CN104914063A - Analytical device - Google Patents

Analytical device Download PDF

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Publication number
CN104914063A
CN104914063A CN201410234044.0A CN201410234044A CN104914063A CN 104914063 A CN104914063 A CN 104914063A CN 201410234044 A CN201410234044 A CN 201410234044A CN 104914063 A CN104914063 A CN 104914063A
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CN
China
Prior art keywords
reactive tank
aqueous solution
glass
solution
analytical equipment
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Pending
Application number
CN201410234044.0A
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Chinese (zh)
Inventor
并河信宽
片冈达哉
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Shimadzu Corp
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Shimadzu Corp
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Publication of CN104914063A publication Critical patent/CN104914063A/en
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  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)

Abstract

The invention provides an analytical device which can restrain the dissolution of a glass container caused by aqueous alkali in the process of abstracting heated aqueous alkali into the glass container, and prolong the service life. The aqueous alkali containing a sample is heated in a reactive tank (2) and reacts; the solution after reaction is abstracted to a glass container (11a) connected with the reactive tank (2) through a liquid flow path (P4) to perform sample analysis; a cooling device (13) is arranged on the liquid flow path (P4) and cools the solution flowing the liquid flow path (P4), thereby restraining the dissolution of glass caused by the aqueous alkali, and prolonging the service life of the glass container (11a).

Description

Analytical equipment
Technical field
The present invention relates to a kind of analytical equipment, in more detail, relate to a kind of analytical equipment comprising operation aqueous slkali being drawn into glass container, described aqueous slkali is heated in the circulation of analysis action.
Background technology
In certain analytical equipment of such as total nitrogen total phosphorus analysis meter (TN/TP analysis meter) etc., comprise in its circulation analyzing action and make the aqueous slkali comprising sample add thermal response, and by this solution extraction to the operation in glass container.
Namely, in order to measure the content of total nitrogen that draining etc. comprises and total phosphorus, when carrying out utilizing the determination of total nitrogen content based on the total nitrogen total phosphorus analysis meter of UV absorbance photometry, general by adding sodium hydrate aqueous solution and persulfate aqueous solution to as in the sample of analytic target, be accommodated in the heating of reactive tank inner edge irradiation ultraviolet radiation limit, make it produce ultra-violet oxidation decomposition reaction, thus, the whole nitrogen compounds comprised in sample just become nitrate ion.This reacted solution is attracted from reactive tank with syringe pump, after utilizing hydrochloric acid to carry out pH adjustment, deliver to absorbance measurement pond, irradiate the ultraviolet light as the wavelength 220nm of the absorption peak of nitrate ion, according to the content (such as with reference to patent documentation 1) of the total nitrogen in its absorbance measurement sample.
In above analysis cycle, the aqueous slkali comprising sample in reactive tank is heated to about 80 DEG C usually, and attracts the material of cylinder many employings glass of the syringe pump of this solution.
Prior art document
Patent documentation
Patent documentation 1 Japanese Unexamined Patent Publication 2007-086041 publication
Summary of the invention
The problem to be solved in the present invention
But, when carrying out the determination of total nitrogen content utilizing total nitrogen total phosphorus analysis meter, the aqueous slkali comprising sample being heated to about 80 DEG C in reactive tank is drawn in the glass rounding cylinder of syringe pump, but glass rounding cylinder can dissolve thus, if use through the long period, then the aggravations such as the dissolving having glass continues to carry out, leak of liquid or devitrification, need the worry carrying out changing below original device lifetime.
Problem of the present invention is to provide a kind of dissolving that can suppress to be caused by this aqueous slkali glass, and then the analytical equipment that the life-span of this device is improved.
The means of dealing with problems
For solving the problem, analytical equipment of the present invention is that a kind of aqueous slkali making to comprise sample heats and reacts in reactive tank, by this reacted solution extraction to the analytical equipment of the glass container be communicated with described reactive tank by liquid flow path for sample analysis, the feature of described analytical equipment is, described liquid flow path is provided with cooling device, and described cooling device cools the solution flowing through this liquid flow path.
At this, the present invention is applicable to total nitrogen total phosphorus analysis meter, as the concrete structure in this situation, following structure can be adopted: described reactive tank is when determination of total nitrogen content, be accommodated with sample liquids, the following heating edge irradiation ultraviolet radiation of state of sodium hydrate aqueous solution and persulfate aqueous solution, make the reactive tank of the reaction generation based on ultra-violet oxidation decomposition method thus, described glass container is the glass rounding cylinder of syringe pump, for measuring sample liquids respectively, sodium hydrate aqueous solution and persulfate aqueous solution by described sample liquids, described sodium hydrate aqueous solution and described persulfate aqueous solution are injected into described reactive tank, and attract the reacted solution in this reactive tank and send to absorbance measurement pond, the pipeline connecting this glass rounding cylinder and described reactive tank is provided with described cooling device.
Dissolution degree due to the glass caused by aqueous slkali depends on the temperature of this aqueous slkali, therefore the present invention by by reactive tank by the solution extraction that heats to glass container time, in stream, cool this solution solve problem.
At this, when Fig. 3 illustrate represent 1mol/1 sodium hydrate aqueous solution/in make glass (borosilicate glass) soak 1 hour corrosion depth and the chart of relation of temperature.As shown, the temperature of aqueous slkali is higher, glass biodissolution more.Therefore, by by before be drawn into glass container by the aqueous slkali heated in reactive tank, the liquid flow path connecting them arrange cooling device the temperature of aqueous slkali is reduced, the dissolving of glass container can be suppressed.
When the present invention being applicable to total nitrogen total phosphorus analysis meter, cooling device is configured by the pipeline that connects between the reactive tank making ultra-violet oxidation decomposition reaction occur and syringe pump, can suppress the dissolving of the glass rounding cylinder of syringe pump, described syringe pump is used for attracting solution from this reactive tank and delivering to absorbance measurement pond.
Invention effect
According to the present invention, owing to arranging cooling device on liquid flow path, before aqueous slkali flows into glass container, its temperature is declined, therefore the dissolving of the glass caused by aqueous slkali can be suppressed, and the life-span of energy extension fixture, described liquid flow path is used for being drawn into glass container by reactive tank by the aqueous slkali heated.
And, the present invention owing to only arranging suitable cooling device on liquid flow path, even if therefore also can improve simply for original analysis meter.
Accompanying drawing explanation
Fig. 1 is the summary construction diagram that embodiments of the present invention are shown.
Fig. 2 is to the schematic diagram that other the key structure of embodiment of the present invention is described is shown.
Fig. 3 is the chart of the relation representing the corrosion depth of glass when aqueous slkali soaking and temperature.
Embodiment
Below, with reference to accompanying drawing, the embodiment that the present invention relates to is described.Fig. 1 is the summary construction diagram of embodiment the present invention being applicable to total nitrogen total phosphorus analysis meter.
On-line sample is the samples such as the plant chimney stalk becoming analytic target, is automatically gathered, be incorporated in analysis meter by on-line sample ingress pipe Pl with the interval set.Again, in addition, the off-line sample gathered by any means is incorporated in analysis meter by off-line Sample introduction pipe P2.
Each of this each ingress pipe Pl, P2 valve 1 logical with the or eight respectively distributes individually port (1) (2) and is connected, and the one or eight leads to reactive tank 2 that other distribution port (3) ~ (8) of valve 1 and the reaction for making based on ultra-violet oxidation decomposition method occur and be connected for the cell 3 etc. measured based on the absorbance of UV absorbance photometry.In addition, be discharged pump 4 through the solution of reactive tank 2 as waste water to process.
The comm port (0) of the one or eight logical valve 1 is connected with the distribution port <1> of the two or eight logical valve 5 by pipeline P3.Other of two or eight logical valve 5 distribute port <2> ~ <7> with as reagent during determination of total nitrogen content sodium hydrate aqueous solution 6, persulfate aqueous solution 7 or be connected for the hydrochloric acid 8 etc. that pH adjusts.In addition, the distribution port of the two or eight logical valve 5 and the described 1 logical valve 1 is connected with for the reagent set of total phosphorus determination or standard model, be connected with drain switching valve door 9 or sample switch valve 10 etc. further, but these and feature of the present invention do not have direct relation, again owing to being common practise, therefore omit detailed description at this.
The common port <0> of the two or eight logical valve 5 is connected with syringe pump 11, and this syringe pump 11 has the cylinder 11a of glass, again, can stir inside by mixing pump 12.
So, the feature of this embodiment is, the pipeline P4 making the one or eight logical valve 1 be communicated with reactive tank 2 is provided with cooling device 13.This cooling device 13 is the use of the air-cooled type cooling device of fan, or employ the water-cooled chiller etc. of tank, be not particularly limited, if can make the solution of about 70 ~ 80 DEG C flowing through its inside from the outside of pipeline P4 be cooled to below set point of temperature, such as less than 55 DEG C.
In the above embodiment, if set forth the action of determination of total nitrogen content, first, drive the logical valve 5 of the one or eight logical valve the 1 and the 28, any one making in on-line sample ingress pipe Pl or off-line Sample introduction pipe P2 is communicated with syringe pump 11, drive syringe pump 11 in this condition, by the sample extraction of ormal weight in glass rounding cylinder 11a.Next, by suitably driving the two or eight logical valve 5 and syringe pump 11, only the sodium hydrate aqueous solution 6 of ormal weight and persulfate aqueous solution 7 being extracted respectively in glass rounding cylinder 11a, stirring by mixing pump 12.Thereafter, drive the logical valve 5 of the one or eight logical valve the 1 and the 28, reactive tank 2 is communicated with syringe pump 11, by the driving of syringe pump 11, the solution in glass rounding cylinder 11a is delivered in reactive tank 2.
In reactive tank 2, while will generate as described above and the sample be admitted to, namely, the aqueous slkali be made up of sodium hydrate aqueous solution 6 and persulfate aqueous solution 7 is heated to temperature (such as 80 DEG C) the limit irradiation ultraviolet radiation of regulation, make it that ultra-violet oxidation decomposition reaction occurs thus, the whole nitrogen compound comprised in sample is become nitrate ion.
Thereafter, drive the logical valve 5 of the one or eight logical valve the 1 and the 28, syringe pump 11 is communicated with reactive tank 2, after in the solution extraction ormal weight in reactive tank 2 to glass rounding cylinder 11a, drive the two or eight logical valve 5, hydrochloric acid 8 is drawn in glass rounding cylinder 11a to carry out pH adjustment, again drive the logical valve 5 of the one or eight logical valve the 1 and the 28, the cell 3 of absorbance measurement is communicated with syringe pump 11, send in cell 3 by the solution in glass rounding cylinder 11a, the light of illumination wavelength 220nm also carries out absorbance measurement.According to this measurement result, obtain the amount of the nitrate ion in solution, and then obtain the amount of the total nitrogen existed in sample.
In above action, by in reactive tank 2, to be drawn into syringe pump 11 by pipeline P4 by the solution that heats glass rounding cylinder 11a in time, be strong basicity due to this solution and be heated to about 80 DEG C, if be therefore directly drawn in glass rounding cylinder 11a, the reason of the glass biodissolution making cylinder 11a will be become.But in the present invention, pipeline P4 arranges cooling device 14, and thus, the solution flow through in pipeline P4 is cooled to less than 55 DEG C, therefore, when flowing into glass rounding cylinder 11a, the temperature (with reference to Fig. 3) needing hardly to worry the degree of dissolving just is become.
At this, in the above embodiment, though show example the present invention being applicable to total nitrogen total phosphorus analysis meter, the present invention is not limited thereto, and also can be widely used in comprising the analytical equipment aqueous slkali being heated to more than about 55 DEG C being drawn into the operation in the container of glass.
Namely, as schematically shown in (A) of Fig. 2, be drawn in the analytical equipment of operation glass container 103 in by the aqueous slkali heated by the liquid flow paths such as pipeline 102 by reactive tank 101 having, as shown in (B) of Fig. 2, by arranging cooling device 104 to cool the solution flow through in liquid flow path 102 on liquid flow path 102, the dissolving of this glass container 103 caused by the solution flowed in glass container 103 can be suppressed, extend the life-span of glass container 103.
Symbol description
Pl on-line sample ingress pipe
P2 off-line Sample introduction pipe
P3 pipeline
P4 pipeline (liquid flow path)
1 the 1 logical valve
2 reactive tanks
3 cells
4 extraction pumps
5 the 28 logical valves
6 sodium hydrate aqueous solutions
7 persulfate aqueous solutions
8 hydrochloric acid
9 drain switching valve doors
10 sample switch valves
11 syringe pumps
11a glass rounding cylinder (glass container)
12 mixing pumps
13 cooling devices.

Claims (2)

1. an analytical equipment, described analytical equipment makes the aqueous slkali comprising sample heat in reactive tank and react, by this reacted solution extraction to the glass container be communicated with described reactive tank by liquid flow path for sample analysis, the feature of described analytical equipment is
Described liquid flow path is provided with cooling device, and described cooling device cools the solution flowing through this liquid flow path.
2. the analytical equipment described in claim 1, is characterized in that,
Described analytical equipment is total nitrogen total phosphorus analysis meter,
Described reactive tank is when determination of total nitrogen content, at the following heating edge irradiation ultraviolet radiation of the state being accommodated with sample liquids, sodium hydrate aqueous solution and persulfate aqueous solution, makes the reactive tank of the reaction generation based on ultra-violet oxidation decomposition method thus,
Described glass container is the glass rounding cylinder of syringe pump, for measuring sample liquids, sodium hydrate aqueous solution and persulfate aqueous solution respectively and described sample liquids, described sodium hydrate aqueous solution and described persulfate aqueous solution being injected into described reactive tank, and attract the reacted solution in this reactive tank and send to absorbance measurement pond
The pipeline connecting this glass rounding cylinder and described reactive tank is provided with described cooling device.
CN201410234044.0A 2014-03-14 2014-05-29 Analytical device Pending CN104914063A (en)

Applications Claiming Priority (2)

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JP2014051647 2014-03-14
JP2014-051647 2014-03-14

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CN (1) CN104914063A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109580480A (en) * 2017-09-28 2019-04-05 株式会社岛津制作所 Total phosphorus determination device
CN112424597A (en) * 2018-07-27 2021-02-26 株式会社岛津制作所 Analysis device

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR102077136B1 (en) * 2018-06-19 2020-02-13 주식회사 위코테크 Apparatus for measuring total phosphorus and total nitrogen

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CN112424597A (en) * 2018-07-27 2021-02-26 株式会社岛津制作所 Analysis device
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JP2015187595A (en) 2015-10-29

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