CN109745880B - Trace gas transfer device and method - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000007789 gas Substances 0.000 claims description 237
- 239000002994 raw material Substances 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 17
- 238000004140 cleaning Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- UUDAMDVQRQNNHZ-UHFFFAOYSA-N (S)-AMPA Chemical compound CC=1ONC(=O)C=1CC(N)C(O)=O UUDAMDVQRQNNHZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 15
- 238000005303 weighing Methods 0.000 abstract description 8
- 238000010790 dilution Methods 0.000 abstract description 5
- 239000012895 dilution Substances 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 28
- 229910000831 Steel Inorganic materials 0.000 description 13
- 239000010959 steel Substances 0.000 description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 229910000838 Al alloy Inorganic materials 0.000 description 4
- 238000004364 calculation method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004868 gas analysis Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention relates to a preparation technology of mixed gas, in particular to a micro gas transfer device and a micro gas transfer method. Solves the technical problem that the preparation of trace gas is difficult to repeatedly dilute in the prior mixed gas preparation. A trace gas transfer apparatus includes a conduit; the system also comprises a component mixed gas cylinder connected to one end of the pipeline and at least one balance gas cylinder connected to the other end of the pipeline; the valve P8, the first branch, the second branch, the third branch, the fourth branch, the fifth branch and the valve P5 are sequentially installed along the pipeline from the component mixed gas bottle to the direction of the balance gas bottle. The invention changes the original method for preparing low-concentration mixed gas by weighing and multi-stage dilution into a method for filling trace gas into a pipeline with a certain capacity, and controls the quality of the trace gas by controlling the pressure of the gas, thereby achieving the aims of reducing the preparation links and improving the production efficiency. Compared with the prior art, the preparation process is easy to operate, and the result is accurate and reliable.
Description
Technical Field
The invention relates to a preparation technology of mixed gas, in particular to a micro gas transfer device and a micro gas transfer method.
Background
At present, a standard mixed gas is prepared by adopting a weighing method, namely a certain amount of pure gas or mixed gas with known components and concentration is transferred into a steel cylinder through a standard gas preparation device, the mass of the steel cylinder before and after filling is weighed by a high-load precision balance, and the difference value of the two times of weighing is the amount of the added component gas.
When a mixed gas with low concentration needs to be prepared, depending on the minimum weighing value of the high-load precision balance, multiple dilutions are required to obtain the mixed gas with the target concentration.
Specifically, in the prior art, a national standard GB/T5274 "preparation and weighing method of mixed gas for gas analysis and calibration" is taken as an example: preparation of 8 liter aluminum alloy Steel CylinderPressure 9Mpa + -1 Mpa, 10.0x10 Mpa -6 As an example of the carbon monoxide mixture gas in the nitrogen of mol/mol,8L aluminum alloy steel cylinder with the pressure of about 10mpa and 10 multiplied by 10 -6 In the nitrogen monoxide mixed gas in mol/mol, through the formula (1),the gas mass of the 8 liter aluminum alloy steel cylinder is about 925 g, wherein the nitrogen monoxide gas mass is 0.01 g, and obviously, the nitrogen monoxide gas cannot be obtained by a high-load precision balance, and the nitrogen monoxide gas can be obtained only by diluting nitrogen monoxide for a plurality of times (shown in fig. 3), so that the process is complicated and the preparation time is long. In the formula (1)m i Is a component in the mixed gasiThe unit of the mass is g;p f final filling pressure of the mixed gas is Pa;V cyl is the volume of the gas cylinder, and the unit is m 3 ；RIs a gas constant (8.31451J/mol X K);Tthe unit is K, which is the ambient temperature;Z f is the temperatureTAnd pressurep f Compression coefficient at the time;M i is composed ofiIn g/mol.
Because the packaging container for preparing the mixed gas generally adopts a steel bottle, the dead weight of the steel bottle is generally more than kilogram, a certain amount of target component raw material gas (namely trace gas) is added into one steel bottle, a high-load precision balance can sense and accurately weigh, and the current balance weighing technology at least needs to be filled with more than 5 grams to obtain reliable measurement data. Thus, for relatively small amounts of gas (e.g., less than 1 gram) existing high load precision balances cannot accurately measure, and therefore there is a great need for an apparatus and method that can accurately produce standard gas mixtures.
Disclosure of Invention
The invention provides a trace gas transfer device and a trace gas transfer method, which aim at solving the technical problem that the preparation of trace gas is difficult to dilute repeatedly in the existing preparation of mixed gas.
The trace gas transfer device is realized by adopting the following technical scheme: a trace gas transfer apparatus includes a conduit; the system also comprises a component mixed gas cylinder connected to one end of the pipeline and at least one balance gas cylinder connected to the other end of the pipeline; starting from the component mixed gas bottle to the direction of the balance gas bottle along the pipeline, a valve P8, a first branch, a second branch, a third branch, a fourth branch and a fifth branch are sequentially arranged, and a valve P5 is arranged; the first branch is connected with four valves Y1, Y2, Y3 and Y4 in parallel, and the other ends of the four valves Y1, Y2, Y3 and Y4 are respectively connected with a pressure gauge; at least one trace gas transfer tube is connected between the second branch and the third branch; two ends of the trace gas transfer tube are provided with a valve; the fourth branch penetrates through the pipeline, the valve P7 is connected in series with the part positioned at one side of the pipeline, and the valve P6 and the vacuum pump are connected in series with the part positioned at the other side of the pipeline; the fifth branch is connected with a valve P4 and a component raw material gas cylinder in series; a valve is connected between each balance gas cylinder and the valve P5; corresponding valves are also arranged on the component mixing gas cylinder, the component raw material gas cylinder and the balance gas cylinder.
A plurality of micro gas transfer pipes which are mutually connected in parallel are connected between the second branch and the third branch.
Quick connectors are respectively arranged at two ends of the trace gas transfer tube; and a valve is arranged on the pipe body at the position close to the two quick connectors.
The balance gas cylinders are mutually connected in parallel.
The trace gas transfer method is realized by adopting the following technical scheme: the micro gas transfer method comprises the steps of obtaining the mass of micro gas according to the mole ratio of mixed gas to be prepared and the total mass of the gas, and calculating the gas pressure bMpa of the micro gas after the micro gas is filled into the micro gas transfer pipe according to the volume and the temperature of the micro gas transfer pipe; the four pressure gauges connected with the Y1, Y2, Y3 and Y4 valves are respectively a high-pressure gauge, a medium-pressure gauge, a low-pressure gauge and a micro-pressure gauge; the method comprises the following steps:
(1) Closing all the gas cylinder valves and valves Y1-Y3, opening valves connected between the balance gas cylinder and the valve P5, and valves P4-P8 and valves Y4 at two ends of the trace gas transfer pipe, and starting a vacuum pump to pump the pressure in the pipeline to below 1 pa;
(2) Closing P7 and Y4, opening a valve arranged on the balance gas cylinder, filling the pipeline with balance gas, and closing the valve arranged on the balance gas cylinder;
(3) P7 is opened, balance gas in the pipeline is exhausted, P7 is closed, Y4 is opened, and a vacuum pump is started to pump the pressure in the pipeline to below 1 pa;
(4) Closing P5, P6, P7 and Y4, opening valves arranged on the component raw material gas cylinders, observing the pressure of the gas cylinders, and determining the valves of low, medium and high pressure gauges and the valves of micro-pressure gauges according to the pressure displayed on the pressure reducing valves on the gas cylinders;
(5) Slowly opening a valve P4, observing the pressure change of a low-pressure gauge, regulating the input gas quantity of the component raw material gas by rotating the valve P4 when the pressure reaches the aMpa, observing the change of a micro-pressure gauge at the moment, closing the valve P4 and a component raw material gas cylinder valve when the micro-pressure changes to the bMpa, observing the change condition of the micro-pressure gauge, closing valves at two ends of a micro-gas transfer pipe when the micro-pressure representation value is stable, observing the micro-pressure gauge again at the moment, and considering that closing the valves at two ends of the micro-gas transfer pipe does not influence the pressure in a pipeline if the change of the micro-pressure gauge is less than 100 Pa; the a < b is used for adjusting the gas flow from small to large so as to be convenient to control;
(6) The valves at two ends of the trace gas transfer pipe are ensured to be closed, the P7 and P6 component raw material gases in the pipeline are opened, the P7 is closed, the vacuum pump is started, and the pressure in the pipeline is pumped to be lower than 1 Pa;
(7) Placing a pre-weighed component mixing gas cylinder on a high-load balance;
(8) Closing P4, P6, P7, Y2, Y3 and Y4, opening a valve Y1 of a high-pressure gauge and a valve of a component mixing gas cylinder, opening a valve of a balance gas cylinder, and sequentially opening a valve connected between the balance gas cylinder and the valve P5, the valve P5 at one end of a trace gas transfer pipe and the valve at the other end of the trace gas transfer pipe;
(9) The quantitative gas in the trace gas transfer tube is filled into the component mixing gas cylinder due to the gas pressure in the balance gas cylinder;
(10) Observing the reading of the gas increased by the high-load balance in the component mixing gas cylinder, and closing a valve on the component mixing gas cylinder when the increment is the value of the total mass of the gas;
(11) Then closing a valve on the balance gas cylinder and a valve connected between the balance gas cylinder and the valve P5, opening P7, and discharging high-pressure gas in the pipeline; the prepared mixed gas is obtained in the component mixed gas cylinder.
Further, after the step (3) is finished, repeating the step (2) and the step (3) at least twice; and (3) after the step (6) is finished, closing valves at two ends of the trace gas transfer pipe, repeating the step (2) and the step (3) at least twice, and cleaning residual component gas in the pipeline.
The invention changes the original method for preparing low-concentration mixed gas by weighing and multi-stage dilution into a method for filling trace gas into a pipeline with a certain capacity, and controls the quality of the trace gas by controlling the pressure of the gas, thereby achieving the aims of reducing the preparation links and improving the production efficiency. Compared with the prior art, the invention does not need complex dilution flow, the preparation process is easy to operate, and the result is accurate and reliable.
Drawings
FIG. 1 is a schematic diagram of a trace gas transfer apparatus according to the present invention.
FIG. 2 is a schematic diagram of a trace gas transfer tube according to the present invention.
FIG. 3 shows a flow chart of dilution when preparing a mixed gas.
1-high pressure gauge, 2-medium pressure gauge, 3-low pressure gauge, 4-micro pressure gauge, 5-first balance gas cylinder, 6-second balance gas cylinder, 7-third balance gas cylinder, 8-component raw material gas cylinder, 9-vacuum pump, 10-component mixed gas cylinder and 11-quick connector.
Detailed Description
As shown in fig. 1, a trace gas transfer apparatus includes a conduit; the system also comprises a component mixed gas cylinder connected to one end of the pipeline and at least one balance gas cylinder connected to the other end of the pipeline; starting from the component mixed gas bottle to the direction of the balance gas bottle along the pipeline, a valve P8, a first branch, a second branch, a third branch, a fourth branch and a fifth branch are sequentially arranged, and a valve P5 is arranged; four valves Y1, Y2, Y3 and Y4 are connected in parallel on the first branch, and the other ends of the four valves Y1, Y2, Y3 and Y4 are respectively connected with a pressure gauge (one end of each of the four pressure gauges Y1, Y2, Y3 and Y4 is connected with the first branch; the four pressure gauges are respectively a high-pressure gauge, a medium-pressure gauge, a low-pressure gauge and a micro-pressure gauge); at least one trace gas transfer tube is connected between the second branch and the third branch; two ends of the trace gas transfer tube are provided with a valve; the fourth branch penetrates through the pipeline, the part positioned at one side of the pipeline is connected in series with a valve P7 (the other side of the valve P7 is communicated with air), and the part positioned at the other side of the pipeline is connected in series with a valve P6 and a vacuum pump (the other side of the vacuum pump is communicated with air); the fifth branch is connected with a valve P4 and a component raw material gas cylinder in series; a valve is connected between each balance gas cylinder and the valve P5; corresponding valves are also arranged on the component mixing gas cylinder, the component raw material gas cylinder and the balance gas cylinder. A plurality of micro gas transfer pipes which are connected in parallel are connected between the second branch and the third branch, and four micro gas transfer pipes are preferable in the figure. The balance gas cylinders are connected in parallel, three balance gas cylinders are preferable in the figure, and valves P1, P2 and P3 are respectively arranged between the three balance gas cylinders and P5.
As shown in fig. 2, two ends of the trace gas transfer tube are respectively provided with a quick connector; and valves W1 and W2 are arranged on the pipe bodies at positions close to the two quick connectors.
According to the scheme, for preparing the mixed gas with low concentration, for example, preparing the mixed gas with ppm concentration, the mixed gas is obtained by gradually diluting after previous weighing, raw material gas for preparing the mixed gas is filled into a pipeline (a trace gas transfer pipe here), and then the filling pressure is controlled according to the volume and the temperature of the pipeline to obtain the desired gas quality.
According to the following: （1）
wherein:
。
the invention adopts a trace gas transfer tube, the length of the trace gas transfer tube is 5000mm, the inner diameter is 8mm, and the temperature is controlled at about 25+/-10 ℃. Under normal atmospheric pressure, the filling pressure is about 10Mpa, and the concentration is 10.0X10 -6 As an example of nitric oxide in mol/mo nitrogen, pure 0.01 g nitric oxide can be obtained by filling the nitric oxide in the trace gas transfer pipeline to about 3.2 Mpa.
Trace gas transfer preparation of low concentration mixed gas examples are presented:
initial parameters: 10.0X10 -6 Nitric oxide in mol/mol nitrogen; the desired pressure is 10Mpa; component purity; NO:99.9% mol/mol.
N 2 ：99.999×10 -2 mol/mol,8L aluminum alloy steel cylinder; the net weight of nitric oxide in nitrogen can be calculated to be about 0.0096 grams.
The method comprises the following specific steps:
(1) Closing all the gas cylinder valves and valves (Y1-Y3), opening the valves P1-P8, W1-W8 and Y4, starting a vacuum pump, and pumping the pressure in the pipeline to below 1 pa.
(2) And closing P7 and Y4, opening a steel cylinder valve of the balance gas (1), and closing a first balance gas steel cylinder valve after the pipeline is filled with the balance gas.
(3) And opening P7, discharging balance gas in the pipeline, closing P7, opening Y4, and starting a vacuum pump to pump the pressure in the pipeline to below 1 pa.
(4) Repeating the step (2) and the step (3) at least twice.
(5) And closing P5, P6, P7 and Y4, opening the valves of the component raw gas cylinders, observing the cylinder pressure, and determining the valves of the low, medium and high pressure gauges and the micro pressure gauge according to the pressure displayed on the pressure reducing valve on the cylinder (because the pressure of the nitric oxide component cylinder is not more than 3.5Mpa, the low pressure gauge Y3 and the micro pressure gauge Y4 are opened at the moment).
(6) Slowly opening the valve P4, observing the pressure change of the low-pressure gauge, regulating the input gas quantity of the component raw material gas by rotating the valve P4 when the pressure reaches about 3Mpa, observing the change of the micro-pressure gauge at the moment, closing the valve P4 and the component raw material gas cylinder valve when the micro-pressure changes to 3.2Mpa, observing the change condition of the micro-pressure gauge, closing the valve W1-W8 when the micro-pressure representation value is stable, at the moment, observing the micro-pressure gauge again, and if the change of the micro-pressure gauge is less than 100pa, considering that the closing of the valve W1-W8 does not influence the pressure in the micro-transfer pipeline.
(7) And (3) closing the W1-W8 valves, opening P7 and P6 to empty component raw material gases in the pipeline, closing P7, starting a vacuum pump, and pumping the pressure in the pipeline to below 1 Pa.
(8) And (3) closing the W1-W8 valve, repeating the step (2) and the step (3) at least twice, and cleaning residual component gas in the pipeline.
(9) The pre-weighed vacuum component mixing cylinder was placed on a high load balance.
(10) Closing P4, P6, P7, Y2, Y3 and Y4, opening a high-pressure gauge Y1, opening a component mixing gas cylinder valve, opening a first balance gas cylinder valve, and sequentially opening valves P1, P5, W1 and W2.
(11) Because the gas pressure in the balance gas cylinder is high pressure, quantitative gas in the trace gas transfer tube can be smoothly filled into the component mixed gas cylinder.
(12) When the reading of the gas increased by the high-load balance in the component mixing gas cylinder is observed and the increasing amount is 920 g (a certain error is caused in actual operation from the theoretical calculation), the valve on the component mixing gas cylinder is closed.
(13) Then the valve on the balance gas cylinder is closed, P1 is opened, P7 is opened, and the high-pressure gas in the pipeline is discharged.
(14) The steel bottle of the component mixed gas bottle is taken down from the gas distribution pipeline, the steel bottle is put on a high-load balance again to weigh the mass, and the mass of the vacuum component mixed gas bottle is subtracted to obtain 921.125g of the filled mixed gas.
(15) The mass of nitric oxide in the trace gas transfer tube can be calculated according to the formula (1)m i =0.009784043g。
(16) From the weighed mass and the measured mass of the trace gas transfer tube, the concentration of nitric oxide in nitrogen can be calculated to be 9.92 multiplied by 10 -6 mol/mol。
(17) 9.92×10 to be developed -6 The mixed gas of nitric oxide in mol/mol nitrogen is tested and compared with a secondary gas standard substance developed by Sichuan standard measuring and testing technologies, and the comparison result is consistent with the calculation result.
Claims (5)
1. A trace gas transfer method, which is realized by adopting a trace gas transfer device, wherein the trace gas transfer device comprises a pipeline; the system also comprises a component mixed gas cylinder connected to one end of the pipeline and at least one balance gas cylinder connected to the other end of the pipeline; starting from the component mixed gas bottle to the direction of the balance gas bottle along the pipeline, a valve P8, a first branch, a second branch, a third branch, a fourth branch and a fifth branch are sequentially arranged, and a valve P5 is arranged; the first branch is connected with four valves Y1, Y2, Y3 and Y4 in parallel, and the other ends of the four valves Y1, Y2, Y3 and Y4 are respectively connected with a pressure gauge; at least one trace gas transfer tube is connected between the second branch and the third branch; two ends of the trace gas transfer tube are provided with a valve; the fourth branch penetrates through the pipeline, the valve P7 is connected in series with the part positioned at one side of the pipeline, and the valve P6 and the vacuum pump are connected in series with the part positioned at the other side of the pipeline; the fifth branch is connected with a valve P4 and a component raw material gas cylinder in series; a valve is connected between each balance gas cylinder and the valve P5; corresponding valves are also arranged on the component mixing gas cylinder, the component raw material gas cylinder and the balance gas cylinder;
obtaining the mass of trace gas according to the mole ratio of the mixed gas to be prepared and the total mass of the gas, and calculating the gas pressure bMpa of the trace gas after the trace gas is filled into the trace gas transfer pipe according to the volume and the temperature of the trace gas transfer pipe; the four pressure gauges connected with the Y1, Y2, Y3 and Y4 valves are respectively a high-pressure gauge, a medium-pressure gauge, a low-pressure gauge and a micro-pressure gauge; characterized in that the method comprises the following steps:
(1) Closing all the gas cylinder valves and valves Y1-Y3, opening valves connected between the balance gas cylinder and the valve P5, and valves P4-P8 and valves Y4 at two ends of the trace gas transfer pipe, and starting a vacuum pump to pump the pressure in the pipeline to below 1 pa;
(2) Closing P7 and Y4, opening a valve arranged on the balance gas cylinder, filling the pipeline with balance gas, and closing the valve arranged on the balance gas cylinder;
(3) P7 is opened, balance gas in the pipeline is exhausted, P7 is closed, Y4 is opened, and a vacuum pump is started to pump the pressure in the pipeline to below 1 pa;
(4) Closing P5, P6, P7 and Y4, opening valves arranged on the component raw material gas cylinders, observing the pressure of the gas cylinders, and determining the valves of low, medium and high pressure gauges and the valves of micro-pressure gauges according to the pressure displayed on the pressure reducing valves on the gas cylinders;
(5) Slowly opening a valve P4, observing the pressure change of a low-pressure gauge, regulating the input gas quantity of component raw gas by rotating the valve P4 when the pressure reaches aMpa, observing the change of a micro-pressure gauge at the moment, closing the valve P4 and a component raw gas cylinder valve when the micro-pressure changes to bMpa, observing the change condition of the micro-pressure gauge, closing valves at two ends of a micro-gas transfer pipe when the micro-pressure representation value is stable, at the moment, observing the micro-pressure gauge again, and if the change of the micro-pressure gauge is smaller than 100Pa, considering that the valves at two ends of the micro-gas transfer pipe are closed without influencing the pressure in a pipeline; the a < b;
(6) The valves at two ends of the trace gas transfer pipe are ensured to be closed, the P7 and P6 component raw material gases in the pipeline are opened, the P7 is closed, the vacuum pump is started, and the pressure in the pipeline is pumped to be lower than 1 Pa;
(7) Placing a pre-weighed component mixing gas cylinder on a high-load balance;
(8) Closing the valves P4, P6, P7, Y2, Y3 and Y4, opening the valves of the high-pressure gauge Y1 and the component mixing gas cylinder, opening the valve of the balance gas cylinder, and sequentially opening the valve connected between the balance gas cylinder and the valve P5, the valve P5 at one end of the trace gas transfer pipe and the valve at the other end of the trace gas transfer pipe;
(9) The quantitative gas in the trace gas transfer tube is filled into the component mixing gas cylinder due to the gas pressure in the balance gas cylinder;
(10) Observing the reading of the gas increased by the high-load balance in the component mixing gas cylinder, and closing a valve on the component mixing gas cylinder when the increment is the value of the total mass of the gas;
(11) Then closing a valve on the balance gas cylinder and a valve connected between the balance gas cylinder and the valve P5, opening P7, and discharging high-pressure gas in the pipeline; the prepared mixed gas is obtained in the component mixed gas cylinder.
2. The trace gas transfer method according to claim 1, wherein step (2) and step (3) are repeated at least two more times after step (3) is completed; and (3) after the step (6) is finished, closing valves at two ends of the trace gas transfer pipe, repeating the step (2) and the step (3) at least twice, and cleaning residual component gas in the pipeline.
3. The micro gas transfer method of claim 1, wherein a plurality of micro gas transfer tubes connected in parallel with each other are connected between the second branch and the third branch.
4. The trace gas transfer method according to claim 3, wherein quick connectors are respectively installed at both ends of the trace gas transfer tube; and a valve is arranged on the pipe body at the position close to the two quick connectors.
5. The micro gas transfer method as set forth in any one of claims 1, 3, and 4, wherein a plurality of balance cylinders are connected in parallel with each other.
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