JPH084603Y2 - X-ray analyzer for liquid samples - Google Patents

Description

[Detailed description of the device]

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a liquid sample X-ray analyzer for analyzing the amount of sulfa contained in a liquid sample while flowing.

[0002]

2. Description of the Related Art Conventionally, there is an X-ray analyzer for X-ray analysis of impurities in a flammable liquid such as petroleum (crude oil). An example of this type of analyzer is shown in FIG.

In FIG. 5, a liquid L having flammability, such as petroleum, is branched from a main stream (not shown), taken out, and flows in the flow path 10. An opening 17 is formed on the side surface of the flow path 10. An irradiation chamber 52 that opens toward the opening 17 faces the opening 17. This irradiation chamber 52 and the flow path
A beryllium foil 53 as a blocking foil is interposed between the inside of the irradiation chamber 52 and the inside of the irradiation chamber 52 to partition the inside of the irradiation chamber 52 from the flow path 10. In the irradiation chamber 52, an X-ray irradiation device 54 for irradiating the liquid L to be analyzed with the primary X-ray B1 and a secondary X-ray B2 which is a fluorescent X-ray from the liquid L to be analyzed are detected through the beryllium foil 53. X-ray detector
55 and an analyzer 56 for selecting the detected secondary X-ray B2 are housed.

[0004]

However, in the above-mentioned conventional technique, the flow passage cross-sectional area in the measuring portion 61 irradiated with the primary X-ray B1 is smaller than that of the introduction flow passage 63 and the discharge flow passage 65. It is getting bigger. Therefore, the flow velocity of the liquid L to be analyzed in the measuring section 61 becomes slow. When the flow velocity is slowed in this way, the solid matter called sludge contained in the liquid L to be analyzed adheres to and accumulates on the inner surface of the beryllium foil 53. Therefore, since the sludge that has adhered is detected, the analysis accuracy of the liquid L to be analyzed decreases over time.

By the way, in the above prior art, the primary X-ray B1
The irradiation area is increased to improve the analysis accuracy. However, since the analyte liquid L flows into the wide measuring section 61 from the narrow upstream introduction flow channel 63, the pressure distribution in the measuring section 61 in the direction perpendicular to the flow direction (direction perpendicular to the paper surface) becomes large, and A stagnation or vortex is likely to occur in the flow of the analysis liquid L. Therefore, sludge easily adheres to the inner surface of the beryllium foil 53,
Therefore, the analysis accuracy is also lowered.

When the temperature of the liquid L to be analyzed is low, the viscosity becomes large and the flow velocity becomes slow, so that sludge easily adheres to the beryllium foil 53. Therefore, the liquid to be analyzed L is warmed at the introduction flow channel 63 or at an upstream thereof to reduce the viscosity of the liquid to be analyzed L. However, since the liquid temperature decreases while the liquid L to be analyzed flows to the measuring section 61 and the viscosity of the liquid L to be analyzed increases, sludge easily adheres to the beryllium foil 53, and thus the analysis accuracy also decreases. To do.

The present invention has been made in view of the above-mentioned conventional problems, and it is possible to prevent solid matter such as sludge from adhering to the blocking foil of the measuring portion and improve the analysis accuracy of the X-ray of the liquid sample. An object is to provide an analyzer.

[0008]

In order to achieve the above object, the present invention is directed to a measuring part irradiated with X-rays, in which a flow path is divided into a plurality of parts by a flow path wall and The total sum of the flow passage cross-sectional areas in the measurement unit is set smaller than the flow passage cross-sectional area of the introduction flow passage communicating with the measurement unit. According to the second aspect of the invention, a heating device for heating the liquid to be analyzed in the measuring section is provided on the opposite side of the irradiation chamber in the vicinity of the measuring section.

[0009]

According to this invention, since the flow passage cross-sectional area of the measuring portion is smaller than the flow passage cross-sectional area of the introducing flow passage, the flow velocity of the analyte liquid becomes faster in the measuring portion. Therefore, the solid matter in the liquid to be analyzed is unlikely to adhere to the inner surface of the blocking foil of the measurement section. Further, since the flow channel is divided into a plurality of channels by the flow channel wall in the measurement section, the width of the flow channel is narrow, so the pressure distribution in the lateral direction becomes small and the flow of the analyte liquid stagnates or There is no danger of it occurring. Further, when the heating device for heating the liquid to be analyzed in the measurement unit is provided, the liquid to be analyzed does not have a low temperature in the measurement unit.

[0010]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT An embodiment of the present invention will be described below with reference to FIGS.
Follow the instructions below. In FIG. 1, the X-ray irradiation device 54
The primary X-ray B1 emitted from the laser beam passes through the flat beryllium foil (closure foil) 53 which is not curved, and is irradiated onto the analyte liquid L in the measurement section 11 of the flow channel 10. The irradiation direction of the primary X-ray B1 is set to the flow direction of the liquid L to be analyzed in the channel 10. Fluorescent X-rays are generated from the elements in the liquid to be analyzed L excited by the primary X-rays B1, and these become secondary X-rays B2 and enter the X-ray detector 55. This incident secondary X-ray B2 is detected by the X-ray detector 55, and then the analyzer 56
Be sorted by.

The measuring portion 11 of the flow passage 10 is communicated with one thick upstream introduction flow passage 13 through the first communication passage 12,
The liquid L to be analyzed flows into the measurement unit 11 from below. In addition, the measurement unit 11 communicates with one thick downstream flow passage 15 via the second communication passage 14, and the liquid L to be analyzed is drawn upward from the measurement unit 11. The introduction flow path 13 and the discharge flow path 15 are in communication with flow paths in a pipe 16 for taking out the liquid L to be analyzed from a main pipe (not shown).

As shown in FIG. 2, the measuring section 11 is formed in the first manifold 20, and the first manifold 20
As shown in FIG. 3, it is divided into, for example, six by the plurality of flow path walls 21 integrally formed with the above. On the other hand, the first and second communication passages 12 and 14 of FIG. 2 pass through the first manifold 20 and the second manifold 22, respectively, and are provided in the same number as the measuring unit 11.

The flow passage cross-sectional area of the measuring section 11 is determined by the first communication passage.
The flow passage cross-sectional areas of 12 and the second communication passage 14 are set to be substantially the same. On the other hand, the sum of the flow passage cross-sectional areas in the six measurement units 11 is the flow passage cross-sectional area of the introduction flow passage 13 and the discharge flow passage in FIG.
The flow passage cross-sectional areas are set to be smaller than 15, for example, about 1/3 to 1/4. Above measuring unit
In No. 11, as it goes from the upstream side to the downstream side (from the lower side to the upper side), the depth h of the flow passage gradually decreases, and the cross-sectional area of the flow passage also gradually decreases.

The first and second manifolds 20, 22 of FIG.
And a reinforcing wall 23 fixed to the second manifold 22 with screws 25.
Constitutes a part of the pressure resistant container whose inside is the irradiation chamber 52. As shown in FIG. 2, a plurality of reinforcing beams 24 are integrally formed on the reinforcing wall 23. The flow path wall 21
The reinforcing beam 24 extends along the flow direction of the liquid L to be analyzed, that is, the irradiation direction of the primary X-ray B1, and opposes each other, and holds the flat beryllium foil 53 therebetween.

Irradiation chamber in the first manifold 20 of FIG.
On the opposite side of 52, the heating device 40 is screwed and fixed. The heating device 40 is made of a copper block and has a steam passage 41 and a steam chamber 42 through which the steam W flows, and heats the liquid L to be analyzed in the measuring unit 11. Note that 43
Is a rubber ring for sealing, and 44 in FIG. 1 is a mounting plate for the analyzer. Other configurations are similar to those of the conventional example of FIG.
The same parts or corresponding parts are designated by the same reference numerals, and detailed description thereof will be omitted.

In the above structure, the flow passage cross-sectional area in the measuring portion 11 of FIG. 4 is smaller than that of the introduction flow passage 13, so that the flow velocity of the liquid L to be analyzed in the measuring portion 11 becomes faster.
Therefore, the sludge in the liquid to be analyzed L is beryllium foil 53.
Hard to adhere to the inner surface of. Therefore, the sludge is not likely to be detected, and the analysis accuracy of the liquid L to be analyzed is improved.

In particular, in this embodiment, since the flow channel depth h of the measuring section 11 is gradually reduced and the flow channel cross-sectional area is gradually reduced from the upstream side to the downstream side, the flow velocity in the measuring section 11 is reduced. Will be faster. Therefore, the sludge is less likely to adhere to the inner surface of the beryllium foil 53.

Further, in this invention, as shown in FIG. 2, the measuring portion 11 is divided into a plurality of parts by the flow path wall 21,
Since the width W (see FIG. 3) of the flow path is narrow, the pressure distribution in the lateral direction becomes small, and the rectifying effect can be obtained. Therefore, there is no possibility of stagnation or vortex occurring in the flow of the liquid to be analyzed L.
After all, sludge is unlikely to adhere to the inner surface of the beryllium foil 53, and as a result, the analysis accuracy is improved.

By the way, since the liquid L to be analyzed is normally fed under pressure by a pump or the like, the liquid L to be analyzed is placed on the thin beryllium foil 53.
Pressure is applied. As a countermeasure against this, in the conventional example of FIG.
Beryllium foil 53 curved into a spherical shell,
Are reinforced. When the beryllium foil 53 is curved in this way, stagnation or vortex is easily generated at the edge portion 61a of the beryllium foil in the measurement portion 61, and sludge is easily attached to the edge portion 61a. Therefore, the analysis accuracy is lowered.

On the other hand, in this embodiment, as shown in FIG. 2, the beryllium foil 53 is set in a flat shape, so that there is no place where stagnation or vortex is likely to occur in the measuring section 11, so that the sludge is beryllium. Difficult to attach to foil 53. Therefore,
After all, the analysis accuracy does not easily deteriorate. Beryllium foil
Since 53 is sandwiched between the channel wall 21 and the reinforcing beam 24, the pressure resistance of the beryllium foil 53 does not decrease even if the area of the opening 17 of the channel 10 is increased.

Further, in this embodiment, the heating device 40 shown in FIG. 4 is provided in the vicinity of the measuring section 11, and the liquid L to be analyzed is passed through the first manifold 20 and the flow path wall 21 having a large heat transfer area. It's warming up. Therefore, unlike the conventional method, the liquid temperature of the liquid to be analyzed L does not decrease by the time it flows into the measurement unit 11, and therefore the viscosity thereof is small, so that the adhesion of sludge can be prevented. In addition, when sludge adheres, the flow of the liquid L to be analyzed is stopped, the measuring section 11 is heated to the steam temperature to dissolve the sludge, and then the liquid L to be analyzed is caused to flow and the sludge may be caused to flow away. it can.

In the above embodiment, the flow passage cross-sectional area of the outlet flow passage 15 is set larger than the flow passage cross-sectional area of the measuring section 11,
The flow passage cross-sectional areas of the outlet flow passage 15 and the measurement unit 11 may be about the same size.

[0023]

As described above, according to the present invention, since the flow passage cross-sectional area of the measuring portion is smaller than the flow passage cross-sectional area of the introducing flow passage, the flow velocity of the analyte liquid in the measuring portion becomes faster. . Further, since the flow channel is divided into a plurality of channels by the flow channel wall in the measurement unit, the flow channel has a narrow width and a rectifying effect can be obtained, so that the flow of the analyte liquid does not stagnant or vortex occurs. . In this way, since the flow velocity is high and there is no risk of stagnation or vortex, it is difficult for the solid matter in the liquid to be analyzed to adhere to the blocking foil of the measurement part, preventing the deterioration of analysis accuracy due to the adhesion of solid matter. By doing so, the accuracy of analysis can be improved.

Further, according to the second aspect of the present invention, since the heating device for heating the liquid to be analyzed in the measuring portion is provided, the liquid temperature of the liquid to be analyzed rises in the measuring portion. The viscosity decreases. Therefore, the liquid to be analyzed becomes easy to flow, and the solid matter is unlikely to adhere to the liquid, so that the analysis accuracy is improved.

[Brief description of drawings]

FIG. 1 is a schematic configuration diagram of an X-ray analysis apparatus showing an embodiment of the present invention.

FIG. 2 is a perspective view showing a measurement part of a flow path and the like.

FIG. 3 is a plan sectional view of a measurement unit.

FIG. 4 is a vertical sectional view showing a main part.

FIG. 5 is a schematic configuration diagram showing a conventional example.

[Explanation of symbols]

10 ... Channel, 11 ... Measuring section, 13 ... Introducing channel, 17 ... Opening section, 21
... Flow path wall, 40 ... Heating device, 52 ... Irradiation chamber, 53 ... Closure foil, 54
... X-ray irradiation device, 55 ... X-ray detector, 56 ... Analyzer, L ... Analyte liquid.

Claims (2)

[Scope of utility model registration request] 1. An opening is formed on a side surface of a flow path for an analyte liquid, and a blocking foil is inserted between the irradiation chamber opening toward the opening and the flow path to form the irradiation chamber and the flow path. Partition and
An X-ray of a liquid sample to be subjected to X-ray analysis through the blocking foil by an X-ray irradiation device and an X-ray detector housed in the irradiation chamber.
In the line analysis device, the flow channel is divided into a plurality of channels by a flow channel wall in a measurement unit irradiated with X-rays, and a total flow channel cross-sectional area in the plurality of measurement units is the above. An X-ray analyzer for a liquid sample, which is set smaller than the flow passage cross-sectional area of the introduction flow passage communicating with the measurement unit. 2. The X-ray analysis apparatus for a liquid sample according to claim 1, wherein a heating device for heating the liquid to be analyzed in the measurement unit is provided on the opposite side of the irradiation chamber near the measurement unit.