CN219417353U - Sample injection device for measuring carbon-oxygen stable isotope ratio in carbon dioxide - Google Patents
Sample injection device for measuring carbon-oxygen stable isotope ratio in carbon dioxide Download PDFInfo
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- CN219417353U CN219417353U CN202223533451.0U CN202223533451U CN219417353U CN 219417353 U CN219417353 U CN 219417353U CN 202223533451 U CN202223533451 U CN 202223533451U CN 219417353 U CN219417353 U CN 219417353U
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Abstract
The utility model belongs to the technical field of stable isotope analysis and test, and particularly relates to a sample injection device for measuring carbon-oxygen stable isotope ratio in carbon dioxide. The sample injection device comprises a sample injection mechanism, a gas guide pipe and a water cooling trap; the sample injection mechanism comprises a sample injection tube, a sealing spacer for air inlet of a sample injection needle is arranged at the top of the sample injection tube, a carrier gas sample injection port and a purging outlet are arranged at two corresponding sides of the side part of the sample injection tube, and a shunt port is further arranged at the side part of the sample injection tube; a liner tube is arranged in the sample injection tube, and an air outlet hole is arranged at the bottom of the liner tube; an air outlet pipe penetrating out of the bottom of the air inlet pipe is arranged at the air outlet hole; the air inlet end of the air duct is connected with the air outlet pipe, and the air outlet end of the air duct is connected with the water cooling trap; and the air outlet end of the water cooling trap is connected with a continuous flow system of the stable isotope ratio mass spectrometer. The device has simple structure and low cost, and can provide more choices for carbon-oxygen stable isotope ratio determination of carbon dioxide.
Description
Technical Field
The utility model belongs to the technical field of stable isotope analysis and test, and particularly relates to a sample injection device for measuring carbon-oxygen stable isotope ratio in carbon dioxide.
Background
In recent years, stable isotope technology is widely researched in the fields of geological investigation, hydrologic analysis, archaeological/archaeological environment research, food authenticity and traceability, and stable isotope analysis technology and application of various light elements (such as carbon, oxygen, hydrogen, nitrogen and sulfur) are increasingly reported. However, the stable isotope ratio mass spectrometer can only measure the stable isotope distribution characteristics of the gas consisting of 5 types of light elements, namely carbon dioxide, nitrogen, carbon monoxide, hydrogen and sulfur dioxide, so that various samples are converted into 5 types of gases and then analyzed, wherein carbon dioxide is the most important target in the carbon and oxygen stable isotope analysis field, for example, the carbon and oxygen isotope ratio of carbonate can be measured after the carbonate is converted into carbon dioxide through phosphoric acid; and (3) after the isotope exchange of the water and the carbon dioxide, measuring the oxygen isotope ratio of the carbon dioxide, and obtaining the oxygen isotope ratio of the water.
With the progress of high-precision instrument manufacturing technology, continuous flow systems combined with stable isotope ratio mass spectrometers are the current trend of development and application focus in the isotope analysis field, and the sample demand can be as low as ng level. It can be seen that for isotope analysis in the food field, samples are very easy to obtain, but the cost of analysis is rather drastically increased with expensive high-precision pretreatment equipment.
The present inventors have invented an off-line pretreatment device and method (ZL 201210473455.6) for simple determination of oxygen stable isotope ratio in water as early as 2012, which avoids the dependence on complex/expensive pretreatment systems, uses high purity carbon dioxide for isotope exchange reaction with water, but uses a gas chromatography-stable isotope ratio mass spectrometry system in the sample injection determination stage, wherein the gas chromatography plays a role of connection/gas guide. The high-temperature reaction module is arranged between the gas chromatograph and the isotope ratio mass spectrometer of the combined system and is used for converting the gas chromatograph separated and purified compounds under the high-temperature condition. However, most of the functions of the gas chromatography and high temperature reaction modules are not exerted in practical use.
Disclosure of Invention
The utility model aims to provide a sample injection device for measuring the carbon-oxygen stable isotope ratio in carbon dioxide, which can effectively save the dependence of stable isotope ratio mass spectrometry on a high-precision instrument module in the process of measuring the indexes, can effectively reduce the analysis and test cost, and is beneficial to the popularization of the application of the oxygen isotope technology in water in food adulteration detection.
The utility model provides a sample injection device for measuring carbon-oxygen stable isotope ratio in carbon dioxide, which comprises a sample injection mechanism, a gas guide pipe and a water cooling trap;
the sample injection mechanism comprises a sample injection tube, a sealing spacer for air inlet of a sample injection needle is arranged at the top of the sample injection tube, a carrier gas sample injection port and a purging outlet are arranged at two corresponding sides of the side part of the sample injection tube, and a shunt port is further arranged at the side part of the sample injection tube; a liner tube is arranged in the sample injection tube, and an air outlet hole is arranged at the bottom of the liner tube; an air outlet pipe penetrating out of the bottom of the air inlet pipe is arranged at the air outlet hole;
the air inlet end of the air duct is connected with the air outlet pipe, and the air outlet end of the air duct is connected with the water cooling trap;
and the air outlet end of the water cooling trap is connected with a continuous flow system of the stable isotope ratio mass spectrometer.
Further, the carrier gas inlet and purge outlet are located above the liner.
Further, the air duct is a capillary tube; preferably, the gas guide tube is a capillary chromatographic column; more preferably, the capillary chromatographic column has a length of 0.1m to 100m and a diameter of 0.2mm to 0.5mm.
Further, the air inlet end of the air duct is connected to the air outlet pipe through a graphite gasket, a stainless steel joint and a nut matched with the stainless steel joint;
the air outlet end of the air duct is connected with the water cooling trap through a graphite gasket, a stainless steel joint and a nut matched with the stainless steel joint.
Further, the water-removal trap is connected to the continuous flow system of the stable isotope ratio mass spectrometer by a graphite gasket, a stainless steel joint, and a nut matching the stainless steel joint.
The utility model has the following advantages:
the sample injection device for measuring the carbon-oxygen stable isotope ratio in the carbon dioxide, which is created by the utility model, does not need to be arranged outside alone, but only adds the sample injection device on the stable isotope ratio mass spectrometer containing the continuous flow system, thereby realizing the measurement of the carbon-oxygen isotope ratio in the carbon dioxide sample, expanding the function of the stable isotope ratio mass spectrometer containing the continuous flow system, avoiding purchasing a full-automatic balance instrument (about 60 ten thousand) and a gas chromatography matching device (about 80 ten thousand) and reducing the analysis cost. The sample injection device has low cost and can provide more choices for carbon-oxygen stable isotope ratio determination of carbon dioxide.
Drawings
The accompanying drawings, which are included to provide a further understanding of the utility model and are incorporated in and constitute a part of this specification, illustrate embodiments of the utility model and together with the description serve to explain the utility model. In the drawings:
FIG. 1 is a schematic view of a device structure according to an embodiment of the present utility model;
reference numerals illustrate:
a sample injection mechanism 1; a sample inlet tube 11; liner 12; a sealing spacer 13; a carrier gas inlet 14; purge outlet 15; a shunt port 16; an air outlet hole 17; an outlet duct 18;
an air duct 2;
except for the water-cooled trap 3.
Detailed Description
It should be noted that, without conflict, the embodiments of the present utility model and features of the embodiments may be combined with each other.
Currently, many stable isotopesThe ratio mass spectrometer is equipped with a continuous flow system, so that the analysis and test of stable isotopes are extremely dependent on pretreatment equipment, but a gas chromatograph and a high-temperature reaction module are not necessarily arranged, in which case, if the analysis and test of carbon-oxygen isotopes in a carbon dioxide gas sample are to be carried out, a separate pretreatment system, such as a gas chromatograph (matched high-temperature reaction module), or a fully automatic water-CO system is required to be arranged outside the stable isotope ratio mass spectrometer 2 Balancing the system, all of which can make the overall cost prohibitive.
Referring to fig. 1, an embodiment of the present utility model provides a sample injection device for determining a carbon-oxygen stable isotope ratio in carbon dioxide, which includes a sample injection mechanism 1, a gas guide tube 2 and a water removal trap 3;
the sample injection mechanism 1 comprises a sample injection tube 11, a sealing spacer 13 for feeding air to a sample injection needle is arranged at the top of the sample injection tube 11, a carrier gas sample injection port 14 and a purge outlet 15 are arranged at two corresponding sides of the side part of the sample injection tube 11, and a shunt port 16 is further arranged at the side part of the sample injection tube 11; a liner tube 12 is arranged in the sample injection tube 11, and an air outlet hole 17 is arranged at the bottom of the liner tube 12; an air outlet pipe 18 penetrating out of the bottom of the air inlet pipe 11 is arranged at the air outlet hole 17;
the air inlet end of the air duct 2 is connected with an air outlet pipe 18, and the air outlet end of the air duct 2 is connected with a water cooling trap 3;
the air outlet end of the water cooling trap 3 is connected with a continuous flow system of the stable isotope ratio mass spectrometer.
In one embodiment of the utility model, the carrier gas inlet 14 and purge outlet 15 are located above liner 12.
Further, the shunt opening 16 is positioned in the middle of the sample tube 11.
In one embodiment of the utility model, a seal may be provided between the components to ensure tightness. For example, a sealing piece can be arranged between the air outlet pipe 18 and the air guide pipe 2 and between the air guide pipe 2 and the water-cooling trap 3 to ensure the tightness of the device.
In an embodiment of the utility model, the air duct is a capillary tube. Preferably, the gas guide tube is a capillary chromatographic column. More preferably, the capillary chromatographic column has a length of 0.1m or more and a diameter of 0.2mm to 0.5mm.
In one embodiment of the utility model, the air outlet pipe 18, the air guide pipe 2, the water-removing trap 3 and the continuous flow system of the stable isotope ratio mass spectrometer are all connected through a graphite gasket, a stainless steel joint and a nut matched with the stainless steel joint.
Specifically, the air inlet end of the air duct is connected to the air outlet pipe of the sample injection pipe through a graphite gasket, a stainless steel joint and a nut matched with the stainless steel joint; the air outlet end of the air duct is connected with the water cooling trap through a graphite gasket, a stainless steel joint and a nut matched with the stainless steel joint.
In one embodiment of the utility model, the water-removal trap is connected to the continuous flow system of the stable isotope ratio mass spectrometer by a graphite washer, a stainless steel fitting, and a nut that mates with the stainless steel fitting.
Therefore, after the sample injection mechanism is adopted, the gas chromatograph does not need to be installed for auxiliary sample injection, and the sample injection mechanism can be independently fixed on a bracket for use.
The embodiment of the utility model also provides a method for measuring the carbon-oxygen stable isotope ratio in carbon dioxide, which comprises the following steps:
the method comprises the steps of measuring by adopting a stable isotope ratio mass spectrometer connected with a continuous flow system, connecting the stable isotope ratio mass spectrometer of the continuous flow system with a sample injection device, injecting a carbon dioxide sample into the sample injection device by a sample injection needle, and transferring the carbon dioxide sample to the stable isotope ratio mass spectrometer through a carrier gas through an air duct 2 and a water removal trap 3 to perform carbon-oxygen stable isotope ratio test;
the sample injection device comprises a sample injection mechanism 1, a gas guide tube 2 and a water removal trap 3;
the sample injection mechanism 1 comprises a sample injection tube 11, a sealing spacer 13 for feeding air to a sample injection needle is arranged at the top of the sample injection tube 11, a carrier gas sample injection port 14 and a purge outlet 15 are arranged at two corresponding sides of the side part of the sample injection tube 11, and a shunt port 16 is further arranged at the side part of the sample injection tube 11; a liner tube 12 is arranged in the sample injection tube 11, and an air outlet hole 17 is arranged at the bottom of the liner tube 12; an air outlet pipe 18 penetrating out of the bottom of the air inlet pipe 11 is arranged at the air outlet hole 17;
the air inlet end of the air duct 2 is connected with the bottom of the air outlet pipe 18, and the air outlet end of the air duct 2 is connected with the water cooling trap 3;
the air outlet end of the water cooling trap 3 is connected with a continuous flow system of the stable isotope ratio mass spectrometer.
Specifically, carrier gas and carbon dioxide enter the gas guide pipe 2 from the gas outlet pipe 18, then enter the stable isotope ratio mass spectrometer containing a continuous flow system for testing after water is removed through the water-removing trap 3.
In one embodiment of the present utility model, the carrier gas may be helium.
In the embodiment of the utility model, the device can be used for expanding the measurement function of the carbon-oxygen stable isotope ratio of the carbon dioxide in the high-concentration sample on any stable isotope ratio mass spectrometer without being provided with a commercial import equipment unit, thereby greatly reducing the experiment cost.
The working of the utility model will be explained in detail below with reference to examples and figures.
Example 1 a method for determining the carbon to oxygen stable isotope ratio in carbon dioxide comprising the steps of:
(1) The respective connection members in the apparatus of fig. 1 were screwed down, and the air tightness was verified to prevent air leakage.
(2) Purging impurity gas in the sample injection device by helium;
(3) Setting a measurement program of a stable isotope ratio mass spectrometer: introducing carbon dioxide reference gas into a mass spectrometer at 20 s-40 s, 70 s-90 s and 120 s-140 s respectively;
(4) 2uL of gas is taken from an air bag or a headspace bottle filled with a carbon dioxide sample by using a 10uL airtight sample injection needle, injected into a sample injection device, and the carbon-oxygen stable isotope ratio (delta) of carbon dioxide is measured by using a stable isotope ratio mass spectrometer 13 C and delta 18 O)。
Example 2
3mL of wine sample is filled into a headspace bottle, carbon dioxide is filled and air is discharged, and after standing for 16h, gas is continuously taken and injected for 8 times according to the method in example 1, and delta is measured 13 C and delta 18 O and tracking the signal strength of m/z=44, the results are shown in table 1.
TABLE 1 carbon dioxide sample delta 13 C and delta 18 O measurement result (mill)
Statistical analysis of the data in Table 1 shows that delta was measured at 10 gas sampling 13 The standard deviation of C is 0.040 per mill, delta 18 The standard deviation of O is 0.058 per mill, the standard deviation meets the measurement requirement of a stable isotope ratio mass spectrometer (the internal precision is better than 0.065 per mill, the two independent measurement precision is better than 0.2 per mill), and the m/z=44 signal intensity can be kept between 5500 and 5900mv when gas and sample are taken for 10 times, which is completely different from the trend that the signal intensity is reduced in a curve when the full-automatic balance meter is used for measurement.
It should be understood that the foregoing description is only of the preferred embodiments of the present utility model and is not intended to limit the utility model, but is intended to cover all modifications, equivalents, alternatives, and modifications falling within the spirit and principles of the utility model.
Claims (7)
1. A sample injection device for measuring carbon-oxygen stable isotope ratio in carbon dioxide is characterized by comprising a sample injection mechanism, a gas guide pipe and a water cooling trap;
the sample injection mechanism comprises a sample injection tube, a sealing spacer for air inlet of a sample injection needle is arranged at the top of the sample injection tube, a carrier gas sample injection port and a purging outlet are arranged at two corresponding sides of the side part of the sample injection tube, and a shunt port is further arranged at the side part of the sample injection tube; a liner tube is arranged in the sample injection tube, and an air outlet hole is arranged at the bottom of the liner tube; an air outlet pipe penetrating out of the bottom of the air inlet pipe is arranged at the air outlet hole;
the air inlet end of the air duct is connected with the air outlet pipe, and the air outlet end of the air duct is connected with the water cooling trap;
and the air outlet end of the water cooling trap is connected with a continuous flow system of the stable isotope ratio mass spectrometer.
2. The sample introduction device of claim 1, wherein the sample introduction device comprises a sample introduction device,
and the carrier gas inlet and the purging outlet are positioned above the liner tube.
3. The sample introduction device of claim 1, wherein the sample introduction device comprises a sample introduction device,
the air duct is a capillary tube.
4. The sample introduction device of claim 3, wherein,
the air duct is a capillary chromatographic column.
5. The sample introduction device of claim 4, wherein,
the length of the capillary chromatographic column is 0.1-100 m, and the diameter is 0.2-0.5 mm.
6. The sample introduction device of claim 1, wherein the sample introduction device comprises a sample introduction device,
the air inlet end of the air duct is connected to the air outlet pipe through a graphite gasket, a stainless steel joint and a nut matched with the stainless steel joint;
the air outlet end of the air duct is connected with the water cooling trap through a graphite gasket, a stainless steel joint and a nut matched with the stainless steel joint.
7. The sample introduction device of claim 1, wherein the sample introduction device comprises a sample introduction device,
the water-cooling trap is connected to a continuous flow system of the stable isotope ratio mass spectrometer through a graphite gasket, a stainless steel joint and a nut matched with the stainless steel joint.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202223533451.0U CN219417353U (en) | 2022-12-29 | 2022-12-29 | Sample injection device for measuring carbon-oxygen stable isotope ratio in carbon dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202223533451.0U CN219417353U (en) | 2022-12-29 | 2022-12-29 | Sample injection device for measuring carbon-oxygen stable isotope ratio in carbon dioxide |
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| CN219417353U true CN219417353U (en) | 2023-07-25 |
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| CN202223533451.0U Active CN219417353U (en) | 2022-12-29 | 2022-12-29 | Sample injection device for measuring carbon-oxygen stable isotope ratio in carbon dioxide |
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