专利标题

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US30912310P| true| 2010-03-01|2010-03-01|

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US61/309,123|2010-03-01|

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