JP2002239301A - Fluorine distillation apparatus and washing apparatus therefor - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a fluorine distillation apparatus for performing fluorine distillation work at the time of fluorine distillation analysis prescribed in JIS K 0102. SOLUTION: The fluorine distillation apparatus is equipped with a steam flask 12 into which water is introduced, a heater 11 for heating the steam flask 12, a distillation flask 14 into which a sample and a reagent are introduced, a heater 13 for heating the distillation flask 14, a solenoid valve 24 provided to a line 23 for sending steam generated in the steam flask 12 to the distillation flask 14, a temperature sensor 18 for detecting the liquid temperation in the steam flask 12, a beaker 17 for storing the distillate from the distillation flask 14 and a level sensor 19 for detecting the liquid level in the beaker 17. When the temperature detected by the temperature sensor 18 reaches a set value, the solenoid valve 24 is opened to send the steam of the steam flask 12 to the distillation flask 14 and the heater 13 is controlled to control the liquid temperature in the distillation flask 14 so as to hold the same to the set value and work is stopped on the basis of the detection value of the level sensor 19.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

TECHNICAL FIELD The present invention relates to JIS K 01
The present invention relates to a fluorine distillation apparatus used in a fluorine distillation analysis for obtaining the concentration of fluoride ions in a fluorine compound specified in 02, and a cleaning apparatus for automatically cleaning the apparatus after the distillation.

[0002]

2. Description of the Related Art Conventionally, a fluorine distillation operation based on JIS K 0102 is performed as follows. That is,
An appropriate amount of a sample containing at least 30 μg of fluorine is placed in an evaporating dish or beaker, and 5 g of phenolphthalein is added to 50 parts of ethanol.
A few drops of a phenolphthalein solution diluted with 0 ml and 1 l of water are added, a sodium hydroxide solution obtained by adding 1 l of water to 100 g of sodium hydroxide is added to make the mixture slightly alkaline, and then the mixture is concentrated by heating to about 30 ml. .

[0003] Next, the concentrated solution in the evaporating dish or beaker is washed into a distillation flask 1 shown in FIG. 1 with about 10 ml of water, and then about 1 g of silicon dioxide, 1 ml of phosphoric acid and about 40 ml of perchloric acid.
Add 30 ml of the reagent specified in JIS K 8951 or 30 ml of sulfuric acid. Then, 20 ml of water is added to a full volume flask (not shown) of a receiver for receiving the distillate distilled out of the cooling pipe 2, and the lower end of the backflow stop (not shown) at the lower end of the cooling pipe is positioned below the water surface. Then, water is put into the steam flask 4 and heated by the heater 5.

[0004] Next, the distillation flask 1 is heated by the heater 6,
When the liquid temperature in the distillation flask reaches about 140 ° C., the cock 7 is opened, and steam is passed from the steam flask 4 into the liquid in the distillation flask and distilled while bubbling. The distilled gas that has been distilled is cooled through the cooling pipe 2 and distilled out into water in the total volume flask. Distillation temperature is 145 ± 5
C., the distillation rate was adjusted to 3 to 5 ml / min, and the distillation was continued until the liquid volume in the total volume flask reached 220 ml.

[0005] As described above, the distillation operation for obtaining a distillate for measuring the concentration of fluoride ions is performed. After the distillation operation, it is confirmed that the apparatus has cooled, and the cooling pipe 2 and the backflow stop are removed. Then, the inside of the cooling pipe 2 and the inside and outside of the backflow stopper are washed with a small amount of washing water, and the washing liquid is also added to the entire flask and further washed by adding water. Thereafter, the cooling pipe and the backflow stopper were assembled again, and the above-described distillation operation was repeated.

[0006]

As described above, in the conventional distillation operation, it is necessary to control the temperature of the heater 6 and operate the cock 7 while monitoring the temperature of the thermometer and the amount of liquid in the total volume flask during the distillation. However, it is difficult to control the temperature to maintain the distillation temperature at 145 ± 5 ° C. by adjusting the heater, and there is a danger of burns when contacting the flask or the heater, and it is also dangerous if the cock operation is incorrect. In addition, during operation, the temperature of the thermometer and the amount of liquid in the total volume flask must be constantly monitored, and the operation requires skill. In addition, washing after the distillation operation is performed manually, and furthermore, it is performed after confirming that the equipment has cooled, so that it takes time and effort.

A first object of the present invention is to provide a fluorine distillation apparatus which can solve the above-mentioned problems by automating the above-mentioned fluorine distillation operation. It is an object of the present invention to provide a washing apparatus capable of automatically washing the above-mentioned fluorine distillation apparatus after distillation.

[0008]

The invention according to claim 1 relates to a fluorine distillation apparatus which achieves the first object, and comprises a steam flask into which water is put, a first heating means for heating the steam flask, and a fluorine compound. And a second flask for heating the distillation flask.
Heating means, a solenoid valve provided in a line for sending steam generated in the steam flask to the distillation flask, a temperature sensor for detecting the liquid temperature of the distillation flask, and a distillation gas generated in the distillation flask and distilled from the distillation flask. A cooling pipe for cooling the container, a container for receiving a distillate distilled from the cooling pipe,
A level sensor for detecting the liquid level of the distillate in the container, a second heating means is controlled based on the temperature detected by the temperature sensor to perform temperature control, and a solenoid valve is controlled to perform distillation from the steam flask. Water vapor is supplied to the flask, and at least a solenoid valve, a first heating means, and a second heating means are provided by a detection signal when the liquid level of the distillate detected by the level sensor reaches a set value. And a sequencer for controlling the second heating means and stopping the heating.

The fluorine distillation in the present invention is performed as follows. With the water in the steam flask and the sample and the reagent made of the fluorine compound in the distillation flask, the first and second heating means are controlled by the sequencer to heat the steam flask and the distillation flask. The temperature of the liquid in the distillation flask is detected by a temperature sensor, and when the liquid temperature reaches the set temperature by heating the distillation flask, the sequencer opens the solenoid valve and sends the steam in the steam flask to the distillation flask, thereby discharging it from the distillation flask. The distilled gas thus cooled is cooled by the cooling pipe and distilled out into the container. The temperature of the liquid in the distillation flask is controlled so as to be maintained at the set temperature, and when the liquid level of the distillate in the container reaches the set level, the heating of the distillation flask is stopped.

According to the present invention, JIS K
Since the fluorine distillation operation at the time of performing the fluorine distillation analysis specified in 0102 can be automatically performed, the liquid temperature of the distillation flask and the liquid level of the distillate in the container are monitored.
Control the temperature so that the liquid temperature of the distillation flask is maintained at the set level, switch the cock that sends steam from the steam flask to the distillation flask when the liquid temperature reaches the set level, or perform distillate There is no need to stop the distillation operation when the liquid level reaches the set level, and it is not necessary to touch the apparatus during the operation, so that the risk of burns can be eliminated. Examples of the first and second heating means used in the present invention include a heater and a gas burner.

[0011] The invention according to claim 2 relates to the cleaning apparatus of the above-mentioned fluorine distillation apparatus, which achieves the second object. In the invention according to claim 1, a shower disposed in a distillation flask and the shower is provided. And a pipe for supplying a washing water to the apparatus and discharging the residual liquid in the distillation flask, a shower and a pump, and a pipe provided with an electromagnetic valve controlled by a sequencer. According to the present invention, the distillation flask is washed by spraying washing water from a shower.

[0012]

FIG. 2 is a schematic view of a fluorine distillation apparatus, and FIG. 3 is a schematic view of a cleaning apparatus. Each apparatus will be described in detail below.

[0013] As shown in FIG.
A steam flask 12 heated by a heater 11 as a heating means, a distillation flask 14 heated by a heater 13 as a second heating means, and a distillation tube 15 attached to the distillation flask 14 are detachably attached. Cooling pipe 16
And a beaker 17 as a container for receiving the distillate. The distillation flask 14 has a temperature sensor 18 for detecting the liquid temperature, and the beaker 17 has a level for detecting the liquid level of the distillate accumulated in the beaker. Lines 2 each of which is provided with a sensor 19 and supplies water to the steam flask 12
1, a solenoid valve 22 is provided. A line 23 for sending steam from the steam flask 12 to the distillation flask 14 is provided with a solenoid valve 24.
Further, a solenoid valve 26 is connected to a line 25 which branches off from the line 23 and discharges the distillation gas in the distillation flask 14 to the atmosphere.
Are respectively attached.

In the distillation operation, first, an appropriate amount of the sample is adjusted and placed in the distillation flask 14 based on JIS K 0102 as described above, and the reagent is added thereto to assemble the apparatus as shown in FIG. Thereafter, distillation is performed as follows.

FIG. 4 shows a control circuit of the sequencer. In this circuit, when a power switch 31 is turned on, a pilot lamp 32 is turned on. In this state, the start button 33 is pressed. Then, the relays R ₁ 34 and R
_{At the same} time, the timer T ₁ 36 starts counting and the solenoid valve 26 closes. At this time, the solenoid valve 22 is open and the solenoid valve 24 is closed.

When the relay R ₁ 34 is energized, the contact 37 of the relay R ₁ 34 closes to perform self-excitation, and the excitation of the relay R ₂ 35 closes the contact 38 to close the heater 11.
Starts heating of the steam flask 12. When the timer T ₁ 36 times out after the set time elapses, the contact 39
Is closed and the relay R ₃ 41 is excited, whereby the contact 4
2 is closed, the heater 13 starts heating the distillation flask 14, and the pilot lamp 43 of the heater 13 is turned on to indicate that the heater 13 is in a heated state.

The temperature of the distillation flask 14 heated by the heater 13 is measured by a temperature sensor 18. When the temperature approaches a set temperature, a temperature controller 45 controls opening and closing of a contact 46 to excite or demagnetize a relay R ₃ 41. Thus, the contact 42 is opened and closed, and heating or stopping of the heating by the heater 13 is performed. At the same time, the pilot lamp 43 is turned on or off.

When the liquid temperature of the flask 14 reaches the set temperature, the temperature controller 45 closes the contact 47. When the contact 47 is closed, it is energized the relay R ₄ 50 is thereby with contacts 40 are self-energized by closing the electromagnetic valve 22 is closed,
The solenoid valve 24 is opened, the supply of water to the steam flask 12 is stopped by closing the solenoid valve 22, and steam is sent from the steam flask 12 to the distillation flask 14 by opening the solenoid valve 24, and this is introduced into the liquid. Start the distillation while discharging and bubbling. The distilled distillation gas is cooled through the cooling pipe 16 and is distilled into a beaker containing a predetermined amount of water. After the start of the distillation, the distillation is continued while controlling the liquid temperature in the distillation flask 14 by the temperature controller 45. When the level of the distillate remaining in the beaker 17 reaches the set value and the level sensor 19 detects this, level detector 48 by the detection signal closes the contacts 49, to energize the relay _R 5 51. As a result, the switch 52 is switched, the relay R ₅ 51 is self-excited, the contact 53 is opened, the relays R ₁ , R ₂ 35 and R ₃ 41 are demagnetized, and the contacts 38 and 42 are opened to open the heaters. The heating of 11 and 13 is stopped. Then, the solenoid valve 26 is opened, and the distillation gas in the distillation flask 14 is released into the atmosphere.

The excitation of the relay R ₅ 51 causes the switch 52
Is switched, the solenoid valve 22 is opened to supply water to the steam flask 12, and the solenoid valve 24 is closed to stop the supply of steam from the steam flask 12 to the distillation flask 14. When the relay R ₅ 51 is excited,
Contact 54 closes and buzzer 55 sounds to signal the end of distillation. The stop of the buzzer 55 is performed by turning off the switch 56.

As shown in FIG. 3, the cleaning device includes a cleaning nozzle 58 disposed in the distillation flask 14, a tank 59 for storing the cleaning water, a suction of the cleaning water in the tank 59, and a cleaning nozzle 58 through a line 61. And the remaining liquid in the distillation flask 14 is discharged by the pump 62 through the line 23, the line 63, the line 61, and the line 64. Line 7 on the tank side from the connection point
A solenoid valve 65, a solenoid valve 66, a solenoid valve 67, and a solenoid valve 68 are provided on the line 0, the line 64, and the line 69 on the cleaning nozzle 58 side from the connection point with the line 64.
This apparatus is configured as described above, and the distillation flask 14 is washed as follows.

In the control circuit of the sequencer shown in FIG. 5, the excitation of the relay R ₅
1, 72 and 80 are closed and relay R ₆ 73 and relay R ₇
74 and relay R ₈ 86 are energized, thereby causing contact 7
5, 76 and 87 are each closed and self-excited, and the timer T ₂ 77 which has been set in advance starts counting. At the same time, the solenoid valves 66 and 67 open (the solenoid valves 65 and 68 are closed) and the relay R
₆ 73, the contact 78 is closed and the pump 62 is started, and the washing water sucked from the tank 59 is discharged through the lines 61 and 64, and the electromagnetic valves 66 and 67, the line 61,
The cleaning of the pumps 64 and 70 and the pump 62 is performed.

When the timer T ₂ 77 times out after the set time elapses, the contact 79 opens and the solenoid valve 67 closes, and the solenoid valve 68 opens, whereby the washing water sucked up from the tank 59 by the pump 62 is supplied to the line 70. ,
The remaining liquid in the distillation flask is supplied to the washing nozzle 58 via the line 61 and the line 69, and the temperature is lowered. The time out of timer T ₂ 77 also causes contact 81
Is closed and a preset timer T ₃ 82 starts counting. After the set time has elapsed, the timer T ₃ 82
Is timed out, the contacts 83 and 85 are closed, the contact 84 is opened, the solenoid valves 65 and 67 are opened, the solenoid valves 66 and 68 are closed, the residual liquid in the distillation flask 14 is sucked up by the pump 62, and the line It is discharged through 63, 61 and 64.

When the residual liquid in the distillation flask 14 is exhausted and the discharge is completed, the operator presses the button 88. Then
When the relay R ₉ 89 is energized, the timer T ₄ 94, which has been set in advance, starts counting. When the relay R ₉ 89 is excited, the contact 91 is closed and self-excited, and the contact 92 is opened. When the contact 93 is closed and the solenoid valve 65 is closed, the solenoid valve 66 is opened and the pump 62 is washed from the tank 59. Line 6
1. Cleaning of the pump 62 and the line 64 is performed.

When the timer T ₄ 94 times out after performing the cleaning for the set time, the contact 95 is opened and the relay R ₅ 73 is opened.
Is demagnetized, the contact 78 opens, and the pump 62 stops.
The washing of the distillation flask 14 is completed as described above.
After the cooling tube 16 and the distillation tube 15 are removed from the distillation flask 14, they are further separated, and the inside and outside are separately washed.
The same applies to beakers.

[0025]

According to the first aspect of the present invention, JIS
Since the fluorine distillation operation at the time of performing the fluorine distillation analysis specified in K0102 is automated, the monitoring operation for monitoring the liquid temperature of the distillation flask and the amount of the distillate in the container is not required. The operation of adjusting the second heating means so that the liquid temperature is maintained at the set level becomes unnecessary, and when the liquid temperature of the distillation flask reaches the set level, the steam of the steam flask is sent to the distillation flask. This eliminates the need for a cock operation, and eliminates the need to stop the distillation operation when the amount of distillate distilled out in the container reaches the set amount, thereby saving labor. Further, since there is no need to touch the apparatus during the distillation operation, the danger of burns can be eliminated.

According to the second aspect of the present invention, after the fluorine distillation operation is completed, the distillation flask can be automatically washed without removing the distillation flask.

[Brief description of the drawings]

FIG. 1 is a diagram showing a conventional fluorine distillation apparatus.

FIG. 2 is a schematic diagram of a fluorine distillation apparatus according to the present invention.

FIG. 3 is a piping diagram of a washing apparatus for a distillation flask.

FIG. 4 is a control circuit diagram relating to a fluorine distillation apparatus of a sequencer.

FIG. 5 is a control circuit diagram relating to a cleaning device of a sequencer.

[Explanation of symbols]

11, 13 · heater 12 · · steam flask 14 · · distillation flask 16 · · cooling tube 17 · beaker 18 · · temperature sensor 19 · · level sensor 22, 24, 26, 65, 66, 67, 68 · · Solenoid valve 31 Power switch 33 Start button 34, 35, 41, 50, 51, 73, 74, 86, 8
9. Relay 36, 77, 82, 94 Timer 45 Temperature controller Level detector 58 Cleaning nozzle 59 Tank 62 Pump

Claims (2)

[Claims] 1. A steam flask for holding water, a first heating means for heating the steam flask, a distillation flask for holding a sample made of a fluorine compound and a reagent, and a second heating means for heating the distillation flask. A solenoid valve provided in a line for sending steam generated in the steam flask to the distillation flask, a temperature sensor for detecting the liquid temperature of the distillation flask, and cooling for cooling the distillation gas generated in the distillation flask and distilled from the distillation flask. A pipe, a vessel for receiving a distillate distilled out of the cooling pipe, a level sensor for detecting a liquid level of the distillate in the vessel, and a second heating means controlled by the temperature detected by the temperature sensor. Control the temperature and control the solenoid valve to supply steam from the steam flask to the distillation flask, and distillate detected by the level sensor. A sequencer for controlling at least the second heating means of the solenoid valve, the first heating means and the second heating means and stopping the heating by a detection signal when the liquid level reaches the set value. A fluorine distillation apparatus, characterized in that: 2. A shower disposed in a distillation flask,
The pump according to claim 1, further comprising a pump for supplying washing water to the shower and for discharging residual liquid in the distillation flask, a pipe having an electromagnetic valve controlled by the shower and the pump, and a sequencer. Cleaning equipment for fluorine distillation equipment.