KR100882770B1 - Operation method of Kjeldahl distillation unit - Google Patents

Abstract

A kjeldahl evaporator and a method for operating the kjeldahl evaporator are provided to experiment in order to calculate nitrogen amount included in corresponding food required in case of calculating amount of the protein included in particular food product. A kjeldahl evaporator contains an analysis tube generating gas by dissembling a sample and injecting steam; a cooling device(115) connected in the analysis tube and cooling the gas generated from the analysis tube by cooling water flowing outside the cooling device; and a flask(110) taking away the condensated water connected to an end of the cooling device. A method for operating the kjeldahl evaporator includes an auto process mode, a command mode, a memory storage mode, a memory erase mode, a sensor mode and an RS-232C mode.

Description

KJELDAHL DISTILLATION APPARATUS AND METHOD FOR OPERATING THE SAME}

The present invention relates to a method of operating a Kjeldahl distillation apparatus, and more particularly, Kjeldahl distillation that can be carried out to calculate the amount of nitrogen contained in the food required to calculate the amount of protein contained in a particular food, etc. An apparatus and a method of operating the same.

In general, in order to determine the amount of protein contained in a particular food, the amount of nitrogen in the food is measured and calculated by multiplying the amount of nitrogen by a certain factor, which is an average of 16% nitrogen in the protein. In consideration of this, it is determined as 6.25 (100/16) (there is a slight difference in the type of food). This is called nitrogen coefficient, and the amount of nitrogen is multiplied by the nitrogen coefficient to calculate the protein amount. It is called crude protein. In addition, a micro Kjeldahl distilling apparatus is used as an experimental apparatus for calculating the amount of nitrogen contained in the sample for the calculation of the crude protein mass as described above. It is configured as shown, that is, steam generating flask (10), gas reservoir tube 20, distillation flask (30), cooling tube (40) and alcohol lamp (50), burette (60), clamping Means 70, tripod 80 and the like.

The steam generating flask 10 is formed as a round bottom flask and a funnel 12 having a cocking device 14 for supplying distilled water or the like is coupled to the top and discharged steam generated therein. The water vapor discharge pipe 16 is coupled, and the discharge end of the water vapor discharge pipe 16 is connected to one end of the generation gas retention pipe 20 by a connection tube 18 and is formed inside the generation gas retention pipe. In communication with the tube (22).

The generator gas retention tube 20 has a sample injection tube 22 having one end in communication with the steam discharge tube 16 and the other end inserted into the distillation flask 30 in the cylindrical appearance, and the sample injection tube A funnel 22 equipped with a cock device 24 is integrally formed at the upper end of the 22 and an ammonia (NH₃) outlet 26 communicating with the distillation flask 20 is formed on the outer surface. Is formed.

And the ammonia outlet 26 is connected to the cooling tube 40 via the connecting tube 27, the cooling tube 40 is a cooling inner tube 42 which is integrally connected to the connecting tube 27 and The cooling casing 44 is formed to have a double tube form on the outside of the cooling inner pipe 42, and the cooling water inlet 46 includes a cooling water inlet 46 through which cooling water is introduced and cooling water introduced therein. A discharge unit 48 is formed to allow inflow and discharge of the cooling water to cool the ammonia that is moved to the cooling inner tube 42.

In addition, the respective devices are fixedly installed at a suitable height and spacing by a plurality of clamping means 70 installed on the burette 60, the steam generating flask 10 is mounted on an alcohol lamp 50 mounted on a tripod By heating.

On the other hand, the experimental process for calculating the amount of nitrogen contained in the sample by the micro Kjeldahl distilling apparatus configured as described above is a general one, so briefly explaining the process, first to decompose the sample to be tested through the decomposition process When the decomposition is completed, the distillation process is performed by a distillation apparatus, and the titration is calculated using the amount of the titrant (NaOH) through titration, and the crude protein mass is obtained by multiplying the calculated nitrogen by the protein nitrogen coefficient.

That is, an appropriate amount of the sample is added to the flask, a decomposition accelerator and sulfuric acid are added, heated to a specific color, cooled, and the sample is decomposed. Then, distilled water is added to the decomposed sample to the distillation flask 30. Water vapor generation flask

Distilled water and a small amount of sulfuric acid are added to (10) and heated, while sulfuric acid is added to the collecting triangular flask 90 at the lower end of the cooling tube 40. In such a state, the water vapor discharged from the steam generating flask is introduced into the distillation flask 30 through a connection pipe to perform a distillation process to cause a distillation reaction. In this process, the fluid collected in the triangular flask 90 for collecting is transferred to a titrator to perform a titration process with a titrant and to obtain an amount of a titrant until a constant color is obtained.

However, the conventional micro Kjeldahl distilling apparatus (Micro kjeldahl distilling apparatus), as described above, the steam generating flask 10, the gas gas retention tube 20, the distillation flask 30, the cooling tube 40 and the alcohol lamp (50). ) And a tripod 80, a plurality of clamping means 70, etc. should be provided, the structure is complicated, the manufacturing process is complicated, there is a problem that the production cost is increased and productivity is reduced, in particular the volume in the assembled state Due to the very large production, transportation and storage process is very difficult and easily broken.

In addition, since each component must be installed on the burette stand 60 by the respective clamping means 70, the experiment preparation process is complicated and takes a lot of time, so the efficiency is reduced in the experiment, and the post-organization arrangement process is also very difficult. There was this.

In addition, the conventional micro Kjeldahl distillation apparatus uses the alcohol lamp 50 for the heating of the steam generating flask 10 is required to adjust the height of the steam generating flask in the test process, and the tripod 80 and the like to adjust the height of the flame In addition to the problems that must be equipped, there was a problem in the safety of the fire or the experimenter burns due to the fall of the alcohol lamp.

The present invention is to solve the above problems, the purpose of the structure is simple and the volume is reduced to reduce the production cost and improve the productivity, easy to transport and storage, can be easily performed experiments In addition, to provide a method of operating the Kjeldahl distillation apparatus to improve the safety in use.

Still another object of the present invention is to provide a method of operating a Kjeldahl distillation apparatus in which the experiment can be performed automatically or manually.

Still another object of the present invention is to provide a method of operating a Kaldal distillation apparatus for performing an experiment according to a program.

According to the present invention, a decomposition tube in which a sample is introduced and decomposed, wherein the decomposition tube includes a caustic soda inlet, and a decomposition tube for decomposing and steam-injecting a sample by connecting steam and water inlets; A cooler, comprising: a cooler communicating with the decomposition tube and cooling gas generated from the decomposition tube by cooling water flowing outside the cooler; And a flask connected to the end of the cooler to collect the cooled condensate.

Preferably, the boric acid inlet for boric acid input is connected to the condensate collection flask.

Preferably, the Kjeldahl distillation apparatus of the present invention is characterized in that it further comprises a control unit for controlling the supply of the caustic soda, steam and water, boric acid.

According to the present invention, the method of operating the Kjeldahl distillation apparatus described above includes an automatic processing menu for automatically inputting data values and setting a program after semi-automatically working a sample, wherein: a) in the flask; Adding a suitable amount of boric acid, b) adding water and caustic soda to the decomposition tube, c) stopping the addition of caustic soda in step b), and the reaction time is displayed on the sample at the same time. Step, d) performing distillation by adding steam to the decomposition tube when the reaction is completed, e) removing wastewater from the decomposition tube when distillation is completed, f) operating time to date It includes a step of displaying on the display window and automatically saving to the empty address.

According to the present invention, the method of operating the Kjeldahl distillation apparatus described above includes a manual processing menu for setting a program by directly inputting data values after working a sample semi-automatically, in which a) displaying a memory mode. B) selecting a desired number using a mode key, c) checking a location using an up / down key, and then adjusting a time using a numeric button.

delete

delete

delete

delete

By implementing the present invention, the structure is simple and the volume is reduced to reduce the production cost and increase the productivity, easy to carry and store, easy to perform experiments as well as to improve the safety in use Kjeldahl It is possible to provide a method of operating a distillation apparatus.

In addition, it is possible to provide a method of operating a Kjeldahl distillation apparatus capable of performing the experiment automatically or manually.

In addition, it is possible to provide a method of operating the Kaldal distillation apparatus for performing the experiment according to the program.

Hereinafter, exemplary embodiments of the present invention will be described with reference to the accompanying drawings. However, the present embodiment is for convenience of description of the invention and is not intended to limit the invention to this embodiment. It can be seen that the technical idea of the present invention is limited only by the claims described below.

2 is a view showing a schematic configuration of a Kaldal distillation apparatus according to the present invention.

Each component of the Kjeldahl distillation apparatus of the present invention, 101 is a glass door of the apparatus, 102 is a caustic soda (NaOH) inlet, 103 is a steam and water inlet, 104 is a decomposition tube. 105 is the Viton-Con, 106 is the test tube and 107 is the test tube clamp. 108 is a leak base, 109 is a boric acid inlet, and 110 is a Erlenmeyer flask. 111 is a steam induction tube, 112 is a coolant outlet, and 113 is a coolant inlet. 114 is a control part, 115 is a cooler. In addition, a bucket, a boric acid tank, a caustic soda tank, a wastewater tank, water, a boric acid, a caustic soda, a wastewater level control sensor, etc. are provided.

Referring to the operation of the Kjeldahl distillation apparatus of the present invention configured as described above are as follows.

When the device is to be used initially, the screen of the control device is in an initial state as shown in FIG. The glass door 101 of the device of the present invention is opened and a test tube, ie an empty dissolution tube, is mounted. Then set the program to use on the initial screen. At first it may be stable to memorize the program using the semi-automatic mode.

The device can set the program in two ways. In other words,

The first is to work with the sample sample semi-automatically and then enter the data values automatically.

In this method, the manual is first selected on the screen of Fig. 3 and then the enter key is pressed. At this time, the next step is prepared after the automatic sensor check.

Then press the Enter or Bor key to add an appropriate amount (5 ml per second) of boric acid to the Erlenmeyer flask and press again to stop. If the amount of boric acid is not enough, press ESC key to add more.

Press enter or caustic soda to add water and caustic soda. If you stop adding caustic soda, the reaction will begin automatically and the reaction time will appear.

When the reaction is completed, press enter key to generate steam and start distillation.

When the distillation is completed, press the enter key again to end the work, remove the Erlenmeyer flask and press the enter key to remove the waste water from the digestion tube.

When the cleaning is completed, the work time up to now is displayed on the LCD window, and when you press the Enter key, it is automatically saved in the empty address starting from 00. At this time, if all are saved as program, it is automatically saved at 99 or at the selected number. Pressing any other key automatically destroys the working data value.

After saving, press ESC key to display the initial screen.

The second is to enter the program directly.

After selecting M-Save Mode in the initial state of Fig. 3, pressing the entry key will display the memory mode.

Select the desired number using the mode key.

After confirming the position using the up / down keys, adjust the time (59 minutes 59 seconds) using the number buttons.

The metering pump is 5 ml per second.

Pressing the entry key will automatically save and display the initial screen.

If you press the Enter key after selecting a program in this way, you will be prompted to wait until Steam is ready.

After waiting, you are ready to start working.

Now, a method of operating the apparatus of the present invention on the menu will be described.

First, auto-P is a menu that automatically selects one of the 100 experimental procedures stored in the memory and automatically processes it. In this menu, all you have to do is to select the required task and press the button.

In this automatic processing, it is possible to process the same experiment repeatedly with the inputted experimental results, so that the same experiment can be processed without errors, and other experiments can be prepared while the experiment is in progress, so that the user's convenience can be achieved.

After all the treatment is finished, after removing the result, press the Enter key to perform the waste water treatment and the tube cleaning process and can be repeated.

Next, manual processing (Manual) is a menu for manually processing the experiment process. The required sample can be adjusted to the amount desired by the user and can be partially processed. Manually processed processes can be stored in memory, or partially processed. Manually processed processes can be stored in memory and used in the automatic processing menu as described above.

 Next is the M-Save menu, which modifies, edits and stores the stored memory. It is a menu that simply handles the stored workflow without experimenting repeatedly. It can memorize and edit the new workflow. Similar experiments can be stored in a single experiment, reducing the number of repeated experiments by the user.

The memory clear (M-Clr) menu is a menu for initializing the EEPROM. The EEPROM is automatically initialized the first time the device is used, but it is used when the user erases all stored contents. Deleted content cannot be recovered.

The sensor menu is a menu for determining whether or not to use the automated sensor used in the present apparatus. Once stored, it is stored in the EEPROM, so there is no inconvenience to set it again every time.

The last menu is the RS-232C menu, which communicates using the computer's RS-232C serial port. The contents stored in the memory can be moved to the computer, and the new contents can be stored on the computer, thereby adding convenience to the user.

After performing the work using the device of the present invention, the cleaning program must be executed and stored. For internal cleaning, an automatic program is set up for cleaning. As shown in Figure 4, to select the conditions for washing, the water is put into the decomposition tube by using a pump for about 25 seconds, and the washing is performed by generating steam for about 7 minutes. If the inside of the digestion tube is heavily contaminated, 10 ml of sulfuric acid can be added to the cleaning program.

Hereinafter, the detailed execution process of the program is as follows.

5 to 8 illustrate a manual execution process of a device according to the present invention.

As can be seen in Figure 5, Manual 2 is selected to execute the program manually (step 510). Then press the Enter key to open the window for boric acid input.

Pressing the Bor or Enter key in this window will turn OFF to ON and begin supplying the boric acid solution. The Esc button then proceeds to the process termination process (step 520).

If the enter button is pressed in the process termination process, the process ends, and if the Esc button is pressed, the process returns to the process again (step 530).

In the boric acid input process 520, if Bor or the enter key is pressed without pressing the Esc button, boric acid is continuously supplied. When boric acid is properly supplied, press the Bor or Enter key to proceed to the next step. At this time, if the Esc key is pressed, the process goes back to the end of the process (step 540).

In step 550, pressing the enter key proceeds to the next process, and pressing the Esc key returns to step 520 to perform the boric acid supply process again.

Fig. 6 is a diagram illustrating a manual execution process of the device according to the present invention.

Step 610 following step 550 is a process of adding water. Pressing the Wat or Enter key once in step 610 will turn OFF to ON in the window and the water will be supplied. Subsequently, pressing the Esc key proceeds to the end of the process (step 620). In step 620, pressing the enter key ends the process, and pressing the Esc button returns to the process again.

Pressing the Wat or Enter key while the window is turned ON in step 610 moves to the next step (step 630). In step 630, when water is properly added, press the Wat or Enter key and proceed to the next step. Pressing the Esc button at this point proceeds to the end of processing (step 620). Pressing the Enter key in step 620 terminates the process, and pressing the Esc button returns to the process (step 630).

Pressing the Wat or Enter key while the window is turned ON in step 630 proceeds to step 640. In step 640, the user presses the Enter key to proceed to the next step, and pressing the Esc button returns to step 610 to execute the water input process again.

Pressing the Enter key in step 640 proceeds to step 650, which is a caustic soda injection process. Pressing the Sod or Enter key once in step 650 turns the window OFF to ON and starts adding caustic soda solution. Pressing the Esc button at this point proceeds to the end of processing (step 620). Instead, pressing the Sod or Enter key moves to the next step (step 660).

In step 660, if the amount of caustic soda is properly added, press the Sod or Enter key and proceed to the next step (step 670). On the other hand, if the Esc button is pressed, the process proceeds to the process termination step (620).

In step 670, pressing the enter key proceeds to the next process, and pressing the Esc button returns to the caustic soda supply process (step 650).

7 is a diagram illustrating a manual execution process of a device according to the present invention.

Step 710 is a step illustrating a reaction time setting process. In step 710, the reaction time (Reac Time) is automatically increased. After watching the chemical reaction, it is time to press the Enter key to proceed to the next step (step 730). At this time, if the Esc key is pressed, the process goes to the end of the process (step 720).

In the process termination process (step 720), press the enter key to terminate the process, press the Esc button to return to the process process (step 710).

Pressing the enter key in step 710 proceeds to the steam supply time setting process (step 730), the steam time is automatically increased as the steam is supplied. Pressing the enter key stops the steam supply and proceeds to the next process (step 740). On the other hand, if the Esc button is pressed in step 730, the process goes to the end of the process (step 720).

Pressing the Enter button in step 740 proceeds to the suction process (step 750), and pressing the Esc button proceeds to the process end process (step 720).

Step 750 is a suction time setting process, in which the suction is activated and the suction time is automatically increased. Pressing the enter key then stops the suction and proceeds to the next process (step 760). On the other hand, if the Esc key is pressed, the process goes to the end of the process (step 720).

Step 760 is a data storage process, in which time is shown for each process. Then press Enter to go to the save confirmation page. At this time, if you press Esc or other button, the processing ends and you are moved to the first page.

When the enter key is pressed in step 770, the data on the page is saved and the page goes to the first page. At this time, press the Esc key to proceed to the end of processing. In this manner, a manual program process is performed.

8 is a diagram illustrating an automatic program process.

If No. 1 is selected on the initial screen, an auto program process (Auto-P) is selected (step 810). Then press Enter to go to the next step.

Step 820 and below are the selection and execution of the stored data. Press the up / down button to view the stored data in step 820 and press the enter key to proceed to the next step.

 In step 830, press the up / down button to view other data, or press the enter button to execute the current data. If you press the enter button once again, it moves to the next step, and if you press the Esc button, the process ends.

In step 840, the experiment is automatically run with the selected current data. When the reaction process is complete, proceed to the next step. Press the Esc button to end the process.

Pressing the enter key in step 840 proceeds to the next step, where processing ends in step 850, where pressing the enter key once again proceeds to the suction process.

Then, in step 850, the suction is executed for the set time and returns to the beginning. If you do not want to run the suction, press the Esc button. If you press the Enter key, you will move to the next step and go to step 840. In this way, an automatic program execution process is performed.

9 is a diagram illustrating a memory storage execution process of the apparatus according to the present invention.

When number 3 is selected on the initial screen, the M-Save process is selected. Then press the enter key to move to the next step (step 910).

In step 920, the selected memory data is stored.

10 is a diagram illustrating a memory deletion execution process of a device according to the present invention.

If you select No. 4 on the initial screen, the process of deleting memory is selected. Pressing the enter key next moves to the next step (step 1010).

In step 1020, the enter button is pressed to delete the stored data. At this time, the entire data will be deleted. To return to the beginning, press the Esc button.

11 is a diagram illustrating a sensor setting process of the apparatus according to the present invention.

If you select 5 on the initial screen, the sensor setup process is selected. Pressing the enter button then moves to the next step (step 1110).

In step 1120, a sensor is set. When each number is pressed on the number plate, ON and OFF are repeated. The sensors operate according to whether or not an external sensor is attached.

12 is a diagram illustrating an external communication execution process of the apparatus according to the present invention.

Selecting No. 6 on the initial screen selects external communication execution (RS232) (step 1210). Then, when the enter key is pressed, a communication program is executed in step 1220. To do this, first, the device of the present invention is connected to the RS232 of the PC by a cable. In this way, control is performed by a program supplied to the PC.

Press the Esc button to return to the beginning.

13 is a view schematically showing a program for communication in the process of performing external communication of the apparatus according to the present invention.

When reading data stored in the distillation apparatus of the present invention, the lead button is pressed. After importing the data, write the title within 15 letters.

To change the time, simply change the minutes and seconds.

Once everything has been saved, press Save to save it to your device.

1 is a view showing the configuration of a conventional semi-micro Kjeldahl distillation apparatus.

Figure 2 shows a schematic configuration of a Kaldal distillation apparatus according to the present invention.

Figure 3 is a view showing the initial state of the control window of the Kjeldahl distillation apparatus according to the present invention.

Figure 4 shows the conditions for washing the decomposition tube in the Kjeldahl distillation apparatus according to the present invention.

5-8 illustrate a manual execution of a device in accordance with the present invention.

Figure 9 illustrates a memory storage execution process of the device according to the present invention.

10 is a diagram illustrating a memory erase execution process of a device according to the present invention.

11 is a diagram illustrating a sensor setting process of the device according to the present invention.

12 illustrates a process of executing external communication of a device according to the present invention.

Figure 13 schematically illustrates a program for communication in the course of executing an external communication of a device according to the present invention.

* Description of the symbols for the main parts of the drawings *

101: glass door 102: caustic soda opening

103: steam and water inlet 104: decomposition tube

105: Viton-con 106: test tube

107: test tube clamp 108: leak support

109: boric acid inlet 110: Erlenmeyer flask

111: steam induction pipe 112: cooling water outlet

113: coolant inlet 114: keyboard

115: cooler

Claims (9)

delete delete delete A decomposition tube in which a sample is introduced and decomposed, wherein the decomposition tube is connected to a caustic soda inlet, and a vapor and water inlet to decompose and steam the sample to generate gas, and the decomposition tube communicates with the decomposition tube. And a condensate collection flask connected to an end of the cooler to collect cooled condensate, a condensate collection flask connected with boric acid inlet for boric acid input, and the caustic. In the operating method of the Kjeldahl distillation apparatus comprising a control unit for controlling the supply of soda, steam, water, boric acid, It includes an automatic processing menu that sets up the program by automatically entering data values after the sample has been semi-automatically operated. a) injecting an appropriate amount of boric acid into the flask, b) injecting water and caustic soda into the decomposition tube; c) starting the reaction to the sample at the same time when stopping the addition of caustic soda in step b), and displaying the reaction time; d) performing distillation by adding steam to the decomposition tube when the reaction is completed, e) removing wastewater from the cracking tube when distillation is finished, and f) displaying a working time to the present on the display window of the control unit and automatically storing the empty address. A decomposition tube in which a sample is introduced and decomposed, wherein the decomposition tube is connected to a caustic soda inlet, and a vapor and water inlet to decompose and steam the sample to generate gas, and the decomposition tube communicates with the decomposition tube. And a condensate collection flask connected to an end of the cooler to collect cooled condensate, a condensate collection flask connected with boric acid inlet for boric acid input, and the caustic. In the operating method of the Kjeldahl distillation apparatus comprising a control unit for controlling the supply of soda, steam, water, boric acid, It includes a manual processing menu for setting a program by directly inputting data values after the sample is semi-automatically operated. a) displaying the memory mode, b) selecting the desired number using the mode key, and c) operating the Kjeldahl distillation apparatus comprising the step of adjusting the time using the numeric buttons after confirming the position using the up / down keys. delete delete delete delete

Images