Integrated heatable spray chamber for introducing single particle analysis sample

Abstract

The utility model discloses an integrated heatable spray chamber for introducing a single particle analysis sample. The integrated heatable spray chamber comprises an outer tube, an inner tube and a base, the outer pipe comprises a main body part, the front end of the main body part is provided with a base socket, the front end surface or the side wall surface of the main body part is provided with a compensation air pipe, the tail end of the main body part extends to form a tapered part, the inner pipe comprises a base connecting part, the tail end of the base connecting part forms an aerosol inlet part, and the tail end of the tapered part extends in the aerosol transmission direction to form a cylindrical extension part; an interface part is arranged at the tail end of the extension part; an atomizer inserting opening is formed in the front end of the base. According to the utility model, the heatable design of the extension part can reduce the condensation effect of aerosol and reduce the number of connectors, so that the spray chamber and the rectangular tube can be directly communicated, good sealing performance is obtained, good concentricity is achieved, the transmission efficiency of samples is improved, and the design of the pluggable base is convenient for daily cleaning and maintenance of the spray chamber.

Description

TECHNICAL FIELD

[0001] The utility model relates to mass spectrum analysis technical field especially relates to a kind of for single particle-inductive coupling plasma mass spectrum (SP-ICP-MS) method's sample introduction system integration can be heated spray chamber. BACKGROUND

[0002] Sample introduced by sample introduction device forms aerosol by atomizer, is transmitted to plasma generator by spray chamber, and plasma is used to ionize and / or atomize aerosol for detection. The introduction system is an important component of SP-ICP-MS, wherein the spray chamber has a greater impact on the transmission efficiency of the sample introduction system. Due to the small sample size and low sample rate, the transmission efficiency of the traditional cyclone spray chamber is poor when the sample is introduced at a low flow rate. Among various types of spray chambers, the pear-shaped spray chamber is suitable for SP-ICP-MS due to its high throughput, high analysis sensitivity, stable signal, and small relative standard deviation. However, as shown in patent ZL202321015354.4, the ordinary pear-shaped spray chamber is relatively short, and when connected to the rear-end rectangular tube, it often needs to be connected through a connecting rod, resulting in too many interfaces and difficulty in calibrating the front and rear concentricities. This leads to a decrease in the sample introduction efficiency and stability of SP-ICP-MS, and it is unable to achieve long-term stable and efficient transmission. The atomizer socket of the ordinary pear-shaped spray chamber is embedded with two rubber rings, which is difficult to disassemble and is not conducive to daily cleaning and maintenance. SUMMARY

[0003] To solve the above technical problems, the utility model designs a kind of for single particle analysis sample introduction integration can be heated spray chamber.

[0004] The utility model adopts the following technical solutions:

[0005] An integrated heatable spray chamber for single particle analysis sample introduction, comprising an outer tube and an inner tube, the outer tube comprising a main body part in a cylindrical shape and extending in an aerosol transmission direction, a base socket being arranged at the front end of the main body part, a compensation gas tube being arranged on the front end surface or the side wall surface of the main body part, a tapered part gradually reducing in size in the aerosol transmission direction being arranged at the end of the main body part, the inner tube comprising a base connecting part extending from the base socket in the aerosol transmission direction, the front end of the base connecting part being connected with the base socket and being integrally formed, an aerosol inlet part being formed at the end of the base connecting part, the aerosol inlet part extending outward from the end of the base connecting part and extending to the middle part of the inner cavity of the main body part, an annular gap being formed between the aerosol inlet part and the outer tube, a cylindrical extension part extending in the aerosol transmission direction at the end of the tapered part, an interface part being arranged at the end of the extension part and being matched with a rectangular tube; a base being sealingly inserted into the base socket, an atomizer socket being arranged at the front end of the base for fixing an atomizer, the atomizer socket being communicated into the inner cavity of the inner tube, the inner cavity of the aerosol inlet part and the inner cavity of the outer tube at the end side of the aerosol inlet part forming an aerosol transmission cavity.

[0006] Preferably, the base is divided into a limiting part and a column part, an atomizer socket being arranged on the front end surface of the limiting part for fixing an atomizer, a rubber ring groove being arranged on the outer wall surface of the column part for fixing the base, a groove for fixing an atomizer being arranged on the inner wall surface, and the column part being inserted into the base socket during use.

[0007] Preferably, the diameter of the main body part is 25-35 mm, and the length is 35-50 mm.

[0008] Preferably, the tapered part has a first tapered part and a second tapered part arranged in sequence in the aerosol transmission direction; the angle between the first tapered part and the vertical direction to the aerosol transmission direction is 60°-85°, and the length is 4-7 mm; the angle between the second tapered part and the vertical direction to the aerosol transmission direction is 50°-75°, and the length is 40-70 mm.

[0009] Preferably, the extension part extends from the end of the tapered part in the aerosol transmission direction, and the length is 80-150 mm, and the inner diameter is 3-7 mm.

[0010] Preferably, the diameter of the limiting part of the base matches the outer diameter of the column part, the thickness is 3-5 mm, and the diameter of the column part is 10-17 mm.

[0011] Preferably, the length of the inner tube is 30-45 mm, and the annular gap between the inner tube and the outer tube is less than 3 mm.

[0012] Preferably, the compensation air tube has an inner diameter of 1-5 mm, the distance between the compensation air tube axis and the front end of the outer tube is 2-8 mm, and the length of the aerosol transmission cavity is set to 30-70 mm.

[0013] Preferably, the aerosol inlet portion comprises, in sequence along the aerosol transmission direction, a first inlet section gradually increasing in size along the aerosol transmission direction from the end of the base connecting portion, and a second inlet section extending from the first inlet section along the aerosol transmission direction.

[0014] Preferably, a waste liquid tube for discharging waste liquid is arranged at the bottom end of the main body portion on the side of the inner tube end.

[0015] The utility model discloses a kind of integrated heating spray chambers for single particle analysis sample introduction, auxiliary gas forms tangential airflow in cylindrical transmission cavity inner wall by compensation air tube, reduces the collision of aerosol and inner wall, the design of extension portion can reduce the condensation effect of aerosol, simultaneously reduce the number of connecting port, so that spray chamber and rectangular tube can be directly communicated, better sealing property is obtained while having good concentricity, to improve the transmission efficiency of sample, and the design of pluggable base facilitates the daily cleaning and maintenance of spray chamber. BRIEF DESCRIPTION OF DRAWINGS

[0016] Figure 1 It is a structure schematic view of the utility model;

[0017] Figure 2 It is the appearance structure schematic view of the utility model;

[0018] Figure 3 It is time resolution spectrum for testing 30nm gold nanoparticles in the utility model;

[0019] Figure 4 It is particle size distribution diagram for testing 30nm gold nanoparticles in the utility model;

[0020] In the drawing: 10, outer tube, 20, inner tube, 30, annular gap, 40, aerosol transmission cavity, 210, main body portion, 211, base socket, 212, compensation air tube, 213, waste liquid tube, 220, base connecting portion, 230, aerosol inlet portion, 240, tapered portion, 250, extension portion, 260, interface portion, 270, base, 271, atomizer socket, 272, limiting portion, 273, column portion, 274, inner rubber ring groove, 275, outer rubber ring groove. DETAILED DESCRIPTION

[0021] The technical scheme of the utility model will be further specifically described below by specific embodiments, and combined with the drawings:

[0022] Embodiment: As shown in Figure 1 and Figure 2 A one-piece spray chamber for single particle analysis sample introduction, which can be heated, has a double-layer structure, including an outer tube 10, an inner tube 20 and a base 270, which are coaxially arranged.

[0023] The outer tube 10 has a cylindrical main body 210 at the front, a gradually tapered portion 240 at the middle, and an extension 250 at the end, wherein the main body 210 extends in the aerosol transmission direction, a base socket 211 for inserting the base is arranged at the front end of the main body 210, and the base socket 211 is formed at the center of the front end face of the main body 210, the wall surface of the main body 210 at the front is provided with a compensation gas pipe 212 for connecting the outside for compensating gas, in this embodiment, two compensation gas pipes 212 are arranged on the side wall surface adjacent to the front end of the main body 210, and in other embodiments, the compensation gas pipe 212 can also be arranged on the front end face of the main body 210 according to the structure of the atomizer.

[0024] The diameter of the main body 210 of the outer tube 10 of the spray chamber is 25-35 mm, preferably 30 mm, and the length of the main body 210 is 30-50 mm, preferably 42 mm; the inner diameter of the base socket 211 is matched with the diameter of the base, which is set to 14 mm in this embodiment; the overall length of the inner tube 20 of the spray chamber is 30-45 mm, preferably 40 mm; the inner diameter of the compensation gas pipe 112 is 1-5 mm, preferably 2 mm; the distance between the axis of the compensation gas pipe 212 and the front end of the outer tube 10 is 2-8 mm, preferably 5 mm.

[0025] A waste liquid pipe 213 for discharging waste liquid is arranged at the bottom end of the main body 210 at the end side of the inner tube 20, which is inclined upward away from the main body 210 in the aerosol transmission direction or the direction opposite to the aerosol transmission direction, and the inclination angle is 30-60°, preferably 60°; the inner diameter of the waste liquid pipe 113 is 2-3 mm, preferably 2.4 mm; the distance between the waste liquid pipe 213 and the front end of the outer tube 10 is 20-38 mm, preferably 36 mm.

[0026] The tapered portion 240 extends from the end of the main body 210, and the size gradually decreases in the aerosol transmission direction, the angle between the first-stage tapered portion and the vertical direction to the aerosol transmission direction is 60°-85°, preferably 80°, and the length is set to 4-7 mm, preferably 5 mm; the angle between the second-stage tapered portion and the vertical direction to the aerosol transmission direction is 50°-75°, preferably 70°, and the length is set to 40-70 mm, preferably 45 mm.

[0027] The extension part 250 is connected to the end of the taper part 240 and extends in the aerosol transmission direction, and the inner diameter thereof is set to 3-7 mm, preferably 5 mm, and the length thereof is set to 80-150 mm, preferably 90 mm. In actual implementation, the extension part can further improve the sample transmission efficiency through heating.

[0028] The interface part 260 matched with the external device is arranged at the end of the extension part 250. In the embodiment, a spherical grinding mouth is selected, and the spherical grinding mouth is formed after extending a certain distance from the end of the extension part 250 in the aerosol transmission direction. The spherical grinding mouth can be used for matched connection with the connector of the ICP-MS torch pipe and other external instruments. According to the different external connection structures, the interface with the corresponding structure can be selected.

[0029] The base 270 is arranged in the base socket 211 at the front end of the main body part 210, and includes the limiting part 272 and the column part 273. The base 270 is provided with the atomizer socket 271 for inserting the atomizer at the front end thereof. The atomizer socket 271 is formed in the center of the front end face of the base 270.

[0030] The diameter of the limiting part 272 matches the main body part 210, and the thickness thereof is set to 3-5 mm, preferably 3 mm. The diameter of the column part 273 is set to 10-17 mm, preferably 14 mm, the length thereof is set to 18-25 mm, preferably 21 mm, and the thickness thereof is set to 2-5 mm, preferably 3 mm. The inner wall face of the column part 273 is provided with two inner rubber ring grooves 274 for fixing the atomizer. The width and depth of the inner rubber ring grooves 274 are set to 0.8-2 mm, preferably 1.1 mm, so that the rubber ring is embedded in the inner rubber ring grooves 274 to fix the atomizer. The outer wall face of the column part 273 is provided with the outer rubber ring groove 275 for fixing the base. The width and depth of the outer rubber ring groove 275 are set to 1-2 mm, preferably 1.5 mm, so that the rubber ring is embedded in the outer rubber ring groove 275 to fix the base.

[0031] The inner tube 20 forms the base connecting part 220 extending from the base socket 211 to the end side in the aerosol transmission direction. The front end of the base connecting part 220 is connected with and integrally formed with the base socket 211. The inner diameter of the base socket 211 and the base connecting part 220 matches the size of the base to be used. After the base is inserted from the base socket 211, the base is connected with the base connecting part 220.

[0032] The base connecting part 220 is spaced apart from the main body part 210 of the outer tube 10, so that the auxiliary gas enters the space between the base connecting part 220 and the main body part 210 of the outer tube 10 from the compensation gas tube 212.

[0033] The annular gap 30 between the aerosol inlet portion 230 and the outer tube 10 is less than 3 mm, preferably 1.5 mm.

[0034] The inner cavity of the aerosol inlet portion 230 at the end side when the atomizer is assembled in the atomizer socket 271 of the base 270 and the inner cavity of the outer tube 10 at the end side of the aerosol inlet portion 230 form the aerosol transmission chamber 40, which has a length of 30-70 mm, preferably 60 mm. After the sample forms an aerosol, the aerosol enters the aerosol transmission chamber 40 from the aerosol inlet portion 230, passes through the main body portion 210, the tapered portion 240, the extension portion 250, and the interface portion 260, and then enters the next structure.

[0035] The size parameters of the spray chamber used in the performance test of the present embodiment include: the diameter of the main body portion 210 of the outer tube 10 is 30 mm, and the length is 42 mm; the inner diameter of the base socket 211 is 14 mm; the inner diameter of the atomizer socket 271 is 6 mm; the length of the inner tube 20 of the spray chamber is 40 mm; the inner diameter of the compensation tube 112 is 2 mm, and the distance between the axis and the front end of the outer tube 10 is 5 mm; the inclination angle of the waste liquid tube 213 is 60°, the inner diameter is 2.4 mm, and the distance from the front end of the outer tube 10 is 36 mm; the angle between the first tapered portion and the direction perpendicular to the aerosol transmission direction is 80°, and the length is set to 5 mm; the angle between the second tapered portion and the direction perpendicular to the aerosol transmission direction is 70°, and the length is set to 45 mm; the inner diameter of the extension portion 250 is set to 5 mm, the length is set to 90 mm, and the end is provided with the interface portion 260 matched with the external device; the base 270 is composed of a limiting portion 273 and a columnar portion 272, the thickness of the limiting portion 273 is set to 3 mm, and the diameter is matched with the main body portion; the diameter of the columnar portion 272 is set to 14 mm, the length is set to 21 mm, the thickness is set to 3 mm, the width and depth of the inner rubber ring groove 274 are set to 1.1 mm, and the width and depth of the outer rubber ring groove 275 are set to 1.5 mm; the annular gap 30 between the aerosol inlet portion 230 and the outer tube 10 is set to 1.5 mm.

[0036] As Figure 3 and Figure 4As shown, in the present embodiment, the commercialized nano-gold standard particles (NIST 8013) are used as the test sample, the time-resolved detection mode (TRA) of the Agilent 8900 model ICP-MS is used, the commercialized concentric nebulizer is used to test the performance of the spray chamber proposed in the above embodiment, the extendable part of the spray chamber is heated during the test, and the test parameters are as follows: the carrier gas flow rate is 0.55 L / min, the auxiliary gas flow rate is 0.38 L / min, the sampling rate is 0.02 ml / min, and the integration time is 0.1 ms.

[0037] For the test of the single-particle sample, the nano-gold particles are ultrasonically treated for 45 s before the test to reduce the agglomeration of the nano-gold particles, and a nano-gold particle solution with a concentration of 50 ppt is configured for the test. 197 As the detection element, the sample sampling flow rate is 0.02 ml / min.

[0038] The test results show that the transmission efficiency of the spray chamber proposed in the above embodiment for the nano-gold particles is 65±2.45 %.

[0039] The spray chamber of the present application shortens the transmission path of the sample, the cylindrical transmission cavity can obtain the optimal airflow distribution, the auxiliary gas forms a tangential airflow on the inner wall of the transmission cavity, reduces the collision between the aerosol and the inner wall of the spray chamber, and in addition, the design that the extension part can be heated slows down the condensation of the aerosol in the transmission path, can work at a low sampling flow rate, greatly improves the transmission efficiency of the sample, and realizes the high-sensitivity detection of the single-cell / single-particle sample.

[0040] The above-described embodiment is only a preferred scheme of the present application, and does not limit the present application in any form, and other variants and modifications can be made without exceeding the technical scheme recorded in the claims.

Claims

1. An integrated heatable spray chamber for single particle analysis sample introduction, comprising an outer tube and an inner tube, the outer tube comprising a main body portion in the shape of a cylinder extending in an aerosol transmission direction, a base socket being provided at a front end of the main body portion, a compensation gas tube being provided on a front end face or a side wall face of the main body portion, a tapered portion gradually decreasing in size in the aerosol transmission direction being extended from a distal end of the main body portion, the inner tube comprising a base connecting portion formed so as to extend from the base socket in the aerosol transmission direction, a front end of the base connecting portion being connected to and integrally formed with the base socket, an aerosol inlet portion being formed at a distal end of the base connecting portion, the aerosol inlet portion extending from the distal end of the base connecting portion to a circumferential outside and extending to a middle portion of an inner cavity of the main body portion toward a distal end side, an annular gap being formed between the aerosol inlet portion and the outer tube, characterized in that, The tapered end extends a cylindrical extension in the aerosol transmission direction, and an interface part matched with the rectangular tube is arranged at the end of the extension; a base is sealingly inserted into the base socket, and an atomizer socket for fixing the atomizer is arranged at the front end of the base, the atomizer socket is communicated into the inner cavity of the inner tube, and the inner cavity of the aerosol inlet part and the inner cavity of the outer tube at the end side of the aerosol inlet part form an aerosol transmission cavity.

2. An integrated, heatable spray chamber for single particle analysis sample introduction according to claim 1, characterized in that The base is divided into a limiting part and a column part, the front end surface of the limiting part is provided with an atomizer socket for fixing the atomizer, the outer wall surface of the column part is provided with a rubber ring groove for fixing the base, and the inner wall surface is provided with a groove for fixing the atomizer, and the column part is inserted into the base socket during use.

3. An integrated, heatable spray chamber for single particle analysis sample introduction according to claim 1, characterized in that The diameter of the main body part is 25-35 mm, and the length is 35-50 mm.

4. An integrated, heatable spray chamber for single particle analysis sample introduction according to claim 1, characterized in that, The tapered part has a first tapered part and a second tapered part arranged in sequence in the aerosol transmission direction; the angle between the first tapered part and the vertical to the aerosol transmission direction is 60°-85°, and the length is set to 4-7 mm; the angle between the second tapered part and the vertical to the aerosol transmission direction is 50°-75°, and the length is set to 40-70 mm.

5. An integrated, heatable spray chamber for single particle analysis sample introduction according to claim 1, characterized in that, The extension part is extended from the end of the tapered part in the aerosol transmission direction, and the length is set to 80-150 mm, and the inner diameter is set to 3-7 mm.

6. An integrated, heatable spray chamber for single particle analysis sample introduction according to claim 1, characterized in that The diameter of the base limiting part matches the outer diameter of the column part, the thickness is set to 3-5 mm, and the diameter of the column part is set to 10-17 mm.

7. An integrated, heatable spray chamber for single particle analysis sample introduction according to claim 1, characterized in that, The length of the inner tube is set to 30-45 mm, and the annular gap between the inner tube and the outer tube is less than 3 mm.

8. An integrated, heatable spray chamber for single particle analysis sample introduction according to claim 1, characterized in that, The inner diameter of the compensation air tube is 1-5 mm, the distance between the axis of the compensation air tube and the front end of the outer tube is 2-8 mm, and the length of the aerosol transmission cavity is set to 30-70 mm.

9. An integrated, heatable spray chamber for single particle analysis sample introduction according to claim 1, characterized in that, The aerosol inlet part includes a first inlet section formed in sequence in the aerosol transmission direction, and the size gradually increases in the aerosol transmission direction from the end of the base connecting part; a second inlet section extending from the first inlet section in the aerosol transmission direction.

10. An integrated, heatable spray chamber for single particle analysis sample introduction according to claim 1, characterized in that, A waste liquid pipe for discharging waste liquid is arranged at the bottom end of the main body part at the end side of the inner tube.

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