Multichannel vaporization detection platform and application thereof
Technical Field
The invention relates to a detection platform, in particular to a multichannel vaporization detection platform and application thereof.
Background
Currently, the samples that are detectable by commercially available concentration and isotope ratio analysis devices are gas samples. For testing of liquid samples, a vaporization platform is required to vaporize the sample, converting it into a gaseous sample for testing, unlike the analytical technique used. The existing vaporization platform and vaporization method for processing liquid samples can not provide better pretreatment samples for analysis and test instruments, and further can influence the accuracy of detection results. Such as isotope ratio measurement of water.
The measurement of the ratio of hydrogen to oxygen isotopes in liquids and vapors has good application in environmental monitoring, biomedical diagnostics, and other industrial, medical and environmental research fields. Since the sample state that can be detected by the in-water oxyhydrogen isotope ratio analysis device is gas, it is necessary for a liquid sample to be converted into gas and then enter the in-water oxyhydrogen isotope ratio analysis device for detection. Isotope ratio analysis is a very precise analysis, so that the process of converting a liquid sample into a gas has a severe requirement, and the gas obtained by a conventional vaporization platform and a vaporization method cannot reach the detection standard of a later analysis instrument. The detection of the hydrogen-oxygen isotope ratio in water requires that 100% of liquid water is converted into water vapor and is totally transmitted to an analyzer for detection, or a part of the water is detected after the water vapor and the water vapor are uniformly mixed. If a certain amount of liquid water evaporates over a period of time, the isotopic content of the water vapor will vary over time. If the evaporation is incomplete and the liquid remains at the end of a certain time, the isotope content in the whole water vapor may differ from the original liquid and the remaining liquid, for example, due to temperature dependent fractionation during evaporation, etc., resulting in uneven entry of the evaporated liquid sample into the analyzer, in which case it is necessary to perform the process of a) having to analyze the whole vapor volume, b) measuring (or precisely controlling) the concentration, isotope ratio and flow rate as a function of time, respectively, during the gas flow, c) calculating the isotope ratio determined by multiplying the measured gas isotope ratio by the concentration and flow rate. The above steps a-c result in complexity and inaccuracy in the liquid isotope ratio determination, require additional measurements or controls (e.g., flow rates), and introduce additional complexity and error sources that can be inconvenient for sample analysis.
Disclosure of Invention
In order to overcome the defects in the prior art, one of the purposes of the invention is to provide a multi-channel vaporization platform, which adopts at least two vaporization channels to start detection at the same time, so as to shorten the sample analysis time.
The second purpose of the invention is to provide an application of the multi-channel vaporization platform, which reduces the memory effect and the liquid residue, and the measurement result is more accurate.
One of the purposes of the invention is realized by adopting the following technical scheme:
A multichannel vaporization detection platform comprises at least two vaporization channels.
Further, the gas analysis device comprises two vaporization channels, namely a first vaporization channel and a second vaporization channel, wherein the first vaporization channel comprises a first vaporization chamber, the second vaporization channel comprises a second vaporization chamber, the gas analysis device further comprises a dryer connected with the first vaporization chamber and the second vaporization chamber, the first vaporization chamber is connected with the second vaporization chamber, and the gas analysis device is connected with the dryer.
Further, the vacuum pump is further included, a first filter is further arranged between the first vaporization chamber and the gas analysis device, a second filter is further arranged between the second vaporization chamber and the gas analysis device, and the first filter and the second filter are both connected with the vacuum pump.
Further, a first control device is arranged between the dryer and the first vaporizing chamber, a third control device is arranged between the first vaporizing chamber and the first filter, a fifth control device is arranged between the first filter and the vacuum pump, a second control device is arranged between the second vaporizing chamber and the dryer, a fourth control device is arranged between the second vaporizing chamber and the second filter, and a sixth control device is arranged between the second filter and the vacuum pump.
Further, a seventh control device is arranged among the first filter, the second filter and the gas analysis device, the seventh control device is respectively connected with the fifth control device and the sixth control device, and the seventh control device is connected with the dryer.
Further, a first communication device is arranged among the first control device, the second control device and the dryer, a second communication device is arranged among the fifth control device, the sixth control device and the vacuum pump, and the fifth control device and the sixth control device are connected through a third communication device and a seventh control device. A fourth communication device is arranged between the dryer and the gas analysis device, an eighth control device and an air supply device are further arranged between the fourth communication device and the gas analysis device, the eighth control device is respectively connected with the air supply device and the seventh control device, and the first communication device is connected with the fourth communication device.
Further, the first control device, the second control device, the third control device and the fourth control device are all two-position three-way electromagnetic valves, and the fifth control device, the sixth control device, the seventh control device and the eighth control device are all three-way connectors.
Further, the first vaporization chamber and the second vaporization chamber are respectively provided with a sample injection device, the sample injection devices comprise sample injection ports, sample injection diaphragms positioned at the sample injection ports, sample injection needles penetrating through the sample injection diaphragms, and porous screens are further arranged in the sample injection ports.
Further, the side walls of the first vaporization chamber and the second vaporization chamber are provided with temperature control devices.
Further, the gas analysis device is one of a spectrometer, a cavity ring-down spectrometer and a cavity enhanced absorption spectrometer. Other gas analysis devices may be selected as desired.
The second purpose of the invention is realized by adopting the following technical scheme:
the application of the multichannel vaporization detection platform is used for introducing the liquid sample into a gas analysis device after vaporization.
Further, the method comprises the following steps:
(1) Carrying out a purging process on the first vaporizing channel by adopting dry gas, then carrying out a complete purging process for 2-3 times by using a liquid sample to be tested, and entering a state of the sample to be tested after the completion of the purging process;
(2) Injecting a sample to be tested into a first vaporizing chamber, standing until vapor is homogenized, then introducing dry gas, standing, balancing mixed gas in the first vaporizing chamber, and preparing the sample to be tested before testing by a first vaporizing channel; the homogeneity of the vapor sample is ensured by standing, and the concentration and the isotope ratio of the condition sample do not change obviously after the condition sample enters an analysis instrument, so that a quick measurement result can be provided for single measurement of the condition sample, the original liquid sample can be correctly represented, and in addition, the condition sample can be measured for multiple times and averaged, so that the measurement precision is improved;
(3) Introducing the gas of the first vaporization chamber after standing into a gas analysis device, and starting analysis test;
(4) When the gas of the first vaporization channel starts to analyze and test, the second vaporization channel starts to be purged, dry gas is firstly adopted to purge, then the liquid sample to be tested is purged for 2-3 times, and the second vaporization channel enters the state of the sample to be tested;
(5) Injecting a liquid sample to be tested into the second vaporization channel, standing for vapor homogenization, then introducing dry gas, standing for balancing the mixed gas in the second vaporization channel, and preparing the second vaporization channel before testing the sample to be tested;
(6) After the gas analysis device which is used for analyzing the first vaporization channel sample is purged with dry gas, starting to analyze and detect the second vaporization channel sample;
(7) The above process needs to be repeated 2 to 3 times to complete the analysis of one sample. .
Further, the method comprises the steps of starting a temperature control device of the first vaporizing chamber and the second vaporizing chamber, heating the first vaporizing chamber and the second vaporizing chamber to the sample vaporizing temperature at the same time, starting a vacuum pump, and performing air running test air by the gas analysis device.
Further, the step (1) includes:
firstly, opening a first control device and a third control device, purging a first vaporization chamber by gas from a dryer, and absorbing dry gas by a vacuum pump;
closing the first control device, vacuumizing the first vaporization chamber to be in a vacuum state, and closing the third control device;
C, injecting a sample to be detected into the first vaporization chamber through a sample injection needle, starting a first control device after homogenization is completed, enabling dry gas to enter the first vaporization chamber, closing the first control device, and standing and mixing the steam of the sample to be detected and the dry gas uniformly;
d, taking the third control device, completely pumping the uniformly mixed gas by a vacuum pump, and closing the third control device when the first vaporization chamber is in a vacuum state;
And E, injecting a sample through the sample injection device again, repeating the processes of the step C and the step D, and enabling the first gasification channel to enter a state of the sample to be detected.
Further, the step (2) includes:
opening the eighth control device, communicating the dryer with the gas analysis device, and purging the gas analysis device from the dryer;
and B, injecting a sample to be detected into the first vaporization chamber through a sample injection needle, starting the first control device after homogenization is finished, enabling the dry gas to enter the first vaporization chamber, closing the first control device, and standing and uniformly mixing the steam of the sample to be detected and the dry gas.
Further, the step (3) includes synchronously opening the fifth control device and the seventh control device, closing the eighth control device, and allowing the sample vapor to be analyzed to enter the gas analysis device for analysis and test.
Further, the purging process of the second vaporizing path in the step (4) is as follows:
firstly, opening a second control device and a fourth control device, purging a second vaporization chamber by gas from a dryer, and absorbing dry gas by a vacuum pump;
closing the second control device, vacuumizing the second vaporization chamber, and closing the fourth control device;
C, injecting a sample to be detected into the second vaporization chamber through a sample injection needle, starting a second control device after homogenization is completed, enabling dry gas to enter the second vaporization chamber, closing the second control device, and standing and mixing the steam of the sample to be detected and the dry gas uniformly;
d, opening a fourth control device, completely pumping the uniformly mixed gas by a vacuum pump, and closing the fourth control device when the second vaporization chamber is in a vacuum state;
And E, injecting the sample through the sample injection device again, repeating the processes of the step C and the step D, and enabling the second vaporization channel to enter a state of the sample to be detected.
Further, the step (5) includes injecting the sample to be measured into the second vaporization chamber through the sample injection needle, opening the second control device after homogenization is completed, allowing the dry gas to enter the second vaporization chamber, closing the second control device, and standing and mixing the steam of the sample to be measured and the dry gas uniformly.
Further, before the analysis and detection of the second vaporization channel sample in the step (6), the fifth control device is turned off, the sixth control device and the seventh control device are turned on, and the sample in the second vaporization chamber enters the gas analysis device to start the analysis and test.
Compared with the prior art, the application has the beneficial effects that: the application discloses a multi-channel vaporization detection platform, which greatly shortens the sample measurement time by arranging a plurality of vaporization channels, wherein one channel is in purging, static balance and the like during measurement, and the application also provides the application of the multi-channel vaporization detection platform, wherein the purging is carried out by adopting dry gas before sample injection, so as to effectively remove the residual liquid in the vaporization channels, the memory effect is reduced to the greatest extent, then the liquid sample is adopted for purging, the same sample can be better homogenized, the measurement result is more similar to the sample, the result is more accurate, the standard liquid sample is calibrated in a traditional mode, long-time preparation work is needed, and the data in a previous period are needed to be discarded.
Drawings
FIG. 1 is a schematic diagram of a multi-channel vaporization platform according to embodiment 1 of the present invention;
the device comprises a first vaporizing chamber 1, a first filter 2, a first control device 3, a first control device 4, a third control device 5, a fifth control device 6, a second vaporizing chamber 7, a second filter 8, a second control device 9, a fourth control device 10, a sixth control device 11, a first communication device 12, a second communication device 13, a third communication device 14, a fourth communication device 15, a dryer 16, an air supply device 17, a vacuum pump 18, a temperature control device 19, a seventh control device 20, an eighth control device 21, a gas analysis device 22, a sample injection device 222, a sample injection diaphragm 223, a sample injection needle 224 and a porous screen.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and detailed description, wherein it is to be understood that, on the premise of no conflict, the following embodiments or technical features may be arbitrarily combined to form new embodiments.
Example 1
A multichannel vaporization detection platform comprises at least two vaporization channels, as shown in figure 1, wherein the arrows in the figure represent the flowing direction of a sample or gas. In this embodiment, two vaporization channels are included, namely, a first vaporization channel and a second vaporization channel, the first vaporization channel includes a first vaporization chamber 1, a first filter 2, and a second vaporization chamber 6 that are sequentially disposed, and a second filter 7, preferably, the first filter 2 and the second filter 7 are stainless steel sintered filters, so as to ensure the cleanliness of the gas entering the gas analysis device 21. The first and second vaporization chambers 1,6 are in communication with a dryer 15 for providing nitrogen or zero air. The first filter 2 and the second filter 7 are both connected to a gas analysis device 21, and the gas analysis device 21 is connected to a dryer 15 and an air supply device 16, respectively. The preferred gas analysis device 21 is one of a spectrometer, a cavity ring down spectrometer, a cavity enhanced absorption spectrometer. Other gas analysis devices 21 may be selected as needed. The first filter 2 and the second filter 7 are also connected with a vacuum pump 17, and the maximum vacuum degree which can be provided by the vacuum pump 17 is less than 1torr, so that the first vaporizing chamber 1 and the second vaporizing chamber 6 can be vacuumized.
A first control device 3 is arranged between the dryer 15 and the first vaporizing chamber 1, a third control device 4 is arranged between the first vaporizing chamber 1 and the first filter 2, a fifth control device 5 is arranged between the first filter 2 and the vacuum pump 17, a second control device 8 is arranged between the second vaporizing chamber 6 and the dryer 15, a fourth control device 9 is arranged between the second vaporizing chamber 6 and the second filter 7, and a sixth control device 10 is arranged between the second filter 7 and the vacuum pump 17. A seventh control device 19 is provided between the first filter 2, the second filter 7 and the gas analysis device 21, the seventh control device 19 being connected to the fifth control device 5 and the sixth control device 10, respectively, and the seventh control device being connected to the dryer 15.
The first control device 3 and the second control device 8 are connected to the dryer 15 via a first communication device 11, the fifth control device 5 and the sixth control device 10 are connected to the vacuum pump 17 via a second communication device 12, and the fifth and sixth control devices 10 are connected to the seventh control device 19 via a third communication device 13. The dryer 15 is connected to the gas analysis device 21 via the fourth communication device 14, an eighth control device 20 is further provided between the fourth communication device 14 and the gas analysis device 21, the eighth control device 20 is connected to the seventh control device 19 and the air supply device 16, respectively, and the first communication device 11 is connected to the fourth communication device 14.
Preferably, the first control device 3, the second control device 8, the third control device 4 and the fourth control device 9 are two-way solenoid valves, and the two-way solenoid valves are opened to enable gas to pass through when power is supplied and closed to disable gas to pass through when power is not supplied. The fifth control device 5, the sixth control device 10, the seventh control device 19 and the eighth control device 20 are all two-position three-way electromagnetic valves, and the two-position three-way electromagnetic valves indicate that gas passes between the interface A and the interface B when power is supplied, and indicate that gas passes between the interface C and the interface B when power is not supplied. The first communication device 11, the second communication device 12, the third communication device 13 and the fourth communication device 14 are all three-way joints. The control device is not limited to the valve types listed above, and those skilled in the art can select other devices that can realize air path control as needed.
The first vaporization chamber 1 and the second vaporization chamber 6 are both provided with a sample injection device 22, the sample injection device 22 comprises a sample injection diaphragm 222 positioned at a sample injection port, a sample injection needle 223 penetrating through the sample injection diaphragm 222, and a porous screen 224 is also arranged in the sample injection port and used for adsorbing salt in a sample. Specifically, the sample may be injected by selecting an automatic injection needle or manually.
The outer side walls of the first vaporizing chamber 1 and the second vaporizing chamber 6 are provided with a temperature control device 18, and the vaporizing temperature of the sample is reached in the measuring process. Preferably, the temperature control device 18 comprises a heating control module and a temperature sensor (not shown in the figure, and can be set by a person skilled in the art according to the prior art), the temperature of the vaporization chamber is adjusted by the temperature control device 18, and the temperature is kept in a stable range, preferably, heat preservation layers are arranged on the shells of the first vaporization chamber 1 and the second vaporization chamber 6, and heat preservation layers can be arranged on other parts of the vaporization platform, so that the fluctuation range of the temperature is reduced, and the accuracy of detection is ensured. The materials of the first vaporization chamber 1 and the second vaporization chamber 6 are preferably corundum with purity of more than 99 percent, or other materials with weak adsorption and rust-proof surface finish are selected. The embodiment is a two-channel vaporization chamber design, but not limited to this, and the three-channel vaporization chamber can be used for performing the cycle test, or more channels, depending on the size of the sample and the requirement of the measurement time.
Example 2
The application of the multi-channel vaporization platform is used for introducing the liquid sample into the gas analysis device 21 after vaporization, and specifically comprises the following steps:
(1) The temperature control device 18 of the first vaporization chamber 1 and the second vaporization chamber 6 is started, the temperature of the first vaporization chamber 1 and the second vaporization chamber 6 is increased to 140 ℃ at the same time, the vacuum pump 17 is opened, the pressure at the interface of the vacuum pump 17 is enabled to be smaller than 1torr, the pressure of the dryer connected to the fourth communication device 14 is controlled to be in a pressure state of 2.5PSI through the pressure reducing valve, before the sample measurement is not started, all electromagnetic valves serving as control devices are not electrified, and the gas analysis device 21 performs air running test air;
(2) First evaporation channel sample measurement purge:
Firstly, the first control device 3 and the third control device 4 are opened, the first vaporization chamber 1 is purged by the gas nitrogen or zero air from the dryer, and simultaneously, the vacuum pump 17 absorbs the dry gas, and the process lasts for 10s;
Closing the first control device 3, vacuumizing the first vaporizing chamber 1 for 10s, and closing the third control device 4;
injecting 2 microliters of liquid water sample into the first vaporization chamber 1 through a sample injection needle, completely vaporizing the liquid water, homogenizing the water vapor in the first vaporization chamber 1 after 30 seconds, starting the first control device 1s, enabling the dry gas to enter the first vaporization chamber 1, closing the first control device 3, and standing and mixing the vapor of the sample to be tested and the dry gas uniformly, wherein the process is 60 seconds;
The third control device 4 is driven, the vacuum pump 17 completely pumps out the uniformly mixed gas, the duration time is 10s, and the third control device 4 is closed when the first vaporization chamber 1 is in a vacuum state;
E, 2 microliter of liquid water sample is injected again through the sample injection device 22, the processes of the step C and the step D are repeated, the first vaporization chamber 1 enters a vacuum state after the completion, and the first vaporization channel enters a sample state to be detected.
(3) The first vaporisation channel performs sample preparation:
Opening the eighth control device, communicating the dryer with the gas analysis device 21, and purging the gas analysis device 21 from the dryer;
Injecting 2 microliters of liquid water sample to be detected into the first vaporization chamber 1 through a sample injection needle, standing for 30s after the liquid water sample is completely vaporized, homogenizing the water vapor, starting a first control device, closing the first control device 3 after dry gas enters the first vaporization chamber 1 for 1s, and uniformly mixing the steam of the sample to be detected and the dry gas for 90s, wherein the mixed gas is balanced in the first vaporization chamber 1;
(4) Synchronously opening the fifth control device 5 and the seventh control device 19, closing the eighth control device 20, and allowing sample vapor to be analyzed to enter the gas analysis device 21 from the first vaporization chamber 1 for analysis and test, wherein the test time is 270s;
(5) And (3) sample measurement and purging of the second vaporization channel, namely when the gas of the first vaporization channel starts to be analyzed and tested, purging the second vaporization channel, wherein the purging process of the second vaporization channel is as follows:
firstly, the second control device 8 and the fourth control device 9 are opened, nitrogen from the dryer sweeps the second vaporization chamber 6, and simultaneously, the vacuum pump 17 absorbs the drying gas, and the process lasts for 10s;
the second control device 8 is closed, the second vaporization chamber 6 is vacuumized, the process lasts for 10s, and the fourth control device 9 is closed;
And C, injecting 2 microliters of liquid water sample to be detected into the second vaporization chamber 6 through a sample injection needle, completely vaporizing the liquid water, homogenizing the vapor in the second vaporization chamber 6 after 30 seconds, starting the second control device 1s, enabling the dry gas to enter the second vaporization chamber 6, closing the second control device 8, and standing the vapor and the dry gas of the sample to be detected for 60 seconds. Mixing and balancing the gas;
d, opening the fourth control device 9, completely pumping the uniformly mixed gas by the vacuum pump 17 for 10 seconds, and closing the fourth control device 9 when the second vaporization chamber 6 is in a vacuum state;
e, 2 microliter of water liquid sample is injected again through the sample injection device 22, the process of the step C and the process of the step D are repeated, and the second vaporization channel enters the state of the sample to be detected.
(6) And (3) carrying out sample preparation on the second vaporization channel, namely injecting 2 microliter of liquid water sample into the second vaporization chamber 6 through a sample injection needle, standing for 30s after the liquid water sample is completely vaporized, homogenizing the water vapor, starting a second control device, enabling dry gas to enter the second vaporization chamber 6, closing the second control device 8 for 1s, standing and mixing the vapor of the sample to be tested and the dry gas uniformly, standing for 90s, balancing the mixed gas in the second vaporization chamber 6, and preparing the sample to be tested before the second vaporization channel completes the test of the sample to be tested.
(7) At this time, after the measurement of the sample in the first vaporizing channel is completed, the gas analysis device 21 which analyzes the sample in the first vaporizing channel is purged with dry gas, the fifth control device 5 is closed after 60s, the sixth control device 10 and the seventh control device 19 are opened, the sample in the second vaporizing chamber 6 enters the gas analysis device 21, and the analysis and detection of the sample in the second vaporizing channel are started, and the test time is 270s;
(8) The first vaporizing channel repeats the steps (2) and (3), after the sample in the second vaporizing channel is analyzed, the sample in the first vaporizing channel enters the process (4), the second vaporizing channel starts the steps (5) to (7), and the processes in the steps (2) to (7) are repeated for 2-3 times until the analysis of one liquid sample is completed.
Comparative example 1
Comparative example 1 is an analysis of a sample using a conventional platform with only one vaporization chamber.
Compared with comparative example 1, the analysis process has the advantages that the traditional method has only one vaporization chamber, measurement cannot be alternately carried out, three dry gas purges are needed, the former time is 60 seconds, the second time is 90 seconds for each dry gas purges, the third time is 150 seconds for preparing a sample, the sample measuring stage is 270 seconds, the gas analysis device is 60 seconds for purges after the test is finished, and each sample is about 630 seconds. The analysis process of the embodiment 2 of the invention adopts a measurement mode of double-channel detection, and the time for completing one-needle test is about 320 seconds, so that the invention can shorten the detection time and improve the efficiency of sample analysis and measurement.
The above embodiments are only preferred embodiments of the present invention, and the scope of the present invention is not limited thereto, but any insubstantial changes and substitutions made by those skilled in the art on the basis of the present invention are intended to be within the scope of the present invention as claimed.