JP2021013897A - Sample extraction method and sample extraction system - Google Patents

Abstract

To provide a sample extraction method and a sample extraction system for easily performing detection inspection on the site and/or continuously performing monitoring inspection for the purpose of detecting deterioration of insulating oil for electric appliances and hydraulic oil for equipment.SOLUTION: There is provided a sample extraction method for extracting a detection target substance in oil and fat into an extraction solvent, comprising; a deriving step of continuously deriving oil and fat O0 from an apparatus 3 using the oil and fat; a parallel laminar flow forming step of causing the derived oil and fat to contact with an extraction solvent A0 to form a parallel laminar flow of both of the oil and fat and the extraction solvent, thereby diffusing the detection target substance in the oil and fat into the extraction solvent; a separation step of separating the parallel laminar flow into the oil and fat, and the extraction solvent; a return step of returning the oil and fat O1 separated from the extraction solvent, to the apparatus 3 using the oil and fat; and a liquid sending step of sending an extraction solvent A1 in which the detection target substance is diffused, to another step. There is also provided a sample extraction system for implementing the method.SELECTED DRAWING: Figure 1

Description

The present invention relates to a sample extraction method and a sample extraction system. The present invention particularly relates to a sample extraction method and a sample extraction system for solvent extraction of a sample containing a substance to be detected in the fat and oil for the purpose of detecting deterioration of the fat and oil used industrially.

As an index for predicting a malfunction or maintenance time of an electric appliance or equipment, a method of measuring the deterioration of the electric appliance insulating oil or the equipment hydraulic oil to be used and detecting a specific amount of substance has been known. Since these oils generally deteriorate over time with the use of equipment, for example, deterioration detection of equipment hydraulic oil used for hydraulic cylinders and insulating oil used for breakers is regularly performed. It has been carried out by extracting oil from the equipment of the above and outsourcing the component analysis to an analysis institution.

For the purpose of testing the degree of deterioration of insulating oil and paper immersed in the insulating oil, a method of detecting furfurals contained in the oil is known (see, for example, Patent Document 1). In this method, the oil to be tested can be mixed with an organic acid solution containing an aromatic amine, and furfurals can be detected from light absorption based on the coloration of the solution.

Further, in an oil-filled electric device in which the insulating oil is depleted, a method of collecting the insulating oil for the purpose of diagnosing deterioration of the insulating oil is known (see, for example, Patent Document 2). In this method, insulating paper or stranded conductors constituting an oil-filled electric device can be taken out and put on a centrifuge to collect insulating oil adhering to the inner wall of the centrifuge container. Then, by subjecting the collected insulating oil to tests such as gas analysis and qualitative analysis, deterioration diagnosis becomes possible.

Japanese Unexamined Patent Publication No. 9-21091 Japanese Unexamined Patent Publication No. 2018-407390

However, it may take time and cost to carry out the outsourced inspection as in the past, and the countermeasure may be delayed.

For the purpose of detecting deterioration of insulating oil and hydraulic oil used in electrical equipment, a sample extraction method and a sample extraction system for easily detecting and inspecting on-site and / or continuously monitoring and detecting are desired.

As a result of diligent studies, the present inventors can extract a sample by forming a parallel laminar flow interface between an oil or fat containing a substance to be detected and an extraction solvent and causing mass transfer at the interface. This led to the completion of the present invention.

That is, according to one embodiment, the present invention is a sample extraction method for extracting a detection target substance in fats and oils into an extraction solvent, and is a derivation step of continuously deriving the fats and oils from an apparatus using the fats and oils, and the derivation thereof. The parallel layer flow forming step of contacting the obtained fat and oil with the extraction solvent to form a parallel layer flow of the fat and oil and the extraction solvent, thereby diffusing the detection target substance in the fat and oil into the extraction solvent, and the above-mentioned A separation step of separating the parallel layer flow into the fat and oil and an extraction solvent, a return step of returning the fat and oil separated from the extraction solvent to an apparatus using the fat and oil, and an extraction solvent in which the detection target substance is diffused. Includes a liquid feeding step of sending the liquid to another step.

In the sample extraction method, it is preferable that the extraction solvent is a hydrophilic solvent and the detection target substance is an ionic substance.

In the sample extraction method, the parallel laminar flow forming step is carried out by a step of introducing the fat and oil and the extraction solvent into an extraction device, and the extraction device has a laminar flow forming portion composed of a single flow path. , At one end of the laminar flow forming portion, the oil and fat introduction port and the extraction solvent introduction port communicating with the laminar flow forming portion, and at the other end of the laminar flow forming portion, the laminar flow forming It is preferable to provide an oil / fat discharge port and an extraction solvent discharge port that communicate with each other.

In the sample extraction method using the extraction device, the extraction device includes an oil / fat introduction flow path provided between the oil / fat introduction port and the layer flow forming portion, and the extraction solvent introduction port and the layer flow forming portion. An extraction solvent introduction flow path provided between the two, an oil / fat discharge flow path provided between the layer flow forming portion and the oil / fat discharge port, and the layer flow forming portion and the extraction solvent discharge port. It is preferable to further provide an extraction solvent discharge flow path provided between them.

In the sample extraction method, it is preferable that the separate step is a detection step for detecting the detection target substance diffused in the extraction solvent, and the sample extraction method further includes a detection step.

In the sample extraction method, it is preferable that the oil or fat is an insulating oil or a mechanical oil.

In the sampling process, the ionic _substance, ^SO 4 _2-, NO ₃ ^- is preferably selected from.

According to another embodiment, the present invention is a sample extraction system for extracting a detection target substance in fats and oils into an extraction solvent, which comprises a laminar flow forming portion composed of a single flow path and one end of the laminar flow forming portion. In the oil and fat introduction port and the extraction solvent introduction port communicating with the layer flow forming portion, and the oil and fat discharge at the other end of the layer flow forming portion and communicating with the layer flow forming portion. A sample extraction device having an outlet and an extraction solvent discharge port, a liquid feeding means for continuously deriving fats and oils from an apparatus using fats and oils and sending them to the fats and oils introduction port of the sample extraction device, and extracting the extraction solvent from the sample. The liquid feeding means for sending the fat and oil to the extraction solvent introduction port of the device, the liquid feeding means for returning the fat and oil discharged from the fat and oil discharge port to the device using the fat and oil, and the liquid feeding means discharged from the extraction solvent discharge port. It is provided with a liquid feeding means for sending an extraction solvent containing a detection target substance diffused from fats and oils to the outside of the sample extraction device.

According to the sample extraction method and the sample extraction system of the present invention, it is possible to extract the detection target substance in the fat and oil into the solvent in a short time, and the maintenance of the apparatus using the fat and oil using the detection target substance amount as a deterioration index. The technology can be strengthened. In particular, in the detection of substances that need to undergo solvent extraction such as water, there is a great advantage that extraction and analysis by an external inspection organization, which has been indispensable in the past, can be performed on-site. Further, such a sample extraction method and a sample extraction system make it possible to perform continuous inspection and constant monitoring, which is advantageous in that the maintenance and inspection timing of the apparatus using fats and oils can be clearly indicated and managed.

FIG. 1 is an explanatory diagram conceptually showing a sample extraction system capable of implementing the sample extraction method according to the embodiment of the present invention. FIG. 2 is a conceptual perspective view of an extraction device that can be used in the sample extraction system shown in FIG. FIG. 3 is a conceptual plan view of the extraction device shown in FIG. 2, and conceptualizes the formation of a parallel laminar flow between fats and oils and an extraction solvent using the extraction device and the extraction mode by molecular diffusion from the parallel laminar flow interface. It is a figure to explain. FIG. 4 is a cross-sectional view taken along the line BB of the extraction device shown in FIG. 3, which conceptually explains a mode of parallel laminar flow of fat and oil and an extraction solvent in a laminar flow forming portion of the extraction device.

Embodiments of the present invention will be described below. However, the present invention is not limited to the embodiments described below.

The present invention relates to a sample extraction method according to one embodiment. The sample extraction method according to the present embodiment is specifically a method of deriving a fat or oil from an apparatus using a fat or oil, diffusing the detection target substance in the fat or oil into an extraction solvent, and obtaining an extraction solvent sample containing the detection target substance. Regarding.

In the sample extraction method according to the present embodiment, the fats and oils may be fluid fats and oils at 40 ° C./100 ° C. under normal pressure (101.325 kPa), and the kinematic viscosity at 40 ° C. and normal pressure is 0. It is preferably an oil or fat of about 5 to 50 mm ² / s. The specified kinematic viscosity value may be a value according to JIS K 2283: 2000 crude oil and petroleum products-kinematic viscosity test method and viscosity index calculation method. Examples of fats and oils may be fats and oils that are mainly sealed in industrial equipment or used together with those equipment, such as insulating oils sealed in a breaker, hydraulic oils sealed in machinery, and the food industry. Examples thereof include, but are not limited to, liquid cooking oils and biological oils derived from biological products. More specifically, it may be an insulating oil conforming to JIS C2320 or the like, a hydraulic oil conforming to JIS B8348, JIS K2213 or the like, but is not limited thereto.

Devices that use oils and fats include, but are not limited to, breakers filled with insulating oil, hydraulic cylinders filled with hydraulic oil , and the like. The sample extraction in the present embodiment is performed for the purpose of detecting deterioration of fats and oils and changes in components in order to prevent malfunction of the apparatus that may occur due to deterioration of these fats and oils and changes in components. Therefore, any device known to those skilled in the art may be used as long as it is such a device.

In the method according to the present embodiment, the substance to be detected contained in the fat and oil (hereinafter, also referred to as the detection target substance) may differ depending on the type of the fat and oil and the type of the device using the fat and oil. In some embodiments, the detection target substance may be a water-soluble ions, e.g., sulfate ion _(SO ^{4 2-),} nitrate ion ^_(NO 3 -), but ^{Ni 2+} ions and the like, but not limited to ..

The extraction solvent used in the method according to the present embodiment can be determined in relation to the type of fat and oil and the substance to be detected. For example, when an ionic substance in an insulating oil or a hydraulic oil is used as a detection target substance, the extraction solvent may be a polar solvent, and examples thereof include water, ethanol, and acetone, but the extraction solvent is not limited thereto. In particular, when water-soluble ions in fats and oils are used as the detection target substance, it is not preferable to use a non-polar solvent such as toluene or hexane as the extraction solvent.

Hereinafter, the present invention will be referred to as an example in which an ionic substance is used as a detection target substance, a hydrophilic solvent is used as an extraction solvent, and a sample containing the detection target substance diffused in the hydrophilic solvent is extracted. Although the invention will be described in detail, the present invention is not limited to this aspect.

The sample extraction method for extracting the detection target substance in the fat and oil according to the present embodiment into the extraction solvent includes the following steps.
(1) Derivation step of continuously deriving fats and oils from an apparatus using fats and oils (2) The derived fats and oils are brought into contact with an extraction solvent to form a parallel layer flow of the fats and oils and the extraction solvent. A parallel layer flow forming step of diffusing the detection target substance in the fat and oil into the extraction solvent (3) A separation step of separating the parallel layer flow into the fat and oil and the extraction solvent (4) Separation from the extraction solvent Return step of returning the fat and oil to the device using the fat and oil (5) Liquid transfer step of sending the extraction solvent in which the detection target substance is diffused to another step.

FIG. 1 is a conceptual diagram showing one aspect of a sample extraction system that can be used in the sample extraction method according to the present embodiment. The sample extraction system shown in FIG. 1 includes an extraction device 1, liquid feed pumps 5, 6 and 7, optionally an extraction solvent storage device 2, a device 3 using fats and oils, and a detection device 4. The extraction device 1 and each device are connected by liquid feeding pipes L1 to L4.

(1) deriving step first step is a deriving step for continuously deriving the oil O ₀ from unit 3 using the oil. A device that uses fats and oils is also hereinafter referred to as a device that uses fats and oils. The oil and fat O ₀ can be derived by the liquid feed pipe L2 and the liquid feed pump 6 connected to the fat and oil using device 3. The means necessary for liquid feeding including the liquid feeding pipe L2 and the liquid feeding pump 6 may be referred to as a liquid feeding means. The liquid feed pump 6 may be a rotary type infusion pump or the like, but is not particularly limited. The liquid feeding means is not limited to the one using a pump, and may be any mechanism capable of feeding liquid. For example, the liquid feeding means is simply opened by opening the oil / fat outlet from the oil / fat using device 3. It may be a mechanism that enables it, or it may be a mechanism that enables liquid transfer due to a pressure difference. Hereinafter, the sample extraction method and another step of the sample extraction system according to the present specification, or the liquid feeding means used at another location can be similarly defined. Liquid feed pipe L2 from fats used device 3 may be a tube that can derive a small amount of oil O ₀ degrees does not affect the operation of the oil used device 3, for example, the cross-sectional area of 1.0 × 10 ^{- 5} m is preferably a liquid feed tube with a ^{2 ~0.005m 2} about the flow path. Using such liquid transfer tube, by the oil used device 3 continuously derivable mechanism grease O _0, as compared with the case where the fat used equipment 3 decomposition takes out the oil sequentially, it is possible to prevent loss of oil O _0. Further, in the range as described above, it derived using the cross-sectional area is small feeding tube L2, by feeding, cooling the oil O ₀ that heating in fats and oils used equipment 3 up to the normal temperature, It can be used for the next process. It is preferable that the fat and oil O ₀ is continuously derived from the fat and oil using device 3 while maintaining a constant flow rate. The speed of deriving fats and oils O ₀ can be appropriately determined by those skilled in the art so as to match the flow velocity V required in the step (2) described later.

In parallel with the derivation of the fat and oil O _0, the step of continuously deriving the extraction solvent A ₀ from the extraction solvent storage device 2 and sending it to the extraction device 1 can be carried out. The extraction of the extraction solvent A ₀ can be carried out by a liquid feeding means which may include a liquid feeding pipe L1 connected to the storage device 2 and a liquid feeding pump 5. The cross-sectional area of the liquid feed pipe L1 is preferably the same as the cross-sectional area of the liquid feed pipe L2, and the speed V for deriving the extraction solvent A ₀ is preferably the same as the speed V for deriving the fat and oil. This is because in the step (2) described later, the same amount of fats and oils O ₀ and the extraction solvent A ₀ are brought into the extraction device 1 at the same speed and brought into contact with each other per unit time.

(2) Laminar flow forming step In the second step, the derived fat and oil O ₀ and the extraction solvent A ₀ are brought into contact with each other to form a parallel laminar flow between the fat and oil and the extraction solvent A _0. This is a laminar flow forming step of diffusing the detection target substance in the fat and oil O ₀ into the extraction solvent A ₀ . In the laminar flow forming step, the fat and oil O ₀ and the extraction solvent A ₀ are introduced into the extraction device 1 from different inlets at the same flow rate, and the fat and oil O ₀ and the fat and oil O ₀ are extracted in a single flow path of the extraction device 1. it can be carried out by flowing two liquids of the solvent a ₀ cocurrently. Here, the parallel laminar flow means that the two liquids flow in parallel with respect to the vertical direction, and is distinguished from the mode in which the two liquids flow in the upper and lower two layers in the vertical direction.

The extraction device 1 will be described with reference to FIGS. 2 to 4. FIG. 2 is a conceptual perspective view of the extraction device 1. In FIG. 2, H indicates the vertical direction (gravity direction), F indicates the flow direction of the flow path (flow direction of fats and oils and extraction solvent), and W indicates the width direction of the flow path (horizontal direction). FIG. 3 is a conceptual plan view of the extraction device 1, and F and W in FIG. 3 indicate the same directions as F and W in FIG. Further, FIG. 4 is a cross-sectional view taken along the line BB of FIG. 3, where H and W in FIG. 4 indicate the same directions as H and W in FIG. 2 to 4 are conceptual diagrams of the extraction device 1, and the dimensions of the parts constituting the extraction device 1 and the relative dimensions between the parts are not limited to the present invention.

Referring to FIGS. 2 and 3, the extraction device 1 is located at one end of the laminar flow forming portion 10 composed of a single flow path and the laminar flow forming portion 10 and communicates with the laminar flow forming portion 10. The extraction solvent introduction port 11 and the oil / fat introduction port 12 and the extraction solvent discharge port 13 and the oil / fat discharge port 14 at the other end of the laminar flow forming portion 10 and communicating with the laminar flow forming portion are provided. ing. An extraction solvent introduction path 110 is arranged between the extraction solvent introduction port 11 and the laminar flow forming portion 10, and an oil and fat introduction path 120 is arranged between the fat and oil introduction port 12 and the laminar flow forming section 10. The laminar flow forming portion 10 extends linearly toward the other end with the confluence portion of the extraction solvent introduction path 110 and the oil / fat introduction path 120 as one end. On the other hand, an extraction solvent discharge path 130 is arranged between the extraction solvent discharge port 13 and the laminar flow forming section 10, and an oil and fat discharge path 140 is arranged between the fat and oil discharge port 14 and the laminar flow forming section 10. The other end of the forming portion 10 is a branch portion, and the extraction solvent discharge path 130 and the oil / fat discharge path 140 are separated.

The laminar flow forming portion 10 is formed from a single flow path having no partition or the like, a substantially flat inner wall surface, and a uniform flow path cross-sectional area in the length direction. The cross-sectional area of the flow path is preferably rectangular, and with reference to FIG. 4, it is more preferable that the width w of the flow path is a rectangle larger than the height (length in the vertical direction) h of the flow path. Further, it is preferable that the laminar flow forming portion 10 has a predetermined flow path length l. The flow path length l is preferably larger than a predetermined threshold value l ₀ , and the threshold value l ₀ will be described later. The shape of the flow path in the laminar flow forming portion 10 is preferably linear. Linear flow path, because most suitable for forming an oil phase is formed by fat O _0, a laminar flow and a solvent phase to be formed is not mixed with the extraction solvent A _0.

As an alternative embodiment, the shape of the flow path is a circular shape having a radius R ₁ sufficiently large with respect to the width w of the flow path or a shape forming a part of the circle, sufficiently large with respect to the width w of the flow path. It may be a spiral shape having a radius R ₂ or an arc shape having a radius of curvature R ₃ sufficiently large with respect to the width w of the flow path (not shown). In this case, R ₁ / w may be approximately 25 or more, R ₂ / w may be approximately 25 or more, and R ₃ / w may be approximately 25 or more, but the present invention is not limited thereto. By forming the flow path in a circular shape or a part of a circular shape, a spiral shape, or an arc shape, the extraction device 1 having a long flow path length l of the laminar flow forming portion 10 can be accommodated in a relatively narrow space. There is an advantage that more accurate sample extraction is possible.

Referring to FIG. 3, the extraction device 1 has a Y-shape whose upstream end is formed by a laminar flow forming portion 10, an extraction solvent introduction path 110, and an oil / fat introduction path 120 when viewed in a plan view from the vertical direction. It has the structure of. The extraction solvent introduction path 110 is outward (distal from the oil / fat introduction path 120) by an angle θ1 with respect to the flow path direction F in the laminar flow forming portion 10 or the direction parallel to the two-component interface S forming the laminar flow. The shape may be such that it joins the laminar flow forming portion 10 at an inclined angle. Further, the oil / fat introduction path 120 is outward by an angle θ2 (distal from the extraction solvent introduction path 110) with respect to the flow path direction F in the extraction device 1 or the direction parallel to the two-component interface S forming the laminar flow. The shape may be such that it joins the laminar flow forming portion 10 at an inclined angle. θ1 and θ2 may be the same or different, and each may be independently about 0 to 40 °, and more preferably about 25 to 35 °. The extraction solvent introduction path 110 and the oil / fat introduction path 120 are formed at an inclination with respect to the flow direction, and the extraction solvent A ₀ and the oil / fat O ₀ are brought into contact with each other at a predetermined angle, whereby both are excessively formed. This is because parallel laminar flows can be formed without mixing.

The angles θ1 and θ2 may both be zero. In that case, the extraction solvent introduction path 110 and the oil / fat introduction path 120 can be formed as two adjacent linear flow paths. Then, in one embodiment, the wall surface partitioning the extraction solvent introduction path 110 and the oil / fat introduction path 120 is formed thin enough to allow heat exchange, or is formed by using a material having high thermal conductivity suitable for heat exchange. Can be done. Thus, the extraction solvent A _0, and oil O ₀ before being introduced into the laminar flow forming unit 10, the extraction solvent A _0, and the heat exchange between the oil O _0, the extraction solvent A _0, fats It can be brought into contact with O ₀ after being brought to substantially the same temperature.

It is preferable that the extraction solvent introduction path 110 and the oil / fat introduction path 120 both have a square cross-sectional shape perpendicular to the flow path and have a constant cross-sectional area along the flow path. Further, the width and height of the flow path can be appropriately determined by those skilled in the art so as to match the width and height of the laminar flow forming portion 10 described later, respectively. Specifically, in each of the extraction solvent introduction path 110 and the oil / fat introduction path 120, the width of the flow path is 1/2 of the width w of the laminar flow forming portion 10, and the height of the flow path is laminar flow formation. It is preferable that the height h of the portion 10 is the same. The length (length along the flow path) of the extraction solvent introduction path 110 and the oil / fat introduction path 120 is not particularly limited. Further, for example, in an embodiment in which the angles θ1 and θ2 are both zero, the extraction solvent introduction path 110 and the oil / fat introduction path 120 are adjacent to each other through a wall surface formed of heat exchangeable members. It can also be formed as a path, and the extraction solvent introduction path 110 and the oil / fat introduction path 120 can be made longer than the above-mentioned general length so that sufficient heat exchange can be performed.

The downstream end of the extraction device 1 has a Y-shaped structure formed by a laminar flow forming portion 10, an extraction solvent discharge passage 130, and an oil / fat discharge passage 140. The extraction solvent discharge port 13 and the oil / fat discharge port 14 are separately provided at separated positions. Then, the extraction solvent discharge path 130 is outward (distal from the oil / fat discharge path 140) by an angle θ3 with respect to the flow path direction F in the extraction device 1 or the direction parallel to the two-component interface S forming the laminar flow. The shape can be branched from the laminar flow forming portion 10 at an inclined angle. Similarly, the oil / fat discharge path 140 is outside the extraction device 1 by an angle θ4 with respect to the flow path direction F or the direction parallel to the two-component interface S forming the laminar flow (distal direction from the extraction solvent discharge path 130). The laminar flow forming portion 10 can be branched at an angle inclined to. θ3 and θ4 may be the same or different, and their numerical ranges and suitable numerical ranges can be independently defined in the same manner as θ1 and θ2, and both θ3 and θ4 are both. It may be zero. In a typical embodiment, θ3 and θ4 may be substantially the same as θ1 and θ2, and all of θ1 to θ4 can have the same angle at about 25 to 35 °. Further, it is preferable that the width and height of the extraction solvent discharge path 130 and the fat and oil discharge path 140 are the same as the width and height of the extraction solvent introduction path 110 and the fat and oil introduction path 120, respectively. The lengths of the extraction solvent discharge passage 130 and the fat and oil discharge passage 140 are not particularly limited, and can be appropriately designed by those skilled in the art.

In the form shown in FIG. 3, the extraction device 1 having Y-shaped ends is illustrated, but the shapes of the upstream end and the downstream end of the extraction device 1 do not have to be symmetrical. The present invention is not limited to the extraction device 1 having such a shape, and only one end on the upstream side serving as an introduction port may be Y-shaped, and one end on the downstream side serving as a discharge port may be formed. Only the Y-shape may be formed, or the structure may not have a Y-shape at the end. Further, in the form shown in FIG. 3, the linear extraction solvent introduction path 110 and the oil / fat introduction path 120 merge and communicate with the laminar flow forming portion 10, and the linear extraction solvent discharge path 130 and the oil / fat discharge path 140. However, the introduction path and discharge path of the extraction solvent and fats and oils may be arcuate, and the occurrence of turbulence can be reduced by making the introduction path and discharge path an arcuate flow path. You may be able to do it.

The extraction device 1 having the above structure is a material that can visually recognize the introduction path, the flow path of the laminar flow forming portion, and the discharge path from the outside, and is not reactive with the extraction solvent A ₀ and the fat O ₀ . Can be manufactured. The extraction device 1 can be produced by a usual method using, for example, a silicone resin having a light transmittance of 80% or more, but the production of the extraction device 1 is not limited to a specific material and production method. ..

Laminar flow forming process, the extraction solvent inlet 11 and the oil inlet 12 of the extraction device 1 comprises a structural feature of the extraction solvent A ₀ and the oil O ₀ same, is flowed at a predetermined speed V, This is carried out by leading to the laminar flow forming portion 10. Factors affecting the formation of laminar flow, the cross-sectional area of the extraction solvent A ₀ and the temperature of the oil O _0, extraction solvent A ₀ and kinematic viscosity of the oil O _0, velocity V, the laminar flow forming unit 10 depends on these temperatures There is d (d = w * h) and the flow path length l of the laminar flow forming portion 10. Therefore, after setting the extraction solvent A ₀ and the fat O ₀ to be used and the temperature conditions for carrying out the method of the present invention, the values of the velocity V, the cross-sectional area d, and the flow path length l are set so as to meet these conditions. Those skilled in the art can appropriately determine by preliminary experiments and simulations. Furthermore, extractable conditions substance to be detected from a two-liquid interface of the parallel laminar flow, the concentration envisaged detection target substance in oil O _0, solubility in the extraction solvent A ₀ of the detection target substance, the extraction solvent A _It is affected by factors such as the detection limit concentration of the substance to be detected in ₀ . By examining these factors and setting the flow path length l to a predetermined threshold value l ₀ or more, it becomes possible to extract the substance to be detected from the two-component interface in a detectable amount. For even threshold l _0, a person skilled in the art can be appropriately determined by prior experiment or simulation.

As an example of the laminar flow formation and extraction conditions, the kinematic viscosity at room temperature is, 1 to 5 mm from the oil _{O 0} of ² / s, the extraction solvent _A typical example water can be extracted _SO ^{4 2-ionic} conditions is _zero The cross-sectional area d can be 0.0001 to 0.0004 m ² , the flow path length threshold l ₀ can be 20 m, and the flow velocity V can be about 0.01 to 1 m / s. Further, the same insulating oil, water NO ₃ ^- ions extractable conditions, except the threshold l ₀ of the channel length of 100m, it is similar to the extractable conditions the SO ₄ ^2-ions Can be done.

Next, the mass transfer in the extraction device 1 in the laminar flow forming step will be described with reference to FIGS. 3 and 4. Referring to FIG. 3, the oil / fat O ₀ introduced into the extraction device 1 from the introduction port 12 flows through the oil / fat introduction path 120, and is similarly introduced into the extraction device 1 from the introduction port 11 and flows through the extraction solvent introduction path 110. It comes into contact with the extraction solvent A ₀ at the confluence of these introduction paths and flows through the laminar flow forming portion 10. In the laminar flow forming portion 10, the fats and oils O ₀ and the extraction solvent A ₀ form parallel laminar flows, and an interface S is formed between them. Referring to FIG. 4, the fats and oils O ₀ and the extraction solvent A ₀ form an interface S and run in parallel at any position in the height direction H of the flow path without being substantially mixed. Then, while the fats and oils O ₀ and the extraction solvent A ₀ flow through the laminar flow forming portion 10, the mass transfer of the substance, particularly the diffusion d of the ionic substance (not shown) occurs through the interface S. Then, the ionic substance diffuses and moves over the flow path length l of the laminar flow forming portion 10, so that the detection target substance can be extracted into the extraction solvent phase. Depending on the nature of the oil O ₀ derived from oils and fats using equipment 3, but the detection target substance in oil O ₀ can may not be present in an amount capable of diffusing into the extraction solvent A _0, this case is also It constitutes a part of the present invention.

(3) separation step third step, the parallel laminar flow, the oil O _1, is separated into an extraction solvent A _1, is the separation process. In this specification, the fats and oils and the extraction solvent before the separation step are designated as O ₀ and A ₀ , and the fats and oils and the extraction solvent after the separation in the separation step are designated as O ₁ and A ₁ for convenience. .. Separation step, detailed in laminar flow forming process, the extraction device 1 using with two separate outlet structure, performed by discharging the oil O ₁ and the extraction solvent A ₁ separately from the extraction device 1 be able to. The laminar flow forming process, through the separation step, oil O ₁ exiting from the outlet 14 of the extraction device 1, the components of the extraction solvent A ₁ is not substantially mixed, and returned to the fats used equipment 3 Can be used again.

(4) returning step the fourth step, the oil O ₁ which is separated from the extraction solvent A _1, a returning step for returning to the oil used instrument 3. The returning step, the oil O ₁ is discharged from the oil discharge port 14, the good fluid feeding means include a liquid feed pipe L3 and feeding pump 7, and returns to the oil used instrument 3. The fat and oil O ₁ is substantially the same as before flowing into the extraction device 1 except that the detection target substance existing therein is diffused into the extraction solvent A ₁ and the amount of the detection target substance is reduced. It retains its composition. By returning the fats and oils O ₁ to the fats and oils-using device 3 and reusing them, the loss and waste of the fats and oils can be reduced.

(5) flowing step fifth step is a liquid feeding process for sending an extraction solvent A ₁ to the detection target substance is diffused into another step. Another step is particularly not limited, an extraction solvent A ₁ detection target substance are diffused may be a process used in accordance with the purposes. The steps used include, but are not limited to, for example, a step of storing, a step of inspecting, and a step of detecting the target substance. The flowing step, the extraction solvent A ₁ discharged from the extraction solvent discharge port 13, the good fluid feeding means also comprise a liquid feed pump (not shown) liquid feed pipe L4 and optionally, send to another process. As a result, the sample containing the detection target substance diffusely extracted from the fat / oil O ₀ derived from the fat / oil using device 3 becomes usable according to the purpose.

The sample extraction method according to the present invention may include a detection step which is an example of another step as an optional step, or may include a detection step of analyzing and detecting the extraction solvent A ₁ by the detection device 4. The method of the present invention including a detection step may also be referred to as a sample detection method including a sample extraction step in which the above first to fourth steps are combined and a detection step of detecting a target substance in the extracted sample. it can. The method carried out by the detection device 4 can be appropriately selected depending on the substance to be detected. For example, infrared spectroscopy, emission spectroscopy, chemical emission / color analysis, ion chromatography, capillary electrophoresis and the like can be used. It may be, but it is not limited to these. In particular, the detection target ^substance, SO 4 _2-, NO ₃ ^- if it is, can be carried out infrared spectroscopy, emission spectrometry, quantitative chemiluminescent / color analysis method.

As a further optional step, a deterioration diagnosis / prediction device (not shown) may be provided after the detection device 4 to carry out the diagnosis / prediction step. Those degradation diagnosis and prediction apparatus, for example, depending on the analysis result, when the extraction is greater than the certain value detecting target substance The amount of the solvent A in _1, in which a diagnosis of deterioration of the oil O _0, warn It may be. Alternatively, in the deterioration diagnosis and prediction apparatus based on the analytical data, to predict the degradation of fats O _0, can also be informed of the timing replacement of oil O _0. By carrying out such a process, it is possible to reduce the loss cost by warning before the spread of damage in the case of an accident in the equipment 3 using oils and fats, and to reduce the cost by reducing the maintenance cost and period.

According to another embodiment, the present invention relates to a sample extraction system that extracts a substance to be detected in fats and oils into an extraction solvent. The sample extraction system is as described above with reference to FIGS. 1 to 4 regarding the sample extraction method. The sample extraction system according to this embodiment is installed at the site of the device that uses fats and oils, and by arbitrarily combining with the detection device, it is possible to extract the substance to be detected from the fats and oils on-site, resulting in deterioration of the fats and oils. It is possible to quickly deal with the malfunction of the device due to this.

Hereinafter, the present invention will be described in more detail with reference to Examples. However, the following examples are examples and do not limit the present invention.

A sample extraction method was carried out in which an ionic substance dissolved in liquid paraffin was used as a detection target substance and extracted with water. As the ionic substance to be detected NO ₃ of SO ₄ ^2-ionic, sparingly soluble easily soluble in water ^- using ion. Using the extraction devices shown in FIGS. 2 to 4, the extraction method was carried out under the conditions shown in Table 1 below. The concentration in Table 1 indicates the concentration of each ion in the fat and oil before extraction. In all the experiments, the flow path cross-sectional area d of the laminar flow forming portion was 0.0002 m ² , the width w of the flow path was 0.02 m, and the height h was 0.01 m. All of θ1 to θ4 in FIG. 3 were set to 30 °. The kinematic viscosity of the liquid paraffin introduced into the extraction device was 1.5 mm ² / s. The temperature of the liquid paraffin and water was 40 ° C., and the same volume of paraffin and water per unit time was flowed into the extraction device at the same flow rate V (m / s). After parallel laminar flow forming, _SO ⁴ 2-of separated aqueous phase, NO ₃ ^- ion concentration was confirmed condition of the flow path length threshold _{l 0} exceeding 10ppm is the detection limit. The results are shown in Table 1.

From Table 1, the required flow path length threshold _{l 0} of _SO ^{4 2-ions} readily soluble is 21.6 m, the poorly soluble NO ₃ ^- required flow path length threshold _{l 0} of the ions was 116.4M. From this embodiment, by securing a predetermined required flow path length threshold l _0, readily soluble Both of sparingly soluble ions it has been shown to be capable of extraction by the method of the present invention.

The sample extraction method and sample extraction system according to the present invention can be suitably used in equipment in a large-scale factory where on-site monitoring of oil deterioration is useful.

1 Extraction device, 2 Extraction solvent storage device, 3 Equipment that uses fats and oils 4 Detection device, 5, 6, 7 Liquid transfer pump

Claims (8)

This is a sample extraction method that extracts the substance to be detected in fats and oils into an extraction solvent.
A derivation process that continuously derives fats and oils from equipment that uses fats and oils,
A parallel laminar flow forming step in which the derived fat and oil and the extraction solvent are brought into contact with each other to form a parallel laminar flow between the fat and oil and the extraction solvent, whereby the substance to be detected in the fat and oil is diffused into the extraction solvent. ,
A separation step of separating the parallel laminar flow into a fat and oil and an extraction solvent.
A return step of returning the fat and oil separated from the extraction solvent to an apparatus using the fat and oil,
A method including a liquid feeding step of sending an extraction solvent in which the detection target substance is diffused to another step. The method according to claim 1, wherein the extraction solvent is a hydrophilic solvent and the detection target substance is an ionic substance. The parallel laminar flow forming step is carried out by a step of introducing the fat and oil and the extraction solvent into an extraction device, and the extraction device is used.
A laminar flow forming part consisting of a single flow path and
An oil / fat introduction port and an extraction solvent introduction port that are located at one end of the laminar flow forming portion and communicate with the laminar flow forming portion.
The method according to claim 1 or 2, further comprising an oil / fat discharge port and an extraction solvent discharge port communicating with the laminar flow forming portion at the other end of the laminar flow forming portion. The extraction device
An oil / fat introduction flow path provided between the oil / fat introduction port and the laminar flow forming portion,
An extraction solvent introduction flow path provided between the extraction solvent introduction port and the laminar flow forming portion,
An oil / fat discharge flow path provided between the laminar flow forming portion and the oil / fat discharge port,
The method according to claim 3, further comprising an extraction solvent discharge flow path provided between the laminar flow forming portion and the extraction solvent discharge port. The method according to any one of claims 1 to 4, wherein the separate step is a detection step for detecting a detection target substance diffused in the extraction solvent, and further comprises a detection step. The method according to any one of claims 1 to 5, wherein the oil is a machine insulating oil or a machine hydraulic oil. The ionic _substance, ^SO 4 _2-, NO ₃ ^- is selected from A method according to any one of claims 1-6. A sample extraction system that extracts the substance to be detected in fats and oils into an extraction solvent.
A laminar flow forming portion consisting of a single flow path, an oil / fat introduction port and an extraction solvent introduction port at one end of the laminar flow forming portion and communicating with the laminar flow forming portion, and the laminar flow forming portion. A sample extraction device provided at the other end of the laminar flow forming portion and having an oil / fat discharge port and an extraction solvent discharge port communicating with the laminar flow forming portion.
A liquid feeding means that continuously derives fats and oils from an apparatus that uses fats and oils and sends them to the fat and oil introduction port of the sample extraction device.
A liquid feeding means for sending the extraction solvent to the extraction solvent introduction port of the sample extraction device, and
A liquid feeding means for returning the fat and oil discharged from the fat and oil discharge port to the device using the fat and oil, and
A sample extraction system including a liquid feeding means for sending an extraction solvent containing a detection target substance diffused from the fat and oil discharged from the extraction solvent outlet to the outside of the sample extraction device.