Spray chamber, sample atomization and introduction device, analysis device and method for analyzing components of a sample

Abstract

Spray chamber (10), which includes: a sample inlet opening area (121) into which a gas stream is introduced containing sample droplets atomized by a nebulizer; an outlet opening area (110) which directs at least a portion of the gas flow introduced through the sample inlet opening area (121) to an exterior thereof; and a flow passage pipe section (13) which has the sample inlet opening area (121) at one end thereof and the outlet opening area (110) at the other end thereof and serves as a flow passage for the introduced gas flow, wherein the flow passage pipe section (13) comprises a first pipe section (11) having the outlet opening area (110) at an end region thereof, and a second pipe section (12), having the sample inlet opening area (121) at another end area thereof, the first pipe section (11) comprises a cylindrical area (112) comprising an end area opposite the end area having the outlet opening area (110) and a conical area (111) with an inner diameter which decreases successively towards one side of the outlet opening area (110), the second pipe section (12) comprises a cylindrical area (120) comprising an end area opposite the end area having the sample inlet opening area (121), wherein an outer diameter of the cylindrical area (120) of the second pipe section (12) is smaller than an inner diameter of the cylindrical area (112) of the first pipe section (11), the spray chamber (10) comprises a double pipe section (100) formed by overlapping at least a part of the cylindrical area (112) of the first pipe section (11) and the cylindrical area (120) of the second pipe section (12), and an outer side surface of the double tube section (100) is provided with an additional gas inlet opening and an additional gas inlet tube section (101), which serves as an introduction channel for introducing an additional gas into the double tube section (100) through the additional gas inlet opening, characterized in that an angle formed between a central axis direction of the sample inlet opening area (121) and a central axis direction of the cylindrical area (112) of the first tube section (11) ranges from 10° to 60°.

Description

Technical field

[0001] The present invention relates to a spray chamber, a sample atomization and introduction device, an analysis device and a method for analyzing components of a sample. State of the art

[0002] A sample atomization and introduction device with nebulizer (atomizer) and spray chamber is provided in various types of analytical devices to atomize a sample liquid and introduce the atomized sample liquid into an analytical unit in the form of droplets (see, for example, Japanese patent application publication JP H06-102249 A, which is expressly incorporated herein by reference in its entirety).

[0003] Document US 2013 / 0181126 A1 discloses a sample transfer device for transferring a dispersion of particles in a sample spray into a mass spectrometer for mass analysis. In this device, a sample of elementally labeled particles from a dispersion is transferred through a carrier aerosol spray into a gas stream for atomization and ionization by an inductively coupled plasma (ICP) source. The sample transfer device's configuration allows for complete sample consumption by passing the sample spray through a deceleration stage to slow the particle spray from its high velocity. After the deceleration stage, the slowed particle sample can be accelerated and focused by an acceleration stage for transfer into the ICP. This effectively improves particle transfer between the sample spray and the ICP.

[0004] Document US 5,969,352 A discloses a spray chamber for preparing a sample for an analytical instrument that may contain a plasma torch. In the chamber, a heated envelope gas is injected into the periphery of the spray mist, surrounding and adjacent to its origin, thereby reducing the size of the recirculated droplets, thus decreasing droplet agglomeration and promoting rapid drying of the spray mist.

[0005] Document US 5,477,048 A discloses an inductively coupled mass spectrometer for the detection of impurities. The basic structure of the spectrometer comprises: an atomizer connected to receive a solution of the sample and a gas, causing the atomizer to produce a spray in the form of a mist of droplets of the sample solution; a spray chamber arranged to receive the spray and classify the droplets within it; a plasma torch that conducts a stream of the sample solution and at least one gas; a radio frequency power source and a working coil connected to the plasma torch to supply energy to generate and maintain a plasma that ionizes the sample solution in the stream; and a mass detector arranged to receive the ionized sample solution from the plasma torch and to detect impurities in the ionized sample solution.

[0006] Document JP H06-102249 A discloses a high-frequency induction-coupled plasma mass spectrometer arranged to convey a sample atomized by an atomizer through a spray chamber to a plasma torch. An outlet port of the spray chamber, connected to the plasma torch, is arranged as a double tube, and the atomized sample is applied to an inner tube of the double tube, while a sheathing gas is applied to its outer tube. Summary of the invention

[0007] In the sample atomization and introduction device described above, the sample liquid is converted into droplets in the nebulizer. Meanwhile, the spray chamber is able to sort the sample droplets according to particle size. Specifically, the spray chamber is primarily capable of sorting the sample droplets according to particle size differences based on gravitational differences, utilizing weight differences generated by variations in droplet particle size, and introducing the fine droplets into the analysis unit of the analytical device.

[0008] The analytical sensitivity (e.g., the signal intensity) in the analytical unit of the analyzer, equipped with the sample atomization and introduction device described above and an analytical unit, is generally proportional to the efficiency of the sample introduction. Therefore, to improve analytical sensitivity, it is desirable to reduce the loss of sample droplets in the spray chamber so that more droplets are introduced into the analytical unit.

[0009] One aspect of the present invention provides novel means that enable an improvement in the sensitivity of an analytical device which introduces droplets of the sample into the device and analyzes the sample.

[0010] One aspect of the present invention relates to a spray chamber, including: a sample inlet opening area into which a gas stream containing sample droplets atomized by a nebulizer is introduced; an outlet opening area which discharges at least a part of the gas flow introduced into the sample inlet opening area to the outside; and a pipe section of a flow passage, comprising the sample inlet opening area at one end thereof and the outlet opening area at the other end thereof, and which serves as a flow passage for the introduced gas flow, wherein the pipe section of the flow passage includes a first pipe section which has the outlet opening area at one end thereof, and a second pipe section which has the sample inlet opening area at one end thereof, the first pipe section has a cylindrical area, including an end area opposite the end area which has the outlet opening area, and a conical area with an inner diameter which decreases successively towards the side of the outlet opening area, the second pipe section has a cylindrical area, including an end area opposite the end area which has the sample inlet opening area, wherein an outer diameter of the cylindrical area of ​​the second pipe section is smaller than an inner diameter of the cylindrical area of ​​the first pipe section, the spray chamber includes a double-pipe section formed by overlapping at least part of the cylindrical area of ​​the first pipe section and the cylindrical area of ​​the second pipe section, and an outer side surface of the double pipe section is provided with an additional gas inlet opening and an additional gas inlet pipe section, which serves as an inlet channel for introducing an additional gas into the double pipe section through the additional gas inlet opening, wherein according to the invention an angle formed between a central axis direction of the sample inlet opening area and a central axis direction of the cylindrical area of ​​the first pipe section ranges from 10° to 60°.

[0011] In one embodiment, an angle formed by a central axis direction of the additional gas inlet pipe section and a central axis direction of the cylindrical area of ​​the first pipe section can lie within a range of 90° to 130°.

[0012] In one embodiment, the additional gas inlet opening, when using the center of the outer side surface of the double tube section as a reference point, which is located at a position on the outer side surface of the double tube section, can be located closer to the second tube section.

[0013] In one embodiment, the length of the double tube section can be within a range of 10.0 mm to 30.0 mm.

[0014] In one embodiment, the difference between the inner diameter of the cylindrical section of the first pipe section and the outer diameter of the cylindrical section of the second pipe section can be within a range of 1.0 mm to 6.0 mm.

[0015] In one embodiment, the ratio (length / maximum inner diameter) of the length of the conical section of the first pipe segment to the maximum inner diameter of the conical section can be within a range of 0.5 to 3.0.

[0016] In one embodiment, the total length of the spray chamber can be within a range of 80.0 mm to 200.0 mm.

[0017] In one embodiment, the first pipe section and the second pipe section can be components made of glass, quartz or a fluorine resin.

[0018] In one embodiment, the outer side surface of the double pipe section can be provided with an opening for waste liquid and a waste liquid pipe section, which serves as a waste liquid channel for the removal of waste liquid, in order to discharge waste liquid from the double pipe section through the waste liquid opening to the outside.

[0019] Another aspect of the present invention relates to a sample atomization and introduction device, including the spray chamber and nebulizer described above.

[0020] Another aspect of the present invention relates to an analysis device, including the sample atomization and introduction device described above, as well as an analysis unit.

[0021] In one embodiment, an angle formed between a horizontal direction of an arrangement surface on which the sample atomization and introduction device is arranged and the central axis direction of the cylindrical area of ​​the first pipe section of the spray chamber can lie within a range of 20° to 90°.

[0022] In one embodiment, the analysis device can be an inductively coupled plasma analysis device, and the analysis device can include a plasma torch.

[0023] In one embodiment, the analysis device can be a mass spectrometry instrument with inductively coupled plasma.

[0024] Another aspect of the present invention relates to a method for analyzing a component of a sample liquid, including analyzing a component of a sample liquid to be subjected to analysis using the analytical apparatus described above, and furthermore including the introduction of an additional gas from the additional gas inlet pipe section when a gas stream containing droplets of the sample liquid atomized by the nebulizer flows through the pipe section of the flow passage of the spray chamber.

[0025] According to one aspect of the present invention, a spray chamber can be provided which can contribute to improving the sensitivity of an analytical device.

[0026] Furthermore, according to one aspect of the present invention, the following can be provided: a sample atomization and introduction device, including the above spray chamber, an analysis device, including the sample atomization and introduction device, and a method for analyzing the components in a sample liquid using the analysis device. Brief description of the drawings Fig. Figure 1 is a schematic view (a side view) showing an example of a spray chamber according to one aspect of the present invention. Fig. Figure 2A is a schematic view (a top view) showing an example of the spray chamber according to one aspect of the present invention. Fig. Figure 2B is a schematic view (a side view) showing an example of the spray chamber according to one aspect of the present invention. Fig.Figure 3A is an illustrative view of an arrangement of an additional gas inlet pipe section in the spray chamber, which is shown in the Fig. 2A and Fig. 2B is shown. Fig. Figure 3B is an illustrative view of the arrangement of the auxiliary gas inlet pipe section in the spray chamber, as shown in the Fig. 2A and Fig. 2B is shown. Fig. Figure 3C is an illustrative view of the arrangement of the auxiliary gas inlet pipe section in the spray chamber, as shown in the Fig. 2A and Fig. 2B is shown. Fig. Figure 4A is a schematic view (a top view) showing another example of the spray chamber according to one aspect of the present invention. Fig. Figure 4B is a schematic view (a side view) showing another example of the spray chamber according to one aspect of the present invention. Fig.Figure 5 is a schematic view (a side view) showing an example of a Scott-type spray chamber according to the prior art, which is widely used as a spray chamber of an inductively coupled plasma analyzer. Description of embodiments

[0027] Exemplary aspects, illustrated in the figures, are described below based on the figures. The present invention is not limited to the aspects shown in the figures. Spray chamber

[0028] A spray chamber according to one aspect of the present invention comprises: a sample inlet opening region into which a gas stream containing sample droplets atomized by a nebulizer is introduced; an outlet opening region which discharges at least a portion of the gas stream introduced into the sample inlet opening region to the outside; and a pipe section of a flow passage comprising the sample inlet opening region at one end and the outlet opening region at the other end, and serving as a flow passage for the introduced gas stream. The pipe section of the flow passage comprises: a first pipe section comprising the outlet opening region at one end, and a second pipe section comprising the sample inlet opening region at one end.The first pipe section has a cylindrical portion with an end section opposite the end section, which contains the outlet opening, and a conical portion with an inner diameter that decreases progressively towards the side of the outlet opening. The second pipe section has a cylindrical portion with an end section opposite the end section, which contains the sample inlet opening. Note that the outer diameter of the cylindrical portion of the second pipe section is smaller than the inner diameter of the cylindrical portion of the first pipe section.The spray chamber includes a double-tube section formed by overlapping at least a part of the cylindrical area of ​​the first tube section and the cylindrical area of ​​the second tube section, and an outer side surface of the double-tube section is provided with an additional gas inlet opening and an additional gas inlet tube section, which serves as an inlet channel for introducing an additional gas into the double-tube section through the additional gas inlet opening.

[0029] The spray chamber described above is described in more detail below.

[0030] First, a conventionally used spray chamber is described.

[0031] Fig. Figure 5 is a schematic view (a side view) showing an example of a Scott-type spray chamber according to the prior art, which is widely used as a spray chamber of an inductively coupled plasma analyzer.

[0032] In a Scott-type spray chamber 20 (double-flow spray chamber according to Scott) according to the prior art, illustrated in Fig.5. Sample droplets, formed by atomizing a sample liquid in a nebulizer 21, are introduced as a gas stream along with a carrier gas. The Scott-type spray chamber 20 is a tubular component in which the entire spray chamber has a double-tube structure. The gas stream containing the sample droplets is introduced from the nebulizer into an inner tube 22 of the double tube. In the spray chamber 20, droplets with small particle sizes and droplets with large particle sizes are sorted according to the difference in gravity using weight differences of the droplets caused by their different particle sizes. The droplets with small particle sizes pass through an outer tube 23 of the double tube to be discharged from the upper region of the spray chamber (through an outlet opening 24 in the Fig.(as illustrated in the embodiment shown in 5), and are subsequently introduced into an analysis unit. Meanwhile, the droplets with a large particle size drip downwards through the spray chamber and are collected in the Fig. In the embodiment shown in section 5, the waste liquid is discharged outside the spray chamber through a waste liquid opening 25, provided at the bottom of the spray chamber.

[0033] In a Scott-type spray chamber, such as the one described above, the flow path for the gas stream containing the sample droplets is typically longer than in other types of spray chambers. Therefore, Scott-type spray chambers are said to have a high ability to sort particles by size based on gravitational differences. However, in a Scott-type spray chamber like the one described above, as well as in other conventional spray chambers, droplets adhere to the inner wall surfaces of the spray chamber, resulting in droplet loss due to wall adhesion. This is thought to reduce the efficiency with which the sample is introduced into the analytical unit.

[0034] In contrast, in the spray chamber according to one aspect of the present invention described above, the additional gas introduced from the double-tube section can contribute to a reduction in the loss of sample droplets due to wall adhesion. In particular, the additional gas introduced into the double-tube section can generate an additional gas flow that swirls in a spiral pattern around the wall surface, from the double-tube section towards the conical region of the first tube section. This additional gas flow can serve both to suppress the adhesion of the droplets to the wall surface and to capture the sample droplets and direct them to the outlet. Consequently, the loss of sample droplets due to wall adhesion can be reduced.

[0035] The spray chamber according to one aspect of the present invention is described in further detail below.

[0036] Fig.Figure 1 is a schematic view (a side view) showing an example of the spray chamber according to one aspect of the present invention. A spray chamber 10, shown in Fig. 1, is formed by a flow-through pipe section 13, including a first pipe section 11 and a second pipe section 12. In the spray chamber 10 of the in Fig. In the embodiment shown in Figure 1, the first pipe section 11 is connected to an analysis unit, which will be described in more detail below. In particular, the first pipe section 11 is connected to an inlet area 14 of a plasma torch, which is part of the analysis unit, via a connecting element 15 located closest to the side of the spray chamber. Furthermore, in the spray chamber 10, the Fig. In the embodiment shown in Figure 1, the second tube section 12 is connected to a nebulizer 16. Furthermore, the Fig. 2A and Fig.2B Schematic views showing the spray chamber alone. Fig. 2A is a top view and Fig. 2B shows a side view. Note that in the figures, dotted lines indicate thicknesses and not double pipes.

[0037] The in the Fig. 2A and Fig.The spray chamber 10 shown in Figure 2B is formed by the flow pipe section 13, which has an outlet opening region 110 at one end and a sample inlet opening region 121 at the other end. The flow pipe section 13 is formed by the first pipe section 11 and the second pipe section 12. The first pipe section 11 is formed by the outlet opening region 110, a conical section 111, and a cylindrical section 112. The second pipe section 12 is formed by a cylindrical section 120 and the sample inlet pipe section 121. A double pipe section 100 is formed by overlapping and coupling at least a portion of the cylindrical section 112 of the first pipe section 11 and the cylindrical section 120 of the second pipe section 12.Thus, an inner wall surface of a space inside the double tube of the double tube section 100 is an outer side surface of the cylindrical area 120 of the second tube section 12, and an outer wall surface of the space inside the double tube of the double tube section 100 is a wall surface of the cylindrical area 112 of the first tube section 11.

[0038] Next, the first pipe section and the second pipe section will be described in more detail.

[0039] In the Fig. 2A and Fig.2B The first pipe section 11 encloses the outlet opening region 110 at one end, and the outlet opening region 110 communicates with the conical region 111. The conical region 111 has a conical shape with an inner diameter that decreases successively towards the side of the outlet opening region. The cylindrical region 112, including the other end region of the first pipe section, communicates with the conical region 111.

[0040] In the second pipe section 12, the cylindrical area 120, which includes one end area of ​​the second pipe section, communicates with the area 121 of the sample inlet opening, which includes the other end area.

[0041] The flow-through pipe section 13 is formed by the first pipe section 11 and the second pipe section 12, having the structures described above. Furthermore, in a connection area between the first pipe section 11 and the second pipe section 12, the cylindrical sections of the corresponding pipe sections overlap to form the double pipe section 100. The double pipe section is the part between an end-area opening of the cylindrical section of the first pipe section and an end-area opening of the cylindrical section of the second pipe section. Thus, the corresponding ends of the double pipe section are open, but an imaginary plane surrounded by the openings is referred to below as the bottom surface. In the Fig. 2A and Fig.In the embodiment shown in 2B, the first pipe section 11 and the second pipe section 12 are separate components, and the flow passage pipe section 13 is formed by inserting the cylindrical area 120 of the second pipe section 12 into the end opening of the cylindrical area 112 of the first pipe section 11 in order to connect the two pipe sections.For example, by shaping the cylindrical section 112 of the first pipe section 11 into a conical shape at its end, and by shaping the inner diameter of the conical end opening in a substantially identical shape to the outer diameter of the end opening of the cylindrical section 120 of the second pipe section 12, the escape of the additional gas introduced into the double pipe section 100, which is formed by joining the two pipe sections, through the connection area between the two pipe sections to the outside can be prevented. Alternatively, a gas tightness can be achieved in the connection area using a sealing element or the like.Note that regarding the gas tightness of the connection area, the escape of the additional gas need not be completely prevented, and a leakage is permitted that does not impede the gas flow created by the additional gas introduced into the twin-pipe section. Alternatively, the flow-through pipe section can be formed by a single-piece casting of the first and second pipe sections.

[0042] The double-tube section 100 has an opening in its outer side surface, or more precisely, in the outer side surface of the cylindrical region 112 of the first tube section 11. This opening is an additional gas inlet opening for introducing the additional gas into the double-tube section (i.e., the space enclosed by the inner and outer wall surfaces of the double-tube section). An additional gas inlet tube section 101 serves as an inlet channel for introducing the additional gas into the double-tube section through the opening. By introducing the additional gas into the double-tube section from the additional gas inlet tube section through the opening, the introduced additional gas can swirl around the double-tube section, thus generating a gas flow (an additional gas flow) that moves spirally towards the conical region 111 of the first tube section 11.The presence of the conical section with an inner diameter that decreases progressively towards the side of the spray chamber's outlet can also contribute to the formation of a spiral gas flow from the additional gas stream. This additional gas flow can form a gas stream that spirals around the wall surfaces of the conical section towards the outlet. This additional gas flow can suppress the adhesion of the sample droplets to the wall surface of the conical section and, furthermore, can capture the sample droplets and guide them towards the outlet.

[0043] In the Fig. 2A and Fig.In the embodiment shown in Figure 2B, the cylindrical section 112 of the first pipe section 11 includes a waste liquid opening, which is provided separately from the auxiliary gas inlet opening, as well as a waste liquid pipe section 113 for discharging waste liquid through the waste liquid opening. The waste liquid pipe section 113 is capable of serving as a waste liquid channel for discharging waste liquid from the interior of the double pipe section 100 to the outside. Furthermore, in the embodiment shown in the Fig. 2A and Fig. In the embodiment shown in Figure 2B, the second pipe section 12 also includes a waste liquid pipe section 122. The waste liquid pipe section 122 is capable of serving as a waste liquid channel for the discharge of waste liquid from the interior of the second pipe section 12 to the outside.

[0044] Next, the relevant components of the spray chamber will be described in more detail.

[0045] The Fig. Figures 3A to 3C are illustrative views of an arrangement of the auxiliary gas inlet pipe section in the spray chamber, as shown in the Fig. 2A and Fig. 2B. Fig. 3A is a view in which explanatory arrows point into the Fig. 2A, the top view shown, was drawn in, and Fig. 3B is a cross-sectional view of the part of the twin-pipe section that includes the auxiliary gas inlet pipe section. Fig. 3C is a view in which explanatory arrows point into the Fig.The side view shown in Figure 2B is indicated. The arrows in the figures denote the following directions. An X-direction is a centerline direction of the auxiliary gas inlet pipe section. A Y-direction is a centerline direction of the cylindrical section of the first pipe section and is aligned with a centerline direction of the conical section of the first pipe section and a centerline direction of the cylindrical section of the second pipe section. The Y-direction is also aligned with a centerline direction of the flow passage pipe section. A Z-direction is a centerline direction of the inlet pipe section.

[0046] The Fig. 4A and Fig. Figures 4B each show a top view and a side view of a spray chamber according to another embodiment. The figures in the Fig. 4A and Fig. The embodiment shown in 4B differs from the one shown in the Fig.The embodiment shown in Figures 1 to 3C differs only in the arrangement of the additional gas inlet pipe section 101 and the sample inlet opening area 121. A description of similarities between the two embodiments is omitted.

[0047] An angle θ1, formed by the X-direction and the Y-direction, is 90° in the Fig. 3A to 3C illustrated embodiment and 110° in the Fig. 4A and Fig.In the embodiment shown in Figure 4B, the angle θ1 is set within a range of 0° to 180°. To ensure that the gas flow of the additional gas, which is introduced through the additional gas inlet pipe section, swirls uniformly around the double pipe section, the angle θ1 is preferably within a range of 90° to 130°. Furthermore, the additional gas inlet opening can be provided at any position on the outer side face of the double pipe section. For example, using the center of the outer side face of the double pipe section as a reference, the additional gas inlet opening can be provided at a position closer to the second pipe section, at a position closer to the first pipe section, or at a position where the center of the additional gas inlet opening is aligned with the center of the outer side face of the double pipe section.To ensure that the gas flow of the additional gas, introduced through the additional gas inlet pipe section, swirls evenly around the double pipe section, the additional gas inlet opening is preferably provided at a position on the outer side surface of the double pipe section which is closer to the second pipe section, and the closer the additional gas inlet opening is to the second pipe section, the better.

[0048] To ensure that the gas flow introduced through the auxiliary gas inlet pipe section swirls uniformly around the double pipe section, the length of the double pipe section, or more precisely, the shortest distance between the bottom surface on the side of the first pipe section and the bottom surface on the side of the second pipe section, is preferably within a range of 10.0 mm to 30.0 mm. Furthermore, the diameter of the auxiliary gas inlet opening is preferably within a range of 0.1 mm to 3.0 mm. Note that this applies similarly to the diameter of the waste liquid opening.

[0049] In the first pipe section, the conical section is the portion located between the cylindrical section and the outlet opening, with the inner diameter decreasing successively towards the outlet opening. Within this first pipe section, the point where the inner diameter begins to vary from the cylindrical section towards the outlet opening is defined as the first end of the conical section, and the point where the inner diameter ceases to vary is defined as the second end. The shortest distance between the first and second ends of the conical section is called the length of the conical section.To reduce sample droplet loss due to wall adhesion in the conical region, the ratio (length / maximum inner diameter) of the length of the conical region to its maximum inner diameter is preferably at least 0.3. By setting this ratio to 0.3 or more (preferably 0.5 or more, and even more preferably 0.8 or more), the gas flow of the additive gas in the conical region can be made to swirl more uniformly in a spiral pattern. Furthermore, as the ratio increases, the length of the conical region increases relative to its maximum inner diameter. The ratio can, for example, be set to 4.0 or less, or to 3.5 or less. However, as the length of the conical region increases, leading to a corresponding increase in the ratio, the overall length of the spray chamber also increases, resulting in an increase in the size of the spray chamber.Meanwhile, the presenting inventors observed no further change in the analysis sensitivity when the conical area was extended beyond the point at which the ratio exceeded 3.0. Therefore, with a view to achieving both an improvement in the analysis sensitivity and a reduction in the size of the spray chamber, the ratio is preferably set at or below 3.0.

[0050] The maximum inner diameter of the conical section of the first pipe segment is preferably within a range of, for example, 25.0 to 65.0 mm. The maximum inner diameter of the conical section refers to the inner diameter of the cylindrical section that communicates with the conical section. As noted above, the cylindrical section may have a tapered shape at its end. In this case, the inner diameter of the cylindrical section refers to the maximum inner diameter of the cylindrical section. Furthermore, the minimum inner diameter of the conical section of the first pipe segment is preferably within a range of, for example, 5.0 to 10.0 mm. The shape of a cross-section passing through the central axis of the conical section need not necessarily form part of a perfect triangle, and at least part of this cross-sectional shape may be a curve.

[0051] In the spray chamber described above, the outer diameter of the cylindrical section of the second pipe segment is smaller than the inner diameter of the cylindrical section of the first pipe segment. Consequently, the double pipe segment can be formed by overlapping at least a portion of the cylindrical section of the first pipe segment and the cylindrical section of the second pipe segment. The difference between the inner diameter of the cylindrical section of the first pipe segment and the outer diameter of the cylindrical section of the second pipe segment is preferably within a range of 1.0 mm to 6.0 mm.Provided this difference lies within a range of 1.0 mm to 6.0 mm, the width of a space within the twin-tube section, which is surrounded by the wall surface of the cylindrical section of the first tube section and the outer side surface of the cylindrical section of the second tube section, or, in other words, the space into which the additive gas is introduced, can be specified within a range of 0.5 mm to 3.0 mm. The width of this space is preferably 0.5 mm or more to facilitate the removal of waste liquid from the twin-tube section. Furthermore, the width of this space is preferably 3.0 mm or less to ensure that the gas flow of the additive gas introduced through the additive gas inlet tube section swirls uniformly around the twin-tube section.For example, the inner diameter of the cylindrical section of the second pipe segment is preferably within a range of, for example, 20.0 mm to 60.0 mm. If the inner diameter of the cylindrical section of the second pipe segment is, for example, 20 mm or more, collisions between the sample droplets in the gas stream introduced through the sample inlet opening can be effectively suppressed, and consequently, droplet loss caused by collisions between droplets can be reduced. Furthermore, the inner diameter of the cylindrical section of the second pipe segment is preferably, for example, 60 mm or less, in order to reduce the size of the second pipe segment and also the size of the spray chamber.

[0052] The second pipe section includes the cylindrical section and the sample inlet opening section and preferably consists of the cylindrical section and the sample inlet opening section. In the case of the Fig. In the embodiment shown in Figure 3C, the angle θ2 formed by the central axis direction of the sample inlet opening area 121 (the Z-direction) and the central axis direction of the cylindrical area of ​​the first pipe section (the Y-direction) is 30°. In the embodiment shown in Fig.In the embodiment shown in Figure 4B, the Z-direction is the same direction as the Y-direction (in other words, the angle θ2 formed by the Z-direction and the Y-direction is 0°). θ2 is fixed within a range of 0° to 90°. If θ2 is 0° and the gas flow containing the sample droplets is introduced into the spray chamber from a direction that is essentially identical to the central axis direction of the sample inlet orifice region, the sample droplets are less likely to collide with the wall surface of the cylindrical section of the second tube. Consequently, the loss of sample droplets due to wall adhesion in the spray chamber can be reduced even more effectively. Therefore, with a view to further improving analytical sensitivity, the Z-direction and the Y-direction are preferably the same.

[0053] If, on the other hand, the Z-direction is inclined relative to the Y-direction and the gas stream containing the sample droplets is introduced into the spray chamber from a direction essentially identical to the central axis direction of the sample inlet orifice region, it is likely that at least some of the sample droplets will collide with the wall surface of the cylindrical section of the second tube. When the sample droplets collide with the wall surface of the cylindrical section of the second tube, the collision can break them into finer droplets, and therefore the droplets discharged from the spray chamber tend to be finer. Finer sample droplets are preferable for stabilizing the sensitivity of the analytical unit of the analyzer.Therefore, if stability is a priority, the Z-direction is preferably inclined relative to the Y-direction, and in this case θ2 is preferably set within a range of, for example, 10° to 60°.

[0054] In the spray chamber described above, the length of the cylindrical section of the second pipe segment is preferably between, for example, 10.0 and 70.0 mm. At least a portion of the cylindrical section forms the double pipe segment, and the above length also includes the length of the portion forming the double pipe segment. As shown, for example, in the Fig. 2B and Fig.As explained in the embodiment shown in Figure 3C, the cylindrical section of the second pipe segment can have a non-perfectly cylindrical shape. The area of ​​its base surface on the side of the sample inlet opening can be inclined relative to the central axis of the cylindrical section of the second pipe segment. In this case, the length of the cylindrical section is the shortest length (l in Fig. 3C, for example).

[0055] In the spray chamber described above, there are no particular restrictions regarding the shape and length of the outlet opening area of ​​the first pipe section, as long as the outlet opening area includes an opening that serves as the outlet. The pointed end of the outlet opening area normally serves as a connector, attached to the analysis unit of the analytical device, and therefore the shape of the pointed end can be determined according to the shape of the analysis unit.

[0056] Meanwhile, there are no specific restrictions regarding the shape and length of the sample inlet opening of the second tube section, as long as the sample inlet opening provides an opening for introducing the gas stream containing the sample droplets from the nebulizer. The sample inlet opening typically serves as an insert port into which the pointed end of the nebulizer is inserted. The sample inlet opening can, for example, be cylindrical, but as noted above, there are no specific restrictions regarding its shape.

[0057] Regarding the overall length of the spray chamber, there is a general tendency for droplet loss within the spray chamber to be more easily reduced with decreasing overall length, while the ability to sort particle sizes tends to improve with increasing overall length. Considering these factors, the overall length of the spray chamber is preferably within a range of, for example, 80.0 mm to 200.0 mm. The overall length of the spray chamber is the shortest distance from one extreme end to the other extreme end when the spray chamber is viewed from the side. This corresponds, for example, to a length L in Fig. 3C and a length L in Fig. 4B.

[0058] In the spray chamber described above, the additional gas can be introduced from the double-tube section, thereby reducing the loss of sample droplets due to wall adhesion. However, if the sample droplets are subjected to particle size sorting within the spray chamber using gravitational differences, some of the sample liquid introduced as droplets may remain in the spray chamber instead of being discharged. Furthermore, some of the sample liquid introduced as droplets may remain in the spray chamber due to wall adhesion. The spray chamber described above preferably includes at least one waste liquid channel to discharge any remaining waste liquid to the outside.For example, a waste liquid channel for draining sample liquid remaining in the first pipe section can be provided at a desired position in the first pipe section, and in one embodiment, the waste liquid channel can be provided in the part forming the double pipe section. In other words, in the spray chamber described above, the outer side surface of the double pipe section can be provided with a waste liquid opening and a waste liquid pipe section that serves as a waste liquid channel for draining waste liquid from the double pipe section outwards through the waste liquid opening (for example, the waste liquid pipe section 113 in ). Fig.2B). Additionally, the outer side surface of the second pipe section can be provided with a waste liquid opening to discharge waste sample liquid remaining in the second pipe section, and a waste liquid pipe section serves as a waste liquid channel for discharging the waste liquid from the second pipe section to the outside through the waste liquid opening (for example, waste liquid pipe section 122 in Fig. 2B).

[0059] In the present invention and in the description, the term "cylindrical," used in reference to the cylindrical region, is not limited to the meaning of a perfectly cylindrical shape and includes, as noted above, embodiments in which a part with a different inner diameter is provided at the end region, which is connected to the part having the cylindrical shape. As noted above, the term "conical," used in reference to the conical region, is not limited to the meaning of a perfectly conical shape. Furthermore, the term "essentially identical," used to refer to a positional relationship between two directions or to the sizes of two diameters, is used to mean, in addition to a completely identical condition, to include a generally acceptable margin of error.This error range refers to a range which, for example, does not exceed 0.1° with respect to a positional relationship between two directions, and a range which, for example, does not exceed 1% with respect to the sizes of two diameters.

[0060] The first and second pipe sections described above can be components made of any material. With regard to chemical stability, such as acid and alkali resistance, the following materials are preferably used: various types of glass, quartz, fluorinated resin, and various types of resins classified as engineering plastics or high-performance plastics, etc. Various types of fluorinated resins, such as polytetrafluoroethylene, can be cited as examples. Various types of engineering plastics, such as polycarbonate (PC), can be cited as examples of engineering plastics, and various types of high-performance plastics, such as polyetheretherketone (PEEK), can be cited as examples of high-performance plastics. Furthermore, the first and second pipe sections can be components with a single-tube structure.The first pipe section and the second pipe section can be manufactured using a well-known mold casting process. Sample atomization and introduction device

[0061] One aspect of the present invention relates to a sample atomization and introduction device, including the spray chamber and a nebulizer described above. Well-known techniques relating to sample atomization and introduction devices can be applied without limiting the use of the sample atomization and introduction device described above, except that the spray chamber is formed according to one aspect of the present invention. A well-known nebulizer capable of generating a gas stream containing the sample droplets by atomizing a sample liquid can be used as the nebulizer.

[0062] The above sample atomization device can be advantageously used to atomize a sample liquid and introduce the atomized sample liquid into various types of analytical instruments. Compared to a conventional sample atomization device, the above sample atomization device achieves higher sample introduction efficiency, which contributes to an improvement in the analytical sensitivity of the instrument. Analysis device

[0063] One aspect of the present invention relates to an analysis device, including the sample atomization and introduction device according to one aspect of the present invention and an analysis unit.

[0064] At the in Fig.In the embodiment shown in Figure 1, the inlet region 14 of the plasma torch is the part of the analytical unit that is located closest to the side of the sample atomization and introduction device. The plasma torch is the part of the analytical device described above that, for example, performs ionization using plasma, with examples of this analytical device being an inductively coupled plasma mass spectrometer (ICP-MS) and an inductively coupled plasma atomic emission spectrometer (ICP-AES).

[0065] With respect to an angle at which the sample atomization and introduction device is arranged within the analysis device, there is an angle θ3 formed by a horizontal direction (an H-direction in Fig. 1) an arrangement surface on which the sample atomization and introduction device is arranged, and the central axis direction (the Y-direction in Fig.1) The cylindrical section of the first tube segment of the spray chamber is preferably positioned within a range of 0° to 90° (i.e., from a parallel to the horizontal direction of the assembly surface to a perpendicular to the horizontal direction of the assembly surface). This allows droplets with a larger particle size, among the sample droplets introduced into the spray chamber by the nebulizer, to fall by gravity, resulting in improved particle size sorting capability. Note that the angle θ3 is specified within a range of 0° to ±90°. If θ3 is negative, the spray chamber is positioned such that the first tube segment is in a lower position than the second tube segment.Furthermore, at least one waste liquid outlet for draining waste sample liquid remaining in the outlet area of ​​the spray chamber can be provided at a desired position on the outer side surface of the outlet area. If θ3 takes on a negative value, the waste liquid outlet is preferably provided on the outer side surface of the outlet area of ​​the spray chamber.

[0066] With a view to improving both the efficiency of sample introduction into the analysis unit and the particle size sorting capability, the angle θ3 is preferably within a range of 20° to 90°, more preferably within a range of 20° to 70°, even more preferably within a range of 20° to 50°, and particularly preferably within a range of 20° to 30°.

[0067] The analytical instrument can be any of various types that require the introduction of a sample liquid in the form of fine droplets. An inductively coupled plasma (ICP) analyzer can be cited as an example of such an instrument. In an ICP analyzer, a plasma torch is located in the part of the analytical unit closest to the sample atomization and introduction device. The sample, contained in the droplets and introduced to the plasma torch, is ionized by plasma generated at the torch's pointed end. Specific examples of ICP analyzers include ICP-MS, ICP-AES, and others.In the case of ICP-MS, for example, ions generated by the ionization described above are introduced into a mass spectrometer. The mass spectrometer then sorts the ions according to their mass, and they are detected by an ion detector. Qualitative analysis can be performed based on the mass of the ions detected, and quantitative analysis can be performed based on the signal intensities of the ions with the corresponding masses. Generally, the signal intensity (the analytical sensitivity) increases with the amount of sample introduced by the sample atomization and introduction device.In the sample atomization and introduction device according to one aspect of the present invention, the efficiency of sample introduction can be improved compared to a conventional sample atomization and introduction device, and thus an improvement in analytical sensitivity can be achieved. Furthermore, in various types of analytical instruments other than ICP-MS, such as ICP-AES, an increase in sample introduction efficiency can contribute to an improvement in analytical sensitivity, and therefore the sample atomization and introduction device according to one aspect of the present invention can be advantageously used in this context. Analytical methods for components

[0068] One aspect of the present invention relates to a method for analyzing a component in a sample liquid, which includes: Analysis of a component in a sample solution to be analyzed using the analytical device according to one aspect of the present invention, and further includes: Introducing an additional gas from the additional gas inlet pipe section when the gas stream, which contains droplets of the sample liquid that have been atomized by the nebulizer, flows through the flow passage pipe section of the spray chamber.

[0069] The above analytical procedure for components is described in more detail below.

[0070] The details of the analytical apparatus used in the above component analysis procedure are as described above. The sample liquid to be analyzed is introduced into the sample atomization and introduction device of the analytical apparatus and atomized in the nebulizer, then flows into the flow-through tube section of the spray chamber and is subsequently introduced into the analysis unit and subjected to component analysis.

[0071] In a nebulizer, a gas stream containing sample droplets (the sample can be atomized) can be generated by mixing the sample liquid with a carrier gas and spraying the result. Typically, one, two, or more types of inert gas are used as the carrier gas. For example, argon gas can be cited as a specific example of a carrier gas. A well-known technique can be applied without being limited to atomizing the sample in the nebulizer.

[0072] The gas stream, containing the sample droplets atomized by the nebulizer, is introduced into the spray chamber according to one aspect of the present invention and flows through the flow passage of the spray chamber. The flow rate of the carrier gas and the quantity of sample droplets (the spray quantity) atomized by the nebulizer and introduced into the spray chamber can be determined taking into account the size of the spray chamber, and so on. For example, the flow rate of the carrier gas can be set to, for example, 0.5 to 1.2 l / min, and the quantity of sample droplets atomized and sprayed by the nebulizer (the spray quantity) can be set to, for example, 25 to 100 µl / min.Note that the carrier gas flow rate and the quantity of sample droplets can be appropriately determined taking into account the nature of the constituents (the types of elements, for example) contained in the sample liquid to be analyzed, and are therefore not limited to the ranges mentioned above. In the constituent analysis procedure described above, as the gas stream containing the sample droplets flows through the flow-through tube section, the additive gas is introduced through the additive gas inlet tube section. Consequently, as described above, the introduced additive gas can swirl around the double tube section, creating a spiral gas stream (the additive gas stream) that moves towards the conical section of the first tube. The various gases mentioned as examples of the carrier gas can be used, for instance.The additional gas can be introduced from an additional gas supply source into the twin-tube section through the additional gas inlet tube section and the additional gas inlet opening by connecting the gas supply source to the additional gas inlet tube section using a tube, such as a resin tube. For durability, a tube made of a fluoropolymer resin such as polytetrafluoroethylene is preferably used. The flow rate of the additional gas can be set within a range of, for example, 0.3 to 0.5 l / min, but is preferably adjusted appropriately taking into account the width of the space in the twin-tube section into which the additional gas is introduced, the size of the conical section, and so on, and is therefore not limited to the range mentioned above.The gas stream containing the sample droplets, which is discharged from the outlet opening of the spray chamber, is introduced into the analysis unit of the analytical device and subjected to qualitative and / or quantitative analysis. Details of specific examples of the analysis unit, etc., are as described above with respect to the analytical device according to one aspect of the present invention. Various metallic components, such as heavy metals, non-metallic components, etc., can be mentioned as examples of components to be analyzed.

[0073] In the component analysis method according to one aspect of the present invention, as described above, an improvement in analytical sensitivity can be achieved compared to a conventional component analysis method. The presenting inventors assume that this improvement is caused by an increase in the efficiency of sample introduction into the analytical unit of the analytical device, which is achieved by reducing the loss of sample droplets due to wall adhesion in the spray chamber. Such an improvement in analytical sensitivity is desirable in component analysis in various fields.As an example, with regard to various types of silicon samples, such as diverse silicon wafers used as semiconductor substrates or the like, and single-crystal ingots from which, for example, silicon wafers are cut, the metallic components of the silicon sample are analyzed, and the presence and / or extent of metallic impurities is evaluated. Contamination by metallic impurities causes defects in semiconductor devices, and therefore it is desirable to determine the presence and / or extent of metallic contamination and to reduce it by excluding silicon wafers contaminated with metallic impurities as defective products, by modifying the manufacturing conditions, and by replacing or repairing the manufacturing equipment.In recent years, improvements in the performance and other aspects of equipment have necessitated a higher quality level for semiconductor substrates. To meet this requirement, it is desirable to reduce the contamination of the silicon sample by metallic impurities, even if the contamination is only a minute amount. To accurately assess the presence and / or extent of such minute amounts of metallic contamination, a high level of sensitivity is required for the analytical device. An improvement in the analytical sensitivity of the device can be achieved according to one aspect of the present invention.Therefore, the method for component analysis according to one aspect of the present invention, which employs this analytical apparatus, can advantageously be used as a method for analyzing the metallic components of various types of silicon samples. By using the above method of component analysis, even if the amount of contamination by metallic foreign substances in the silicon sample is minute, a qualitative and / or quantitative analysis of the metallic components can be carried out with a high degree of sensitivity.To assess the contamination of the silicon sample by metallic foreign substances, a sample solution obtained by dissolving all or part of the silicon sample to be assessed, or a sample solution obtained by scanning the surface of the silicon sample with a recovery liquid such as an acid solution, so that metallic components adhering to the surface are captured by the recovery liquid, can be introduced into a nebulizer and subjected to analysis of the metallic components, possibly after pretreatment such as dilution in an acid solution or the like.The presence and / or extent of different types of contamination of the silicon sample by metallic foreign substances, such as metal contamination of a surface layer area, metal contamination of the entire body and surface metal contamination, can then be assessed based on the obtained analysis results.

[0074] However, the present invention is not limited to the evaluation of contamination by metallic foreign substances in a silicon sample, but can be applied to component analysis in various fields, and by applying the present invention an improvement in the sensitivity of the analysis can be achieved. Examples

[0075] The present invention is further described below using examples. However, the present invention is not limited to the embodiments illustrated in the examples.

[0076] In the following examples, gas was introduced by connecting a polytetrafluoroethylene tube to the additional gas inlet area of ​​the spray chamber, and waste liquid was discharged by connecting a polyvinyl chloride tube to the waste liquid tube section. Furthermore, the first and second tube sections of the spray chamber used in the examples described below were made of glass. Example 1

[0077] An ICP-MS from Example 1 was prepared by modifying the spray chamber of a commercially available ICP-MS to the spray chamber of the embodiment described in the Fig. 4A and Fig.4B is shown, with the exception that θ1 has been set to θ1 = 90°. In the ICP-MS from Example 1, θ1 = 90°, θ2 = 0°, θ3 = 30°, the maximum inner diameter of the conical section of the first pipe segment was set to 45.0 mm, the ratio (length / maximum inner diameter) of the length of the conical section to the maximum inner diameter of the conical section was set to 0.5, the length of the double pipe segment was set to 20.0 mm, the diameter of the auxiliary gas inlet port, as well as the waste liquid ports in the double pipe segment and the second pipe segment, were set to 3.0 mm, the inner diameter (the maximum inner diameter) of the cylindrical section of the first pipe segment was set to 45.0 mm, the outer diameter of the cylindrical section of the second pipe segment was set to 42.0 mm, and the total length of the spray chamber was set to 130.0 mm.

[0078] In the ICP-MS from Example 1, the analysis was performed on a 0.5 N nitric acid solution containing 0.2 ppb (based on volume) of 115The sample liquid contained In. A gas stream containing sample droplets was generated by atomizing the sample liquid in the nebulizer using a carrier gas (argon gas; flow rate 0.75 l / min). The gas stream containing the sample droplets was then introduced into the flow tube section of the spray chamber (sample droplet quantity (spray rate): 100 µl / min) through the sample introduction tube section of the spray chamber. While the gas stream passed through the flow tube section, argon gas was continuously introduced into the double tube section as an additive gas from the additive gas inlet tube section through the additive gas inlet opening at a flow rate of approximately 0.4 l / min. The analysis was performed 10 times, and the arithmetic mean of the signal intensity of the In ions obtained in each of the 10 analyses was determined.

[0079] For comparison, as example 1, the sample liquid described above was analyzed 10 times using a similar procedure to that in example 1, except that the Scott spray chamber (the Scott double-pass spray chamber) was the one described in Fig. In the embodiment shown in Figure 5 (prior art), a spray chamber was used, and the arithmetic mean of the In ion signal intensity obtained in each of the 10 analyses was determined. The In ion signal intensity (the arithmetic mean) obtained in Comparative Example 1 was then set to 1.0, after which the In ion signal intensity (the arithmetic mean) obtained by the ICP-MS analysis from Example 1 was determined as a relative value in relation to Comparative Example 1. The resulting value is shown in Table 1. Examples 2 to 4

[0080] The ICP-MS instruments of Examples 2 to 4 were prepared similarly to those in Example 1, except that the ratio (length / maximum inner diameter) of the length of the conical region to the maximum inner diameter of the conical region was varied by varying the length of the conical region. Using the ICP-MS instruments of Examples 2 to 4, the signal intensities (the arithmetic means), obtained by analyzing the sample liquid in a manner similar to that described above, were determined as relative values ​​in relation to Comparison Example 1, and the results are presented in Table 1. Table 1 Comparative example 1 Example 1 Example 2 Example 3 Example 4 Length / maximum inner diameter of the tapered section 0,5 0,8 3,0 3,2 Signal intensity (relative value) 1,0 1,7 2,0 1,9 1,9

[0081] The results presented in Table 1 confirm that the ICP-MS instruments of Examples 1 to 4 improve the analytical sensitivity (signal intensity) compared to the ICP-MS using the conventional spray chamber. This is thought to be because, while the gas stream containing the sample droplets of the sample liquid flows through the single-pipe section of the spray chamber, the additional gas is introduced into the double-pipe section. This generates an additional gas stream that spirals from the double-pipe section towards the conical area of ​​the first pipe section, swirling around the wall surface. Consequently, the loss of droplets due to wall adhesion is reduced.

[0082] A standard deviation (variation) of the signal intensities obtained in the 10 analyses was determined for each of examples 1 to 4. The standard deviation obtained for example 3 was then set to 1.0, after which the standard deviations obtained for the corresponding examples were determined as relative values ​​in relation to example 3. The results are shown in Table 2. Table 2 Example 1 Example 2 Example 3 Example 4 Length / maximum inner diameter of the conical section 0,5 0,8 3,0 3,2 Variation in signal intensity (relative value) 2,0 1,5 1,0 0,8

[0083] Comparing the signal intensities of Examples 1 to 3, listed in Table 1, with the signal intensity from Example 4, it was confirmed that no further improvement in the analysis sensitivity (signal intensity) was achieved by increasing the ratio (length / maximum inner diameter) of the length to the maximum inner diameter of the conical region beyond 3.0. Meanwhile, as this ratio increases, the overall length of the spray chamber also increases. Therefore, based on the results listed in Table 1, it can be said that, in order to achieve both a reduction in the size of the spray chamber and an improvement in the analysis sensitivity, the ratio should preferably be 3.0 or less.

[0084] Meanwhile, the variation in signal intensity, shown in Table 2, decreases with increasing ratio (length / maximum inner diameter) of length to maximum inner diameter of the conical region. Note that in Example 1, a tiny amount of droplets adhering to the wall surface of the conical region was confirmed, whereas such droplet adhesion was not confirmed in Examples 2 to 4.

[0085] With a view to improving the reliability of the analysis results, the variation in analysis sensitivity is preferably small. To further reduce the variation in analysis sensitivity (signal intensity), based on the results listed in Table 2, it can be said that the ratio (length / maximum inner diameter) of length to the maximum inner diameter of the conical region is preferably 0.8 or more. Examples 5 to 8

[0086] ICP-MS instruments were prepared in a similar manner to Example 1, except that θ1 and / or the length of the double tube section were modified as shown in Table 3, and the sample liquid was analyzed.

[0087] The signal intensity (the arithmetic mean of 10 analyses) obtained from each of the examples was determined as a relative value to comparison example 1, similar to Example 1, and the results are presented in Table 3. As shown in Table 3, the signal intensity (relative value) exceeded 1.0 in Examples 5 to 8, confirming that the analytical sensitivity (signal intensity) can be improved compared to that of ICP-MS using the conventional spray chamber (comparison example 1). Note that in Example 8, a minute quantity of droplets adhering to the wall surface of the conical region was confirmed, whereas such droplet adhesion was not confirmed in Examples 5 to 7. Table 3 Comparative example 1 Example 5 Example 6 Example 7 Example 8 Length of the double pipe section - 10.0 mm 30.0 mm 20.0 mm 20.0 mm θ1 - 90° 90° 110° 130° Signal intensity (relative value) 1,0 1,1 1,1 1,3 1,1 Example 9

[0088] An ICP-MS from Example 9 was prepared by modifying the spray chamber of a commercially available ICP-MS to the spray chamber described in the Fig.The embodiment shown in Figures 1 to 3C is described. In the ICP-MS from Example 9, θ1 = 90°, θ2 = 10°, θ3 = 30°, the maximum inner diameter of the conical section of the first pipe segment was set to 50.0 mm, the ratio (length / maximum inner diameter) of the length of the conical section to the maximum inner diameter of the conical section was set to 0.5, the length of the double pipe segment was set to 20.0 mm, the diameter of the auxiliary gas inlet port, as well as the waste liquid ports in the double pipe segment and the second pipe segment, were set to 3.0 mm, the inner diameter (the maximum inner diameter) of the cylindrical section of the first pipe segment was set to 45.0 mm, the outer diameter of the cylindrical section of the second pipe segment was set to 42.0 mm, and the overall length of the spray chamber was set to 130.0 mm.

[0089] Using the ICP-MS from Example 9, the signal intensity obtained by analyzing the sample liquid in a manner similar to Example 1 was determined as a relative value in relation to comparison example 1, similar to Example 1. The result is shown in Table 4.

[0090] Furthermore, the variation in signal intensity (a relative value in relation to Example 3) of Example 9 was determined in a similar manner to that described above. Example 10

[0091] An ICP-MS from Example 10 was prepared in a similar way to Example 9, except that θ2 was set to θ2 = 45°.

[0092] Using the ICP-MS from Example 10, the signal intensity obtained by analyzing the sample liquid in a similar manner to Example 1 was determined as a relative value in relation to comparison example 1, similar to Example 1. The result is shown in Table 4.

[0093] Furthermore, the variation in signal intensity (a relative value in relation to Example 3) in Example 10 was determined in a similar way to that described above. Example 11

[0094] An ICP-MS from Example 11 was prepared in a similar way to Example 9, except that θ2 was set to 60°.

[0095] Using the ICP-MS from Example 11, the signal intensity, obtained by analyzing the sample liquid in a similar manner to Example 1, was determined as a relative value in relation to comparison Example 1, similar to Example 1. The result is shown in Table 4.

[0096] Furthermore, the variation in signal intensity (a relative value in relation to Example 3) in Example 11 was determined in a similar manner to that described above.

[0097] The results obtained for Example 2 are also listed in Table 4. Table 4 Comparative example 1 Example 2 Example 9 Example 10 Example 11 θ2 - 0° 10° 45° 60° Signal intensity (relative value) 1,0 2,0 1,7 1,3 1,1 Variation in signal intensity (relative value) - 1,5 1,2 0,8 0,5

[0098] As shown in Table 4, in examples 9 to 11, the signal intensity (relative value) exceeds 1.0, confirming that the analysis sensitivity (signal intensity) can be improved compared to that of ICP-MS using the conventional spray chamber (comparative example 1).

[0099] Furthermore, a comparison of Example 2 with Examples 9 to 11 confirmed that the variation in signal intensity in Examples 9 to 11 was smaller than in Example 2.

[0100] From the above results, it can be said that if a further improvement in signal intensity is to be prioritized, θ2 is preferably between 0° and 10°, and if both an improvement in signal intensity and a reduction in the variation of signal intensity are to be prioritized, then θ2 is preferably within a range of 10° to 60°.

[0101] From the above results it can be confirmed that, according to one aspect of the present invention, an improvement in the analysis sensitivity can be achieved, and, according to one aspect of the present invention, an improvement in the analysis sensitivity can be achieved while reducing the variation in signal intensity.

Claims

Spray chamber (10) comprising: a sample inlet opening region (121) into which a gas stream containing sample droplets atomized by a nebulizer is introduced; an outlet opening region (110) which discharges at least a part of the gas stream introduced through the sample inlet opening region (121) to an exterior thereof; and a flow passage pipe section (13) having the sample inlet opening region (121) at one end region thereof and the outlet opening region (110) at the other end region thereof and serving as a flow passage for the introduced gas flow, wherein the flow passage pipe section (13) comprises a first pipe section (11) having the outlet opening region (110) at one end region thereof, and a second pipe section (12) having the sample inlet opening region (121) at another end region thereof, the first pipe section (11) comprising a cylindrical section (112) comprising an end region,which is opposite the end region having the outlet opening region (110), and a conical region (111) with an inner diameter which decreases successively towards one side of the outlet opening region (110), the second pipe section (12) comprises a cylindrical region (120) comprising an end region which is opposite the end region having the sample inlet opening region (121), wherein an outer diameter of the cylindrical region (120) of the second pipe section (12) is smaller than an inner diameter of the cylindrical region (112) of the first pipe section (11), the spray chamber (10) comprises a double pipe section (100) formed by overlapping at least a part of the cylindrical region (112) of the first pipe section (11) and the cylindrical region (120) of the second pipe section (12),and an outer side surface of the double tube section (100) is provided with an additional gas inlet opening and an additional gas inlet tube section (101), which serves as an introduction channel for introducing an additional gas into the double tube section (100) through the additional gas inlet opening, characterized in that an angle formed between a central axis direction of the sample inlet opening area (121) and a central axis direction of the cylindrical area (112) of the first tube section (11) ranges from 10° to 60°. Spray chamber (10) according to claim 1, wherein an angle formed by a central axis direction of the additional gas inlet pipe section (101) and a central axis direction of the cylindrical area (112) of the first pipe section (11) ranges from 90° to 130°. Spray chamber (10) according to claim 1 or 2, wherein the additional gas inlet opening, using the center of the outer side surface of the double tube section (100) as a reference, is arranged at a position on the outer side surface of the double tube section (100) which is closer to the second tube section (12). Spray chamber (10) according to one of claims 1 to 3, wherein the length of the double tube section (100) ranges from 10.0 mm to 30.0 mm. Spray chamber (10) according to one of claims 1 to 4, wherein the difference between the inner diameter of the cylindrical section (112) of the first pipe section (11) and the outer diameter of the cylindrical section (120) of the second pipe section (12) ranges from 1.0 mm to 6.0 mm. Spray chamber (10) according to one of claims 1 to 5, wherein a ratio, length / maximum diameter, of a length of the conical section (111) of the first pipe section (11) to a maximum inner diameter of the conical section (111) ranges from 0.5 to 3.

0. Spray chamber (10) according to one of claims 1 to 6, wherein the total length of the spray chamber (10) ranges from 80.0 mm to 200.0 mm. Spray chamber (10) according to one of claims 1 to 7, wherein the first pipe section (11) and the second pipe section (12) are components which are made of glass, quartz or a fluorine resin. Spray chamber (10) according to one of claims 1 to 8, wherein the outer side surface of the double pipe section (100) is provided with a waste liquid opening and a waste liquid pipe section (113), which serves as a waste liquid channel for the discharge of waste liquid from an interior of the double pipe section (100) to an exterior of the double pipe section (100) through the waste liquid opening. Sample atomization and introduction device comprising a spray chamber (10) and a nebulizer, wherein the spray chamber (10) is the spray chamber according to any one of claims 1 to 9. Analysis device comprising the sample atomization and introduction device according to claim 10 and an analysis unit. Analysis device according to claim 11, wherein an angle formed by a horizontal direction of an arrangement surface on which the sample atomization and introduction device is arranged and a central axis direction of the cylindrical region (112) of the first pipe section (11) of the spray chamber (10) ranges from 20° to 90°. Analysis device according to claim 11 or 12, which is an analysis device with inductively coupled plasma and the analysis device comprises a plasma torch. Analysis device according to claim 13, which is a mass spectrometer device with inductively coupled plasma. Method for analyzing a component in a sample liquid, comprising: analysis of a component in a sample liquid to be analyzed using the analysis device according to one of claims 11 to 14, and further comprising: introducing an additional gas from the additional gas inlet pipe section (101) when a gas stream containing droplets of the sample liquid, which have been atomized by the nebulizer, flows through the flow passage pipe section (13) of the spray chamber (10).

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