阅读说明：本技术 送液装置以及液相色谱仪 (Liquid feeding device and liquid chromatograph ) 是由 山口忠行 浅川直树 佐藤友纪 福泽兴祐 村越干昭 于 2017-07-04 设计创作，主要内容包括：送液装置包括：送液泵,经由端部浸渍于收容作为液体的流动相的流动相容器的所述流动相的抽吸用配管,从所述流动相容器中抽吸所述流动相并输送；以及至少一个溶解物质除去过滤器,设于所述流动相的流动路径上的比所述送液泵更靠上游的位置,且填充有填充剂,所述填充剂具有吸附所述流动相中的溶解物质的性质。(The liquid feeding device comprises: a liquid feeding pump that sucks and feeds a mobile phase from a mobile phase container, which contains the mobile phase as a liquid, through a pipe for sucking the mobile phase, the pipe having an end immersed in the mobile phase container; and at least one dissolved substance removal filter which is provided upstream of the liquid sending pump on the flow path of the mobile phase and is filled with a filler having a property of adsorbing the dissolved substance in the mobile phase.)

1. A liquid feeding apparatus comprising:

a liquid feeding pump that sucks and feeds a mobile phase from a mobile phase container, which contains the mobile phase as a liquid, through a pipe for sucking the mobile phase, the pipe having an end immersed in the mobile phase container; and

and at least one dissolved substance removal filter which is provided upstream of the liquid sending pump on the flow path of the mobile phase and is filled with a filler having a property of adsorbing the dissolved substance in the mobile phase.

2. The liquid feeding apparatus according to claim 1, wherein the dissolved substance removing filter includes a dissolved substance removing filter in which the filler is filled in a suction filter provided at the end of the suction pipe.

3. The liquid feeding apparatus according to claim 1 or 2, wherein a plurality of the dissolved substance removal filters are provided in series along a flow path of the mobile phase.

4. The liquid feeding apparatus according to claim 3, wherein the plurality of dissolved substance removal filters are dissolved substance removal filters filled with a filler having a property of adsorbing dissolved substances different from each other.

5. The liquid conveying apparatus according to any one of claims 1 to 4, wherein the filler is any one of activated carbon, silica gel, a polymer, silica gel whose surface is modified with a functional group, or a polymer whose surface is modified with a functional group.

6. A liquid chromatograph comprising:

analyzing the flow path;

the liquid feeding apparatus according to any one of claims 1 to 5, wherein a mobile phase is fed in the analysis flow path;

a sample injection unit configured to inject a sample into the analysis channel;

an analysis column provided downstream of the sample injection section in the analysis channel and configured to separate a sample injected into the analysis channel by the sample injection section for each component; and

and a detector provided downstream of the analytical column in the analytical flow path, for detecting the sample component separated by the analytical column.

Technical Field

The present invention relates to a liquid feeding device for feeding a mobile phase as a liquid, and a liquid chromatograph (liquid chromatograph) using the liquid feeding device.

Background

An analysis device such as a liquid chromatograph is provided with a liquid feeder that feeds a liquid as a mobile phase. The liquid feeding device immerses an end of a suction pipe in the mobile phase contained in the mobile phase container, and sucks and feeds the mobile phase by a liquid feeding pump through the suction pipe.

A filter called a suction filter (see patent document 1) is generally attached to an end of a pipe for sucking the mobile phase immersed in the mobile phase container. By providing a suction filter at an end of the suction pipe, it is possible to remove solid substances in the mobile phase while sucking the mobile phase from the mobile phase container.

[ Prior art documents ]

[ patent document ]

Patent document 1: japanese patent laid-open No. 2006-038738

Disclosure of Invention

[ problems to be solved by the invention ]

A liquid used as a mobile phase in an analysis apparatus such as a liquid chromatograph may be contaminated in all places such as the use environment of the apparatus (a laboratory, a pretreatment substance, and the like), an ultrapure water purification apparatus, and a mobile phase container. For example, carbon dioxide in the intake air dissolves in the liquid contained in the mobile phase container, or the residue of a cleaning agent for cleaning the mobile phase container dissolves in the liquid that becomes the mobile phase, and the mobile phase is contaminated.

In recent years, liquid chromatography is typified by mass spectrometry and has improved detector sensitivity, and compounds at lower concentrations can be analyzed. However, in the high sensitivity analysis, even if the mobile phase is slightly contaminated as described above, substances other than the analysis target substance dissolved in the mobile phase may be detected by the detector, which may hinder the analysis. Further, the mobile phase, which is only slightly contaminated, enters the analysis system, and a contaminant may adhere to the inside of the pipe or the column to contaminate the analysis system itself, which may cause a reduction in detection sensitivity.

However, conventionally used suction filters cannot remove contaminants dissolved in a mobile phase. On the other hand, if a member for removing such contaminants is provided in the analysis system, the dead volume (dead volume) may become large and the separation capacity may be reduced. In particular, when gradient analysis (gradient analysis) is performed in which a sample is separated and analyzed while changing the composition of a mobile phase in a liquid chromatograph, if the internal capacity in the system downstream of a liquid sending pump is large, the change in the composition of the mobile phase is also slowed down by that amount, and the analysis efficiency is lowered.

Therefore, an object of the present invention is to remove contaminants dissolved in a mobile phase without increasing the dead volume in the system.

[ means for solving problems ]

The liquid feeding device of the present invention includes: a liquid feeding pump that sucks and feeds a mobile phase from a mobile phase container, which contains the mobile phase as a liquid, through a pipe for sucking the mobile phase, the pipe having an end immersed in the mobile phase container; and at least one dissolved substance removal filter which is provided upstream of the liquid sending pump on the flow path of the mobile phase and is filled with a filler having a property of adsorbing the dissolved substance in the mobile phase.

In the liquid feeding device according to the present invention, it is preferable that the dissolved substance removing filter includes a dissolved substance removing filter in which the filler is filled in a suction filter provided at the end of the suction pipe. In general, since a suction filter is provided at an end of a pipe for sucking the mobile phase immersed in the mobile phase container, an increase in the internal capacity of the system between the mobile phase container and the liquid sending pump can be suppressed by filling the filler in the suction filter to form a dissolved substance removing filter.

In addition, there may be a case where the contaminant dissolved in the mobile phase cannot be completely removed by only one dissolved substance removal filter. In this case, the plurality of dissolved substance removal filters may be provided in series along the flow path of the mobile phase.

In this case, the plurality of dissolved substance removing filters provided in series are preferably dissolved substance removing filters filled with a filler having a property of adsorbing dissolved substances different from each other. In this way, even when a plurality of contaminants are dissolved in the mobile phase, these contaminants can be removed from the mobile phase.

The filler to be filled in the dissolved substance removing filter includes: activated carbon, silica gel, polymers, silica gel with a surface modified with functional groups, polymers with a surface modified with functional groups, and the like.

The liquid chromatograph of the present invention comprises: analyzing the flow path; the liquid feeding device described above that feeds a mobile phase in the analysis flow path; a sample injection unit configured to inject a sample into the analysis channel; an analysis column provided downstream of the sample injection section in the analysis channel and configured to separate a sample injected into the analysis channel by the sample injection section for each component; and a detector provided downstream of the analytical column in the analytical flow path, for detecting the sample component separated by the analytical column.

[ Effect of the invention ]

The liquid feeding device of the present invention includes at least one dissolved substance removal filter filled with a filler having a property of adsorbing dissolved substances in a mobile phase, and therefore can remove contaminants dissolved in the mobile phase. Further, the dissolved substance removing filter does not increase the system volume of the analyzer on the downstream side of the liquid feeding pump even at the upstream side of the liquid feeding pump in the flow path of the mobile phase.

The liquid chromatograph of the present invention is provided with the liquid feeding device, and therefore, the detection of substances other than the substance to be analyzed in the highly sensitive analysis is suppressed by removing the contaminating substance in the mobile phase. In addition, the mobile phase from which the contaminant is removed flows in the analysis flow path, and therefore contamination in the analysis system is prevented.

Drawings

Fig. 1 is a flow path configuration diagram schematically showing an embodiment of a liquid chromatograph.

FIG. 2 is a sectional view showing an example of the dissolved substance removing filter of the liquid feeding apparatus according to the embodiment.

Fig. 3 is a sectional view showing another example of the dissolved substance removing filter.

Fig. 4 is a cross-sectional view showing another example of the dissolved substance removal filter.

Detailed Description

Hereinafter, an embodiment of the present invention will be described with reference to the drawings.

First, an embodiment of a liquid chromatograph will be described with reference to fig. 1.

The liquid chromatograph of the present embodiment includes a liquid feeding device 1 for feeding a mobile phase. The liquid feeding device 1 is configured to suck a mobile phase solvent (hereinafter referred to as a mobile phase) as a liquid from a mobile phase container 8a and a mobile phase container 8b by two liquid feeding pumps 2a and 2b, respectively, mix the mobile phases in a mixer 10, and feed the mixed mobile phases to an analysis channel 12. The analysis channel 12 is provided with a sample injection unit 14, an analysis column 16, and a detector 18 from the upstream side.

The sample injection unit 14 is, for example, an autosampler (autosampler) that collects a sample to be analyzed from a sample container using a needle (needle) and injects the collected sample into the analysis channel 12. The analytical column 16 is used for separating the sample injected into the analytical flow path 12 by the sample injection section 14 for each component. The separated sample components in the analytical column 16 are detected by a detector 18.

The liquid- sending pumps 2a and 2b of the liquid-sending device 1 suck the mobile phase from the sample solutions 8a and 8b via the suction pipes 4a and 4 b. A dissolved substance removing filter 6a and a dissolved substance removing filter 6b for removing contaminants dissolved in the mobile phase are provided upstream of the liquid-sending pumps 2a and 2b on the flow path of the mobile phase drawn by the liquid-sending pumps 2a and 2 b. In the present embodiment, the dissolved substance removing filter 6a and the dissolved substance removing filter 6b are provided at the ends of the suction pipe 4a and the suction pipe 4b, but the dissolved substance removing filter 6a and the dissolved substance removing filter 6b may be provided at any positions as long as they are upstream of the liquid-sending pumps 2a and 2 b.

The structure of the dissolved substance removal filter 6a and the dissolved substance removal filter 6b will be described with reference to fig. 2. Since the dissolved substance removal filter 6a and the dissolved substance removal filter 6b have the same structure, only the dissolved substance removal filter 6a will be described here.

The dissolved substance removal filter 6a includes a cylindrical (for example, cylindrical) main body 20 having a bottom surface and an opening at the upper side, and a lid portion 22 attached to the upper portion of the main body 20. The main body 20 is made of a porous material such as ceramic, and functions as a filter that allows liquid to pass therethrough and prevents solid contaminants such as dust and dirt in the liquid from passing therethrough. The cap portion 22 may contain a resin material such as Polytetrafluoroethylene (hereinafter referred to as PTFE), for example, but any material may be used as long as it is a material that is not reactive to the mobile phase.

The internal space of the body 20 is filled with a filler 28. The filler 28 has a property of adsorbing the contaminant dissolved in the mobile phase. Examples of the filler 28 include: activated carbon, silica gel, polymers, silica gel with a surface modified with functional groups, polymers with a surface modified with functional groups, and the like. When the contaminant dissolved in the mobile phase is a hydrophobic compound, the contaminant can be removed by using activated carbon as the filler 28. When the contaminant dissolved in the mobile phase is a surfactant from the air or a detergent, the contaminant can be removed by using activated carbon as the filler 28. When the contaminant dissolved in the mobile phase is an anionic surfactant, the contaminant can be removed by using the ion exchange substrate as the filler 28.

An annular projection 24 is provided on the lower surface of the lid 22. The projection 24 is fitted into the upper surface opening of the main body 20, and the lid 22 is attached to the upper portion of the main body 20 by fitting the projection 24 into the upper surface opening of the main body 20. A filter 30 made of, for example, stainless steel is provided inside the annular projection 24. The filter 30 is used to prevent the filler 28 filled in the body portion 20 from flowing out. A connection hole 26 for inserting and connecting the suction pipe 4a is provided in the upper surface of the lid portion 22, and the connection hole 26 is opened to the internal space of the main body portion 20 through a filter 30.

The dissolved substance removal filter 6a is used by immersing the mobile phase in the mobile phase container 8a, and functions as a suction filter, that is: the body section 20 containing the porous material removes solid contaminants from the mobile phase while pumping the mobile phase. That is, when the liquid sending pump 2a is driven in a state where the dissolved substance removing filter 6a is immersed in the mobile phase, the mobile phase is sucked from the main body 20 functioning as a suction filter while removing solid contaminants, and further contaminants dissolved in the mobile phase are removed by the filler filled in the main body 20. Thereby, the mobile phase in which both the solid contaminant and the soluble contaminant are removed is supplied to the analysis flow path 12 of the liquid chromatograph.

However, when the contaminants dissolved in the mobile phase container 8a cannot be completely removed by only one kind of filler, as shown in fig. 3, a dissolved substance removing filter 6a' may be provided in addition to the dissolved substance removing filter 6 a. In this case, the dissolved substance removal filter 6a and the dissolved substance removal filter 6a 'are connected in series, and the mobile phase is passed through the dissolved substance removal filter 6a and the dissolved substance removal filter 6a' in this order. When the contaminants dissolved in the mobile phase container 8b cannot be completely removed only by the dissolved substance removal filter 6b, the dissolved substance removal filter 6b' can be provided in the same manner as in fig. 3.

The structure of the dissolved substance removing filter 6a' shown in fig. 3 will be described.

The dissolved substance removal filter 6a' includes a cylindrical (for example, cylindrical) main body 32 having an opening at the upper part thereof, and a lid 36 attached to the upper part of the main body 32. A connection hole 34 is provided in the bottom surface of the main body 32, and the connection hole 34 is used to insert and connect an end of the suction pipe 4a' for connection with the dissolved substance removing filter 6 a. The body portion 32 and the lid portion 36 may each include a resin material such as PTFE, but any material may be used as long as it is a material that is not reactive to the mobile phase.

A filter 43 is disposed at the bottom of the internal space of the main body 32, and a filler 42 is filled above the filter 43. The filter 43 is for preventing the filler 42 from flowing out. The filler 42 has the following properties: the contaminant dissolved in the mobile phase is adsorbed, and a different contaminant is adsorbed from the filler 28 of the dissolved substance removing filter 6 a. Examples of the filler 42 include activated carbon, silica gel, polymer, silica gel whose surface is modified with a functional group, polymer whose surface is modified with a functional group, and the like.

An annular projection 38 is provided on the lower surface of the cover 36. The projection 38 is fitted into the upper surface opening of the main body 32, and the lid 36 is attached to the upper portion of the main body 32 by fitting the projection 38 into the upper surface opening of the main body 32. A filter 44 made of, for example, stainless steel is provided inside the annular projection 38. The filter 44 serves to prevent the filler 42 from flowing out. A connection hole 40 for inserting and connecting the suction pipe 4a is provided in the upper surface of the lid portion 36, and the connection hole 40 is opened to the internal space of the body portion 32 via a filter 44.

In the example of fig. 3, two dissolved substance removal filters 6a and 6a' are connected in series, but more dissolved substance removal filters may be connected in series.

In the above-described embodiment, the dissolved substance removing filter 6a is used as a premise, and the dissolved substance removing filter 6a also functions as a suction filter for removing solid contaminants in the mobile phase, but the present invention is not limited to this. As shown in fig. 4, the solid contaminants in the mobile phase may be removed by using a conventionally used suction filter 46, and the contaminants dissolved in the mobile phase may be removed by a dissolved substance removing filter 6a' connected in series to the suction filter 46. Further, the suction filter 46 of fig. 4 includes: a cylindrical main body 48 made of a porous material, and a lid 50 attached to the upper part of the main body.

In the above-described embodiment, the liquid chromatograph has been described as an example of the analysis device provided with the liquid feeding device 1, but the liquid feeding device of the present invention provided with the dissolved substance removing filter can be applied to any device as long as it is a device having a configuration in which the mobile phase in the mobile phase container is sucked and transported. Examples of such an apparatus include a separation and purification apparatus, an elution tester, and an apparatus for performing filtration and cleaning of a solvent or the like.

[ description of symbols ]

1: liquid feeding device

2a, 2 b: liquid feeding pump

4a, 4a', 4 b: suction pipe

6a, 6a', 6 b: dissolved substance removing filter

8a, 8 b: flow compatilizer

10: mixing device

12: analytical flow path

14: sample injection part

16: analytical column

18: detector

20. 32: body part

22. 36: cover part

24. 38: protrusion

26. 34, 40: connecting hole

28. 42: filler

30. 43, 44: filter

46: and (4) sucking a filter.