KR101761216B1 - An analysis apparatus for total phosphorus or total nitrogen capable of reducing constant injection error rate of a sample and an analysis method for total phosphorus or total nitrogen using the same - Google Patents

Abstract

The present invention relates to a total phosphorus or total nitrogen measuring device and a total phosphorus or total nitrogen measuring method using the same. More particularly, the present invention relates to an apparatus for measuring total phosphorus or total nitrogen contained in a sample, The present invention relates to a total nitrogen or total nitrogen measuring device and a total nitrogen or total nitrogen measuring method using the same. To this end, the total phosphorus or total nitrogen measuring device includes a sample and reagent supply unit for supplying the sample and the reagent to be measured; A sample and reagent supply pump for transferring a sample and reagent supplied from the sample and reagent supply unit in a fixed amount; An oxidation reaction tank for preheating the transferred sample by pressurization heating; A mixing tank transfer pump for transferring the pretreated sample in the oxidation tank; A mixing tank for diluting and mixing the pretreated sample, the diluted water and the pretreated sample supplied with the reaction reagent; A detector transfer pump for transferring diluted and mixed samples to a detector in a mixing chamber; A detector for measuring the concentration of total phosphorus or total nitrogen contained in the sample; And a 3-way valve disposed downstream of the sample supply pump for supplying the sample to the oxidation reaction tank or the mixing tank.

Description

TECHNICAL FIELD [0001] The present invention relates to a total phosphorus or total nitrogen measuring device capable of reducing a quantitative injection error rate of a sample, and a total phosphorus or total nitrogen measuring method using the same. [0002] TOTAL PHOSPHORUS OR TOTAL NITROGEN USING THE SAME}

The present invention relates to a total phosphorus or total nitrogen measuring device and a total phosphorus or total nitrogen measuring method using the same. More particularly, the present invention relates to an apparatus for measuring total phosphorus or total nitrogen contained in a sample, The present invention relates to a total nitrogen or total nitrogen measuring device and a total nitrogen or total nitrogen measuring method using the same.

In general, phosphorus (P) and nitrogen (N) components are known to be the main cause of the rapid growth of algae in the summer due to eutrophication.

The eutrophication (eutrophication) is a process in which nutrients (nitrogen, phosphorus) are released into water by flowing salts such as nitrate, ammonia and phosphate into rivers, rivers and lakes and the growth of phytoplankton And breeding proceeds very quickly, causing a large amount of phytoplankton to grow in a short period of time, resulting in a red tide phenomenon that turns into sour blue.

Such eutrophication reduces the value of aesthetics of rivers or streams due to the growth of attached algae, and when water of river or stream is used as a monastery, it closes the filter paper in the production of tap water, It is also a cause.

In addition, high-grade fish species disappear and fishes with low economic value become large, and when large algae or aquatic plants are killed, they are rapidly decomposed to generate odors, consume a large amount of dissolved oxygen, It produces detrimental substances that affect the quality of the water.

(N), phosphorus (P), iron (Fe), magnesium (Mg), potassium (K), sodium (Na), sulfur (S) (Mo), cobalt (Co), manganese (Mn), zinc (Zn), copper (Cu) and the like are required in addition to the inorganic carbon (P) and nitrogen (N).

Therefore, a water quality measurement system is being used to measure the amount of phosphorus (P) and nitrogen (N) contained in water for continuous water quality management in consideration of the self-sufficiency of the river.

However, in the conventional total phosphorus and total nitrogen measurement apparatuses, since the sample to be injected is injected by the rotary pump and the pump and the valve are used for each contact point of each flow channel, the pumping capacity There is a problem in that it is difficult to inject the sample in a fixed amount, and it is troublesome to correct each pump when the pumping capacity error of each pump occurs, and the installation cost is also increased because each pump has a pump there was. In addition, when the oxidation reaction tank of the conventional apparatus is used in an alkaline state, corrosion occurs and the container melts. As a result, the use period of the oxidation reaction tank is only about six months, and the heating tank is periodically replaced.

Therefore, there is a demand for development of a technique capable of improving the durability of the oxidation reaction tank by minimizing the error of the measurement value by quantitatively injecting the sample.

Korean Registered Patent No. 10-1588798

SUMMARY OF THE INVENTION The present invention has been made to solve the above problems, and it is an object of the present invention to reduce the injection error rate of a sample to improve the reliability of a total phosphorus or total nitrogen concentration measurement value included in a sample, And a total nitrogen or total nitrogen measurement method using the same.

These and other objects and advantages of the present invention will become apparent from the following description of a preferred embodiment.

The above objects are accomplished by a reagent supply system comprising: a sample and reagent supply unit for supplying a sample to be measured and a reagent necessary for measurement; A sample and reagent supply pump for transferring a sample and reagent supplied from the sample and reagent supply unit in a fixed amount; An oxidation reaction tank for heating and pretreating the transferred sample and the reagent; A mixing tank transfer pump for transferring the pretreated sample in the oxidation tank; A mixing tank for diluting and mixing the pretreated sample, the diluted water and the pretreated sample supplied with the reaction reagent; A detector transfer pump for transferring diluted and mixed samples to a detector in a mixing chamber; A detector for measuring the concentration of total phosphorus or total nitrogen contained in the sample; And a 3-way valve disposed at the rear end of the sample and reagent supply pump for supplying the sample to the oxidation reaction tank or the mixing tank.

Preferably, the sample and reagent supply unit is provided with a multi-channel valve to selectively supply one or more samples, and can supply reagents necessary for the pretreatment and color reaction, and the sample and reagent supply pump is provided within the pump A predetermined amount of sample can be transferred by controlling the number of revolutions of the motor.

Preferably, the oxidation reaction tank further comprises: a chamber capable of receiving the transferred sample; And a heating module surrounding the chamber, wherein the chamber may be formed of a dual structure including an outer tube and an inner tube, the heating module including: a heater for heating the chamber; And a temperature sensor for measuring the temperature inside the chamber.

Preferably, the 3-way valve has a first port, a second port and a third port, the first port being connected to the oxidation reaction tank, the second port being connected to the sample and reagent supply pump, Can be connected to the mixing tank.

The above object may also be accomplished by a method for measuring total phosphorus or total nitrogen using the total phosphorus or total nitrogen measuring apparatus described above, comprising the steps of: a) supplying a sample and a reagent to be analyzed to a oxidation reaction tank; b) a pretreatment step in which the sample is heated in the oxidation reaction tank and pretreated; c) mixing the pretreated sample with diluting water and a reaction reagent; And d) a detection step of measuring the concentration of total phosphorus or total nitrogen contained in the sample.

Preferably, the sample and reagent supply step (a) includes a first step (a-1) of supplying the sample up to the 3-way valve and removing the air filled in the front end and the rear end flow path of the sample and reagent supply pump; A second step (a-2) of supplying the sample into the oxidation reaction tank; A third step (a-3) of supplying air through the sample and reagent supply unit to drain the sample filled in the flow path between the sample and reagent supply unit and the 3-way valve; And a fourth step (a-4) of supplying air through the sample and reagent supply unit to supply the sample filled in the flow path between the 3-way valve and the oxidation reaction tank into the oxidation reaction tank.

Preferably, the mixing step (c) comprises a first step (c-1) of diluting and cooling the sample by mixing the pretreated sample with dilution water; And a second step (c-2) of mixing the diluted and cooled sample with the reaction reagent.

According to the present invention, it is possible to remarkably reduce the injection error rate of the sample, thereby improving the reliability of the total phosphorus or total nitrogen concentration measurement value contained in the sample.

Further, the structure of the oxidation reaction tank can be improved to easily replace the oxidation reaction tank, and the durability can be improved, so that the maintenance and repair cost of the equipment can be reduced.

However, the effects of the present invention are not limited to the above-mentioned effects, and other effects not mentioned can be clearly understood by those skilled in the art from the following description.

1 is a schematic view of a total phosphorus or total nitrogen measuring device according to an embodiment of the present invention.
FIG. 2 is a schematic view showing a front face (a), a side face (b), and an upper face (c) of the oxidation reaction tank according to an example.
3 is a schematic illustration of a vertical section (a) and a top surface (b) of a chamber according to an example.
FIG. 4 is an enlarged schematic view of a vertical section and an inner tube of the chamber according to an example.
5 is an enlarged view schematically showing a part of part A in Fig.
Figure 6 is a schematic representation of a detector according to an example.
7 is a schematic view illustrating a total phosphorus or total nitrogen measurement method using a total phosphorus or total nitrogen measurement apparatus according to an embodiment of the present invention.

Hereinafter, the present invention will be described in detail with reference to embodiments and drawings of the present invention. It will be apparent to those skilled in the art that these embodiments are provided by way of illustration only for the purpose of more particularly illustrating the present invention and that the scope of the present invention is not limited by these embodiments .

Also, unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains and, where contradictory, Will be given priority.

In order to clearly illustrate the claimed invention, parts not related to the description are omitted, and like reference numerals are used for like parts throughout the specification. And, when a section is referred to as "including " an element, it does not exclude other elements unless specifically stated to the contrary. In addition, "part" described in the specification means one unit or block performing a specific function.

In each step, the identification code (first, second, etc.) is used for convenience of explanation, the identification code does not describe the order of each step, and each step does not explicitly list a specific order in the context May be performed differently from the above-described sequence. That is, each of the steps may be performed in the same order as described, or may be performed substantially concurrently or in the reverse order.

1 is a schematic view of a total phosphorus or total nitrogen measuring device 10 according to an embodiment of the present invention. 1, a total phosphorus or total nitrogen measurement apparatus 10 according to an embodiment of the present invention includes a sample and reagent supply unit 100 for supplying samples and reagents to be measured; A sample and reagent supply pump 200 for transferring a sample and a reagent supplied from the sample and reagent supply unit 100 in a predetermined amount; An oxidation reaction tank 300 for heating and pretreating the transferred sample; A mixing tank transfer pump 400 for transferring the pretreated sample in the oxidation tank 300; A mixing tank 500 for diluting and mixing the pretreated sample, the diluted water, and the pretreated sample supplied with the reaction reagent; A detector 700 transfer pump 600 for transferring the diluted and mixed sample in the mixing tank 500 to the detector 700; A detector 700 for measuring the concentration of total phosphorus or total nitrogen contained in the sample; And a 3-way valve 800 disposed at the rear end of the sample supply pump for supplying the sample to the oxidation reaction tank 300 or the mixing tank 500.

Conventional gun or total nitrogen measuring apparatuses have limited their ability to inject a sample in a fixed amount due to the air filled in the flow path during the initial sample injection. However, since the three-way valve 800 is provided at the front end of the oxidation reaction tank 300, it is possible to effectively remove air, which is a problem in the initial injection, The reliability of the measured value can be improved.

In one embodiment, the sample and reagent supply unit supplies a sample to be measured and a reagent necessary for measurement, and may include a multi-channel valve 110 to selectively supply one or more samples. Specifically, the supply path connected to each of the plurality of valves and the main flow path through which the sample supplied from each supply path is included, so that one or more samples to be measured can be selected and sequentially supplied. In addition, not only the sample but also the sample and reagent supply unit 100 may be connected to various storage containers to supply the pretreatment reagents required for achieving the measurement purpose, distilled water and air necessary for washing, diluting, and cooling the reaction reagent.

In one example, when the concentration of total phosphorus is to be measured from a sample, the sample and reagent supply unit 100 may be a sample, as well as air, distilled water, phosphorus (P) standard solution, ascorbic acid, potassium persulfate, ammonium molybdate (N) standard solution, zero standard solution, alkaline potassium persulfate, hydrochloric acid, and the like can be supplied as well as the sample when measuring the total nitrogen.

In one embodiment, the sample and reagent supply pump 200 is for transferring samples and reagents supplied from the sample and reagent supply unit 100 to the oxidation reaction tank 300 or the mixing tank 500 at the subsequent stage, And the number of revolutions of the motor provided in the reagent supply pump 200 can be controlled to supply a predetermined amount of sample or reagent.

In one embodiment, the oxidation reaction tank 300 can be heated by pretreating the sample transferred through the three-way valve 800. FIG. 2 is a schematic view of a front surface (a), a side surface (b), and an upper surface (c) of the oxidation reaction tank 300 according to an exemplary embodiment of the present invention. A chamber 310 capable of receiving a sample and a reagent necessary for measurement, and a heating module 320 surrounding the chamber 310.

FIG. 3 is a schematic view of a vertical section (a) and a top section (b) of the chamber 310 according to an exemplary embodiment. Referring to FIG. 3, the chamber 310 receives a sample and a reagent And a double structure including an outer tube 312 and an inner tube 311 can be formed. The chamber 310 may be manufactured in various shapes and is preferably formed in a cylindrical shape, but is not limited thereto.

The outer tube 312 may be made of stainless steel (SUS). When the outer tube 312 is made of a stainless steel material, when the chamber 310 is heated by the heating module 320, the heat transfer is well performed and the sample in the chamber 310 can be effectively heated (pretreated). That is, the pretreatment efficiency of the sample can be increased.

The inner tube 311 may be formed of a polytetrafluoroethylene (PTFE) coating layer. Teflon is chemically inert because it forms a very stable compound due to strong chemical bonding between fluorine and carbon, and has properties such as heat resistance, corrosion resistance, non-stickiness, excellent insulation stability, and low coefficient of friction. Therefore, even when potassium alkaline persulfate is injected into the chamber 310 together with the sample to be heated, corrosion of the chamber 310 can be prevented, so that the service life of the chamber 310 can be extended. It is preferable that the inner pipe 311 has a thickness of 0.2 to 1 mm in order to maximize heat transfer efficiency. When the thickness of the inner pipe 311 is less than 0.2 mm, mechanical damage or heat deformation can be caused. When the thickness of the inner pipe 311 is more than 1 mm, the heat transfer efficiency may be reduced and the pre-

4 is an enlarged schematic view of a vertical section of the chamber 310 and its inner tube 311 according to an example. The inner tube 311 of the chamber 310 may be formed with a concavo-convex structure having grooves at predetermined intervals. When the inner pipe 311 is formed in a concavo-convex structure, the contact area with the sample supplied into the chamber 310 is widened, so that the heating can be performed more easily, and the pre-treatment efficiency can be further improved. The contact area between the inner tube 311 and the outer tube 312 is widened so that the inner tube 311 and the outer tube 312 can be stably stuck to each other so that the inner tube 311 can be prevented from being detached from the outer tube 312 have.

3 and 5, the heating module surrounds the chamber 310 and surrounds the chamber 310. The heating module 320 includes a heating chamber 320 and a heating chamber 320, And a temperature sensor 322 for measuring the temperature inside the chamber 310. The heater 321 and the temperature sensor 322 may be installed side by side. The chamber 310 is coupled to the upper cover 324 of the heating module 320 and can be coupled to and detached from the lower cover 325. The lower cover 325 may include a chamber 310, And a reagent such as a sample or an alkaline potassium persulfate can be supplied into the chamber 310. In addition, The lower end of the chamber 310 coupled with the lower cover 325 is formed in a structure that the inner tube 311 surrounds the outer tube 312 and is engaged with the O-ring of the lower cover 325 to thereby connect the outer tube 312 and the inner tube 311 to prevent corrosion of the outer tube 312 and to facilitate separation of the inner tube 311 when the inner tube 311 is replaced.

In one embodiment, the heating module 320 may include an overtaking sensor 323. The overheat prevention sensor 323 may be positioned between the heater 321 and the temperature sensor 322 and may display visual or auditory information when a fire due to overheating is concerned, 310 may be shut off.

In one embodiment, the oxidation reaction tank 300 may include a pressurization valve 330 (see FIG. 1). The pressurization valve 330 is installed at the upper end of the upper cover 324 of the oxidation reaction tank 300. When the sample and the reagent are injected or drained, the pressurization valve 330 is kept open to smoothly inject the sample and the reagent. In the case of thermal oxidation, the pressurization valve 330 is changed to the closed state, ) Is maintained up to 2 atmospheres so that the temperature inside the oxidation reaction tank 300 is increased to 120 degrees so that the oxidation reaction can be smoothly performed. Also, in order to maintain the pressurized state, the 3-way valve 800 of the sample injection line opens the third port 803 to shut off the inflow line of the oxidation reaction tank 300, thereby preventing pressure leakage to the outside do.

In one embodiment, the mixing tank transfer pump 400 is a pump for transferring the sample pretreated in the oxidation reaction tank 300 to the mixing tank 500, and the same pump as the sample and reagent supply pump 200 described above can be used have.

In one embodiment, the mixing tank 500 dilutes and mixes the pretreated sample, the diluted water and the reaction reagent, and the pretreated sample is diluted and mixed. The present invention does not include a separate cooling device, (Distilled water) is supplied to the sample. Unlike the prior art, unlike the prior art, the dilution water is not heated in the oxidation reaction tank 300, so that energy can be saved. By passing the diluted water after the pretreated sample, the oxidation reaction tank 300 (precisely, inside the chamber 310) It is possible to obtain the effect of cooling the sample without any separate cooling device by mixing the sample and the diluting water in the mixing tank 500. [

In one embodiment, the detector 700 transfer pump 600 is a pump that is diluted and cooled in the mixing chamber 500 and transfers the sample mixed with the reaction reagent to the detector 700. The sample and reagent supply The same pump as the pump 200 can be used.

In one embodiment, the detector 700 measures the concentration of total phosphorus or total nitrogen contained in the sample, and may use a spectrophotometric method, but not limited thereto, The concentration can be measured. FIG. 6 is a schematic view of a detector 700 according to an exemplary embodiment. Referring to FIG. 6, the detector 700 includes a light source unit 701, a cell 702 in which a measurement sample is received, and a light metering unit. . The light source 701 may be a deuterium lamp that generates an ultraviolet wavelength required for absorbance and the light emitted from the deuterium lamp may be a condensing UV lens provided between the deuterium lamp and the cell 702 Cell 702 through the cell 702. At this time, a connection part 703 is preferably provided at one side of the cell 702, and a sample moving pipe (not shown) is connected to the connection part 703, so that the measurement sample can be introduced into the cell 702.

In one example, when the concentration of total nitrogen contained in the sample is measured, the light transmitted through the cell 702 is preferably transmitted to the beam splitter 705 through the secondary condenser lens 704, The light reflected after being split in half by the spectroscope 705 is filtered by the second interference filter 706b at a wavelength of 275nm and detected at the reference photodiode 707b and is separated in half by the spectroscope 705 The transmitted light is preferably filtered by the first interference filter 706a at a wavelength of 220 nm and then detected by the measuring photodiode 707a. Here, the reference photodiode 707b measures the absorbance of residual organic matter and nitrate ions, and the measured photodiode 707a preferably measures the absorbance of turbidity with residual organic matter. The absorbance conversion formula is not limited to any particular formula but may be an appropriate formula. For example, the formula of the reference photodiode 707b and the output of the photodiode 707a Can be converted as the difference of the log value for the signal.

In one example, when the concentration of total phosphorus contained in the sample is measured, the absorbance is measured by passing a wavelength of 880 nm through the cell 702, and when the absorbance measurement value is unstable, the absorbance is measured at a wavelength of 710 nm It is possible to obtain a more stable and accurate absorbance measurement value.

Way valve 800 is disposed at the downstream end of the sample and reagent supply pump 200 and at the front end of the oxidation reaction tank 300. The sample or reagent supplied by the sample and reagent supply pump 200 May be supplied to the oxidation reaction tank (300) or the mixing tank (500). The three-way valve 800 includes a first port 801, a second port 802 and a third port 803. The first port 801 is connected to the oxidation reaction tank 300, The second port 802 is connected to the sample and reagent supply pump 200 and the third port 803 is connected to the mixing tank 500. The present invention can improve the reliability of the final measured value by reducing the quantitative error rate of the sample through the 3-way valve 800.

More specifically, when the sample is initially supplied to the oxidation reaction tank 300, the flow path from the sample and reagent supply unit 100 to the oxidation reaction tank 300 is filled with air. Due to the volume difference between the air and the liquid, The sample in the state is not injected in a fixed amount and an error occurs. In addition, such an error occurs more largely when the sample and reagent supply unit 100 includes the multi-channel valve 110 because the moving distance of each sample is changed. However, when the three-way valve 800 is provided, it is possible to remove the air existing in the flow path by supplying the sample up to the three-way valve 800. When the flow path is filled with the sample, It is possible to eliminate the error due to the change in the volume of the flow path. The third port 803 of the three-way valve 800 is opened to drain some of the sample. The first port 801 is opened to supply a predetermined amount of the sample to the oxidation reaction tank 300. After supplying a predetermined amount of sample, air is injected from the sample and reagent supply unit 100 to supply all the samples present in the flow path between the 3-way valve 800 and the oxidation reaction tank 300 to the oxidation reaction tank 300 So that a predetermined amount of sample can be injected.

In one embodiment, a sensing sensor 900 may be further included at the front end of the three-way valve 800. The detection sensor 900 can check whether the sample injected from the sample and reagent supply unit 100 is properly injected into the 3-way valve 800 and can calibrate the sample so as to additionally supply the sample when it is not used.

Next, a total phosphorus or total nitrogen measurement method will be described. The total phosphorus or total nitrogen measuring device 10 described above will be mainly described, but the present invention is not limited thereto, and it is also possible to apply the present method using a modified apparatus.

7 is a schematic view illustrating a total phosphorus or total nitrogen measurement method using a total phosphorus or total nitrogen measurement apparatus according to an embodiment of the present invention. 7, the total phosphorus or total nitrogen measurement method includes the steps of: a) supplying a sample and a reagent to be analyzed to the oxidation reaction tank 300; b) a pretreatment step of preheating the sample in the oxidation reaction tank 300; c) mixing the pretreated sample with diluting water and a reaction reagent; And d) measuring the concentration of total phosphorus or total nitrogen contained in the sample.

In one embodiment, the sample and reagent supply step (a) is a step of supplying the sample to be analyzed and the pretreatment reagent to the oxidation reaction tank 300, and the sample and reagent supply unit 100 having the multi-channel valve 110 A sample to be measured or a reagent necessary for measurement may be sequentially or simultaneously selected and supplied. Specifically, the sample and reagent supply step includes a first step (a-1) of supplying a sample up to the three-way valve 800 to remove the air filled in the front end and the rear end flow path of the sample and reagent supply pump 200; A second step (a-2) of supplying the sample into the oxidation reaction tank; A third step (a-3) of supplying air through the sample and reagent supply unit 100 to drain the sample filled in the flow path between the sample and reagent supply unit 100 and the 3-way valve 800; And a fourth step (a-4) of supplying air through the sample and reagent supply unit 100 to supply the sample filled in the flow path between the 3-way valve 800 and the oxidation reaction tank into the oxidation reaction tank 300 . This reduces the quantitative error rate of the sample and improves the reliability of the final measured value. That is, when the sample is initially supplied to the oxidation reaction tank 300, the air filled in the flow path from the sample and reagent supply unit 100 to the oxidation reaction tank 300 is removed to eliminate an error caused by volume differences between air and liquid And an error caused by the difference in distance from the end of the main flow path (the point where the sample flows out from the sample and reagent supply unit 100) in each valve of the sample and reagent supply unit 100 can be also excluded.

In one embodiment, the pretreatment step (b) is a step of heating a sample supplied in a predetermined amount from the sample and reagent supply unit 100, wherein only the sample to be measured and the pretreatment reagent are supplied. That is, conventionally, diluted water (distilled water) and a sample are supplied together and heated, but the present invention is characterized in that only necessary samples are supplied without diluted water (distilled water) and heated. The size of the oxidation reaction tank 300 can be reduced by injecting only the sample, and a separate cooling step for cooling the heated sample can be avoided.

In one embodiment, the mixing step (c) is a step of mixing the pretreated sample with the diluting water and the reaction reagent. In the first step (c-1) of diluting and cooling the sample by mixing the pretreated sample with diluted water, ; And a second step (c-2) of mixing the diluted and cooled sample with the reaction reagent. In the present invention, since only the sample is heated in the pretreatment step and then supplied to the mixing tank 500, not only the cooling step by the separate cooling module between the pretreatment step and the mixing step can be excluded, Energy can be saved.

In one embodiment, the detecting step (d) is a step of measuring the concentration of total phosphorus or total nitrogen contained in the sample, and the concentration of total phosphorus or total nitrogen contained in the sample is measured using various experimental techniques such as a spectrophotometric method .

Hereinafter, the structure and effect of the present invention will be described in more detail with reference to examples and comparative examples. However, this embodiment is intended to explain the present invention more specifically, and the scope of the present invention is not limited to these embodiments.

[Experimental Example]

(Not shown in Fig. 1) and a 3-way valve without a separate cooling device and equipped with a separate cooling device at the downstream end of the oxidation reaction tank A total phosphorus or total nitrogen measuring device (comparative example) was prepared to compare the dosing effect and cooling effect.

Confirmation of reduction effect of sample injection error rate with 3-way valve

A sample was injected to the front end of the 3-way valve to remove air existing in the flow path, and the sample was injected in a predetermined amount using a sample and reagent supply pump using a comparative example , And the results are shown in Table 1 below.

[Table 1]

As shown in Table 1, it can be seen that the quantitative error rate of the sample injection of the embodiment is reduced, and it is found that the effect is better when the sample is low in capacity.

Check energy savings

The pretreatment step and the mixing step of the sample were carried out using the examples and the comparative examples. The specific process is shown in Table 2 below, and the overall results are shown in Table 3 below. In the case of washing, distilled water was used as the distilled water, and a large amount of distilled water was added thereto (N, a, b, c means a positive number exceeding 0) in comparison with the amount of the previously introduced liquid (sample, reagent, etc.).

[Table 2]

[Table 3]

As can be seen from Tables 2 and 3, the embodiment can reduce the energy consumption, the cost of manufacturing the facility (the size of the oxidation tank, etc.) as compared with the comparative example, and has the effect of shortening the overall measurement time Could know. In addition, by supplying the diluted water after the sample is heated, an additional cleaning step can be omitted.

Confirmation of decrease in error rate of concentration measurement value in preprocessing

The error ratios of the sample concentration measurement values of Examples and Comparative Examples were measured according to the process of Table 2 and are shown in Table 4 below. The samples were compared with the concentrations of the initially introduced samples and the concentrations measured at the detector (diluted with distilled water).

[Table 4]

As can be seen from the above Table 4, it can be seen that the error rate of the sample concentration measurement value is significantly reduced in the Examples, compared with Comparative Example, and that the effect is better when the concentration is low.

Check cooling efficiency

The cooling efficiencies of the examples and comparative examples were confirmed according to the process of Table 2 and are shown in Table 5 below.

[Table 5]

It was judged that the cooling efficiency was excellent in that the cooling efficiency was lowered to a temperature close to 25 ° C required in the water pollution process test standard. As can be seen from Table 5, the examples and the comparative examples showed a difference of 5.52 ° C and 25.39 ° C compared to 25 ° C, respectively, and it was found that the cooling efficiency was better in the examples.

It is to be understood that the present invention is not limited to the above embodiments and various changes and modifications may be made by those skilled in the art without departing from the spirit and scope of the invention.

10: Total phosphorus or total nitrogen measuring device
100: sample and reagent supply unit
110: Multi-channel valve
200: Sample and reagent feed pump
300: oxidation reaction tank
310: chamber
311: Inner pipe
312: Appearance
320: Heating module
321: Heater
322: Temperature sensor
323: Overheat prevention sensor
324: upper cover
325: Lower cover
326: O ring
330: Pressure valve
400: Mixing feed pump
500: mixing tank
600: Detector feed pump
700: detector
800: 3-way valve
801: First port
802: second port
803: Third port
900: Sensing sensor

Claims (10)

A sample and reagent supply unit for supplying the sample to be measured and the sample necessary for the measurement;
A sample and reagent supply pump for transferring a sample and reagent supplied from the sample and reagent supply unit in a fixed amount;
An oxidation reaction tank for heating and pretreating the transferred sample;
A mixing tank transfer pump for transferring the pretreated sample in the oxidation tank;
A mixing tank for diluting and mixing the pretreated sample, the diluted water and the pretreated sample supplied with the reaction reagent;
A detector transfer pump for transferring diluted and mixed samples to a detector in a mixing chamber;
A detector for measuring the concentration of total phosphorus or total nitrogen contained in the sample; And
A first port, a second port, and a third port, the first port being connected to the oxidation reaction tank, the second port being connected to the sample and reagent supply pump, And a 3-way valve connected to the mixing tank and supplying the sample to the oxidation reaction tank or the mixing tank to remove the air remaining in the flow path,
In the oxidation tank,
A chamber capable of receiving the transferred sample; And a heating module surrounding the chamber,
In the chamber,
And is formed as a double structure including an outer tube and an inner tube,
Wherein the inner pipe is a concavo-convex structure having a groove formed at a predetermined interval. The apparatus according to claim 1, wherein the sample and reagent supply unit
And a multi-channel valve is provided to selectively supply one or more samples. The apparatus of claim 1, wherein the sample and reagent supply pump comprises:
Characterized in that the number of revolutions of the motor provided in the pump is controlled to transfer a specified amount of the sample. delete delete The heating module according to claim 1,
A heater for heating the chamber; And
And a temperature sensor for measuring the temperature inside the chamber. delete A total phosphorus or total nitrogen measuring method using the measuring device according to claim 1,
a) supplying a sample to be analyzed and a reagent necessary for the measurement to the oxidation reaction tank;
b) a pretreatment step in which the sample is heated in the oxidation reaction tank and pretreated;
c) mixing the pretreated sample with diluting water and a reaction reagent; And
and d) measuring the concentration of total phosphorus or total nitrogen contained in the sample. 9. The method of claim 8, wherein the sample and reagent supply step (a)
A first step (a-1) of supplying the sample up to the 3-way valve and removing the air filled in the front end and the rear end flow path of the sample and reagent supply pump;
A second step (a-2) of supplying the sample into the oxidation reaction tank;
A third step (a-3) of supplying air through the sample and reagent supply unit to drain the sample filled in the flow path between the sample and reagent supply unit and the 3-way valve; And
And a fourth step (a-4) of supplying air through the sample and reagent supply unit to supply the sample filled in the flow path between the 3-way valve and the oxidation reaction tank into the oxidation reaction tank. Method of measuring nitrogen. 9. The method of claim 8, wherein the mixing step (c)
A first step (c-1) of diluting and cooling the sample by mixing the pretreated sample with dilution water; And
And a second step (c-2) of mixing the diluted and cooled sample with the reaction reagent.

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