ISOTOPE ANALYSIS SYSTEM
20230045177 · 2023-02-09
Inventors
Cpc classification
H01J49/04
ELECTRICITY
B01L2300/1805
PERFORMING OPERATIONS; TRANSPORTING
B01L2400/0622
PERFORMING OPERATIONS; TRANSPORTING
B01L2200/16
PERFORMING OPERATIONS; TRANSPORTING
B01L3/502715
PERFORMING OPERATIONS; TRANSPORTING
International classification
Abstract
An isotope analysis system includes: a first liquid channel, second liquid channels, third liquid channels, fourth liquid channels connected with a heating reactor, a diverter, and a selector valve. The diverter is configured to divert liquid from the first liquid channel to the third liquid channels. The selector valve comprises a first liquid outlet and a plurality of first liquid inlets. A third liquid channel and a fourth liquid channel are assigned to each of the plurality of second liquid channels; an end of the fourth liquid channel is connected to both an end of the second liquid channel and an end of the third liquid channel; and a first liquid inlet is assigned to each of the plurality of fourth liquid channels, and another end of the fourth liquid channel is connected to the first liquid inlet.
Claims
1. An isotope analysis system, comprising: a first liquid channel; a plurality of second liquid channels; a plurality of third liquid channels; a plurality of fourth liquid channels, wherein a heating reactor is provided at the fourth liquid channels; a diverter configured to divert liquid from the first liquid channel to the plurality of third liquid channels; and a first selector valve comprising a first liquid outlet and a plurality of first liquid inlets; wherein a third liquid channel and a fourth liquid channel are assigned to each of the plurality of second liquid channels; an end of the fourth liquid channel is connected to both an end of the second liquid channel and an end of the third liquid channel; wherein a first liquid inlet is assigned to each of the plurality of fourth liquid channels, and another end of the fourth liquid channel is connected to the first liquid inlet.
2. The isotope analysis system according to claim 1, further comprising an actuator configured to drive liquid flow in the plurality of second liquid channels and the plurality of third liquid channels.
3. The isotope analysis system according to claim 2, wherein the actuator is a peristaltic pump.
4. The isotope analysis system according to claim 1, wherein the heating reactor is an electric heating source; and each of the plurality of fourth liquid channels comprises a segment wrapping around the electric heating source.
5. The isotope analysis system according to claim 1, further comprising: a fifth liquid channel communicating with the first liquid outlet and a cooler provided at the fifth liquid channel.
6. The isotope analysis system according to claim 5, further comprising a membrane inlet mass spectrometer communicating with the fifth liquid channel.
7. The isotope analysis system according to claim 1, further comprising: a degassing device configured to remove a gas in the first liquid channel and the plurality of second liquid channels.
8. The isotope analysis system according to claim 1, wherein the diverter comprises a liquid inlet pipe and a plurality of liquid outlet pipes; wherein an inlet of the liquid inlet pipe communicates with an outlet of the first liquid channel, and an outlet of the liquid inlet pipe communicates with an inlet of the plurality of liquid outlet pipes; and an outlet of each of the plurality of liquid outlet pipes is connected to an inlet of a specific third liquid channel.
9. The isotope analysis system according to claim 1, further comprising a second selector valve and/or a third selector valve, wherein the second selector valve comprises a second liquid outlet and a plurality of second liquid inlets, and the second liquid outlet communicates with an inlet of the first liquid channel; wherein the third selector valve comprises a third liquid outlet and a plurality of third liquid inlets, and the third liquid outlet communicates with an inlet of the plurality of second liquid channels.
10. The isotope analysis system according to claim 1, wherein the isotope analysis system is provided with four second liquid channels.
11. The isotope analysis system according to claim 2, wherein the isotope analysis system is provided with four second liquid channels.
12. The isotope analysis system according to claim 3, wherein the isotope analysis system is provided with four second liquid channels.
13. The isotope analysis system according to claim 4, wherein the isotope analysis system is provided with four second liquid channels.
14. The isotope analysis system according to claim 5, wherein the isotope analysis system is provided with four second liquid channels.
15. The isotope analysis system according to claim 6, wherein the isotope analysis system is provided with four second liquid channels.
16. The isotope analysis system according to claim 7, wherein the isotope analysis system is provided with four second liquid channels.
17. The isotope analysis system according to claim 8, wherein the isotope analysis system is provided with four second liquid channels.
18. The isotope analysis system according to claim 9, wherein the isotope analysis system is provided with four second liquid channels.
Description
BRIEF DESCRIPTION OF THE DRAWINGS
[0026] To more clearly illustrate the embodiments of the present disclosure, the accompanying drawings required for describing the embodiments or the prior art are briefly described below. The accompanying drawings described below only illustrate some embodiments of the present disclosure. Other drawings can be obtained by the skilled person based on these accompanying drawings without creative efforts.
[0027]
[0028]
[0029]
[0030] Reference numerals in the figures: [0031] 11 represents a first liquid channel; 12 represents a second liquid channel; 13 represents a third liquid channel; 14 represents a fourth liquid channel; 15 represents a fifth liquid channel; 2 represents a diverter; 21 represents a liquid inlet pipe; 22 represents a liquid outlet pipe; 31 represents a heating reactor; 32 represents a actuator; 33 represents a cooler; 34 represents a mass spectrometer; 35 represents a degassing device; 41 represents a first selector valve; 411 represents a first liquid inlet; 412 represents a first liquid outlet; 42 represents a second selector valve; 421 represents a second liquid inlet; 422 represents a second liquid outlet; 43 represents a third selector valve; 431 represents a third liquid inlet; 432 represents a third liquid outlet; A1 represents a first reagent; A2 represents a second reagent; A3 represents a third reagent; B1 represents a fourth reagent; B2 represents a fifth reagent; B3 represents a sixth reagent; C1 represents a liquid sample to be tested; C2 represents a first standard sample liquid; C3 represents a second standard sample liquid; C4 represents a third standard sample liquid; and C5 represents a fourth standard sample liquid.
DETAILED DESCRIPTION
[0032] To make the technical problems to be solved, the technical solutions, and the beneficial effects of the present disclosure clearer, the present disclosure is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific examples described herein are merely intended to explain the present disclosure, rather than to limit the present disclosure.
[0033] It should be noted that, when a component is “fixed” or “provided” on another component, the component may be “fixed” or “provided” on the another component directly or indirectly. When a component is “connected” to another component, the component may be “connected” to the another component directly or indirectly.
[0034] It should be noted that, in the description of the embodiments of the present disclosure, unless otherwise specified, “I” means “or”, for example, “A/B” may mean “A or B”. The term “and/or” herein means that there are three relationships, for example, “A and/or B” may indicate that A exists alone, A and B coexist, and B exists alone. “A” and “B” may be singular or plural.
[0035] It should be understood that orientations or position relationships indicated by terms “length”, “width”, “upper”, “lower”, “front”, “rear”, “left”, “right”, “vertical”, “horizontal”, “top”, “bottom”, “inside”, “outside”, and the like are based on the orientation or position relationships shown in the accompanying drawings. These terms are just used to facilitate the description of the present disclosure and simplify the description, but not to indicate or imply that the mentioned device or elements must have a specific orientation and must be established and operated in a specific orientation, and thus these terms cannot be understood as a limitation to the present disclosure.
[0036] Moreover, the terms such as “first” and “second” are used only for the purpose of description and should not be construed as indicating or implying a relative importance, or implicitly indicating a quantity of indicated technical features. Thus, features defined with “first” and “second” may explicitly or implicitly include one or more of the features. In the description of the present disclosure, “a plurality of” means two or more, unless otherwise specifically defined.
[0037] With reference to
[0038] a first liquid channel 11, a plurality of second liquid channels 12, a plurality of third liquid channels 13, a diverter 2 configured to deliver a liquid in the first liquid channel 11 to the plurality of third liquid channels 13, a plurality of fourth liquid channels 14, and a first selector valve 41 including a first liquid outlet 412 and a plurality of first liquid inlets 411. A heating reactor 31 is provided at the fourth liquid channels 14. A third liquid channel 13 and a fourth liquid channel 14 are assigned to each of the plurality of second liquid channels 12; an inlet of the fourth liquid channel 14 is connected to both an outlet of the second liquid channel 12 and an outlet of the third liquid channel 13; and a first liquid inlet is assigned to each of the plurality of fourth liquid channels, and an outlet of the fourth liquid channel is connected to the first liquid inlet.
[0039] During detection, a liquid sample containing .sup.15N is introduced into a diverter 2 through a first liquid channel 11. The diverter then diverts the liquid sample to a plurality of third liquid channels 13 (that is, the liquid sample in the first liquid channel 11 flows into various third liquid channels 13 through the diverter 2). The second liquid channels 12 of the system are each introduced with a unique reagent that can react with a particular .sup.15N-containing substance (a molecule or an ion). In a fourth liquid channel 14, a reagent from a particular second liquid channel 12 combines with a liquid sample from a particular third liquid channel 13 to form a liquid mixture. A heating reactor 31 heats the liquid mixture to a predetermined temperature to react. The liquid mixture then flows from this fourth liquid channel 14 to a first selector valve 41 through a particular first liquid inlet 411 designated to this fourth liquid channel 14. The first selector valve 41 enables the communication between this first liquid inlet 411 and a first liquid outlet 41, allowing the liquid mixture to be directed out of the system through this outlet. In brief, a liquid sample from a third liquid channel 13 reacts with a specific reagent from a designated second liquid channel 12 in a designated fourth liquid channel 14. The post-reaction liquid mixture is directed out of the system through a designated first liquid inlet 411 and first liquid outlet 412 and is then monitored. In this way, reactions between the .sup.15N-containing substance in a liquid sample with different reagents can be monitored separately and continuously.
[0040] Further, please refer to
[0041] In an embodiment, the actuator 32 may be a peristaltic pump.
[0042] In an embodiment, the peristaltic pump may be Ecoline VC-360 (8 channels) produced by Ismatec.
[0043] In an embodiment, the first selector valve 41 may further include a valve body including communication holes that define communication passages. As a result, the valve body is switchable between a plurality of communication passages through rotation. When the valve body rotates to a specific communication passage, a first liquid inlet 411 to which the communication passage is assigned communicates with a first liquid outlet 412.
[0044] In an embodiment, the heating reactor 31 can heat a liquid in the fourth liquid channel 14 to 75° C. At this temperature, the reaction can proceed at a desired rate without producing an excessive amount of steam.
[0045] In an embodiment, the liquid sample may be a water sample taken from soil leachate, river water, seawater, or groundwater.
[0046] In an embodiment, different reagents may be delivered by different second liquid channels 12.
[0047] In an embodiment, the first liquid channel 11 may be PEEK tubing with the following dimension: 0.1 m to 1 m (length)×1,580 μm (outer diameter)×508 μm (inner diameter).
[0048] In an embodiment, the fifth liquid channel 15 may be FS-coated PEEK tubing with the following dimension: 6 m (length)×1,580 μm (outer diameter)×530 μm (inner diameter). This type of tubing facilitates liquid flow, reduces product adhesion, and thus reduces the likelihood of channel blockage.
[0049] In an embodiment, the second liquid channel 12, the third liquid channel 13, and the fourth liquid channel 14 may each include a plurality of segments, and different segments may be adopt tubing of different types and sizes.
[0050] In an embodiment, a segment of the second liquid channel 12 in the actuator 32 may be Tygon® S3 E-LFL tubing with the following dimension: 15 cm (length)×508 μm (inner diameter)×1,600 μm (outer diameter). This type of tubing facilitates liquid flow and controls liquid flow rate. The other segments of the second liquid channel 12 may be PEEK tubing with the following dimension: 0.1 m to 1 m (length)×1,580 μm (outer diameter)×508 μm (inner diameter).
[0051] In an embodiment, a segment of the third liquid channel 13 in the actuator 32 may be Santoprene tubing with the following dimension: 15 cm (length)×320 μm (inner diameter)×1,600 μm (outer diameter). This type of tubing facilitates liquid flow and controls liquid flow rate. The other segments of the third liquid channel 13 may be PEEK tubing with the following dimension: 0.1 m to 1 m (length)×1,580 μm (outer diameter)×508 μm (inner diameter).
[0052] In an embodiment, segments of the fourth liquid channel 14 at a reaction tower 31 and after the reaction tower 31 may each be FS-coated peek tubing with the following dimension: 6 m (length)×1,580 μm (outer diameter)×530 μm (inner diameter); and segments of the fourth liquid channel 14 before the reaction tower 31 may each be PEEK tubing with the following dimension: 1 m (length)×0.508 mm (inner diameter)×1.6 mm (outer diameter). This type of tubing facilitates liquid flow, reduces the adhesion of a product, and reduces the possibility of pipe blockage.
[0053] In an embodiment, the first selector valve 41 may be Low Pressure Stream Selector manufactured by VICI. In an embodiment, the first selector valve 41 may be a selector valve with 1/16″ Valco ZDV fittings. In an embodiment, the first selector valve 41 could be a 4 position selector, a 6 position selector, or an 8 position selector. In an embodiment, a communication interface of the first selector valve 41 may be an RS232 interface.
[0054] Further, please refer to
[0055] In an embodiment, the reaction at the heating reactor 31 may be conducted for 7 min. In an embodiment, the reaction system may be heated to and kept at 75° C.
[0056] In an embodiment, the heating reactor 31 may include a hollow aluminum column, a fourth liquid channel 14 may wrap the hollow aluminum column, and the heat source may heat a liquid in the fourth liquid channel 14 through the hollow aluminum column.
[0057] In an embodiment, the heat source may be an electric heating wire.
[0058] In an embodiment, the heat source may include an electric heater, a temperature sensor, and a temperature control element.
[0059] Further, please refer to
[0060] Further, please refer to
[0061] In an embodiment, the membrane-inlet mass spectrometer 34 may be Hiden HPR-40 MIMS System manufactured by Hiden Analytical, UK.
[0062] Further, please refer to
[0063] In an embodiment, the degassing device 35 may be a membrane degassing device.
[0064] In an embodiment, the degassing device 35 may be DEGASi Compact Stand Alone Degasser, Systec AF.
[0065] Further, please refer to
[0066] Further, please refer to
[0067] In an embodiment, the second selector valve 42 may further include a valve body including communication holes that define communication passages. As a result, the valve body is switchable between a plurality of communication passages through rotation. When the valve body rotates to a specific communication passage, a second liquid inlet 421 to which the communication passage is assigned communicates with a second liquid outlet 422.
[0068] In an embodiment, the second selector valve 42 may be Low Pressure Stream Selector manufactured by VICI. In an embodiment, the second selector valve 42 may be a selector valve with 1/16″ Valco ZDV fittings. In an embodiment, the second selector valve 42 may be a 4 position selector, a 6 position selector, or an 8 position selector. In an embodiment, a communication interface of the second selector valve 42 may be an RS232 interface.
[0069] In an embodiment, the isotope analysis system may further include: a third selector valve 43 including a third liquid outlet 432 and a plurality of third liquid inlets 431, where an inlet of a second liquid channel 12 communicates with the third liquid outlet 432. Different third liquid inlets 431 can be used to input different reagents into the third selector valve 43, and by enabling communication between the third liquid outlet 432 and various third liquid inlets 431, different reagents in the various third liquid inlets 431 can be discharged separately into the second liquid channel 12 through the third liquid outlet 432.
[0070] In an embodiment, the third selector valve 43 may further include a valve body including communication holes that define communication passages. As a result, the valve body is switchable between a plurality of communication passages through rotation. When the valve body rotates to a specific communication passage, a third liquid inlet 431 to which the communication passage is assigned communicates with a third liquid outlet 432.
[0071] In an embodiment, the third selector valve 43 may be Low Pressure Stream Selector manufactured by VICI. In an embodiment, the third selector valve 43 may be a selector valve with 1/16″ Valco ZDV fittings. In an embodiment, the third selector valve 43 may be a 4 position selector, a 6 position selector, or an 8 position selector. In an embodiment, a communication interface of the third selector valve 43 may be an RS232 interface.
[0072] In an embodiment, a fourth reagent B1 may enter a second liquid channel 12 through a third liquid inlet 431 of the third selector valve 43. In an embodiment, a fifth reagent B2 may enter another second liquid channel 12 through another third liquid inlet 431 of the third selector valve 43. In an embodiment, a sixth reagent B3 may enter still another second liquid channel 12 through still another third liquid inlet 431 of the third selector valve 43.
[0073] In an embodiment, the fifth reagent B2 may be HCl. In an embodiment, the sixth reagent B3 may be water. In this way, the second liquid channels 12 can be rinsed with HCl and water. In an embodiment, the rinsing may be conducted as follows: after the fourth reagent B1 stayed in the second liquid channel 12 for 3 minutes, the second liquid channel is rinsed with H.sub.2O for 1 min, then with HCL for 1 min. The fourth reagent B1 can be introduced again afterwards. In an embodiment, the fourth reagent B1 may be a NaBrO solution.
[0074] Further, please refer to
[0075] In the present disclosure, M stands for mol/L (moles per liter).
[0076] In the present disclosure, mg N/mL stands for mg/mL nitrogen.
[0077] In an embodiment, an inlet of a second liquid channel 12 may communicate with a container filled with a first reagent A1. The first reagent A1 reacts with NH.sub.2OH in the first liquid channel 11 for subsequent detection. In an embodiment, the reaction may be (1) NH.sub.2OH+NO.sub.2.sup.−.fwdarw.N.sub.2O+H.sub.2O+OH.sup.−; and/or (2) 4Fe.sup.3++2 NH.sub.2OH.fwdarw.4Fe.sup.2++N.sub.2O+H.sub.2O+4H+NH.sub.2OH.
[0078] In an embodiment, the first reagent A1 may enter a second liquid channel 12 after passing through the degassing device 35.
[0079] In an embodiment, an inlet of a second liquid channel 12 may communicate with a container filled with a second reagent A2. The second reagent reacts with NO.sub.2.sup.− in the first liquid channel 11 for subsequent detection. In an embodiment, the reaction is as follows: NO.sub.2.sup.−+2 KI+H.sup.+.fwdarw.NO+KI.I+KOH. In an embodiment, the second reagent A2 is prepared from reagents including 78% H.sub.3PO.sub.4, 0.2 mol KI, and distilled water. Preparation method of A2: 33.2 g (0.2 mol) of KI is dissolved in 1 L of water with stirring to produce a 0.2 M KI solution; and 75 mL of 78% H.sub.3PO.sub.4, 30 mL of the 0.2 M KI solution, and 95 mL of distilled water are mixed to obtain the second reagent A2; alternatively, 70 mL of 78% H.sub.3PO.sub.4, 30 mL of the 0.2 M KI solution, and 100 mL of distilled water are mixed to obtain the second reagent A2.
[0080] In an embodiment, the second reagent A2 may enter a second liquid channel 12 after passing through the degassing device 35.
[0081] In an embodiment, an inlet of a second liquid channel 12 may communicate with a container filled with a third reagent A3. The third reagent reacts with NO.sub.3.sup.− in the first liquid channel 11 for subsequent detection. In an embodiment, the reaction is as follows: NO.sub.3.sup.−+3 V.sup.3++4 H.sup.+.fwdarw.NO+3 V.sup.4++2H.sub.2O. In an embodiment, the third reagent A3 is prepared from reagents including H.sub.2O, 0.1 M VCl.sub.3, and 37% HCl. Preparation of 100 mL of A3: 1.57 g of VCl.sub.3 and 16 mL of 37% HCl are mixed, and then distilled water is added until a total volume is 100 mL. When a segment of the second liquid channel 12 in the actuator 32 is Tygon® S3 E-LFL tubing with the following dimension: 15 cm (length)×508 μm (inner diameter)×1,600 μm (outer diameter) and a segment of the third liquid channel 13 in the actuator 32 is Santoprene tubing with the following dimension: 15 cm (length)×320 μm (inner diameter)×1,600 μm (outer diameter), the ratio of A3 volume to sample volume is at least 1:1; for example, 3 mL of A3 may be used for 2 mL to 3 mL of a sample.
[0082] In an embodiment, the third reagent A3 may enter a second liquid channel 12 after passing through the degassing device 35.
[0083] In an embodiment, an inlet of a second liquid channel 12 may communicate with a container filled with a fourth reagent B 1, where the fourth reagent B1 reacts with NH.sub.4.sup.+ in the first liquid channel 11 for subsequent detection. In an embodiment, a reaction process for the NH.sub.4.sup.+ can be as follows: 2 NH.sub.4.sup.++3 BrO.sup.−+2 OH.sup.−.fwdarw.N.sub.2+5 H.sub.2O+3 Br.sup.−. In an embodiment, the fourth reagent B4 is prepared from reagents including Br.sub.2, H.sub.2O, KI, and NaOH. Preparation of the fourth reagent B1: 20 g of NaOH is dissolved in 200 mL of H.sub.2O under cooling to obtain a solution; after the solution is cooled to 4° C., 2 mL of Br.sub.2 is added with vigorous shaking until the solution turns orange-yellow; the solution is placed overnight in a refrigerator; and then 50 mL of H.sub.2O, in which 0.25 g of KI is dissolved, is added to the solution to stabilize the NaOBr solution obtained. A chemical reaction that takes place during the preparation is as follows: 2 NaOH+Br.sub.2.fwdarw.NaOBr+NaBr+H.sub.2O. The NaOBr solution can be used directly to react with a sample. It should be noted that the NaOBr solution is stable only under alkaline conditions and should always be stored at 4° C. to maintain the molarity of the hypobromite. According to theoretical calculations, a freshly-prepared NaOBr solution includes 0.156 M BrO.sup.−; the molarity should be examined every 4 weeks. In addition, the NaOBr solution should be subjected to visual inspection for suspended particles; if necessary, particles are filtered through G3 frit.
[0084] In an embodiment, the fourth reagent B1 may enter a second liquid channel 12 after passing through the degassing device 35.
[0085] In an embodiment, the fifth reagent B2 may enter a second liquid channel 12 after passing through the degassing device 35.
[0086] In an embodiment, the sixth reagent B3 may enter a second liquid channel 12 after passing through the degassing device 35.
[0087] In an embodiment, the liquid sample C1 to be tested may be a water sample from soil leachate, river water, seawater, or groundwater.
[0088] In an embodiment, a first standard sample liquid C2 may be a NH.sub.2OH solution with a predetermined concentration. In an embodiment, a NH.sub.2OH standard sample liquid may be prepared as follows: hydroxylamine hydrochloride is dissolved in deionized water according to the following standards: 10 mg N/mL=49.257 g NaNO.sub.3; 1 mg N/mL=4.9257 g NaNO.sub.3; 0.1 mg N/mL=0.4926 g NaNO.sub.3; .sup.15N content: 1 to 10 atom %.
[0089] In an embodiment, a second standard sample liquid C3 may be a NO.sub.2.sup.− solution with a predetermined concentration. In an embodiment, the second standard sample liquid can be prepared according to Chinese Patent CN110763535A. In an embodiment, a nitrite standard sample liquid may be prepared as follows: NaNO.sub.2 is dissolved in deionized water according to the following standards: 10 mg N/mL=49.257 g NaNO.sub.2; 1 mg N/mL=4.9257 g NaNO.sub.2; 0.1 mg N/mL=0.4926 g NaNO.sub.2; .sup.15N content: 1 to 10 atom %.
[0090] In an embodiment, a third standard sample liquid C4 may be a NO.sub.3.sup.− solution with a predetermined concentration. In an embodiment, a nitrate standard sample liquid may be prepared as follows: NaNO.sub.3 is dissolved in deionized water according to the following standards: 10 mg N/mL=49.257 g NaNO.sub.3; 1 mg N/mL=4.9257 g NaNO.sub.3; 0.1 mg N/mL=0.4926 g NaNO.sub.3; .sup.15N content: 1 to 10 atom %.
[0091] In an embodiment, a fourth standard sample liquid C5 may be a NH.sub.4.sup.+ solution with a predetermined concentration.
[0092] In an embodiment, the liquid sample C1 to be tested may enter the first liquid channel 11 after passing through the degassing device 35.
[0093] In an embodiment, the first standard sample liquid C2 may enter the first liquid channel 11 after passing through the degassing device 35.
[0094] In an embodiment, the second standard sample liquid C3 may enter the first liquid channel 11 after passing through the degassing device 35.
[0095] In an embodiment, the third standard sample liquid C4 may enter the first liquid channel 11 after passing through the degassing device 35.
[0096] In an embodiment, the fourth standard sample liquid C5 may enter the first liquid channel 11 after passing through the degassing device 35.
[0097] In an embodiment, the peristaltic pump, the reactor, and the mass spectrometer 34 may be each controlled by LabVIEW.
[0098] The above are merely preferred embodiments of the present disclosure, and are not intended to limit the present disclosure. Any modifications, equivalent replacements, improvements, and the like made within the spirit and principle of the present disclosure shall be all included in the protection scope of the present disclosure.