Integrated Sampling Device for Liquefied Gas, Cylinder Gas and Gas in Sampling Bag

Abstract

The present invention provides an integrated sampling device for liquefied gas, cylinder gas and sampling bag gas, which has a liquefied gas sample sampling device, a gas sample sampling device and a sample gas bag. The liquefied gas sample sampling device is connected to a heating device through a liquid path cut-off valve and a liquid path flow-limiting tube, and then connected to the inlet of a first switching valve; the gas sample sampling device is connected to the other inlet of the first switching valve through a gas path cut-off valve and a gas path flow-limiting tube; the outlet of the first switching valve is connected to the inlet of a flow observation window, the outlet of the flow observation window is connected to the first port of a drain tee, a pipeline is reserved at the second port of the drain tee and can be led to an exhaust device, and the third port of the drain tee is connected to the inlet of a second switching valve; the other inlet of the second switching valve is connected to the sample gas bag; the outlet of the second switching valve is sequentially connected to a sampling / injection valve, an injection / drain valve and a sampling tee, and the sampling tee is also connected to a carrier gas and an analytical instrument.

Description

Technical Field

[0001] The invention relates to an integrated sample introduction device for component and content analysis of liquefied gas samples, cylinder gas samples and sampling bag samples. Background Art

[0002] When analyzing the components and contents of liquefied gas samples, cylinder gas samples and sampling bag samples, since the samples have different shapes and pressures, and the analytical instruments have requirements for the shape and pressure of the samples, it is necessary to process the samples in different forms, and process the liquefied gas samples, cylinder gas samples and collection bag samples into gases with the same shape and pressure. This eliminates the need to correct the measurement results due to the different shapes of the samples, thereby ensuring the accuracy and uniformity of the measurement results of different samples; it also reduces manual operations and enables repeated analysis of the same sample.

[0003] Liquefied gas: Liquefied gas samples exist in the cylinder in both gaseous and liquid forms, which means that some heavy components in the sample exist more in the liquid state, while light components exist more in the gas state; the liquid part is more uniform and representative than the gaseous part, so the liquid part should be sampled for component and content analysis. Due to the particularity of liquefied gas samples, a certain pressure must be maintained inside the cylinder to keep the sample in a gas-liquid equilibrium state; when the sample is reduced, in order to maintain the pressure, part of the liquid sample will be converted into gas to maintain gas-liquid equilibrium.

[0004] When the taken liquid sample is placed in an environment with a pressure lower than its liquefaction pressure, the liquid sample will vaporize, but a considerable portion of the heavy components cannot be completely vaporized and need to be heated to completely vaporize them. Therefore, liquefied gas samples require additional heating devices to fully vaporize the samples.

[0005] Cylinder gas: When using cylinders to collect gas samples, the internal pressure varies and may change as the analysis proceeds, so the cylinder pressure needs to be adjusted to maintain the same pressure during injection.

[0006] Sampling bag gas: When using an air bag to collect gas samples, the air bag has very limited pressure resistance and cannot maintain too much pressure. It is impossible to inject the sample into the analyzer by relying on its own pressure. Summary of the invention

[0007] In summary, the forms, pressures and component uniformities of liquefied gas, cylinder gas and sampling bag gas are all different. In order to be able to use one device to analyze both liquefied gas samples and cylinder gas and sampling bag gas, the present invention provides an integrated sampling device for liquefied gas, cylinder gas and sampling bag gas, which can process the above three forms of samples into devices with the same form and pressure, and can perform component and content analysis on the same analytical instrument.

[0008] To achieve the above object, the technical solution adopted by the present invention is:

[0009] An integrated sampling device for liquefied gas, cylinder gas and sampling bag gas, characterized in that it comprises a liquefied gas sample sampling device, a gas sample sampling device and a sample gas bag, wherein:

[0010] The liquefied gas sample injection device is connected to the heating device through the liquid circuit stop valve and the liquid circuit flow limiting tube, and then connected to the inlet of the first switching valve;

[0011] The gas sample injection device is connected to another inlet of the first switching valve through a gas circuit stop valve and a gas circuit flow limiting tube;

[0012] The outlet of the first switching valve is connected to the inlet of the flow observation window, the outlet of the flow observation window is connected to one of the working ports of the emptying tee, the other two working ports of the emptying tee are respectively connected to the exhaust device and the inlet of the second switching valve, and the other inlet of the second switching valve is connected to the sample air bag;

[0013] The outlet of the second switching valve is connected to the sampling / injection valve, the injection / drain valve and the injection tee in sequence, and the injection tee is also connected to the carrier gas and the analytical instrument.

[0014] The integrated sampling device for liquefied gas, cylinder gas and sampling bag gas, wherein: the common port of the second switching valve is connected to a port of the sampling / injection valve, and the common port of the sampling / injection valve is connected to the syringe;

[0015] The other port of the sampling / injection valve is connected to the common port of the injection / drain valve, and the two outlets of the injection / drain valve are respectively connected to the self-ventilation system and a working port of the injection tee.

[0016] The integrated sampling device for liquefied gas, cylinder gas and sampling bag gas, wherein: another working port of the sampling tee is connected to the carrier gas, and the last working port is directly connected to the analytical instrument or is connected to the analytical instrument after being mixed with the carrier gas by a mixer.

[0017] The integrated sampling device for liquefied gas, cylinder gas and sampling bag gas, wherein: the mixer is a double-layer structure, one end of the inner tube has a No. 1 interface, the other end extends into the outer tube and is in close contact with the outer tube, one end of the outer tube is opposite to the extending end of the inner tube and has a No. 2 interface, and the side of the other end of the outer tube is provided with an outlet; the No. 1 interface is connected to the last working port of the sampling tee, the No. 2 interface is for carrier gas to enter, and the outlet is connected to the analytical instrument.

[0018] The integrated sampling device for liquefied gas, cylinder gas and sampling bag gas, wherein: the heating device is equipped with a temperature control device, a U-shaped quartz tube is placed in the heating device, and the two tube ends of the U-shaped quartz tube are placed vertically upward, the two tube ends are placed up and down, or tilted.

[0019] The integrated sampling device for liquefied gas, cylinder gas and sampling bag gas, wherein: the liquid path flow limiting tube and the gas path flow limiting tube are both made of peek material or polytetrafluoro material or passivated stainless steel material.

[0020] The integrated sampling device for liquefied gas, cylinder gas and sampling bag gas, wherein: a flow observation window is provided on the pipeline between the first switching valve and the exhaust tee.

[0021] The integrated sampling device for liquefied gas, cylinder gas and sampling bag gas, wherein: the liquefied gas sample sampling device is equipped with a cylinder rack, the liquefied gas sample cylinder is vertically or obliquely inverted on the cylinder rack, the liquid bottle switch valve of the liquefied gas sample cylinder is connected downstream with a liquid bottle filter and an opening of a liquid bottle tee in sequence, the other two openings of the liquid bottle tee are respectively connected to the downstream sampling pipeline and the liquid circuit manual stop valve, the liquid circuit manual stop valve is connected to the drain pipeline, and the liquid circuit manual stop valve is in a closed state under normal circumstances.

[0022] The integrated sampling device for liquefied gas, cylinder gas and sampling bag gas, wherein: the gas sample sampling device is equipped with a cylinder rack, an opening of the cylinder tee is connected downstream of the cylinder switch valve of the gas sample cylinder, the other two openings of the cylinder tee are respectively connected to the downstream sampling pipeline and the manual gas circuit stop valve, the manual gas circuit stop valve is connected to the exhaust pipeline, and the manual gas circuit stop valve is in a closed state under normal circumstances.

[0023] The present invention can not only realize automatic cleaning between samples, but also realize consistency of gas pressure inhaled into a syringe, thereby ensuring that the states of liquefied gas samples, cylinder gas samples and air bag samples during injection are completely consistent, and there is no need to calibrate for different types of samples, thereby ensuring the accuracy of measurement results of different samples. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 It is a structural schematic diagram of the liquefied gas sample injection device of the present invention.

[0025] Figure 2 It is a structural schematic diagram of the gas sample injection device of the present invention.

[0026] Figure 3 It is a schematic diagram of the overall structure of the present invention.

[0027] Figure 4 It is a schematic diagram of the overall structure of another embodiment of the present invention.

[0028] Figure 5 It is a structural diagram of the mixer. DETAILED DESCRIPTION

[0029] like Figure 1 As shown, it is a liquefied gas sample injection device of the present invention, which has a cylinder rack 11, and a liquefied gas sample cylinder 12 is vertically or obliquely inverted on the cylinder rack 11 (in this way, it can be ensured that the gaseous form of the sample in the liquefied gas sample cylinder 12 is at the upper part, and the liquid form is at the lower part, so that the liquid part of the sample can be taken), the liquefied gas sample cylinder can be installed with a liquid bottle pressure gauge 13, and the end where the liquid bottle pressure gauge is installed should generally be above the liquefied gas sample cylinder 12, and the downstream of the liquid bottle switch valve 14 of the liquefied gas sample cylinder 12 is connected with a liquid bottle filter 15 and a liquid bottle tee 16 in sequence, and the other two openings of the liquid bottle tee 16 are respectively connected to the downstream injection pipeline and one port of the liquid manual stop valve 20, and the other port of the liquid manual stop valve 20 is connected to the drain pipe The manual stop valve 20 is normally closed; since most liquefied gases contain tiny solid particles, the liquid bottle filter 15 can avoid clogging the sample pipeline and also avoid damaging the components of the sampling device; in order to avoid cross contamination between different samples and to achieve rapid flushing of the samples, the liquid bottle tee 16 is installed to connect the manual stop valve 20; before replacing the liquefied gas sample cylinder 12, the liquid bottle switch valve 14 is closed, and the liquid circuit manual stop valve 20 is opened to quickly empty the original sample in the pipeline; after replacing the liquefied gas sample cylinder 12, the liquid bottle switch valve 14 is opened, and since the liquid circuit manual stop valve 20 is in an open state, the current sample can be used to quickly flush the pipeline, and then the liquid circuit manual stop valve 20 is closed, so that cross contamination can be avoided;

[0030] like Figure 2As shown, the gas sample injection device of the present invention is a gas sample cylinder. The gas in the gas sample cylinder is uniform gas. Whether taking the upper part or the lower part of the sample, the uniformity of the sample can be guaranteed. Therefore, the gas sample cylinder can be placed horizontally, vertically or tilted. However, for safety reasons, the present invention also places the gas sample cylinder 22 on another cylinder rack 21. The gas sample cylinder can be installed with a cylinder pressure gauge 23. The end where the cylinder pressure gauge 23 is installed should generally be at the top. The downstream of the switch valve 24 of the gas sample cylinder 22 is connected to the cylinder tee 26 and the pressure reducing valve 27 in sequence. The cylinder tee 26 is also connected to one port of the manual gas circuit stop valve 25. The other port of the manual gas circuit stop valve 25 is connected to the emptying pipeline. The manual gas circuit stop valve 25 is normally closed. In order to avoid cross contamination between different samples and realize rapid flushing of samples, the cylinder tee 26 and the manual gas circuit stop valve 25 are installed. Before replacing the gas sample cylinder 22, the cylinder is opened. The shut-off valve 24 is closed, and the manual gas circuit stop valve 25 is opened to quickly drain the original sample in the pipeline; after replacing the gas sample cylinder 22, the cylinder switch valve 24 is opened. Since the manual gas circuit stop valve 25 is in an open state, the pipeline can be quickly flushed with the current sample, and then the manual gas circuit stop valve 25 is closed, so that cross contamination can be avoided; since the pressures in the gas sample cylinders 22 are different, when the filling pressure is very high, it is possible to damage the device by sampling. The present invention installs the pressure reducing valve 27 on the downstream sampling pipeline of the gas cylinder tee 26 to ensure that the outlet pressures of different sample sources are roughly the same;

[0031] like Figure 3 , Figure 4 , which is a schematic diagram of the overall structure of the present invention, a liquid circuit stop valve 17 is provided on the downstream injection pipeline of the liquid bottle tee 16 of the liquefied gas sample injection device, and the downstream of the liquid circuit stop valve 17 is connected to the heating device 19 through the liquid circuit limiting pipe 18, and then connected to the inlet of the first switching valve 41;

[0032] A gas circuit stop valve 28 is provided on the downstream sampling pipeline connected to the gas cylinder tee 26 of the gas sample injection device via a pressure reducing valve 27, and the downstream of the gas circuit stop valve 28 is connected to another inlet of the first switching valve 41 via a gas circuit limiting pipe 29;

[0033] The outlet of the first switching valve 41 is connected to the inlet of the flow observation window 50, and the outlet of the flow observation window 50 is connected to one of the working ports of the exhaust tee 42. The other two working ports of the exhaust tee 42 are respectively connected to an exhaust device (such as a fume hood or an exhaust hood) and the inlet of the second switching valve 43. The other inlet of the second switching valve 43 is connected to the sample air bag 30.

[0034] The common port of the second switching valve 43 is connected to one port of the sampling / injection valve 44, and the common port of the sampling / injection valve 44 is connected to the syringe 45;

[0035] The other port of the sampling / injection valve 44 is connected to the common port of the injection / drain valve 46, and the two outlets of the injection / drain valve 46 are respectively connected to the self-ventilation system and a working port of the injection tee 47;

[0036] Another working port of the injection tee 47 is connected to the carrier gas, and the last working port is directly connected to the analytical instrument 48 (such as Figure 3 ) or mixed with carrier gas through mixer 49 and connected to analytical instrument 48 (such as Figure 4 ).

[0037] in:

[0038] Components and fittings used in the sampling device should be made of quartz, peek, polytetrafluoroethylene or stainless steel as much as possible to avoid adsorption of gas samples.

[0039] Because most gas samples and liquefied gas samples are flammable and explosive, in order to avoid the accumulation of emptied samples in the room, an exhaust hood should be installed above the instrument or a fume hood should be placed near the instrument. The emptied samples through the liquid manual stop valve 20, the gas manual stop valve 25, the exhaust tee 42 and the injection / exhaust valve 46 should be discharged into the exhaust hood or fume hood through pipelines.

[0040] The heating device 19 is equipped with a temperature control device, which can set the required temperature as needed and maintain a constant temperature during the entire test process. To ensure that the sample is completely gasified, a U-shaped quartz tube is placed in the heating device 19, and the U-shaped quartz tube cannot be placed horizontally in the heating device 19, but can be placed vertically with the two tube openings facing upward, placed up and down, or tilted.

[0041] When the two ends of the U-shaped quartz tube are placed vertically upward, any end can be used as the air inlet; when the two ends are placed upside down or tilted, only the end at the bottom can be used as the air inlet.

[0042] The heating area of ​​the U-shaped tube can be doubled compared to that of the straight tube, and the above placement method can ensure to the greatest extent that only the completely vaporized part enters the analysis instrument 48.

[0043] The liquid flow limiting tube 18 and the gas flow limiting tube 29 are both microporous tubes, made of peek material, polytetrafluoroethylene material, passivated stainless steel material or other materials that have no adsorption or low adsorption to the analysis components;

[0044] The gasified liquefied gas sample and the cylinder gas sample pass through the flow observation window 50, and the float position can be used to determine whether there is gas flowing out, thereby ensuring that there is sample entering the sampling device.

[0045] The structure of the mixer 49 is as follows Figure 5 As shown, it is a double-layer structure, one end of the inner tube has a No. 1 interface 491, and the other end extends into the outer tube and is in close contact with the outer tube. One end of the outer tube is opposite to the extending end of the inner tube and has a No. 2 interface 492, and the side of the other end of the outer tube is provided with an outlet 493.

[0046] exist Figure 4 In the illustrated embodiment, interface No. 1 491 is connected to the last working port of the injection tee 47, interface No. 2 492 is for carrier gas to enter, and the outlet 493 is connected to the analytical instrument 48; by virtue of the relative blowing of the airflows of interface No. 1 491 and interface No. 2 492, uniform mixing of the sample can be achieved.

[0047] When the present invention is used, by means of the switching operation of the first switching valve 41 and the second switching valve 43, any one of the liquefied gas sample injection device, the gas sample injection device, and the sample gas bag 30 can be selected as the sample gas source; this is a basic operation in the art and will not be described in detail here;

[0048] When the liquefied gas sample injection device is selected as the sample gas source, the liquid sample in the liquefied gas sample cylinder 12 is connected to the sampling / injection valve 44 through the liquid bottle filter 15, the liquid bottle tee 16, the liquid circuit stop valve 17, the liquid circuit limiting tube 18, the heating device 19 (converted into gas), the first switching valve 41, the flow observation window 50, the emptying tee 42, and the second switching valve 43;

[0049] When the gas sample injection device is selected as the sample gas source, the gas sample in the gas sample cylinder 22 is connected to the sampling / injection valve 44 through the gas cylinder tee 26, the pressure reducing valve 27, the gas circuit stop valve 28, the gas circuit flow limiting tube 29, the first switching valve 41, the flow observation window 50, the emptying tee 42, and the second switching valve 43;

[0050] When the sample gas bag 30 is selected as the sample gas source, the gas sample in the sample gas bag 30 is connected to the sampling / injection valve 44 via the second switching valve 43;

[0051] After the gas sample is connected to the sampling / injection valve 44, the negative pressure generated by the suction of the syringe 45 can cause the gas sample to enter the syringe 45 to achieve quantitative sampling; then the connection relationship of the sampling / injection valve 44 is switched, and the syringe 45 is pushed again to send the gas sample into the injection / emptying valve 46;

[0052] At this time, if the injection / drain valve 46 is switched to be connected to the ventilation system, sample cleaning can be achieved; if the injection / drain valve 46 is switched to be connected to the injection tee 47, injection operation can be achieved; by virtue of the injection action of the syringe 45 and the switching action of the injection / drain valve 46, no matter which of the optional liquefied gas sample injection device, the gas sample injection device and the sample gas bag 30 is used as the sample gas source, the injection state of the gas sample can be unified;

[0053] After the gas sample enters the injection tee 47, it enters the analysis instrument 48 under the carrier gas for subsequent analysis.

[0054] The present invention can not only realize automatic cleaning between samples, but also realize consistency of gas pressure in the suction syringe 45, thereby ensuring that the states of liquefied gas samples, cylinder gas samples and air bag samples during injection are completely consistent, and no calibration is required for different types of samples, thereby ensuring the accuracy of measurement results of different samples.

[0055] By installing the integrated sampling device for liquefied gas, cylinder gas and sampling bag gas of the present invention on an ultraviolet fluorescence sulfur analyzer, the sulfur content of liquefied gas samples, cylinder gas samples and sampling bag gas is analyzed. It is found that after the ultraviolet fluorescence sulfur analyzer uses this device to analyze standard samples, a standard curve that meets the requirements can be obtained.

[0056] In addition, liquefied gas samples, cylinder gas samples and sampling bag gas samples were tested separately. From the obtained measurement results, it can be seen that the parallelism of the samples is very good and can meet the test requirements.

[0057] The above description is only illustrative rather than restrictive of the present invention. Those skilled in the art will understand that many modifications, changes or equivalents may be made without departing from the spirit and scope defined by the claims, but all will fall within the scope of protection of the present invention.

Claims

1. An integrated sampling device for liquefied gas, cylinder gas and sampling bag gas, characterized in that: it has a liquefied gas sample injection device, a gas sample injection device and a sample gas bag, wherein: the liquefied gas sample injection device is connected to a heating device through a liquid line stop valve and a liquid line flow limiter tube, and then connected to the inlet of a first switching valve; the gas sample injection device is connected to the other inlet of the first switching valve through a gas line stop valve and a gas line flow limiter tube; the outlet of the first switching valve is connected to the inlet of a flow observation window, the outlet of the flow observation window is connected to one of the working ports of an exhaust tee, and the other two working ports of the exhaust tee are respectively connected to an exhaust device and the inlet of a second switching valve, and the other inlet of the second switching valve is connected to the sample gas bag; the outlet of the second switching valve is sequentially connected to a sampling / injection valve, an injection / vent valve and an injection tee, and the injection tee is also connected to a carrier gas and an analytical instrument; wherein, the common port of the second switching valve is connected to one port of the sampling / injection valve, and the common port of the sampling / injection valve is connected to a syringe; the other port of the sampling / injection valve is connected to the common port of the injection / vent valve, and the two outlets of the injection / vent valve are respectively connected to a self-ventilation system and one of the working ports of the injection tee; wherein, the other working port of the injection tee is connected to a carrier gas, and the last working port is directly connected to the analytical instrument or connected to the analytical instrument after being mixed with the carrier gas through a mixer; wherein, downstream of the liquid bottle switch valve of the liquefied gas sample cylinder, a liquid bottle filter and one opening of a liquid bottle tee are sequentially connected, and the other two openings of the liquid bottle tee are respectively connected to a downstream sampling pipeline and a manual liquid line stop valve, and the manual liquid line stop valve is connected to an exhaust pipeline, and the manual liquid line stop valve is in a closed state under normal conditions.

2. The integrated sampling device for liquefied gas, cylinder gas and sampling bag gas according to claim 1, characterized in that: the mixer is of a double-layer structure, one end of the inner tube has a No. 1 interface, the other end extends into the outer tube and is in close contact with the outer tube, one end of the outer tube is opposite to the extending end of the inner tube and has a No. 2 interface, and the side of the other end of the outer tube is provided with an outlet; the No. 1 interface is connected to the last working port of the injection tee, the No. 2 interface allows the carrier gas to enter, and the outlet is connected to the analytical instrument.

3. The integrated sampling device for liquefied gas, cylinder gas and sampling bag gas according to claim 1, characterized in that: the heating device is equipped with a temperature control device, a U-shaped quartz tube is placed in the heating device, and the two tube openings of the U-shaped quartz tube are placed vertically upward, placed one above the other or placed obliquely.

4. The integrated sampling device for liquefied gas, cylinder gas and sampling bag gas according to claim 1, characterized in that: both the liquid line flow limiter tube and the gas line flow limiter tube are made of peek material, or polytetrafluoro material, or passivated stainless steel material.

5. The integrated sampling device for liquefied gas, cylinder gas and sampling bag gas according to claim 1, characterized in that: a flow observation window is provided on the pipeline between the first switching valve and the exhaust tee.

6. The integrated sampling device for liquefied gas, cylinder gas and sampling bag gas according to claim 1, characterized in that: the liquefied gas sample injection device is equipped with a cylinder rack, and the liquefied gas sample cylinder is placed vertically or inclinedly upside down on the cylinder rack.

7. The integrated sampling device for liquefied gas, cylinder gas and sampling bag gas according to claim 1, characterized in that: the gas sample injection device is equipped with a cylinder rack, one opening of a cylinder tee is connected downstream of the cylinder switch valve of the gas sample cylinder, and the other two openings of the cylinder tee are respectively connected to the downstream injection pipeline and the manual gas circuit shut-off valve, and the manual gas circuit shut-off valve is connected to the evacuation pipeline, and the manual gas circuit shut-off valve is in a closed state under normal conditions.

Images