JP2000298096A - Water analyser - Google Patents

Abstract

PROBLEM TO BE SOLVED: To suppress the deterioration of an apparatus after the power supply of a water analyser is cut off and to reduce the operation of an operator after the power supply is cut off. SOLUTION: When power supply cutting-off operation is applied to a power supply switch 65, a signal is sent to a control circuit 63 from a CPU 61 to cut off the power supply of an electric furnace 27 and the power supply of an ozone generator 43. The temp. of the electric furnace 27 is monitored by a temp. sensor 47 and the temp. data thereof is sent to the CPU 61. The temp. and power supply cutting-off temp. of the electric furnace 27 are compared with each other by the CPU 61 and, the temp. of the electric funace 27 becomes the power supply cutting-off temp. or lower, a signal is sent to the CPU 61 to cut off the power supply of a cooling fan 45 and a ventilation fan 49. After a power supply cutting-off set time elapsed from a point of time when the power supply of the ozone generator 43 is cut off, a signal is sent to a control circuit 63 from the CPU 61 to close a solenoid valve 41 and the supply of the gas of an ozone source to the ozone generator 43 is stopped.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a water quality analyzer for measuring pollutants contained in sewage, river water, industrial waste water, and the like.

[0002]

2. Description of the Related Art As a conventional water quality analyzer, a TOC meter for measuring total organic carbon (TOC) contained in a sample, a total nitrogen
There is a TN meter for measuring (TN) and a total organic carbon / nitrogen meter (TOCN meter) that can measure both of them. T
When measuring the TOC concentration in an OC meter or a TOCN meter, first, all the carbon components in a predetermined amount of the sample are oxidized using an electric furnace to be converted into carbon dioxide (CO ₂ ), and the CO ₂ concentration is measured. Convert to total carbon (TC) concentration. Then acidified with a small amount of acid in a predetermined amount of the sample, subjected to aeration treatment with purified air, leading to an infrared gas detector converts inorganic body carbon in the sample (IC) to CO _2, CO ₂ Measure the concentration and IC
Convert to concentration. Next, the TOC concentration is determined by subtracting the IC concentration from the TC concentration.

When measuring the TN concentration in a TN meter or a TOCN meter, all nitrogen components in a predetermined amount of a sample are oxidized using an electric furnace to be converted into nitric oxide (NO), and the oxidized nitrogen component is supplied to a chemiluminescence detector. Then, the NO concentration is measured based on the detected intensity of chemiluminescence generated by the reaction between NO and ozone, and is converted into a TN concentration. The TN meter or the TOCN meter is provided with an ozone generator for supplying ozone of a chemiluminescence detector. The pipes in the ozone generator, the pipes from the ozone generator to the detector, the pipes in the detector, and the pipes from the detector to the ozone decomposer are subjected to oxidation-resistant treatment to prevent oxidation by ozone.

[0004]

The TOC meter, the TN meter and the TOCN meter have a cooling fan for cooling the electric furnace and a ventilation fan for ventilating the inside of the device so that the temperature inside the electric furnace and the device does not rise excessively. Is provided. After using the device,
When the power supply is cut off, when the main power supply is cut off, the cooling fan and the ventilation fan also stop, and the temperature of the piping around the electric furnace becomes high due to the residual heat of the electric furnace, causing a problem that the power supply is damaged.

When the main power is turned off with a TN or TOCN meter, air is no longer supplied to the ozone generator, so that the inside of the ozone generator, the piping from the ozone generator to the detector, the detector, and the detector Ozone remaining in the piping connected to the ozone decomposer flows back to the piping that supplies air to the ozone generator and the piping that supplies sample vaporized gas to the detector. There was a problem that damages.

[0006] In the TOC meter, TN meter, and TOCN meter, in order to solve the problem of damage to the apparatus due to the residual heat of the electric furnace, first, the power of the electric furnace is turned off, and after the temperature of the electric furnace is sufficiently lowered, the main operation is started. An operation of turning off the power was required. Further, in the TN meter and the TOCN meter, it is necessary to first turn off the power of the ozone generator, and then turn off the main power after all the ozone in the pipe is discharged. Such an operation is complicated for the operator. SUMMARY OF THE INVENTION It is an object of the present invention to suppress the deterioration of the water quality analyzer after the power is turned off and to reduce the operation of the operator after the power is turned off.

[0007]

According to one aspect of the present invention, there is provided a sample combustion section for thermally decomposing and vaporizing an aqueous solution sample and converting a carbon component in the sample into CO ₂ , and a CO ₂ gas in a sample vaporized gas. and CO ₂ detector for detecting, a water quality analyzer, comprising: a temperature measuring unit for measuring the temperature of the sample combustion portion, a cooling means for cooling the sample combustion portion, and a ventilation means for ventilating the inside of the apparatus, The temperature of the sample combustion unit when turning off the power of the cooling fan and the ventilation fan after turning off the power of the sample combustion unit is set, and when the power is turned off, the temperature of the sample combustion unit is turned off. Based on the temperature information from the measuring unit,
When the temperature of the sample burning section becomes equal to or lower than a preset temperature, the power supply of the cooling means and the ventilation means is also cut off.

When the power supply is turned off, the power supply of the sample burning section is turned off by the power supply disconnecting section, and the temperature of the sample burning section is lowered. Then, the temperature of the sample combustion unit is monitored by the temperature measurement unit, and when the temperature falls below a preset temperature, the power of the cooling unit and the ventilation unit is also cut off. As a result, the operator can stop the apparatus while suppressing the deterioration of the apparatus due to the residual heat of the sample combustion section only by performing the operation of turning off the power of the apparatus.

In another aspect of the present invention, the aqueous solution sample is thermally decomposed and vaporized, and a sample combustion section for converting a nitrogen component in the sample into NO is generated by a reaction between ozone and NO in the sample vaporized gas. A water quality analyzer comprising a chemiluminescence detector for detecting chemiluminescence and an ozone generator for supplying ozone to the chemiluminescence detector, wherein after the ozone generator is turned off, an ozone source to the ozone generator is provided. The time until the supply of gas is stopped is set, and when the power is turned off, the power of the ozone generator is turned off. It has a power cutoff unit for stopping the supply of the ozone source gas to the generator.

When the power supply is turned off, the power supply of the ozone generator is first turned off by the power supply cutoff unit to stop the generation of ozone. Then, after the preset time has elapsed from the power-off operation and the ozone in the apparatus is eliminated, the supply of the ozone source gas from the ozone source supply unit to the ozone generator is stopped. As a result, the operator can stop the apparatus while suppressing the deterioration of the apparatus due to the backflow of ozone only by performing the operation of turning off the power of the apparatus.

[0011] Still another aspect of the present invention is a sample combustion section for thermally decomposing and vaporizing an aqueous solution sample and converting a target component in the sample into a detection component, and a sample combustion section for converting ozone and the detection component in the sample vaporized gas. A chemiluminescence detector for detecting chemiluminescence caused by the reaction, an ozone generator for supplying ozone to the chemiluminescence detector, a temperature measuring unit for measuring the temperature of the sample burning unit, and a cooling means for cooling the sample burning unit. A water quality analyzer having ventilation means for ventilating the inside of the apparatus, wherein the temperature of the sample combustion section when the power supply of the cooling fan and the ventilation fan is turned off after the power supply of the sample combustion section is turned off, and the power supply of the ozone generator After the cutting, the time until the supply of the ozone source gas to the ozone generator is stopped is set.If the power is turned off, the power of the sample combustion unit is turned off, and the temperature measurement unit Based on temperature information Then, when the temperature of the sample burning section becomes equal to or lower than the preset temperature, the power of the cooling means and the ventilation means is also turned off, and when the power is turned off, the power of the ozone generator is turned off. After the set time has elapsed, the power supply disconnecting unit for stopping the supply of the ozone source gas from the ozone source supply unit to the ozone generator is provided.

In the case of a water quality analyzer provided with both a sample combustion section and an ozone generator, the power of the sample combustion section is turned off when the power is turned off, and then the sample combustion section is turned on based on the temperature information from the temperature measurement section. The function of turning off the power of the cooling means and the ventilating means when the temperature of the ozone generator becomes equal to or lower than the preset temperature, and the power of the ozone generator is cut off. By providing both the function of stopping the supply of the ozone source gas to the ozone generator to the power-off section, the operator only needs to turn off the power of the apparatus, and suppresses the deterioration of the apparatus due to the residual heat of the sample combustion section. Further, it is possible to stop the apparatus while suppressing the deterioration of the apparatus due to the backflow of ozone. In this mode, the TN meter or T
The present invention can be applied to a water quality analyzer including both a sample combustion unit and an ozone generator, such as an OCN meter.

[0013]

FIG. 1 is a schematic diagram showing an embodiment in which the present invention is applied to a TOCN meter. A channel for discharging a part of the sample to a drain outlet 5 through a branch portion 3 in the TOCN meter main body is connected to a water sampling pipe 1 through which a sample such as environmental water flows continuously. In the branching section 3, one of the 8-port valves 7 of the sample injection mechanism 11 is used to collect a sample and guide it to the analysis section.
Ports are connected.

The sample injection mechanism 11 comprises an 8-port valve 7 and a micro syringe 9 connected thereto.
The micro syringe 9 is connected to any port of the 8-port valve 7. 8 port valve 7
Each of the ports has a flow path for the sample connected to the branch portion 3, a flow path for the acid 13 added to make the sample acidic when measuring the IC, and a standard solution 1 for calibration.
A flow path leading to 5, a flow path leading to dilution water 17 used for dilution and washing, a flow path leading to an off-line sample 19, and an oxidation catalyst that converts carbon components in the sample into CO ₂ and nitrogen components into NO. Sample injection part 2 of sample combustion part 29 provided
3, a flow path connected to a drain outlet 21 for discharging unnecessary gas, and a flow path connected to a drain outlet 5 for discharging unnecessary liquid.

A gas purification / flow rate control unit 33 is provided for removing a carbon component from the air taken in from the air inlet 31 to generate a purified gas, adjusting the flow rate, and sending out the purified gas. The gas outlet 33 has a flow path 35 for supplying the purified gas generated by the gas purification / flow rate control unit 33 to the micro syringe 9 as a sparging gas or a carrier gas, and a flow path 37 for supplying the sample gas to the sample combustion unit 29 as a carrier gas. And the ozone generator 43 via the purified gas.
An ozone source flow path 39 for supplying an ozone source gas as an ozone source gas is connected. The ozone source channel 39 includes an ozone generator 43.
Valve 4 for switching between supply and non-supply of purified gas
1 is provided.

The sample combustion section 29 converts the carbon component in the sample into C
A combustion tube 25 filled with an oxidation catalyst for converting O ₂ and converting a nitrogen component to NO, a sample injection portion 23 for introducing a sample and a carrier gas into the combustion tube 25, and an electric furnace 27 for heating the combustion tube 25 It is composed of A cooling fan 45 is provided near the sample injection section 23 to prevent the temperature of the sample injection section 23 from becoming too high due to the heating of the electric furnace 27. The electric furnace 27 is provided with a temperature sensor 47 for measuring the temperature of the electric furnace 27. Further, a ventilation fan 49 for ventilating the inside of the apparatus main body is provided in order to prevent the temperature inside the apparatus main body from excessively rising due to the heating of the electric furnace 27.

The downstream portion of the combustion tube 25 is connected to an infrared gas detector 53 for detecting CO ₂ through a dehumidifier / gas processor 51 having a dehumidifier for removing moisture and a halogen scrubber for removing halogen components. ing. Downstream of the infrared gas detector 53 is a chemiluminescence detector 5 for detecting NO.
5 is connected. Ozone is supplied from the ozone generator 43 to the chemiluminescence detector 55. Chemiluminescence detector 55
Is connected to a drain outlet 59 via an ozone decomposing device 57 for decomposing ozone.

The output of the infrared gas detector 53, the output of the chemiluminescence detector 55 and the output of the temperature sensor 47 are input to a CPU (central processing unit) 61. In the CPU 61,
8-port valve 7, micro syringe 9, electric furnace 27,
Operation of electromagnetic valve 41, ozone generator 43, cooling fan 45 and ventilation fan 49, and infrared gas detector 53
And a control circuit 63 for controlling the detector sensitivity of the chemiluminescence detector 55 is connected. A power switch 65 for turning off the power of the entire apparatus is provided outside the apparatus main body, and ON / OFF of the power switch 65 is input to the CPU 61.

Further, the CPU 61 has a predetermined power supply for turning off the cooling fan 45 and the ventilation fan 49 after the power of the electric furnace 27 is turned off and the temperature of the electric furnace 27 becomes lower than a predetermined temperature. The temperature (power cutoff temperature) is stored. Further, the power supply of the ozone generator 43 is cut off to stop the supply of ozone, and the ozone generator 43, the chemiluminescence detector 55, the ozone decomposer 57, and the predetermined ozone at which ozone is discharged from the flow path between these devices. A predetermined time (power-off setting time) for closing the electromagnetic valve 41 after a lapse of time is also stored. The power supply disconnection unit according to the present invention includes a CPU
61 and the control circuit 63.

When the power switch 65 is turned on, the CP
The operation of the device is started by the U61 and the control circuit 63. During operation of the apparatus, the electric furnace 27 is heated and the combustion tube 25 is heated to, for example, 720 ° C. The temperature of the electric furnace 27 is monitored by a temperature sensor 47. Since the heat of the electric furnace 27 is also transmitted to the sample injection unit 23 via the combustion tube 25, the sample injection unit 23 is cooled by the cooling fan 45. Further, the inside of the apparatus is ventilated by the ventilation fan 49 so that the temperature inside the apparatus does not excessively increase due to the heating of the electric furnace 27.

Further, during operation of the apparatus, a carrier gas is supplied from the gas purification / flow rate control unit 33 to the sample injection unit 23 via the flow path 37. The carrier gas is discharged from a drain outlet 59 via a dehumidification / gas processing unit 51, an infrared gas detector 53, a chemiluminescence detector 55, and an ozone decomposer 57. Further, during operation of the apparatus, the electromagnetic valve 41 is opened, and the gas purification / flow rate control unit 33
The purified gas is supplied to the ozone generator 43 via the ozone source channel 39. In the ozone generator 43, ozone is generated from oxygen in the purified gas and supplied to the chemiluminescence detector 55. The ozone supplied to the chemiluminescence detector 55 is sent to the ozone decomposer 57 together with the carrier gas and decomposed.

Next, the operation of this embodiment when measuring a sample will be described with reference to FIG. (TC measurement and TN measurement) Switching of the 8-port valve 7 and micro-syringe 9 by the control signal from the control circuit 63
Is driven. First, the micro syringe 9 is connected to the branch portion 3, and a certain amount of a sample is collected in the micro syringe 9. When a predetermined dilution rate is set, the micro syringe 9 is connected to the dilution water 17, and a predetermined amount of dilution water is added to the sample in the micro syringe 9. next,
The sample of the microsyringe 9 is injected into the combustion tube 25 via the sample injection part 23 of the sample combustion part 29, and the carbon component in the sample is converted into CO ₂ and the nitrogen component is converted into NO. The CO ₂ and NO generated in the combustion tube 25 are sent to the dehumidification / gas processing unit 51 together with the carrier gas supplied from the gas purification / flow rate control unit 33 through the flow path 37 and cooled, dehumidified, and halogen-removed. CO ₂ is detected by the infrared gas detector 53, and NO is subsequently detected by the chemiluminescence detector 55. These detection signals are sent to the CPU 61, from which the TC concentration and the TN concentration are obtained.

(IC Measurement) A fixed amount of a sample is collected in the micro syringe 9 in the same manner as in the TC measurement and the TN measurement. When a predetermined dilution rate is set, the micro syringe 9 is connected to the dilution water 17 and a predetermined amount of the dilution water is added to the sample in the micro syringe 9. Next, the micro syringe 9 is connected to the acid 13 and a small amount of acid is added to the sample in the micro syringe 9. Next, the micro syringe 9 is connected to the sample injection unit 23, and a sparge gas is supplied to the micro syringe 9 from the gas purification / flow rate control unit 33 via the flow path 35. C generated from IC in sample
O ₂ is sent to the dehumidification / gas processing unit 51 together with the sparge gas, and after cooling, dehumidification, and halogen removal, CO ₂ is detected by the infrared gas detector 53. The detection signal is CPU6
1 and the IC density is obtained from the signal. CP
U61 determines the TOC concentration from the difference between the TC concentration and the IC concentration.

FIG. 2 is a flow chart showing the operation of this embodiment when the power is turned off. FIG. 3 is a schematic configuration diagram showing a main part according to the present invention of an embodiment in which the present invention is applied to a TOC meter. FIG. 4 is a schematic configuration diagram illustrating a main part according to the present invention in an embodiment in which the present invention is applied to a TN meter. The operation of the present invention when the power is turned off will be described with reference to FIGS. First, turning off of the power supply of the cooling fan 45 and the ventilation fan 49 will be described with reference to FIGS. When the power switch 65 is turned off, a signal is sent from the CPU 61 to the control circuit 63, and the power of the electric furnace 27 is turned off. The temperature of the electric furnace 27 is monitored by the temperature sensor 47, and the temperature information is sent to the CPU 61. CPU 61
Thus, the temperature of the electric furnace 27 is compared with a preset power-off temperature. When the temperature of the electric furnace 27 becomes equal to or lower than the power cutoff temperature, a signal is sent from the CPU 61 to the control unit 61, and the power of the cooling fan 45 and the ventilation fan 49 is cut off. As described above, the power supply of the cooling fan 45 and the ventilation fan 49 is turned off after the electric furnace 27 becomes lower than the power cutoff temperature, thereby preventing the sample injection part 23 and the piping around it from being damaged due to the residual heat of the electric furnace 27. can do.

Next, the operation of stopping the supply of the ozone source gas to the ozone generator 43 will be described with reference to FIGS. 1, 2 and 4. When the power switch 65 is turned off, a signal is sent from the CPU 61 to the control circuit 63, and the power of the ozone generator 43 is turned off. Then, the generation of ozone in the ozone generator 43 stops. At this time, since the electromagnetic valve 41 is opened and the gas generation / flow path control unit 33 is operated, the purified gas (ozone source gas) is continuously supplied to the ozone generator 43.

After the power supply of the ozone generator 43 is turned off, and during a lapse of a power-off setting time preset in the CPU 61, the ozone generator 43, the chemiluminescence detector 55, the ozone decomposer 57, and those devices The ozone existing in the flow path between them is sent to the ozone decomposing device 57 and decomposed. After the power-off set time has elapsed since the power of the ozone generator 43 was turned off, a signal was sent from the CPU 61 to the control circuit 63, the electromagnetic valve 41 was closed, and the supply of the ozone source gas to the ozone generator 43 was stopped. Stopped. Thereafter, the power supply of the gas purification / flow rate control unit 33 is also cut off.

After the ozone generator 43, the chemiluminescence detector 55, the ozone decomposing device 57, and the ozone remaining in the flow path between these devices are decomposed, the supply of the ozone source gas to the ozone generator is performed. Since the operation is stopped, damage to the apparatus due to the backflow of ozone can be prevented. In the embodiment of FIG. 1, the present invention is applied to a TOCN meter, and in the embodiment of FIG.
Although the present invention is applied to the TN meter in the embodiment of FIG. 4, the present invention is not limited to these, and can be applied to a water quality analyzer equipped with an electric furnace or an ozone generator or both. .

[0028]

According to the present invention, in a water quality analyzer having a sample burning section, the temperature of the sample burning section when the power supply of the cooling fan and the ventilation fan is turned off after the power supply of the sample burning section is turned off is set. When the power-off operation is performed, the power supply of the sample burning unit is turned off by the power-off unit, the temperature of the sample burning unit is reduced, the temperature of the sample burning unit is monitored by the temperature measuring unit, and a preset value is set. When the temperature becomes lower than the temperature, the power of the cooling means and the ventilation means is also cut off, so that the operator simply turns off the power of the apparatus and stops the apparatus while suppressing the deterioration of the apparatus due to the residual heat of the sample combustion section. be able to. In a water quality analyzer equipped with an ozone generator, a time period is set from when the power of the ozone generator is turned off to when the supply of the ozone source gas to the ozone generator is stopped. Then, the power supply disconnecting unit turns off the power of the ozone generator, stops the generation of ozone, and removes ozone from the inside of the apparatus after a preset time has elapsed from the operation of turning off the ozone power. Since the supply of the ozone source gas from the source supply unit to the ozone generator is stopped, the operator simply stops the power supply of the apparatus and stops the apparatus while suppressing the deterioration of the apparatus due to the backflow of ozone. be able to. As described above, according to the present invention, it is possible to suppress the deterioration of the water quality analyzer after the power is turned off, and to reduce the operation of the operator after the power is turned off.

[Brief description of the drawings]

FIG. 1 is a schematic configuration diagram of one embodiment.

FIG. 2 is a flowchart illustrating an operation at the time of power off according to the embodiment.

FIG. 3 is a schematic configuration diagram of another embodiment.

FIG. 4 is a schematic configuration diagram of still another embodiment.

[Explanation of symbols]

 11 Sample Injection Mechanism 23 Sample Injection Unit 25 Combustion Tube 27 Electric Furnace 29 Sample Combustion Unit 33 Gas Purification / Flow Control Unit 39 Ozone Source Flow Path 41 Electromagnetic Valve 43 Ozone Generator 45 Cooling Fan 47 Temperature Sensor 49 Ventilation Fan 51 Dehumidification / Gas Processing Unit 53 Infrared gas detector 55 Chemiluminescence detector 57 Ozone decomposer 61 CPU 63 Control circuit 65 Power switch

──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. ⁷ Identification symbol FI Theme coat ゛ (Reference) G01N 31/12 G01N 31/12 B 33/18 33/18 B

Claims (3)

[Claims] With a 1. A solution sample is vaporized by thermal decomposition, and CO ₂ detector for detecting a sample combustion portion for converting the carbon component in the sample to CO _2, the CO ₂ in the sample vaporization gas,
In a water quality analyzer provided with a temperature measuring unit for measuring the temperature of the sample burning unit, a cooling unit for cooling the sample burning unit, and a ventilating unit for ventilating the inside of the apparatus, the cooling fan after turning off the power of the sample burning unit And the temperature of the sample combustion unit when the power supply of the ventilation fan is turned off is set. When the power supply is turned off, the power supply of the sample combustion unit is turned off, and the temperature from the temperature measurement unit is turned off. A water quality analyzer, comprising: a power cutoff unit that cuts off the power of the cooling unit and the ventilation unit when the temperature of the sample combustion unit falls below a preset temperature based on the information. 2. A sample combustion section for thermally decomposing and vaporizing an aqueous solution sample and converting a nitrogen component in the sample into NO,
In a water quality analyzer including a chemiluminescence detector that detects chemiluminescence generated by a reaction between ozone and NO in a sample vaporized gas, and an ozone generator that supplies ozone to the chemiluminescence detector, the ozone generator includes: After the power is turned off, the time until the supply of the ozone source gas to the ozone generator is stopped is set, and when the power is turned off, the power of the ozone generator is turned off, and further set in advance. A water quality analyzer, comprising: a power cut-off unit for stopping the supply of the ozone source gas from the ozone source supply unit to the ozone generator after a lapse of the set time. 3. A sample combustion section for thermally decomposing and vaporizing an aqueous solution sample and converting a target component in the sample into a detection component, and detecting chemiluminescence generated by a reaction between ozone and a detection component in the sample vaporization gas. Chemiluminescence detector, an ozone generator for supplying ozone to the chemiluminescence detector, a temperature measuring unit for measuring the temperature of the sample burning unit, a cooling means for cooling the sample burning unit, and ventilation for ventilating the inside of the apparatus In the water quality analyzer provided with means, the temperature of the sample combustion unit when the power supply of the cooling fan and the ventilation fan is turned off after the power supply of the sample combustion unit is turned off, and after the power supply of the ozone generator is turned off, The time until the supply of the ozone source gas to the ozone generator is stopped is set. When the power is turned off, the power of the sample combustion unit is turned off, and the temperature from the temperature measurement unit is turned off. Emotion Based on, the power is also cleavage of the cooling means and said ventilating means if the temperature below the temperature preset for the sample combustion portion, and,
When the power is turned off, the power of the ozone generator is turned off, and after a preset time has elapsed, the supply of the ozone source gas from the ozone source supply unit to the ozone generator is stopped. A water quality analyzer comprising a power cut-off part.