Light scattering detector and its sample cell

By designing the sample cell of the light scattering detector, using a cylindrical inner section and a truncated conical outer section, combined with a lens and detector, the problem of insufficient sensitivity and resolution of conventional light scattering detectors in small molecule analysis is solved, achieving a highly efficient detection effect.

CN116337760BActive Publication Date: 2026-06-19TOSOH CORP

Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
TOSOH CORP
Filing Date
2019-01-02
Publication Date
2026-06-19

AI Technical Summary

Technical Problem

Conventional light scattering detectors have limited sensitivity and resolution in analyzing small molecules, and increasing laser power increases cost and footprint, while increasing sample cell volume leads to peak broadening.

Method used

A sample cell for a light scattering detector was designed, comprising a cylindrical inner section and a truncated conical outer section. By combining a lens and a detector, the beam path was optimized to improve sensitivity and resolution while reducing peak broadening.

🎯Benefits of technology

This improves the sensitivity and resolution of the light scattering detector for small molecules, while avoiding the cost and space issues associated with increasing laser power and sample cell volume.

✦ Generated by Eureka AI based on patent content.

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Abstract

A sample cell, a light scattering detector utilizing the sample cell, and a method for using the light scattering detector are provided. The sample cell may include a body defining a flow path extending axially through it. The flow path may include a cylindrical inner section interposed between a first outer section and a second outer section. The first outer section may be truncated conical. A first end portion of the first outer section may be in direct fluid communication with the inner section and may have a cross-sectional area relatively smaller than that at its second end portion. The body may also define an inlet in direct fluid communication with the inner section. The inlet may be configured to guide a sample into the inner section of the flow path.
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Description

Background Technology

[0001] Conventional light scattering detectors are typically used in conjunction with chromatographic techniques to determine one or more physical properties or characteristics of various molecules or solutes suspended in solution. For example, light scattering detectors are often used in conjunction with gel permeation chromatography (GPC) to determine the molecular weight and radius of gyration of various polymers. In a light scattering detector, a sample or effluent containing molecules (e.g., polymers) flows from an inlet through a sample cell to an outlet located at its opposite end. As the effluent flows through the sample cell, it is illuminated by a collimated light beam (e.g., a laser). The interaction of the light beam with the polymer in the effluent produces scattered light. The scattered light is then measured and analyzed for different properties (such as intensity and angle) to determine the physical properties of the polymer.

[0002] While conventional light scattering detectors have proven effective for determining the physical properties of a wide variety of molecules, they are limited in their ability to analyze small molecules. For example, conventional light scattering detectors typically lack the sensitivity and / or resolution to measure the Rg of molecules with a radius of gyration less than approximately 10 nm. Given the foregoing, conventional light scattering detectors often incorporate lasers with relatively high power or energy to increase detector sensitivity. However, incorporating high-power lasers is expensive and typically requires larger equipment due to the relatively large footprint of lasers. Alternatively, the volume of the sample cell in a conventional light scattering detector can be increased to increase the intensity of the scattered light. However, increasing the volume of a conventional sample cell leads to excessive peak broadening.

[0003] What is needed next is an improved light scattering detector and its sample cell, as well as methods for increasing the sensitivity and / or resolution of the light scattering detector without increasing peak broadening. Summary of the Invention

[0004] This overview is merely intended to provide a simplified overview of some aspects of one or more embodiments of this disclosure. Further areas of application of this disclosure will become apparent from the detailed description provided below. This overview is not a broad summary, nor is it intended to identify key or essential elements of this teaching, nor is it intended to depict the scope of this disclosure. Rather, its purpose is simply to present one or more concepts in a simplified form as a prelude to the detailed description that follows.

[0005] The foregoing and / or other aspects and utility implemented in this disclosure can be achieved by providing a sample cell for a light scattering detector. The sample cell may include a body defining a flow path extending axially therethrough. The flow path may include a cylindrical inner section interposed between a first outer section and a second outer section. The first outer section may be truncated conical, and a first end portion of the first outer section may be in direct fluid communication with the inner section and may have a cross-sectional area relatively smaller than that at its second end portion. The body may also define an inlet in direct fluid communication with the inner section and configured to guide a sample into the inner section of the flow path.

[0006] In at least one embodiment, the second outer section is truncated conical, and the first end portion of the second outer section is in direct fluid communication with the inner section and has a cross-sectional area that is relatively smaller than the cross-sectional area at its second end portion.

[0007] In at least one embodiment, the body further defines a first outlet and a second outlet extending therethrough, wherein the first outlet and the second outlet are configured to fluidly connect respective second end portions of the first outer section and the second outer section to the waste line.

[0008] In at least one embodiment, the body defines a first notch extending axially through it, the first notch being in fluid communication with a first outer segment and configured as a first lens to receive a light scattering detector.

[0009] In at least one embodiment, the body defines a second notch extending axially through it, the second notch being in fluid communication with a second outer segment and configured as a second lens to receive a light scattering detector.

[0010] In at least one embodiment, the body defines an orifice extending radially through it, wherein the orifice is in direct fluid communication with an internal section of the flow path.

[0011] In at least one embodiment, the sample cell further includes an optically transparent material disposed in the aperture.

[0012] The foregoing and / or other aspects and utility implemented in this disclosure can be achieved by providing a light scattering detector. The light scattering detector may include: a laser configured to emit a light beam; a sample cell including a body defining a flow path extending therethrough, the flow path having a centerline aligned with the light beam, the flow path including a cylindrical inner section interposed between a first outer section and a second outer section. The first outer section is truncated conical, and a first end portion of the first outer section is in direct fluid communication with the inner section and has a cross-sectional area relatively smaller than that at its second end portion. The body also defines an inlet in direct fluid communication with the inner section and configured to guide a sample into the inner section of the flow path. The light scattering detector may also include at least one detector operatively coupled to the sample cell and configured to receive scattered light emitted from the sample cell.

[0013] In at least one embodiment, the second outer section is truncated conical, and the first end portion of the second outer section is in direct fluid communication with the inner section and has a cross-sectional area that is relatively smaller than the cross-sectional area at its second end portion.

[0014] In at least one embodiment, the light scattering detector may include a first lens and a second lens, the first lens being configured to be adjacent to a first outer segment of the flow path, and the second lens being configured to be adjacent to a second outer segment of the flow path.

[0015] In at least one embodiment, the light scattering detector further includes a first mirror and a first detector, the first mirror being disposed near the first lens and configured to reflect forward-scattered light from the sample cell to the first detector.

[0016] In at least one embodiment, the light scattering detector may further include a second mirror and a second detector, the second mirror being disposed near the second lens and configured to reflect backscattered light from the sample cell to the second detector.

[0017] In at least one embodiment, the body defines an orifice extending radially through it, wherein the orifice is in direct fluid communication with an internal section of the flow path.

[0018] In at least one embodiment, the light scattering detector may further include a third detector disposed in the aperture and configured to receive right-angle scattered light from the sample cell.

[0019] In at least one embodiment, the body further defines a first outlet and a second outlet extending therethrough, wherein the first outlet and the second outlet are configured to fluidly connect respective second end portions of the first outer section and the second outer section to the waste line.

[0020] The foregoing and / or other aspects and utility implemented in this disclosure can be achieved by providing a method using any of the light scattering detectors disclosed herein. The method may include emitting a light beam from a laser into and through a flow path of a sample cell, flowing a sample through an inlet of the sample cell into an inner section of the flow path, flowing a first portion of the sample from the inner section into a first truncated conical outer section and from a first end portion through the first truncated conical outer section to a second end portion thereof, and flowing the first portion of the sample through a first outlet from the second end portion of the first truncated conical outer section to a waste line.

[0021] In at least one embodiment, the method may further include causing a second portion of the sample to flow from an inner section to a second truncated conical outer section and from a first end portion through the second truncated conical outer section to its second end portion, and causing the second portion of the sample to flow from the second end portion of the second truncated conical outer section to a waste line via a second outlet.

[0022] In at least one embodiment, the method may further include using a first mirror to guide forward-scattered light emitted from the flow path to a first detector.

[0023] In at least one embodiment, the method may further include using a second mirror to guide backscattered light emitted from the flow path to a second detector.

[0024] In at least one embodiment, the method may include guiding right-angle scattered light emitted from the flow path to a third detector.

[0025] Further areas of application of this disclosure will become apparent from the detailed description provided below. It should be understood that while the detailed description and specific examples indicate some typical aspects of this disclosure, they are intended for illustrative purposes only and not to limit the scope of this disclosure. Attached Figure Description

[0026] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of variations of this disclosure. These and / or other aspects and advantages of the embodiments of this disclosure will become apparent and more readily understood from the following description of various embodiments accompanied by the accompanying drawings. It should be noted that some details in the drawings have been simplified and drawn to facilitate understanding of this disclosure, rather than to maintain strict structural accuracy, detail, and scale. These drawings / figures are intended to be illustrative and not restrictive.

[0027] Figure 1A A schematic diagram of an exemplary light scattering detector including an exemplary sample cell, according to one or more disclosed embodiments, is shown.

[0028] Figure 1BThe illustration shows one or more embodiments according to the disclosure. Figure 1A A schematic diagram of an exemplary sample cell.

[0029] Figure 1C This illustrates a method according to one or more disclosed embodiments that does not have analyte-scattered light. Figure 1A A schematic diagram of an exemplary sample cell.

[0030] Figure 1D The illustration shows a method based on one or more disclosed embodiments, using... Figure 1C A magnified view of the sample cell portion indicated by the box labeled 1D. Detailed Implementation

[0031] The following description of various typical aspects is merely exemplary in nature and is in no way intended to limit this disclosure, its application or use.

[0032] As used throughout this disclosure, the range is used as a shorthand to describe each value within the range. It should be recognized and understood that the range format is merely for convenience and brevity and should not be construed as an inflexible limitation on the scope of any embodiment or implementation disclosed herein. Therefore, the disclosed range should be interpreted as specifically disclosing all possible subranges and the individual numerical values ​​within that range. In this regard, any value within the range may be chosen as the end point of the range. For example, a description of a range (e.g., from 1 to 5) should be considered as specifically disclosing subranges (e.g., from 1.5 to 3, from 1 to 4.5, from 2 to 5, from 3.1 to 5, etc.) and the individual numbers within that range (e.g., 1, 2, 3, 3.2, 4, 5, etc.). This applies regardless of the breadth of the range.

[0033] Furthermore, all numerical values ​​are indicated as "approximately" or "approximately," and take into account experimental errors and biases that would be expected by those skilled in the art. It should be understood that all numerical values ​​and ranges disclosed herein are approximate values ​​and ranges, whether or not the word "approximately" is used in conjunction with them. It should also be understood that, as used herein in conjunction with numbers, the term "approximately" means a value that may be ±0.01% (inclusive), ±0.1% (inclusive), ±0.5% (inclusive), ±1% (inclusive), ±2% (inclusive), ±3% (inclusive), ±5% (inclusive), ±10% (inclusive), or ±15% (inclusive) of that number. It should be further understood that when numerical ranges are disclosed herein, any numerical values ​​falling within those ranges are also specifically disclosed.

[0034] All references cited in this document are hereby incorporated herein by reference in their entirety. In the event of any conflict between the definitions in this disclosure and the definitions in the cited references, this disclosure shall prevail.

[0035] As used herein, the term "sensitivity" may refer to the signal-to-noise ratio. Those skilled in the art will recognize that increasing laser power does not necessarily improve sensitivity.

[0036] Figure 1A A schematic diagram of an exemplary light scattering detector (LSD) 100, including an exemplary sample cell 102, is shown according to one or more embodiments. The LSD 100 may be operatively coupled to a sample source or device 104 and is capable of or configured to receive samples or effluents therefrom. For example, as... Figure 1A As shown, LSD 100 may be fluidly coupled to a sample source or device 104 via line 106 and configured to receive effluent therefrom. The exemplary sample source or device 104 may include, but is not limited to, a chromatograph capable of or configured to separate one or more analytes of a sample or eluent from each other. For example, sample source or device 104 may be a liquid chromatograph capable of or configured to separate analytes of the eluent from each other based on their respective charges (e.g., ion exchange chromatography), sizes (e.g., size exclusion or gel permeation chromatography), etc. In an exemplary embodiment, LSD 100 is operatively coupled to a liquid chromatograph configured to separate analytes from each other based on their respective sizes. For example, LSD 100 is operatively coupled to a liquid chromatograph including a gel permeation column.

[0037] LSD 100 may include an exemplary sample cell 102, a collimated light source (such as laser 108) beam, and one or more detectors 110, 112, 114 (three shown) operatively coupled to each other. Detectors 110, 112, 114 may be any suitable detector capable of or configured to receive light scattered by the analyte. For example, any one or more of detectors 110, 112, 114 may be photodetectors, such as silicon photodetectors. LSD 100 may include one or more lenses 116, 118, 120, 122, 124 (five shown) and one or more mirrors 126, 128 (two shown), the lenses 116, 118, 120, 122, 124 capable of or configured to refract, focus, attenuate, and / or collect light transmitted through LSD 100, and the mirrors 126, 128 capable of or configured to reflect or redirect light transmitted through LSD 100.

[0038] In at least one embodiment, the first lens 116 and the second lens 118 may be disposed on opposite sides of the sample cell 102 and configured to refract, focus, attenuate, and / or collect light transmitted through it. In another embodiment, the body 130 of the sample cell 102 may define recesses 132, 134 configured to receive the first lens 116 and the second lens 118. For example, as Figure 1A As shown in and further in Figure 1B As shown in detail, the body 130 of the sample cell 102 may define a first notch 132 and a second notch 134, which extend longitudinally or axially through the body 130 and are configured to receive a first lens 116 and a second lens 118, respectively. Figure 1A and Figure 1B As shown, each of the first lens 116 and the second lens 118 may define a convex surface along its respective first or outer end portion 136, 138. Although the first end portions 136, 138 of the first lens 116 and the second lens 118 are shown defining convex surfaces, it should be understood that either of the respective first end portions 136, 138 of the first lens 116 and the second lens 118 may alternatively define a plane. Figure 1A As further shown herein, each of the first lens 116 and the second lens 118 may define a plane along its respective second or inner end portion 140, 142. As further described herein, the respective second end portions 140, 142 of the first lens 116 and the second lens 118 may seal and / or at least partially define a channel or flow path 144 extending through the sample cell 102.

[0039] Laser 108 can be any suitable laser capable of or configured to provide a beam 146 with sufficient wavelength and / or power. For example, laser 108 can be a diode laser, a solid-state laser, etc. Laser 108 can be configured to emit the beam 146 through sample cell 102. For example, as... Figure 1A As shown, laser 108 can be arranged or positioned around LSD 100 such that the beam 146 emitted from it is transmitted through sample cell 102. Figure 1A As further shown, a third lens 120 can be inserted between the sample cell 102 and the laser 108, and is configured to focus and guide the beam 146 to and through the sample cell 102.

[0040] In at least one embodiment, at least one of the mirrors 126, 128 may be associated with a corresponding detector 110, 112 and configured to reflect or redirect light (e.g., scattered light or analyte scattered light) toward the corresponding detector 110, 112. For example, as Figure 1AAs shown, a first mirror 126 may be disposed near the first lens 116 and configured to reflect at least a portion of the light from the first lens 116 toward the first detector 110. In another embodiment, a second mirror 128 may be disposed near the second lens 118 and / or interposed between the second lens 118 and the third lens 120, and configured to reflect at least a portion of the light from the second lens 118 toward the second detector 112. In at least one embodiment, one or more lenses 122, 124 may be interposed between the first mirror 126 and the second mirror 128 and the first detector 110 and the second detector 112 to focus, refract, or otherwise guide light from the mirrors 126, 128 to the detectors 110, 112. For example, as Figure 1A As shown, the fourth lens 122 can be inserted between the first detector 110 and the first mirror 126, and the fifth lens 124 can be inserted between the second detector 112 and the second mirror 128.

[0041] In at least one embodiment, at least one of the detectors 110, 112, 114 may be configured to receive light (e.g., scattered light or analyte scattered light) from the sample cell 102 without the aid or reflection of one of the mirrors 126, 128. For example, as Figure 1A and Figure 1B As shown, the third detector 114 may be positioned adjacent to or coupled to the sample cell 102 and configured to receive light (e.g., scattered light) from the sample cell 102 at an angle of approximately 90° relative to the beam 146. As further discussed herein, an optically transparent material or a sixth lens 186 may be configured to refract or guide the scattered light toward the third detector 114.

[0042] like Figure 1A As shown, at least one of the sample cell 102, the first lens 116, the second lens 118, and the third lens 120, as well as the first mirror 126 and the second mirror 128, can be arranged parallel to each other, coaxially, or otherwise aligned along the direction of the beam 146 emitted by the laser 108. Figure 1AAs further shown, each of the first detector 110 and the second detector 112 may be configured or positioned to receive light (e.g., scattered light or analyte scattered light) from the respective mirrors 126, 128 in a direction substantially perpendicular to the beam 146 emitted by the laser 108. Each of the first mirror 126 and the second mirror 128 may define a respective opening or path 150, 152 extending through it. For example, the first mirror 126 may define an opening 150 extending through it in a direction parallel, coaxial, or otherwise aligned with the beam 146. Similarly, the second mirror 128 may define an opening 152 extending through it in a direction parallel, coaxial, or otherwise aligned with the beam 146. It should be recognized that the openings 150, 152 extending through the respective mirrors 126, 128 allow the beam 146 emitted from the laser 108 to be transmitted through the first mirror 126 and the second mirror 128, thereby preventing the beam 146 from being reflected toward the first detector 110 and the second detector 112.

[0043] Figure 1D This illustrates a method based on one or more embodiments, using... Figure 1C The diagram shows an enlarged view of a portion of the exemplary LSD100 indicated by the 1D box. As previously discussed, the body 130 of the sample cell 102 may at least partially define a channel or flow path 144 extending through it. For example, as... Figure 1D As shown, the inner surface 154 of the body 130 may at least partially define a flow path 144 extending through it. The flow path 144 may define the volume of the sample cell 102. The flow path 144 may include a central axis or centerline 156 extending through it and configured to define the general orientation of the flow path 144. Figure 1B As shown, the flow path 144 and its central axis 156 can be aligned with or coaxial with the beam 146 emitted from the laser 108. The flow path 144 of the sample cell 102 can be inserted between the first lens 116 and the second lens 118. In at least one embodiment, the first lens 116 and the second lens 118 can be sealingly engaged with the body 130 of the sample cell 102 on opposite sides of the body 130, thereby preventing the flow of sample or effluent from the flow path 144 via the mating portion between the body 130 and the respective first lens 116 and second lens 118. In another embodiment, a seal (e.g., a gasket, O-ring, etc.) (not shown) can be provided between the body 130 and the first lens 116 and the second lens 118 to provide a fluid-proof seal between them.

[0044] The flow path 144 may include an internal segment 158 ​​and two external segments 160, 162 arranged along its centerline 156. For example... Figure 1DAs shown, the internal segment 158 ​​can be inserted between the two external segments 160, 162. The internal segment 158 ​​can be fluidly connected to the sample source 104 and configured to receive a sample or effluent from the sample source 104. For example, as continuing to refer to... Figure 1A of Figure 1D As shown, the body 130 of the sample cell 102 may define an inlet 164 that extends through the body 130 and is configured to fluidly connect the sample source 104 to the internal section 158 via a line 106. In a preferred embodiment, the inlet 164 is configured such that a sample from the sample source 104 is directed to the middle or center of the flow path 144 or its internal section 158.

[0045] In at least one embodiment, the inner segment 158 ​​may be cylindrical or define a cylindrical volume and may have a circular cross-sectional profile. However, it should be appreciated that the cross-sectional profile may be represented by any suitable shape and / or size. For example, the cross-sectional profile may be elliptical, rectangular (such as a rounded rectangle), etc. The inner segment 158 ​​may have any suitable dimensions. In at least one embodiment, the inner segment 158 ​​may have a length from about 4 mm to about 12 mm or greater, extending between the two outer segments 160, 162. For example, the inner segment 158 ​​may have a length from about 4 mm, about 5 mm, about 6 mm, about 7 mm, or about 7.5 mm to about 8.5 mm, about 9 mm, about 10 mm, about 11 mm, about 12 mm or greater. In another example, the inner segment 158 ​​may have a length from about 4 mm to about 12 mm, about 5 mm to about 11 mm, about 6 mm to about 10 mm, about 7 mm to about 9 mm, or about 7.5 mm to about 8.5 mm. In a preferred embodiment, the inner segment 158 ​​may have a length from about 7 mm to about 9 mm, preferably from about 7.5 mm to about 8.5 mm, more preferably about 8 mm. In at least one embodiment, the inner segment 158 ​​may have a diameter from about 1.2 mm to about 2.0 mm or greater. For example, the inner segment 158 ​​may have a diameter from about 1.2 mm, about 1.3 mm, about 1.4 mm, about 1.5 mm, or about 1.55 mm to about 1.65 mm, about 1.7 mm, about 1.8 mm, about 1.9 mm, about 2.0 mm or greater. In another example, the inner segment 158 ​​may have a diameter from about 1.2 mm to about 2.0 mm, about 1.3 mm to about 1.9 mm, about 1.4 mm to about 1.8 mm, about 1.5 mm to about 1.7 mm, or about 1.55 mm to about 1.65 mm. In a preferred embodiment, the inner section 158 may have a diameter of about 1.5 mm to about 1.7 mm, preferably about 1.55 mm to about 1.65 mm, and more preferably about 1.6 mm.

[0046] The outer sections 160, 162 of the flow path 144 may be fluidly connected to the inner section 158 and configured to receive samples or effluents therefrom. In at least one embodiment, at least one of the first outer section 160 and the second outer section 162 may be cylindrical or define a cylindrical volume and may have a circular cross-sectional profile. For example, at least one of the first outer section 160 and the second outer section 162 may be sized and shaped similar to... Figure 1DThe internal section 158. In another embodiment, at least one of the first outer section 160 and the second outer section 162 may be conical or truncated conical, such that the cross-sectional area at its respective first end portion or inlet 166, 168 may be relatively smaller than the cross-sectional area at its respective second end portion or outlet 170, 172. In a preferred embodiment, both the first outer section 160 and the second outer section 162 may be truncated conical or defined truncated cone, wherein the respective first end portion or inlet 166, 168 is configured to receive a sample from the internal section 158, while the respective second end portion or outlet 170, 172 is configured to convey a sample to the waste line 174 (see Figure 1A ).

[0047] The inner surface 154 of the body 130 may at least partially define the corresponding cone angles (θ1, θ2) of the first outer segment 160 and the second outer segment 162. For example, as Figure 1D As shown, a portion of the inner surface 154 of the first outer segment 160 defining or forming the flow path 144 and the centerline 156 of the flow path 144 may define a corresponding cone angle (θ1) for the first outer segment 160. In another example, a portion of the inner surface 154 of the second outer segment 162 defining or forming the flow path 144 and the centerline 156 of the flow path 144 may define a corresponding cone angle (θ2) for the second outer segment 162. The first outer segment 160 and the second outer segment 162 may have any cone angle (θ1, θ2), which is capable of or configured to allow the LSD 100 and its detectors 110, 112, 114 to receive scattered light at any desired angle. Although Figure 1D The cone angles (θ1, θ2) of the first outer segment 160 and the second outer segment 162 are shown as being relatively equal to each other; however, it should be understood that one of the cone angles (θ1, θ2) may be relatively larger than the other. It should also be understood that any one or more attributes (e.g., length, cone angle, diameter, shape, size, etc.) of the first outer segment 160 and the second outer segment 162 may be different. In a preferred embodiment, the attributes (e.g., length, cone angle, diameter, shape, size, etc.) of the first outer segment 160 and the second outer segment 162 are the same or substantially the same.

[0048] Each of the outer sections 160 and 162 can be fluidly connected to the waste line 174. For example, as... Figure 1A and Figure 1D As shown, body 130 may define a first outlet 176 and a second outlet 178, which extend through body 130 and are configured to fluidly connect the first outer section 160 and the second outer section 162 to waste line 174 via first outlet line 180 and second outlet line 182, respectively. Figure 1DAs further illustrated, the first outlet 176 and the second outlet 178 may be fluidly connected to the corresponding second end portions 170, 172 of the outer sections 160, 162. It should be understood that the orientation (e.g., circumferential orientation) or location of the inlet 164 and the first outlet 176 and the second outlet 178 may vary. For example, the inlet 164 may be circumferentially aligned with at least one of the first outlet 176 and the second outlet 178. In another example, the inlet 164 may be circumferentially offset from at least one of the first outlet 176 and the second outlet 178. In yet another example, the first outlet 176 and the second outlet 178 may be circumferentially aligned with each other or circumferentially offset from each other.

[0049] like Figure 1D As shown, the body 130 of the sample cell 102 may define an aperture 184 extending through at least a portion of the body 130 and configured to allow light (e.g., scattered light) from the inner segment 158 ​​to be directed or transmitted to the third detector 114. The aperture 184 may be sealed using an optically transparent material 186 (such as a quartz crystal) to thereby allow light from the inner segment 158 ​​to be directed to the third detector 114. Figure 1B and Figure 1D In the exemplary embodiment shown, the optically transparent material 186 may be shaped to refract a portion of the light toward the third detector 114. For example, the optically transparent material 186 may be a sixth lens (e.g., a spherical lens) configured to seal the aperture 184 and refract light toward the third detector 114 at least partially.

[0050] Body 130 may comprise or be made of any suitable material. Body 130 may be configured such that its inner surface 154 attenuates light reflection. For example, body 130 may be made of a non-reflective material. In another instance, body 130 may be at least partially made of a reflective material and at least partially coated with a non-reflective material. In at least one embodiment, sample cell 102 may be made of quartz (such as black quartz). In exemplary embodiments, body 130 may comprise or be made of a polymer. Exemplary polymers may be, or include, polyolefin-based polymers, acrylic-based polymers, polyurethane-based polymers, ether-based polymers, polyester-based polymers, polyamide-based polymers, formaldehyde-based polymers, silicon-based polymers, any copolymers thereof, or any combination thereof. For example, polymers may include, but are not limited to, poly(ether ether ketone) (PEEK), TORLON, etc. ®Polyamide-imide, polyethylene (PE), polyvinyl fluoride (PVF), polyvinyl chloride (PVC), polyvinylidene fluoride (PVDF), polyvinylidene chloride (PVDC), polyvinyl trifluoroethylene (PCTFE), polytetrafluoroethylene (PTFE), polypropylene (PP), poly(1-butene), poly(4-methylpentene), polystyrene, polyvinylpyridine, polybutadiene, polyisoprene, polychloroprene, styrene-acrylonitrile copolymer, acrylonitrile-butadiene-styrene terpolymer, ethylene-methacrylic acid copolymer Polymers, styrene-butadiene rubber, tetrafluoroethylene copolymers, polyacrylates, polymethacrylates, polyacrylamide, polyvinyl acetate, polyvinyl alcohol, polyvinyl butyral, polyvinyl ether, polyvinylpyrrolidone, polyvinylcarbazole, polyurethane, polyacetal, polyethylene glycol, polypropylene glycol, epoxy resins, polyphenylene ether, polyethylene terephthalate, polybutylene terephthalate, polydimethylolcyclohexyl terephthalate, cellulose esters, polycarbonate, polyamides, polyimides, any copolymers thereof, or any combination thereof. The polymer may be, or is not limited to, elastomers or elastomeric materials, synthetic rubbers, etc. Exemplary elastomers and synthetic rubbers may include, but are not limited to, VITON. ® Nitriles, polybutadiene, acrylonitrile, polyisoprene, chloroprene rubber, butyl rubber, chloroprene, polysiloxane, styrene-butadiene rubber, alcohol rubber, silicone rubber, ethylene-propylene-diene terpolymer, any copolymer thereof, or any combination thereof.

[0051] In the exemplary operation of LSD100, continue to refer to Figure 1A-1D Sample source 104 (e.g., a liquid chromatograph including a gel permeation column) can inject or direct a sample or effluent (e.g., a diluted polymer solution) into and through the flow path 144 of sample cell 102 via line 106 and inlet 164. Figure 1D As shown, the sample from sample source 104 can be directed toward the center or middle of the flow path 144 or inner section 158 of sample cell 102. As the sample flows to the center of inner section 158, the sample flow can split such that a first portion of the sample flows toward a first outer section 160, while a second portion flows toward a second outer section 162. Portions of the sample in the first outer section 160 and the second outer section 162 can then be directed from sample cell 102 and toward waste line 174 via first outlet 176 and second outlet 178, and first outlet line 180 and second outlet line 182, respectively.

[0052] The flow rate of the sample through the first outer section 160 and the second outer section 162 can be modified or adjusted (i.e., increased or decreased) by adjusting the corresponding lengths of the first outlet line 180 and the second outlet line 182. In at least one embodiment, the flow rates of the first portion and the second portion of the sample through the first outer section 160 and the second outer section 162 may be the same or substantially the same. For example, the flow rate of the first portion of the sample through the first outer section 160 may be the same or substantially the same as the flow rate of the second portion of the sample through the second outer section 162. In another embodiment, the flow rates of the first portion and the second portion of the sample through the first outer section 160 and the second outer section 162 may be different. However, it should be recognized that if the flow rates through the first outer section 160 and the second outer section 162 are different, time correction may be applied.

[0053] As the sample flows through the flow path 144 of the sample cell 102, the laser 108 can emit a beam 146 along and through the centerline 156 of the flow path 144 via the opening 152 of the second mirror 128. Figure 1A In at least one embodiment shown, the beam 146 can be transmitted through the third lens 120, which allows the beam 146 to be at least partially focused along the centerline 156 of the flow path 144. In another embodiment, the third lens 120 may be omitted. In at least one embodiment, an optional grid or aperture 188 may be disposed between the laser 108 and the sample cell 102 and configured to “clear”, isolate, or otherwise filter stray light (e.g., light halo) from the beam 146. For example, the aperture 188 may define an aperture or orifice (e.g., an adjustable aperture / aperture) that is capable of or configured to filter stray light from the beam 146.

[0054] At least a portion of the beam 146 may travel from or be transmitted from the laser 108 to and through the sample cell 102, the opening 152 of the first lens 116, the second mirror 128, and / or the optional aperture 196. For example, at least a portion of the beam 146 may be transmitted from the laser 108 to and through the sample cell 102, the opening 152 of the first lens 116, the second mirror 128, and / or the optional aperture 188 without obstruction or interaction with any of the analytes in the sample. The remaining portion of the beam 146 transmitted through the flow path 144 may interact with or otherwise contact the analytes, which are suspended, dispersed, or otherwise disposed in the sample and / or flow through the sample cell 102.

[0055] Contact between beam 146 and the analyte in the sample can generate or cause scattered light or analyte scattered beams 190, 192, 194 (see...) Figure 1A and Figure 1BFor example, contact between the beam 146 and the analyte contained in or flowing through the sample cell 102 via the flow path 144 can generate a forward analyte-scattered beam 190 and a backward analyte-scattered beam 192. In another example, contact between the beam 146 and the analyte contained in or flowing through the sample cell 102 via the flow path 144 can generate right-angle scattered light 194 in a direction generally perpendicular to the beam 146.

[0056] It should be recognized that the flow of the sample through inlet 164 to the center of flow path 144 allows the sample to interact immediately with beam 146, thereby minimizing peak broadening. For example, allowing the sample to flow directly to the center of flow path 144 allows the sample to interact with beam 146 without flow across at least half the length or volume of sample cell 102 and its flow path 144 (e.g., in a lateral or axial direction). Allowing the sample to flow directly to the center of flow path 144 also minimizes the amount of time required for the sample to interact with beam 146 and generate analyte scattered beams 190, 192, 194. It should also be recognized that one or more components of LSD 100 are configured such that light scattered only from the center of flow path 144 is collected by detectors 110, 112, 114. For example, at least one of the first lens 116, the first mirror, and the fourth lens 122 may be configured to isolate forward-scattered light 190 originating from the center of the flow path 144 from forward-scattered light 190 originating from other regions of the flow path 144, such that the first detector 110 receives only the forward-scattered light 190 originating from the center of the flow path 144. Similarly, at least one of the second lens 116, the second mirror 128, and the fifth lens 124 may be configured to isolate backscattered light 192 originating from the center of the flow path 144 from backscattered light 192 originating from other regions of the flow path 144, such that the second detector 112 receives only the backscattered light 192 originating from the center of the flow path 144.

[0057] like Figure 1A As shown, the forward-scattered beam or forward-scattered light 190 can be guided toward the first detector 110 via a first lens 116, a first mirror 126, and a fourth lens 122. At least a portion of the forward-scattered light 190 can be at least partially refracted by a convex surface defined along a first end portion 136 of the first lens 116. Figure 1A As shown, forward-scattered light 190 can be refracted towards the first mirror 126 by the convex surface, and the first mirror 126 can reflect the forward-scattered light 190 towards the first detector 110 via the fourth lens 122. The fourth lens 122 can collect the forward-scattered light 190 and guide and / or focus the forward-scattered light 190 towards the first detector 110.

[0058] Relative to the beam 146 emitted from laser 108, forward-scattered light 190 can be scattered at angles ranging from greater than 0° to less than 90°. For example, forward-scattered light 190 can be scattered at any angle from greater than 0°, approximately 5°, approximately 10°, approximately 15°, approximately 20°, approximately 25°, approximately 30°, approximately 35°, approximately 40°, or approximately 45° to approximately 50°, approximately 55°, approximately 60°, approximately 65°, approximately 70°, approximately 75°, approximately 80°, approximately 85°, or less than 90°. In another example, relative to the beam 146 emitted from laser 108, forward-scattered light 190 can be scattered at any angle from approximately 5°, approximately 6°, approximately 7°, approximately 8°, approximately 9°, or approximately 9.5° to approximately 10.5°, approximately 11°, approximately 12°, approximately 13°, approximately 14°, or approximately 15°. In yet another example, the forward-scattered light 190 can be scattered at angles ranging from approximately 5° to approximately 15°, approximately 6° to approximately 14°, approximately 7° to approximately 13°, approximately 8° to approximately 12°, approximately 9° to approximately 11°, or approximately 9.5° to approximately 10.5°. It should be understood that the LSD 100 and any of its components can be configured to receive the forward-scattered light 190 scattered at any angle greater than 0° and less than 90°. For example, any one or more properties (e.g., shape, location, orientation, etc.) of the first detector 110, first lens 116, first mirror 126, fourth lens 122, and / or any additional optional aperture can be adjusted, modified, or otherwise configured such that the first detector 110 can receive any of the forward-scattered light 190. In a preferred embodiment, the LSD100 and its first detector 110 are configured to receive or collect forward-scattered light 190 at an angle of about 9° to about 11°, preferably about 9.5° to about 10.5°, and more preferably about 10°, relative to the beam 146.

[0059] like Figure 1A As shown, the backscattered beam or backscattered light 192 can be guided toward the second detector 112 via the second lens 118, the second mirror 128, and the fifth lens 124. At least a portion of the backscattered light 192 can be at least partially refracted by the convex surface of the second lens 118. Figure 1A As shown, the backscattered light 192 can be refracted towards the second mirror 128 by the convex surface, and the second mirror 128 can reflect the backscattered light 192 towards the second detector 112 via the fifth lens 124. The fifth lens 124 can collect the backscattered light 192 and guide and / or focus the backscattered light 192 towards the second detector 112.

[0060] Relative to the beam 146 emitted from laser 108, backscattered light 192 can be scattered at varying angles from greater than 90° to less than 180°. For example, backscattered light 192 can be scattered at any angle from greater than 90°, approximately 95°, approximately 100°, approximately 105°, approximately 110°, approximately 115°, approximately 120°, approximately 125°, approximately 130°, or approximately 135° to approximately 140°, approximately 145°, approximately 150°, approximately 155°, approximately 160°, approximately 165°, approximately 170°, approximately 175°, or less than 180°. In another example, the backscattered light 192, relative to the beam 146 emitted from the laser 108, can be scattered at any angle from approximately 165°, approximately 166°, approximately 167°, approximately 168°, approximately 169°, or approximately 169.5° to approximately 170.5°, approximately 171°, approximately 172°, approximately 173°, approximately 174°, or approximately 175°. In yet another example, the backscattered light 192 can be scattered at an angle from approximately 165° to approximately 175°, approximately 166° to approximately 174°, approximately 167° to approximately 173°, approximately 168° to approximately 172°, approximately 169° to approximately 171°, or approximately 169.5° to approximately 170.5°. It should be appreciated that the LSD 100 and any of its components can be configured to receive the backscattered light 192 scattered at any angle greater than 90° and less than 180°. For example, any one or more properties (e.g., shape, location, orientation, etc.) of the second detector 112, second lens 118, second mirror 128, fifth lens 124, and / or any additional optional apertures may be adjustable, modified, or otherwise configured such that the second detector 112 may receive any of the backscattered light 192. In a preferred embodiment, the LSD 100 and its second detector 112 are configured to receive or collect the backscattered light 192 at an angle of approximately 169° to approximately 171°, preferably approximately 169.5° to approximately 170.5°, and more preferably approximately 170°, relative to the beam 146.

[0061] like Figure 1D As shown, a right-angle analyte scattered beam or right-angle scattered light 194 can be guided toward a third detector 114 via an aperture 184 extending between the third detector 114 and an inner section 158 of the flow path 144. In at least one embodiment, the third detector 114 may be disposed in the aperture 184 adjacent to the inner section 158. Figure 1DIn another embodiment shown, an optically transparent material 186 may be disposed in the aperture 184 to seal the internal section 158 of the flow path 144. The optically transparent material 186 may be any suitable material capable of allowing right-angled scattered light 194 to be transmitted to the third detector 114. The optically transparent material 186 may be shaped to refract at least a portion of the right-angled scattered light 194 toward the third detector 114. For example, as previously discussed, the optically transparent material 186 may be a spherical lens shaped to refract the right-angled scattered light 194 toward the third detector 114.

[0062] The right-angle scattered light 194 can be scattered in a direction substantially perpendicular to the beam 146. For example, the right-angle scattered light 194 can be scattered at angles ranging from approximately 87°, approximately 88°, approximately 89°, approximately 89.5°, or approximately 90° to approximately 90.5°, approximately 91°, approximately 92°, or approximately 93°. In another example, the right-angle scattered light 194 can be scattered at angles ranging from approximately 87° to approximately 93°, approximately 88° to approximately 92°, approximately 89° to approximately 91°, or approximately 89.5° to approximately 90.5°. It should be appreciated that the LSD 100 and any of its components can be configured to receive the right-angle scattered light 194 scattered in a direction substantially perpendicular to the beam 146. For example, the shape, location, orientation, or any other property of the optically transparent material 186 (e.g., a sixth lens) and / or the third detector 114 may be adjusted, modified, or otherwise configured such that the third detector 114 can receive any of the right-angled scattered light 194. In a preferred embodiment, the LSD 100 and its third detector 114 are configured to receive or collect the right-angled scattered light 194 at an angle of approximately 89° to approximately 91°, preferably approximately 89.5° to approximately 90.5°, and more preferably approximately 90°, relative to the beam 146.

Claims

1. A sample cell for a light scattering detector, comprising: A body defining a flow path extending through it, the flow path including a cylindrical inner section inserted between a first outer section and a second outer section; An inlet extends from the outer surface of the body through the body to the inner section, and the inlet is configured to guide fluid toward the center of the inner section. Wherein, the first outer section is truncated conical, wherein the first end portion of the first outer section is in direct fluid communication with the inner section and has a cross-sectional area relatively smaller than that at its second end portion, and The second outer section is truncated conical, wherein the first end portion of the second outer section is in direct fluid communication with the inner section and has a cross-sectional area that is relatively smaller than the cross-sectional area at its second end portion.

2. The sample cell according to claim 1, wherein, The body also defines a first outlet and a second outlet extending through it, wherein the first outlet and the second outlet are configured to fluidly connect respective second end portions of the first outer section and the second outer section to the waste line.

3. The sample cell according to claim 1, wherein, The body defines a first notch extending axially through it, the first notch being in fluid communication with the first outer section and configured to receive a first lens of the light scattering detector.

4. The sample cell according to claim 3, wherein, The body defines a second notch extending axially through it, the second notch being in fluid communication with the second outer segment and configured to receive a second lens from the light scattering detector.

5. The sample cell according to claim 1, wherein, The body defines an orifice extending radially through it, wherein the orifice is in direct fluid communication with the internal section of the flow path.

6. The sample cell according to claim 5, wherein, The sample cell also includes an optically transparent material disposed in the orifice.

7. A light scattering detector, comprising: A laser, which is configured to emit a beam of light; The sample cell according to claim 1, wherein the flow path of the sample cell has a centerline aligned with the beam of the laser; as well as At least one detector is operatively coupled to the sample cell and configured to receive scattered light emitted from the sample cell.

8. A method of operating the light scattering detector according to claim 7, comprising: The light beam is emitted from the laser into the flow path of the sample cell and passes through the flow path of the sample cell; The sample flows through the inlet of the sample cell to the inner section of the flow path; The first portion of the sample is allowed to flow from the inner section to the first outer section and through the first outer section; The first portion of the sample is allowed to flow from the first external section to the waste line via the first outlet of the sample cell.

9. The method according to claim 8, wherein, The method further includes: The second portion of the sample flows from the inner section to the second outer section and through the second outer section; and The second portion of the sample is allowed to flow from the second outer section to the waste line via the second outlet of the sample cell.

10. The method according to claim 8, wherein, The method further includes guiding forward-scattered light emitted from the flow path to a first detector.

11. The method according to claim 10, wherein, The method further includes guiding the backscattered light emitted from the flow path to a second detector.

12. The method according to claim 11, wherein, The method further includes guiding right-angle scattered light emitted from the flow path to a third detector.

13. A sample cell for a light scattering detector, comprising: A body defining a flow path extending through it, the flow path including a cylindrical inner section inserted between a first outer section and a second outer section; An inlet extends from the outer surface of the body through the body to the inner section, and the inlet is configured to guide fluid toward the center of the inner section; A first notch extends axially from the outer surface through the body to the first outer section; A first lens, wherein the first lens is disposed in the first recess; A second notch extends axially from the outer surface through the body to the second outer section; The second lens is disposed in the second recess; as well as An opening that extends radially from the outer surface through the body to the inner section; An optically transparent material is disposed in the aperture. The first outer section is truncated conical in shape. Wherein, the first end portion of the first outer section is in direct fluid communication with the inner section and has a cross-sectional area relatively smaller than that at its second end portion; and The second outer section is truncated conical, wherein the first end portion of the second outer section is in direct fluid communication with the inner section and has a cross-sectional area that is relatively smaller than the cross-sectional area at its second end portion.

14. The sample cell according to claim 13, wherein, The body also defines a first outlet extending through it, the first outlet being configured to fluidly connect a second end portion of the first outer section to a waste line.

15. The sample cell according to claim 14, wherein, The body also defines a second outlet extending through it, the second outlet being configured to fluidly connect a second end portion of the second outer section to a waste line.

Citation Information

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