JPH03242550A - Metal component analyzer - Google Patents

Abstract

(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

[Detailed description of the invention] [Industrial application field]

The present invention relates to a metal component analyzer, and more particularly to an analyzer that prevents a decrease in the concentration and separation capabilities of a column that concentrates or separates ions to be analyzed.

[Conventional technology]

FIG. 4 shows a metal component analyzer previously proposed by the present inventors in Japanese Patent Application No. 180529/1983. The symbol l in the figure is an automatic flow path switching valve. A sample supply path 3o is connected to the outlet of the automatic flow path switching valve 1. The sample liquid supply path 30 includes an acid feeding pump 2 and a reactor 3.
, an overflow valve i+"fr 4 , a three-way automatic switching valve 5, a pressurizing pump 6, and a pressure filter A are attached, and this sample liquid supply path 30 is ultimately connected to the first four-way switching valve 7. This first four-way switching valve 7 has a first
The inflow path 8a to the R condensation column 8, the inflow path 9a to the second concentration column 9, and the eluent supply path 31 are connected, and the eluent supply path 31 is connected to the pressurized horn 17 and the eluent storage section 18. It is provided. The outflow path 8b from the 1711th condensation column 8 and the outflow path 9b from the second concentration column 9 are connected to a second four-way switching valve 10. This second four-way switching valve lO is further connected with a flow path 33 that connects to an analysis means 32 consisting of a separation column 11 and an absorption photometer 12, and a flow path 35 that connects to a water channel 34. A flow meter 19 is attached to 35. Next, the operation of the metal component analyzer will be explained. The automatic flow path switching valve l has six sample liquid optical input paths IA-
IF is connected, and these sample liquid inflow paths lA to IF -
are selectively connected to the sample liquid supply path 30. At night, the sample liquid sold to the supply path 30 is sent to the reaction "AX3" by the liquid sending pump 2. Jx of the reactor 3
On the 1Ilt side, there is a reaction limb storage section 15 and a supply pump 16.
A reaction wave supply path 37 equipped with a reaction wave is connected to the sample liquid, and a reaction wave for ionizing metals in the sample liquid is added to the sample liquid. The sample solution to which this reaction mixture has been added is mixed in the reactor 3 at a predetermined temperature. The sample liquid that has passed through this reactor 3 is transferred to an overflow container 4.
Trial E is stored once and exceeds a certain storage amount.
The l liquid is discharged to the drainage channel 34 through the flow path indicated by . The sample liquid that has passed through the overflow container 4 reaches the three-way switching valve 5. Moreover, the three-way automatic switching valve 5 guides a part of the sample liquid flowing through the sample liquid supply path 30 to the drainage path 34 through a flow path indicated by the symbol L3, and is configured so that the automatic flow path switching valve 1 is switched. If another sample solution is supplied,
First, the flow path is switched to the flow path L3 side to completely wash away the previous sample liquid remaining between the automatic flow path switching valve 1 and the three-way switching valve 5, and then the sample liquid is sampled by switching the flow path. The liquid is strained so that it flows along the sample liquid supply path 30. The sample liquid that has passed through the three-way switching valve 5 is pressurized by a pressure pump 6. Note that when the sample liquid is pressurized to a predetermined pressure or higher by this pressure pump 6, the pressure switch 6A is
is turned on and outputs a detection signal to the control unit C to stop the operation of the pressurizing pump 6. The sample liquid pressurized by the pressurizing pump 6 is fed to the pipe 1 concentrating column 8 or the second concentrating column 9 by the first four-way switching valve 7. The four-way switching valve 10 is a metal ion layer wire process in which the sample e (j) is supplied from the supply path 30 and is passed through the concentration column 8 or 9 and then guided to the drainage path 34 via the flow path 35. The flow path and the flow path for the metal ion elution process in which the eluent supplied from the eluent supply path 31 passes through the concentration column 9 or 8 and then leads to the analysis means 32 are connected to the concentration columns 8 and 9. The switching of the four-way switching valve 710 is transmitted from the control unit C when the flow rate of the sample liquid passing through the flow path 35 measured by the flow meter 19 reaches a set value. This is done by the signal. Then, the sample l that has passed through the concentration column 8 or 9
The metal ions in ll are adsorbed on column 8 or 9,
The metal ions adsorbed on the column 8 or 9 or the eluent supplied from the eluent supply path 31
9 and sent to the analysis means 32. Further, the metal ions carried to the analysis means 32 are purified by the separation column 11 and then subjected to N g! A color is developed by the colored liquid supplied from the liquid supply path 38, and the degree of color development is chromatographed in the spectrophotometer 12 and the concentration is measured.

[Invention or problem to be solved]

However, in the case of the analyzer having the structure described in 2, the sample liquid is heated in the reactor 3 at a temperature of 100°C or higher (specifically, at 150° to +60°C, which is sufficient to reliably dissolve the cladding of the metal wall). C
), and furthermore, since there is an atmosphere in the overflow III volume 4, bubbles are generated and the temperature is 0<,
There is a problem that the pump 6 cannot operate normally after pumping in air %jQ. Therefore, it is possible to omit the overflow pipe 4 and close the pipe d8. There is a problem that this causes deterioration of the ion exchange resin in the column. In addition, in the above analyzer, ion exchange processing is essential in the concentration columns 8 and 9 or the separation column 10, but since the ion exchange capacity of these changes depending on the temperature, the temperature conditions at the time of analysis may affect the ion exchange processing in each column. concentrated,
There is a problem that the time required for separation is different and it is difficult to maintain reliability of analysis. The present invention has been made in view of the above circumstances, and aims to prevent air entrainment in the sample feed pump and to perform highly reliable analysis regardless of the temperature conditions during analysis.

[Means for Solving the Problems] In order to achieve the above object, the invention according to claim 1 of the present application is such that a cooling device is provided downstream of a reactor in which a reaction is prepared while heating a sample liquid. be. The invention according to claim 2 of the present application is the invention according to claim I, in which the cross-sectional area of the sample liquid flow path in the cooling device is made smaller than that of the flow path on the upstream side. The invention set forth in claim 3 of the present application is such that an element that performs an ion exchange action in a metal component analyzer is housed in a constant temperature bath. The invention as set forth in claim 4 of the present application is directed to the lower part of the reactor in which the reaction is prepared while heating the sample liquid. A cooling device is provided on the ε side, and a column for concentrating and separating metal components in the sample liquid by ion exchange action is housed in a constant temperature bath. [Operation] According to the structure of the invention in claim 1, trial 1 in a heated state
After 1ffl is cooled down, it is sucked into the pump, so
Air bubbles are not sucked into the pump. With the configuration of the invention of claim 2, it is possible to generate back pressure at the outlet of the heater and keep the pressure high. According to the configuration of the invention described in claim 3, the ion exchange treatment can be performed at a constant temperature. With the configuration of the invention of claim 4, the temperature of the sample liquid sucked into the pump can be lowered to prevent bubbles from being sucked in, and the ion exchange treatment can be performed at a constant temperature.

[Example] Hereinafter, the present invention will be described in detail with reference to the drawings. In addition,
Components common to the conventional example are given the same reference numerals to simplify the explanation. FIG. 1 shows a first embodiment of the present invention, in which a cooling device 40 for cooling the sample liquid is provided downstream of the reactor 3, and a cooling device 40 is provided downstream of the cooling device 40. Then, there is a branch 4 which branches the sample to a pump 6 and a drain 34.
1 is provided, and a check valve 42 is provided between this branch portion 41 and the pump 6. The cooling device 40 includes a thin pipe 4 formed into a coil shape.
3, and a fan 44 that supplies cooling air to the pipe 43. The total length of the pipe 43 is set to 2 m, and the inner diameter of the pipe 43 is, for example, 1.5 m. If the diameter is set to 5 mm, the inner diameter is set to a smaller diameter of about 0.5 mm, which functions as a throttle in the flow path and applies back pressure to the discharge side of the heater 3. There is. The fan 44 also forces air into contact with the pipe 43, which is formed into a coil shape and has a predetermined flow path length, to promote heat exchange (cooling) between the sample liquid and the outside air. There is. Note that when the flow rate of the sample at night is low, the fan 44
may be omitted to rely on self-thermal cooling. Also,
The coiled piping may be immersed in a cooling element such as water to exchange heat with the cooling element. Furthermore, the check valve 42 is set at an operating pressure lower than the suction pressure of the pump 6, i! When the pump 6 operates to send a sample wave to the A-shrinking column 8, the sample liquid is sucked in, while when the pump is stopped during the analysis of the sample 1, the gas that has risen from the lower drainage channel 34 is sucked in. This prevents suction into the pump 6. In this first embodiment, since the constricted pipe 43 is present in the cooling device 40 downstream of the heater 3, the pressure of the sample liquid increases, and bubbles are not generated when the sample liquid is sucked into the pump 6. It's fleeting. In addition, since the sample liquid is cooled by the Leahy flow through the concentration columns 8 and 9, the concentration columns 8 and 9
Deterioration of the ion exchange resin provided in 9 etc. can be prevented. Next, FIGS. 2 and 3 show a second embodiment of the present invention. In this example, 1
By housing the g3 condensation columns 8 and 9 and the separation column 11 in a constant temperature bath 50, the t temperature conditions for ion exchange are made constant. The concentration columns 8 and 9 accommodated in the above-mentioned WI 50 are provided in the middle of the pipes La and Lb between the four-way switching valves 7 and 10, as in the first embodiment, and the separation columns 11 is provided in the middle of the conduit Lc between the four-way switching valve 10 and the absorption photometer 12. Furthermore, the pipe La
On the upstream side of the column in -Lb-Lc, coiled portions LaLb' and Lc' are provided, giving a certain heat exchange area, and these coiled portions La',
By bringing Lb'Lc' into contact with a heat medium (e.g. heated air or water) in a constant temperature Fu5o, each pipe L
The sample liquid in aLb and Ic can be maintained at a predetermined art-. Furthermore, a coiled portion Ld' is also provided in the middle of the pipe line Ld that supplies the separated liquid to the iR condensation columns 8 and 9, so that the temperature of the liquid fed into the column from outside the system is made as equal as possible to that inside the column. is now possible. Further, the heat medium in the constant temperature bath 50 is maintained at a constant temperature by the control device C. Note that instead of exchanging heat using the coiled portion in the pipe, it is of course possible to directly heat each column or the pipe on the upstream side thereof using an electric heater, a steam heater, or the like. By maintaining the temperature of the column that performs the ion exchange function constant in this way, the concentration or separation ability of these columns becomes constant, and therefore reliability and reproducibility can be maintained without being influenced by the usage environment. A high level of analysis can be performed. [Effects of the Invention] As is clear from the above explanation, the water head has the following effects. ■Since a cooling device is installed downstream of the reactor that heats the sample solution and prepares the reaction, the heated sample will be sucked into the pump after it has cooled down, and air bubbles will not be sucked into the pump. , malfunction or be prevented. (2) If the area of the flow path constituting the cooling device is narrowed down, back pressure can be generated at the outlet of the heater to keep the pressure high, thereby further reliably preventing the generation of bubbles. ■Place the elements for ion exchange treatment in a constant temperature bath,
The ion exchange treatment can be performed at a constant temperature, and therefore analysis can be performed with good reproducibility while maintaining conditions such as concentration and separation treatment times constant.

[Brief explanation of drawings]

Fig. 1 is a piping diagram showing a first embodiment of the present invention, Figs. 2 and 3 are a piping diagram showing a second embodiment of the invention, Fig. 2 is a piping diagram, and Fig. 3 is a piping diagram. FIG. 4 is a piping diagram of a conventional analyzer. 2 ・Night pump, 3... Reactor, 6...
...pressurized pop, 8.9...concentration column, 30.
...Sample l night (j (feed path, 11 ・ Separation column,
12... Absorption light change, 21... Color development l night, 4
0...Cooling device, 41 Branch, 42...Cheer/return valve, 43...Piping, 44...Fan, 50...↑Wataru Variety.

Claims (4)

[Claims] (1) a reactor that is installed in a flow path through which a sample liquid containing a metal component flows and prepares a reaction while heating the sample liquid;
Metal component analysis consisting of a column that adsorbs metal ions in a sample solution prepared by the reactor and sent out by a pump, and an analysis means that analyzes metal ions separated into an eluent from the column. A metal component analysis apparatus, characterized in that the sample liquid flow path between the reactor and the pump is provided with a cooling device for cooling the sample liquid in the flow path. (2) The metal component analysis apparatus according to claim 1, wherein the sample liquid flow path in the cooling device has a cross-sectional area smaller than that of the flow path upstream thereof. (3) Provided in a flow path through which a sample liquid containing metal components flows, the sample liquid is heated and subjected to reaction preparation, the reaction-prepared sample liquid is concentrated, and metal ions are separated into the eluent. , a metal component analyzer configured to analyze separated metal ions, comprising an element installed in a sample liquid flow path of the metal component apparatus and having a function of ion-exchanging the sample liquid, housed in a constant temperature bath. A metal component analyzer characterized by: (4) a reactor that is installed in a flow path through which a sample liquid containing a metal component flows and prepares a reaction while heating the sample liquid;
Metal component analysis consisting of a column that adsorbs metal ions in a sample solution prepared by the reactor and sent out by a pump, and an analysis means that analyzes metal ions separated into an eluent from the column. A metal component analyzer, characterized in that the sample liquid flow path between the reactor and the pump is provided with a cooling device for cooling the sample liquid in the flow path, and the column is housed in a constant temperature bath. .