Abstract

A hybrid trap including a replaceable open-tubular capillary trap followed by a packed trap is used to collect, preconcentrate, and recover a sample, such as VOCs and SVOCs found in air. The capillary stage prevents losses and carryover of the heavy fraction and can also collect the particles in air that contain the heavier SVOCs, also preventing them from reaching the packed stage. The packed stage traps lighter organic compounds that are not as prone to carryover due to channeling. The ionic species within the collected VOCs and SVOCs at the capillary trap can be converted to volatile compounds that allow gas chromatography-mass spectrometry.

IPC Classes  ?

• G01N 1/22 - Devices for withdrawing samples in the gaseous state
• G01N 1/40 - Concentrating samples
• G01N 30/00 - Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography
• G01N 30/16 - Injection
• G01N 30/60 - Construction of the column
• G01N 30/88 - Integrated analysis systems specially adapted therefor, not covered by a single one of groups

Abstract

A diffusive sampling device is used for quantitative measurement of chemicals in indoor and outdoor air. The sampling device includes a vial containing a sorbent on the inside bottom of the vial. The sampling device can be thermally vacuum cleaned before transport to the sampling location, and the sorbent can be chosen to allow the collection of either volatile or semi-volatile compounds (VOCs or SVOCs). After a diffusive sampling period (1 hour to 1 month), the vial is closed, and the collected sample is transferred to a laboratory for analysis. Using a thermal vacuum extraction focusing technique, the collected sample is rapidly delivered to a GCMS-compatible preconcentration device including a second sorbent for either split or splitless injection into a capillary based GCMS. No solvents are used during sampler preparation or analysis, and detection limits needed for monitoring of ambient or indoor air can be achieved for thousands of chemicals.

IPC Classes  ?

• G01N 1/40 - Concentrating samples

Abstract

A diffusive sampling device is used for quantitative measurement of chemicals in indoor and outdoor air. The sampling device includes a vial containing a sorbent on the inside bottom of the vial. The sampling device can be thermally vacuum cleaned before transport to the sampling location, and the sorbent can be chosen to allow the collection of either volatile or semi-volatile compounds (VOCs or SVOCs). After a diffusive sampling period (1 hour to 1 month), the vial is closed, and the collected sample is transferred to a laboratory for analysis. Using a thermal vacuum extraction focusing technique, the collected sample is rapidly delivered to a GCMS-compatible preconcentration device including a second sorbent for either split or splitless injection into a capillary based GCMS. No solvents are used during sampler preparation or analysis, and detection limits needed for monitoring of ambient or indoor air can be achieved for thousands of chemicals.

IPC Classes  ?

• G01N 1/22 - Devices for withdrawing samples in the gaseous state
• G01N 1/40 - Concentrating samples

Abstract

A hybrid gas sampling device can combine the functionality of both whole air and sorbent based samplers. The sampling device can be used for collecting light to very heavy organic compounds, for subsequent thermal desorption into a GC or GCMS for quantitative measurement. The sampling device isolates collected samples of gas phase matrices in a sample vessel, provided with sorbent elements from a removable sample extraction device. The sampling device is operated by drawing a vacuum on the chamber through the sample extraction device after sampling, and then completing the extraction of the heavier organic compounds using a static, diffusive extraction under vacuum to allow optimal deposition of the heavier compounds on the sorbent. The vacuum container is cooled to draw any excess water back into the container, thereby dehydrating attached sorbent element(s) in preparation for thermal desorption into a GC or GCMS, eliminating interferences in the MS analyzer.

IPC Classes  ?

• G01N 33/497 - Physical analysis of biological material of gaseous biological material, e.g. breath
• G01N 31/22 - Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroups; Apparatus specially adapted for such methods using chemical indicators
• G01N 33/00 - Investigating or analysing materials by specific methods not covered by groups

Abstract

A hybrid gas sampling device (100) can combine the functionality of both whole air and sorbent based samplers. The sampling device can be used for collecting light to very heavy organic compounds, for subsequent thermal desorption into a GC or GCMS for quantitative measurement. The sampling device isolates collected samples of gas phase matrices in a sample vessel (132), provided with sorbent elements (202, 256a, 256b, 256c) from a removable sample extraction device (150). The sampling device is operated by drawing a vacuum on the chamber through the sample extraction device after sampling, and then completing the extraction of the heavier organic compounds using a static, diffusive extraction under vacuum to allow optimal deposition of the heavier compounds on the sorbent. The vacuum container is cooled to draw any excess water (450) back into the container, thereby dehydrating attached sorbent element(s) (202, 256a, 256b, 256c) in preparation for thermal desorption into a GC or GCMS, eliminating interferences in the MS analyzer.

IPC Classes  ?

• G01N 1/24 - Suction devices
• G01N 1/22 - Devices for withdrawing samples in the gaseous state
• G01N 1/40 - Concentrating samples
• G01N 1/44 - Sample treatment involving radiation, e.g. heat
• G01N 33/497 - Physical analysis of biological material of gaseous biological material, e.g. breath

Abstract

Techniques disclosed herein can improve the extraction of chemicals prior to analysis by GC or GCMS. A liquid or solid sample can be placed in a sample container of a closed system under vacuum that further includes a sample extraction device. The assembly can be placed in a 3-zone heater that can separately control the temperature of the bottom of the sample container, the top of the sample container, and the sample extraction device. Vapor flux from the bottom of the sample container into the headspace of the sample container can deliver compounds of interest to the sample extraction device, whereas matrix compounds can re-condense in the headspace of the sample container to avoid delivery to the sample extraction device. Extraction can continue until substantial transfer of compounds of interest to the sorbent occurs, followed by thermal desorption of the extract into a GCMS for analysis.

IPC Classes  ?

• G01N 30/12 - Preparation by evaporation
• H01J 49/00 - Particle spectrometers or separator tubes
• H01J 49/04 - Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
• G01N 30/72 - Mass spectrometers
• G01N 1/40 - Concentrating samples

Abstract

Techniques disclosed herein can improve the extraction of chemicals prior to analysis by GC or GCMS. A liquid or solid sample can be placed in a sample container of a closed system under vacuum that further includes a sample extraction device. The assembly can be placed in a 3-zone heater that can separately control the temperature of the bottom of the sample container, the top of the sample container, and the sample extraction device. Vapor flux from the bottom of the sample container into the headspace of the sample container can deliver compounds of interest to the sample extraction device, whereas matrix compounds can re-condense in the headspace of the sample container to avoid delivery to the sample extraction device. Extraction can continue until substantial transfer of compounds of interest to the sorbent occurs, followed by thermal desorption of the extract into a GCMS for analysis.

IPC Classes  ?

• G01N 1/22 - Devices for withdrawing samples in the gaseous state
• G01N 1/40 - Concentrating samples
• G01N 1/44 - Sample treatment involving radiation, e.g. heat
• G01N 30/06 - Preparation

Abstract

Techniques disclosed herein can be used to perform a rapid, splitless injection of a sample including SVOCs and VOCs. In some embodiments, a system includes two focusing traps combined in series, one inside of a GC oven and one in a separate oven to concentrate the SVOCs inside of the GC oven and concentrate the VOCs outside of the GC oven. Heating the VOC focusing trap and reversing the flow through both focusers allows splitless injection of compounds boiling from as low as -100 ⁰C to as high as 600 ⁰C in a single analysis, with a narrow injection bandwidth to optimize both sensitivity and the resolving power of the analyzer.

IPC Classes  ?

• G01N 30/16 - Injection
• G01N 30/06 - Preparation
• G01N 30/88 - Integrated analysis systems specially adapted therefor, not covered by a single one of groups
• G01N 30/08 - Preparation using an enricher
• G01N 30/20 - Injection using a sampling valve
• H01J 49/04 - Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
• G01N 30/12 - Preparation by evaporation

Abstract

Techniques disclosed herein can be used to perform a rapid, splitless injection of a sample including SVOCs and VOCs. In some embodiments, a system includes two focusing traps combined in series, one inside of a GC oven and one in a separate oven to concentrate the SVOCs inside of the GC oven and concentrate the VOCs outside of the GC oven. Heating the VOC focusing trap and reversing the flow through both focusers allows splitless injection of compounds boiling from as low as −100° C. to as high as 600° C. in a single analysis, with a narrow injection bandwidth to optimize both sensitivity and the resolving power of the analyzer.

IPC Classes  ?

• G01N 30/14 - Preparation by elimination of some components
• G01N 30/12 - Preparation by evaporation
• G01N 30/02 - Column chromatography

Abstract

A flow controller for filling evacuated canisters can be operated at different reference pressures to produce substantially the same flow rates to facilitate inertness testing of the flow controller through demonstrated recovery of trace level chemicals in a challenge standard prior to using the flow controllers to collect air samples for measurement of VOCs during time weighted sampling events. The flow controller can include a first chamber and a second chamber divided by a diaphragm. The first chamber can be fluidly coupled to an inlet of the flow controller and an outlet of the flow controller. The second chamber can be coupled to a reference port of the flow controller. The outlet of the flow controller can be coupled to an initially (e.g., substantially) evacuated canister that can be used to collect a sample of ambient air or challenge standard (e.g., during testing).

IPC Classes  ?

• G01N 33/00 - Investigating or analysing materials by specific methods not covered by groups
• G05D 7/01 - Control of flow without auxiliary power

Abstract

A flow controller for filling evacuated canisters can be operated at different reference pressures to produce substantially the same flow rates to facilitate inertness testing of the flow controller through demonstrated recovery of trace level chemicals in a challenge standard prior to using the flow controllers to collect air samples for measurement of VOCs during time weighted sampling events. The flow controller can include a first chamber and a second chamber divided by a diaphragm. The first chamber can be fluidly coupled to an inlet of the flow controller and an outlet of the flow controller. The second chamber can be coupled to a reference port of the flow controller. The outlet of the flow controller can be coupled to an initially (e.g., substantially) evacuated canister that can be used to collect a sample of ambient air or challenge standard (e.g., during testing).

IPC Classes  ?

• G05D 7/01 - Control of flow without auxiliary power
• F17C 13/00 - VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES - Details of vessels or of the filling or discharging of vessels
• G01F 25/00 - Testing or calibration of apparatus for measuring volume, volume flow or liquid level or for metering by volume
• G01N 1/00 - Sampling; Preparing specimens for investigation

Abstract

Embodiments of the disclosure relate to chemical analysis systems, including autosampler systems. In some embodiments, an autosampler system can analyze gas phase samples using a single inlet for better consistency. The autosampler system can move the sample container closer to the sample introduction/preconcentration system prior to accessing the contents of the container to reduce exposure of the sample to reactive surfaces. The autosampler system is able to couple the sample containers to a sampling wand automatically, thereby eliminating the need to pre-attach each container using a gas transfer line. The autosampler system can be disposed on top of a chemical analysis system (e.g., a GC or GCMS), thereby conserving laboratory bench space. In some embodiments, the modules (e.g., sample trays, thermal conditioning systems, support legs) of the autosampler system can be coupled to the autosampler system using clamps that include magnetic codes associated with autocalibration information.

IPC Classes  ?

• G01N 35/00 - Automatic analysis not limited to methods or materials provided for in any single one of groups ; Handling materials therefor
• G01N 30/24 - Automatic injection systems
• G01N 35/10 - Devices for transferring samples to, in, or from, the analysis apparatus, e.g. suction devices, injection devices

Abstract

Embodiments of the disclosure relate to chemical analysis systems, including autosampler systems. In some embodiments, an autosampler system can analyze gas phase samples using a single inlet for better consistency. The autosampler system can move the sample container closer to the sample introduction/preconcentration system prior to accessing the contents of the container to reduce exposure of the sample to reactive surfaces. The autosampler system is able to couple the sample containers to a sampling wand automatically, thereby eliminating the need to pre-attach each container using a gas transfer line. The autosampler system can be disposed on top of a chemical analysis system (e.g., a GC or GCMS), thereby conserving laboratory bench space. In some embodiments, the modules (e.g., sample trays, thermal conditioning systems, support legs) of the autosampler system can be coupled to the autosampler system using clamps that include magnetic codes associated with autocalibration information.

IPC Classes  ?

• G01N 30/24 - Automatic injection systems
• G01N 30/18 - Injection using a septum or microsyringe

Abstract

The disclosed system and method improve measurement of trace volatile chemicals, such as by Gas Chromatography (GC) and Gas Chromatography/Mass Spectrometry (GCMS). A first trapping system can include a plurality of capillary columns in series and a focusing column fluidly coupled to a first detector. The first trapping system can retain and separate compounds in a sample, including C3 hydrocarbons and compounds heavier than C3 hydrocarbons (e.g., up to C12 hydrocarbons, or compounds having a boiling point around 250 °C), and can transfer the compounds from the focusing column to the first detector. A second trapping system can receive compounds that the first trapping system does not retain, and can include a packed trap and two columns. The second trapping system can remove water from the sample and can separate and detect compounds including C2 hydrocarbons and Formaldehyde.

IPC Classes  ?

• B01D 15/12 - Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the preparation of the feed
• B01D 15/18 - Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns
• G01N 30/14 - Preparation by elimination of some components
• G01N 30/40 - Flow patterns using back flushing
• G01N 30/46 - Flow patterns using more than one column
• G01N 30/08 - Preparation using an enricher

Abstract

While sample extraction device including a sorbent is coupled to a sample vial containing a sample, a vacuum is drawn through the sample extraction device to evaporate the volatile matrix of the sample and carry volatilized target compounds of the sample to the sorbent. Optionally, once the volatile matrix is evaporated, the sample vial is heated and/or the vacuum level is increased to transfer heavier target compounds to the sorbent. Multiple sampling devices can be extracted in parallel. The sample extraction device can be inserted into a thermal desorption device that directly couples the sample extraction device to a gas chromatograph. In some embodiments, the sample is desorbed and analyzed using gas chromatography or another suitable technique. The techniques disclosed herein are used for analysis of volatile organic compounds and semi-volatile organic compounds in water, food, beverages, soils, and other matrices.

IPC Classes  ?

• G01N 1/40 - Concentrating samples
• G01N 1/22 - Devices for withdrawing samples in the gaseous state
• G01N 30/12 - Preparation by evaporation
• G01N 30/08 - Preparation using an enricher

Abstract

While sample extraction device including a sorbent is coupled to a sample vial containing a sample, a vacuum is drawn through the sample extraction device to evaporate the volatile matrix of the sample and carry volatilized target compounds of the sample to the sorbent. Optionally, once the volatile matrix is evaporated, the sample vial is heated and/or the vacuum level is increased to transfer heavier target compounds to the sorbent. Multiple sampling devices can be extracted in parallel. The sample extraction device can be inserted into a thermal desorption device that directly couples the sample extraction device to a gas chromatograph. In some embodiments, the sample is desorbed and analyzed using gas chromatography or another suitable technique. The techniques disclosed herein are used for analysis of volatile organic compounds and semi-volatile organic compounds in water, food, beverages, soils, and other matrices.

IPC Classes  ?

• G01N 30/14 - Preparation by elimination of some components
• G01N 1/14 - Suction devices, e.g. pumps; Ejector devices
• G01N 1/22 - Devices for withdrawing samples in the gaseous state
• G01N 30/72 - Mass spectrometers
• G01N 30/00 - Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography

Abstract

Pressure-controlled splitting can be used to inject a chemical sample from an injection source to a detector (e.g., a mass spectrometer) for chemical analysis (e.g., gas chromatography or gas chromatography-mass spectrometry) with reduced peak widths. For example, the sample is first transferred to a first compression volume; then pressure in the system is increased to compress the sample to split it between a second compression volume and a column. The fraction of the sample split to the column can have reduced peak widths compared to the peak widths prior to compression and splitting yet can maintain the same peak height to preserve high sensitivity for trace level analysis. This portion of the sample can traverse the column and elute to the detector for analysis with reduced chemical noise. Faster injection rates can allow faster analysis times, as less separation of chemicals is needed before the sample reaches the detector.

IPC Classes  ?

• G01N 30/72 - Mass spectrometers
• G01N 30/20 - Injection using a sampling valve
• G01N 30/10 - Preparation using a splitter

Abstract

Pressure-controlled splitting can be used to inject a chemical sample from an injection source to a detector (e.g., a mass spectrometer) for chemical analysis (e.g., gas chromatography or gas chromatography-mass spectrometry) with reduced peak widths. For example, the sample is first transferred to a first compression volume; then pressure in the system is increased to compress the sample to split it between a second compression volume and a column. The fraction of the sample split to the column can have reduced peak widths compared to the peak widths prior to compression and splitting yet can maintain the same peak height to preserve high sensitivity for trace level analysis. This portion of the sample can traverse the column and elute to the detector for analysis with reduced chemical noise. Faster injection rates can allow faster analysis times, as less separation of chemicals is needed before the sample reaches the detector.

IPC Classes  ?

• B01D 15/14 - Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the introduction of the feed to the apparatus
• B01D 15/18 - Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to flow patterns
• G01N 30/38 - Flow patterns
• G01N 30/32 - Control of physical parameters of the fluid carrier of pressure or speed
• G01N 30/16 - Injection

Abstract

A hybrid trap including a replaceable open-tubular capillary trap followed by a packed trap is used to collect, preconcentrate, and recover a sample, such as VOCs and SVOCs found in air. The capillary stage prevents losses and carryover of the heavy fraction and can also collect the particles in air that contain the heavier SVOCs, also preventing them from reaching the packed stage. The packed stage traps lighter organic compounds that are not as prone to carryover due to channeling. The capillary and packed traps together provide quantitative recovery of compounds boiling from as low as −50° C. to as high as 600° C. The sample can be directly desorbed onto the GC column, which avoids losses and contamination caused by other approaches that thermally desorb samples through transfer lines and rotary valves more remote to the GC oven.

IPC Classes  ?

• G01N 30/38 - Flow patterns
• G01N 1/40 - Concentrating samples
• G01N 30/54 - Temperature
• G01N 30/60 - Construction of the column
• G01N 30/72 - Mass spectrometers
• G01N 30/88 - Integrated analysis systems specially adapted therefor, not covered by a single one of groups
• G01N 30/00 - Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography
• G01N 30/02 - Column chromatography

Abstract

A hybrid trap including a replaceable open-tubular capillary trap followed by a packed trap is used to collect, preconcentrate, and recover a sample, such as VOCs and SVOCs found in air. The capillary stage prevents losses and carryover of the heavy fraction and can also collect the particles in air that contain the heavier SVOCs, also preventing them from reaching the packed stage. The packed stage traps lighter organic compounds that are not as prone to carryover due to channeling. The capillary and packed traps together provide quantitative recovery of compounds boiling from as low as -50 ⁰C to as high as 600 ⁰C. The sample can be directly desorbed onto the GC column, which avoids losses and contamination caused by other approaches that thermally desorb samples through transfer lines and rotary valves more remote to the GC oven.

IPC Classes  ?

• G01N 30/08 - Preparation using an enricher
• G01N 30/12 - Preparation by evaporation
• G01N 30/16 - Injection
• G01N 1/22 - Devices for withdrawing samples in the gaseous state
• G01N 1/40 - Concentrating samples
• G01N 30/24 - Automatic injection systems

Abstract

The disclosed system and method improve measurement of trace volatile chemicals, such as by Gas Chromatography (GC) and Gas Chromatography/Mass Spectrometry (GCMS). A first trapping system can include a plurality of capillary columns in series and a focusing column fluidly coupled to a first detector. The first trapping system can retain and separate compounds in a sample, including C3 hydrocarbons and compounds heavier than C3 hydrocarbons (e.g., up to C12 hydrocarbons, or compounds having a boiling point around 250° C.), and can transfer the compounds from the focusing column to the first detector. A second trapping system can receive compounds that the first trapping system does not retain, and can include a packed trap and two columns. The second trapping system can remove water from the sample and can separate and detect compounds including C2 hydrocarbons and Formaldehyde.

IPC Classes  ?

• G01N 30/46 - Flow patterns using more than one column
• G01N 30/20 - Injection using a sampling valve
• G01N 30/10 - Preparation using a splitter
• G01N 30/60 - Construction of the column
• G01N 30/02 - Column chromatography

Abstract

A sample collection device collects Volatile Organic Compounds (VOCs) in exhaled breath in the outlet of a breathing assisted ventilator. The sample collection device is attached to the ventilator outlet line through a coupler containing either two check valves, or a check valve and a restrictive outlet flow path. During sampling, the exhaled air flows through a sorbent contained in the sample collection device as the ventilator pressure increases and decreases during the assisted breathing process. The flow of the exhaled air through the sample collection system is driven by the alternating pressure in the ventilator line without the need for an additional pump or power supply separate from the ventilator pump and power supply. The sample collection device can be used to monitor levels of bacteria-produced VOCs as an early detection of pneumonia and to allow feedback on the effectiveness of antibiotic treatment.

IPC Classes  ?

• A61B 5/097 - Devices for facilitating collection of breath or for directing breath into or through measuring devices
• A61M 16/20 - Valves specially adapted to medical respiratory devices
• A61M 16/08 - Bellows; Connecting tubes
• A61M 16/00 - Devices for influencing the respiratory system of patients by gas treatment, e.g. mouth-to-mouth respiration; Tracheal tubes
• A61B 5/08 - Measuring devices for evaluating the respiratory organs
• G01N 1/22 - Devices for withdrawing samples in the gaseous state
• G01N 33/497 - Physical analysis of biological material of gaseous biological material, e.g. breath
• A61B 10/00 - Other methods or instruments for diagnosis, e.g. for vaccination diagnosis; Sex determination; Ovulation-period determination; Throat striking implements

Abstract

A sample collection device collects Volatile Organic Compounds (VOCs) in exhaled breath in the outlet of a breathing assisted ventilator. The sample collection device is attached to the ventilator outlet line through a coupler containing either two check valves, or a check valve and a restrictive outlet flow path. During sampling, the exhaled air flows through a sorbent contained in the sample collection device as the ventilator pressure increases and decreases during the assisted breathing process. The flow of the exhaled air through the sample collection system is driven by the alternating pressure in the ventilator line without the need for an additional pump or power supply separate from the ventilator pump and power supply. The sample collection device can be used to monitor levels of bacteria-produced VOCs as an early detection of pneumonia and to allow feedback on the effectiveness of antibiotic treatment.

IPC Classes  ?

• A61B 5/097 - Devices for facilitating collection of breath or for directing breath into or through measuring devices

Abstract

The disclosed system and method improve measurement of trace volatile chemicals, such as by Gas Chromatography (GC) and Gas Chromatography /Mass Spectrometry (GCMS). A first trapping system can include a plurality of capillary columns in series and a focusing column fluidly coupled to a first detector. The first trapping system can retain and separate compounds in a sample, including C3 hydrocarbons and compounds heavier than C3 hydrocarbons (e.g., up to C12 hydrocarbons, or compounds having a boiling point around 250 °C), and can transfer the compounds from the focusing column to the first detector. A second trapping system can receive compounds that the first trapping system does not retain, and can include a packed trap, a polar column and a PLOT column fluidly coupled to one or more second detectors. The second trapping system can remove water from the sample and can separate and detect compounds including C2 hydrocarbons and Formaldehyde.

IPC Classes  ?

• G01N 30/06 - Preparation
• G01N 30/08 - Preparation using an enricher
• G01N 30/46 - Flow patterns using more than one column
• G01N 30/88 - Integrated analysis systems specially adapted therefor, not covered by a single one of groups
• G01N 30/40 - Flow patterns using back flushing
• B01D 53/04 - Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases or aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
• G01N 30/60 - Construction of the column
• G01N 30/72 - Mass spectrometers

Abstract

The disclosed system and method improve measurement of trace volatile chemicals, such as by Gas Chromatography (GC) and Gas Chromatography/Mass Spectrometry (GCMS). A first trapping system can include a plurality of capillary columns in series and a focusing column fluidly coupled to a first detector. The first trapping system can retain and separate compounds in a sample, including C3 hydrocarbons and compounds heavier than C3 hydrocarbons (e.g., up to C12 hydrocarbons, or compounds having a boiling point around 250° C.), and can transfer the compounds from the focusing column to the first detector. A second trapping system can receive compounds that the first trapping system does not retain, and can include a packed trap, a polar column and a PLOT column fluidly coupled to one or more second detectors. The second trapping system can remove water from the sample and can separate and detect compounds including C2 hydrocarbons and Formaldehyde.

IPC Classes  ?

• G01N 30/08 - Preparation using an enricher
• G01N 30/10 - Preparation using a splitter
• G01N 30/46 - Flow patterns using more than one column
• G01N 30/40 - Flow patterns using back flushing
• G01N 30/06 - Preparation
• G01N 30/88 - Integrated analysis systems specially adapted therefor, not covered by a single one of groups
• G01N 30/02 - Column chromatography
• G01N 30/72 - Mass spectrometers
• G01N 30/60 - Construction of the column

Abstract

The disclosed system and method improve analysis of chemical samples for measurement of trace volatile chemicals, such as by Gas Chromatography (GC) and Gas Chromatography/Mass Spectrometry (GCMS). The system can include two traps in series, the first of which removes most of the unwanted water vapor, while the second trap preconcentrates the sample using a series of capillary columns of increasing adsorption strength. The sample can be backflushed from the second trap directly to a chemical analyzer without splitting which can maximize sensitivity. The system improves elimination of water vapor and fixed gases from the sample prior to analysis, resulting in detection limits as low as 0.001PPBb. The second trap allows faster release of the sample upon injection to the chemical analyzer without additional focusing, and can be cleaned up faster when exposed to high concentration samples relative to packed traps.

IPC Classes  ?

• G01N 30/40 - Flow patterns using back flushing
• G01N 1/40 - Concentrating samples
• G01N 30/46 - Flow patterns using more than one column

Abstract

The disclosed system and method improve analysis of chemical samples for measurement of trace volatile chemicals, such as by Gas Chromatography (GC) and Gas Chromatography/Mass Spectrometry (GCMS). The system can include two traps in series, the first of which removes most of the unwanted water vapor, while the second trap preconcentrates the sample using a series of capillary columns of increasing adsorption strength. The sample can be backflushed from the second trap directly to a chemical analyzer without splitting which can maximize sensitivity. The system improves elimination of water vapor and fixed gases from the sample prior to analysis, resulting in detection limits as low as 0.001 PPBb. The second trap allows faster release of the sample upon injection to the chemical analyzer without additional focusing, and can be cleaned up faster when exposed to high concentration samples relative to packed traps.

IPC Classes  ?

• G01N 30/72 - Mass spectrometers
• G01N 33/00 - Investigating or analysing materials by specific methods not covered by groups
• G01N 30/46 - Flow patterns using more than one column
• G01N 30/60 - Construction of the column
• G01N 1/40 - Concentrating samples
• G01N 30/02 - Column chromatography
• G01N 30/12 - Preparation by evaporation
• G01N 30/40 - Flow patterns using back flushing

Abstract

The disclosed system and method concentrates and enriches a chemical sample while removing water and/or CO2 prior to analysis, improving detection limits and repeatability of quantitative chemical analysis without the need for cryogenic or sub-ambient cooling. The system can include a valve system, a dewpomt control zone, and a multi-capillary column trapping system (MCCTS). During a first time period, the valve system can couple the dewpoint control zone to the MCCTS. During a second time period, the valve system can couple the MCCTS to the chemical separation column such the dewpoint control zone is bypassed. Excess water included in the sample can condense in the dewpoint control zone as the sample transfers to the dewpoint control zone and MCCTS. When the sample is transferred from the MCCTS to the chemical separation column, the condensed water in the dewpoint control zone is not transferred to a chemical separation column.

IPC Classes  ?

• G01N 30/08 - Preparation using an enricher
• G01N 30/20 - Injection using a sampling valve
• G01N 1/40 - Concentrating samples
• G01N 30/60 - Construction of the column
• G01N 30/14 - Preparation by elimination of some components
• G01N 30/46 - Flow patterns using more than one column

Abstract

The disclosed system and method concentrates and enriches a chemical sample while removing water and/or CO2 prior to analysis, improving detection limits and repeatability of quantitative chemical analysis without the need for cryogenic or sub-ambient cooling. The system can include a valve system, a dewpoint control zone, and a multi-capillary column trapping system (MCCTS). During a first time period, the valve system can couple the dewpoint control zone to the MCCTS. During a second time period, the valve system can couple the MCCTS to the chemical separation column such the dewpoint control zone is bypassed. Excess water included in the sample can condense in the dewpoint control zone as the sample transfers to the dewpoint control zone and MCCTS. When the sample is transferred from the MCCTS to the chemical separation column, the condensed water in the dewpoint control zone is not transferred to a chemical separation column.

IPC Classes  ?

• B01L 3/00 - Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
• G01N 1/40 - Concentrating samples
• G01N 1/44 - Sample treatment involving radiation, e.g. heat
• G01N 30/12 - Preparation by evaporation
• G01N 30/14 - Preparation by elimination of some components
• G01N 30/46 - Flow patterns using more than one column
• G01N 30/72 - Mass spectrometers
• G01N 30/30 - Control of physical parameters of the fluid carrier of temperature
• G01N 30/20 - Injection using a sampling valve
• G01N 30/08 - Preparation using an enricher
• G01N 30/60 - Construction of the column
• G01N 1/22 - Devices for withdrawing samples in the gaseous state

Abstract

Trace Volatile and Semi-Volatile compounds within a sample can be extracted and concentrated on an sorbent in the headspace of a closed sample vial by alternating the temperature of the sample repeatedly from hot to cold. As the sample heats, mass transport can occur from the sample into the headspace that can increase the speed of ejection of one or more chemicals from the sample into the headspace where they can be collected on the sorbent, for example. In some examples, re-cooling and then re-heating the sample can allow faster transport to continue until significant transport has occurred of one or more target compounds from the sample to the adsorbent, leaving behind the non-volatile chemicals and most of the liquid matrix that would otherwise interfere with the chemical analysis device. The pulsed heating and cooling can be performed under vacuum to increase the speed of the extraction process.

IPC Classes  ?

• G01N 1/40 - Concentrating samples
• G01N 1/44 - Sample treatment involving radiation, e.g. heat
• G01N 1/22 - Devices for withdrawing samples in the gaseous state
• B01L 7/00 - Heating or cooling apparatus; Heat insulating devices

Abstract

A system to thermally desorb a sample into a multi-column GC or GC/MS system that can use both the desorption system and GC system for optimizing injection rates, matrix management (e.g., water elimination), optimizing recovery of a specific range of chemicals, and system cleanup is described. Reversing the flow through a first column (332) inside the GC can facilitate the elimination of excess, condensed water as well as heavy chemicals that could otherwise affect the operation and background of the GC. The elimination of flow through both the thermal desorber (320) and a first column (332) in the GC during sample preheat can accommodate the pre-expansion of the sample that could otherwise result in pre-release to the active carrier gas flow in other systems. Transfer lines and rotary valves can be avoided, improving system performance and longevity, with simple maintenance achieved by replacing a desorption liner (322) and the first GC column (332).

IPC Classes  ?

• G01N 30/12 - Preparation by evaporation
• G01N 30/46 - Flow patterns using more than one column

Abstract

A system to thermally desorb a sample into a multi-column GC or GCMS system that can use both the desorption system and GC system for optimizing injection rates, matrix management (e.g., water elimination), optimizing recovery of a specific range of chemicals, and system cleanup is described. Reversing the flow through a first column inside the GC can facilitate the elimination of excess, condensed water as well as heavy chemicals that could otherwise affect the operation and background of the GC. The elimination of flow through both the thermal desorber and a first column in the GC during sample preheat can accommodate the pre-expansion of the sample that could otherwise result in pre-release to the active carrier gas flow in other systems. Transfer lines and rotary valves can be avoided, improving system performance and longevity, with simple maintenance achieved by replacing a desorption liner and the first GC column.

IPC Classes  ?

• G01N 30/54 - Temperature
• G01N 30/60 - Construction of the column
• G01N 30/46 - Flow patterns using more than one column
• G01N 30/12 - Preparation by evaporation
• G01N 30/72 - Mass spectrometers
• G01N 30/02 - Column chromatography

Abstract

The disclosure is related to preparing a sample for chemical analysis by evaporating at least a portion of solvent included in the sample. After depositing the sample into a sample container, in some examples, at l east a portion of the solvent can be evaporated. Solvent evaporation can be achieved at room temperature, at an elevated temperature, at atmospheric pressure, or by drawing a vacuum in the sample container, for example. The one or more compounds of interest can pass through a sample delivery port on the sample container into the chemical analysis device for analysis, for example. Preliminary reduction or elimination of the solvent can increase the overall amount of compounds of interest delivered into the chemical analysis device, for example, in some examples, when extra sensitivity may not be needed, less solvent can be used, which can result in a greener analytical technique that is better for the environment.

IPC Classes  ?

• G01N 30/12 - Preparation by evaporation
• G01N 1/40 - Concentrating samples
• G01N 30/72 - Mass spectrometers
• G01N 30/60 - Construction of the column
• G01N 1/10 - Devices for withdrawing samples in the liquid or fluent state

Abstract

A sample extraction device and a desorption device for use in gas chromatography (GC), gas chromatography-mass spectrometry (GCMS), liquid chromatography (LC), and/or liquid chromatography-mass spectrometry (LCMS) are disclosed. In some examples, the sample extraction device includes a lower chamber holding a sorbent. The sample extraction device can extract sample headspace gas from a sample vial by placing the sorbent inside the vial and creating a vacuum to increase recovery of low volatility compounds, for example. Once the sample has been collected, the sample extraction device can be inserted into a desorption device. The desorption device can control the flow of a carrier fluid (e.g., a liquid or a gas) through the sorbent containing the sample and into a pre-column and/or a primary column of a chemical analysis device for performing GC, GCMS, LC, LCMS, and/or some other chemical analysis process.

IPC Classes  ?

• G01N 30/06 - Preparation
• G01N 1/10 - Devices for withdrawing samples in the liquid or fluent state
• G01N 1/40 - Concentrating samples
• G01N 30/00 - Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography
• G01N 33/487 - Physical analysis of biological material of liquid biological material
• G01N 33/497 - Physical analysis of biological material of gaseous biological material, e.g. breath
• G01N 30/88 - Integrated analysis systems specially adapted therefor, not covered by a single one of groups

Abstract

A sample extraction device and a desorption device for use in gas chromatography (GC), gas chromatography-mass spectrometry (GCMS), liquid chromatography (LC), and/or liquid chromatography-mass spectrometry (LCMS) are disclosed. In some examples, the sample extraction device includes a lower chamber holding a sorbent. The sample extraction device can extract sample headspace gas from a sample vial by placing the sorbent inside the vial and creating a vacuum to increase recovery of low volatility compounds, for example. Once the sample has been collected, the sample extraction device can be inserted into a desorption device. The desorption device can control the flow of a carrier fluid (e.g., a liquid or a gas) through the sorbent containing the sample and into a pre-column and/or a primary column of a chemical analysis device for performing GC, GCMS, LC, LCMS, and/or some other chemical analysis process.

IPC Classes  ?

• A61B 10/00 - Other methods or instruments for diagnosis, e.g. for vaccination diagnosis; Sex determination; Ovulation-period determination; Throat striking implements
• G01N 33/497 - Physical analysis of biological material of gaseous biological material, e.g. breath
• G01N 33/487 - Physical analysis of biological material of liquid biological material
• G01N 30/06 - Preparation
• G01N 1/20 - Devices for withdrawing samples in the liquid or fluent state for flowing or falling materials
• G01N 1/40 - Concentrating samples
• G01N 1/22 - Devices for withdrawing samples in the gaseous state
• G01N 30/00 - Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography

Abstract

A multi-capillary column pre-concentration trap (300) for use in various chromatography techniques (e.g., gas chromatography (GC) or gas chromatography-mass spectrometry (GCMS)) is disclosed. The trap (300) includes a first trap (204) comprising a plurality of capillary columns (208A, 208B, 208C) connected in series in order of increasing strength (i.e., increasing chemical affinity for one or more sample compounds). A sample enters the trap (204), flowing from a sample vial (202) to a relatively weak column (208A) to the relatively strongest column (208C) of the trap by way of any additional columns (208B) included in the trap, for example. The trap is backflushed so that the sample exits the trap through the head of the relatively weak column. The trap may further be heated to aid in the desorption of the sample. Next, the sample can be injected into a chemical analysis device (206) for performing the chromatography technique (e.g., GC or GCMS) or it can be injected into a second trap (304) for further concentration.

IPC Classes  ?

• G01N 30/12 - Preparation by evaporation
• G01N 1/40 - Concentrating samples
• G01N 30/40 - Flow patterns using back flushing
• G01N 30/60 - Construction of the column
• G01N 30/46 - Flow patterns using more than one column

Abstract

A multi-capillary column pre-concentration trap for use in various chromatography techniques (e.g., gas chromatography (GC) or gas chromatography-mass spectrometry (GCMS)) is disclosed. In some examples, the trap can include a plurality of capillary columns connected in series in order of increasing strength (i.e., increasing chemical affinity for one or more sample compounds). A sample can enter the trap, flowing from a sample vial to a relatively weak column to the relatively strongest column of the trap by way of any additional columns included in the trap, for example. In some examples, the trap can be heated and backflushed so that the sample exits the trap through the head of the relatively weak column. Next, the sample can be injected into a chemical analysis device for performing the chromatography technique (e.g., GC or GCMS) or it can be injected into a secondary multi-capillary column trap for further concentration.

IPC Classes  ?

• G01N 30/14 - Preparation by elimination of some components
• G01N 30/12 - Preparation by evaporation
• B01L 3/00 - Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
• G01N 1/40 - Concentrating samples
• G01N 1/44 - Sample treatment involving radiation, e.g. heat
• G01N 30/30 - Control of physical parameters of the fluid carrier of temperature
• G01N 30/46 - Flow patterns using more than one column
• G01N 30/72 - Mass spectrometers
• G01N 30/60 - Construction of the column
• G01N 30/40 - Flow patterns using back flushing

Abstract

A sample extraction device and a desorption device for use in gas chromatography (GC), gas chromatography-mass spectrometry (GCMS), liquid chromatography (LC), and/or liquid chromatography-mass spectrometry (LCMS) are disclosed. In some examples, the sample extraction device includes a lower chamber holding a sorbent. The sample extraction device can extract sample headspace gas from a sample vial by placing the sorbent inside the vial and creating a vacuum to increase recovery of low volatility compounds, for example. Once the sample has been collected, the sample extraction device can be inserted into a desorption device. The desorption device can control the flow of a carrier fluid (e.g., a liquid or a gas) through the sorbent containing the sample and into a pre-column and/or a primary column of a chemical analysis device for performing GC, GCMS, LC, LCMS, and/or some other chemical analysis process.

IPC Classes  ?

• G01N 1/20 - Devices for withdrawing samples in the liquid or fluent state for flowing or falling materials
• G01N 30/14 - Preparation by elimination of some components
• G01N 30/06 - Preparation
• G01N 1/22 - Devices for withdrawing samples in the gaseous state
• G01N 30/72 - Mass spectrometers
• G01N 30/02 - Column chromatography
• G01N 30/00 - Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography

Abstract

A sample extraction device (100, 200,210) and a desorption device for use in gas chromatography (GC), gas chromatography-mass spectrometry (GCMS), liquid chromatography (LC), and/or liquid chromatography-mass spectrometry (LCMS) are disclosed. The sample extraction device includes a lower chamber (220) holding a sorbent (202). The sample extraction device can extract sample headspace gas from a sample vial by placing the sorbent inside the vial and creating a vacuum to increase recovery of low volatility compounds, for example. Once the sample has been collected, the sample extraction device can be inserted into a desorption device. The desorption device can control the flow of a carrier fluid (e.g.,a liquid or a gas) through the sorbent containing the sample and into a pre-column and/or a primary column of a chemical analysis device for performing GC, GCMS, LC, LCMS, and/or some other chemical analysis process.

IPC Classes  ?

• G01N 30/06 - Preparation
• G01N 1/22 - Devices for withdrawing samples in the gaseous state
• G01N 30/00 - Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography