CN101477040B - On-line digestion and detection apparatus for total nitrogen content in solution - Google Patents
On-line digestion and detection apparatus for total nitrogen content in solution Download PDFInfo
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- CN101477040B CN101477040B CN2009100424915A CN200910042491A CN101477040B CN 101477040 B CN101477040 B CN 101477040B CN 2009100424915 A CN2009100424915 A CN 2009100424915A CN 200910042491 A CN200910042491 A CN 200910042491A CN 101477040 B CN101477040 B CN 101477040B
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- digestion
- lamp guide
- nitrogen content
- total nitrogen
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 230000029087 digestion Effects 0.000 title claims abstract description 54
- 238000001514 detection method Methods 0.000 title claims abstract description 39
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 37
- 230000007246 mechanism Effects 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- 238000009833 condensation Methods 0.000 claims description 34
- 230000005494 condensation Effects 0.000 claims description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 238000010992 reflux Methods 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 125000006850 spacer group Chemical group 0.000 claims description 12
- 230000003287 optical effect Effects 0.000 claims description 6
- 230000009467 reduction Effects 0.000 claims description 5
- 238000005259 measurement Methods 0.000 abstract description 7
- 230000011514 reflex Effects 0.000 abstract 3
- 238000005070 sampling Methods 0.000 abstract 2
- 239000000523 sample Substances 0.000 description 22
- 239000000243 solution Substances 0.000 description 15
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000012488 sample solution Substances 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000009977 dual effect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 235000004279 alanine Nutrition 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000006396 nitration reaction Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- -1 nitrogen-containing compound Chemical class 0.000 description 1
- YPJKMVATUPSWOH-UHFFFAOYSA-N nitrooxidanyl Chemical compound [O][N+]([O-])=O YPJKMVATUPSWOH-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- CHKVPAROMQMJNQ-UHFFFAOYSA-M potassium bisulfate Chemical compound [K+].OS([O-])(=O)=O CHKVPAROMQMJNQ-UHFFFAOYSA-M 0.000 description 1
- 229910000343 potassium bisulfate Inorganic materials 0.000 description 1
- 235000010333 potassium nitrate Nutrition 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
The invention discloses an on-line digestion and detection device for total nitrogen content in a solution, which comprises a light source, a digestion device, a reflex condenser, a sampling detection mechanism, and a light guide stick, wherein a top end of the digestion device is connected with the reflex condenser; the outer surface of the digestion device is provided with a heating device; the light guide stick is inserted into the digestion device and the reflex condenser; the upper end of the light guide stick corresponds to a detection disk of the sampling detection mechanism, and the lower end of the light guide stick corresponds to the light source. The invention is the on-line digestion and detection device for the total nitrogen content in the solution which has a simple and compact structure, low cost, simple and convenient operation, high measurement accuracy, and quick measurement speed.
Description
Technical field
The present invention is mainly concerned with the checkout equipment field of nitrogen content in the solution, refers in particular to the in-line digestion and the pick-up unit of total nitrogen content in a kind of solution.
Background technology
In fields such as environmental protection, food, medical and health, often need to measure the nitrogen content or the protein content of material, the general practice is that elder generation changes into liquid phase with material, again the nitrogen in the liquid phase sample is all changed into nitrate ion (NO
3 -), by mensuration, extrapolate the nitrogen pool content in the material to be measured to nitrate ion concentration, its reaction principle is as follows:
In the aqueous solution, potassium persulfate can decompose generation potassium acid sulfate and atomic oxygen more than 60 ℃.Under 120～124 ℃ of conditions, the oxygen of atomic state makes that the nitrogen of nitrogen-containing compound is converted into nitrate in the water sample.Its equation is
K
2S
2O
8+H
2O→2KHSO
4+1/2O
2↑
Because in the conversion process of nitride, therefore organism oxidized decomposition simultaneously measures absorbance A with ultraviolet spectrophotometry respectively in wavelength 220nm and 275nm place
220And
And obtain the correction absorbance A by following formula:
A＝A
220-2A
275
Value by A is calculated total nitrogen (with NO according to working curve
3-N) content.
Aforesaid operations process majority is to carry out in the laboratory, and manually operation is analyzed one by one to sample.For realizing clearing up, just need design and produce special-purpose closed heating pressure vessel, after one hour high temperature is cleared up nearly, lower the temperature again, break seal, take a sample, the phenomenon of frequent do not open color comparison tube or color comparison tube washing pipe, trivial operations, time-consuming, be difficult to satisfy the requirement of the information of obtaining fast, accurately and timely in environmental administration or the technological process.
These technological improvements have positive meaning for traditional manual operations.But it still need adopt sealed pressure vessel, and operating process has a significant impact measuring accuracy, and this has just limited the practical application of this technology in on-line measurement.
Summary of the invention
The problem to be solved in the present invention just is: at the technical matters that prior art exists, the invention provides the in-line digestion and the pick-up unit of total nitrogen content in a kind of simple and compact for structure, with low cost, easy and simple to handle, measuring accuracy is high, measuring speed is fast solution.
For solving the problems of the technologies described above, the solution that the present invention proposes is: the in-line digestion of total nitrogen content and pick-up unit in a kind of solution, it is characterized in that: it comprises light source, digestion instrument, condensation reflux device, sample detecting mechanism and lamp guide, the top of described digestion instrument links to each other with condensation reflux device, be equiped with heating arrangement on the outside surface of digestion instrument, lamp guide is inserted in digestion instrument and the condensation reflux device, the upper end of lamp guide is corresponding with the detection dish of sample detecting mechanism, and the lower end of lamp guide is corresponding with light source.
Described sample detecting mechanism comprises detects control box, detection dish, drive motor, driving shaft and photoelectric conversion unit, the detection dish is installed in the detection control box and is fixed on the driving shaft of drive motor, photoelectric conversion unit is installed on the detection dish top of detecting the hole and detected light signal is converted into electric signal and sends to and detect control box and handle, and lamp guide is positioned at the below of detection dish.
Offer pilot hole on the described detection dish, detect hole and reference hole, detect the optical filter that 220nm is placed at the place, hole, the optical filter of 275nm is placed at place, reference hole.
Described condensation reflux device comprises condensation chamber and condensate water spacer, and described condensate water spacer is wrapped on the outside surface of condensation chamber, is used for offering water inlet and water delivering orifice on the condensate water spacer of logical chilled water, and the lower end of condensation chamber links to each other with digestion instrument.
The upper end of described condensation chamber is provided with upper head plate, is equiped with the reduction valve assembly on the upper head plate.
Described lamp guide comprises lamp guide transmitter unit and lamp guide receiving element, the lamp guide transmitter unit be installed in digestion instrument bottom and with the corresponding position of light source on, the lamp guide receiving element be installed in digestion pool the top and with sample detecting mechanism corresponding position on.
Compared with prior art, advantage of the present invention just is:
1, the in-line digestion and the pick-up unit of total nitrogen content in the solution of the present invention have advantages such as simple and compact for structure, with low cost, easy and simple to handle, that measuring accuracy is high, measuring speed is fast;
2, the in-line digestion and the pick-up unit of total nitrogen content in the solution of the present invention, it has abandoned general in the past pressure sealing container, has the pressure apparatus of condensation reflux device but adopt, thereby make digestion process can be safer, thoroughly, finish efficiently;
3, the in-line digestion and the pick-up unit of total nitrogen content in the solution of the present invention, a kind of dual wavelength detection method has been proposed, the first can form the maximum absorption wavelength (λ=220nm) of maximum absorption band to nitrate ion, it two is the wavelength that will not absorb nitrate ion (λ=275nm), by contrast to two kinds of wavelength absorption peaks, the concentration that can reflect nitrate ion in the sample, detection speed is fast, precision is high;
4, the in-line digestion and the pick-up unit of total nitrogen content in the solution of the present invention adopt lamp guide, can increase the light intensity signal under the ultraviolet condition thus, significantly improve and measure signal to noise ratio (S/N ratio), improve measuring accuracy;
5, the in-line digestion and the pick-up unit of total nitrogen content in the solution of the present invention, clearing up reaction, cooling, measure and be integrated in one sample, realize the quick accurate on-line measurement of sample nitrogen pool,, realize that technological process control provides foundation in time circulating a notice of field data.
Description of drawings
Fig. 1 is a structural representation of the present invention;
Fig. 2 is the structural representation of detection dish among the present invention;
Fig. 3 is the signal collection of illustrative plates of the nitrogen pool detection and the usefulness of surveying.
Marginal data
1, light source 2, digestion instrument
201, resistance wire 202, digestion pool
203, injection port 3, condensation reflux device
301, condensation chamber 302, condensate water spacer
303, water inlet 304, water delivering orifice
305, upper head plate 306, reduction valve assembly
4, sample detecting mechanism 401, detection dish
402, photoelectric conversion unit 403, drive motor
404, driving shaft 405, detection control box
4011, pilot hole 4012, detection hole
4013, reference hole 501, lamp guide transmitter unit
502, lamp guide receiving element
Embodiment
Below with reference to the drawings and specific embodiments the present invention is described in further details.
As depicted in figs. 1 and 2, the in-line digestion of total nitrogen content and pick-up unit in the solution of the present invention, it comprises light source 1, digestion instrument 2, condensation reflux device 3, sample detecting mechanism 4 and lamp guide, the top of digestion instrument 2 links to each other with condensation reflux device 3, be equiped with heating arrangement on the outside surface of digestion instrument 2, lamp guide is inserted in digestion instrument 2 and the condensation reflux device 3, and it is 401 corresponding that the upper end of lamp guide and the detection of sample detecting mechanism 4 are coiled, and the lower end of lamp guide is corresponding with light source 1.In the present embodiment, lamp guide comprises lamp guide transmitter unit 501 and lamp guide receiving element 502, lamp guide transmitter unit 501 be installed in digestion pool 202 bottoms and with light source 1 corresponding position on, lamp guide receiving element 502 be installed in digestion pool 202 the top and with sample detecting mechanism 4 corresponding positions on.By increase distance between lamp guide transmitter unit 501 upper ends and lamp guide receiving element 502 lower ends can increase solution the absorption light path, the decay of light intensity simultaneously is very little, has improved the sensitivity and the degree of accuracy of apparatus measures so greatly.Sample detecting mechanism 4 comprises detects control box 405, detection dish 401, drive motor 403, driving shaft 404 and photoelectric conversion unit 402, detection dish 401 is installed in the driving shaft 404 that detects in the control box 405 and be fixed in drive motor 403, photoelectric conversion unit 402 is installed on the detection dish 401 top of detecting the hole and detected light signal is converted into electric signal and sends to and detect control box 405 and handle, and lamp guide receiving element 502 is positioned at the below of detecting the hole on the detection dish 401.Referring to Fig. 2, offer three circular holes on the detection dish 401, these three circular holes are respectively pilot hole 4011, detect hole 4012 and reference hole 4013, pilot hole 4011 is determined accurate start time point in order to give to detect, detect 4012 places, hole and place the optical filter of 220nm, be used to pass through the detection light beam of wavelength X=220nm; The optical filter of 275nm is placed at 4013 places, reference hole, is used to pass through the reference beam of wavelength X=275nm.
In the present embodiment, digestion instrument 2 comprises heating arrangement and digestion pool 202, and heating arrangement adopts resistance wire 201, and this resistance wire 201 is installed on digestion pool 202 outside surfaces, offers injection port 203 on the digestion pool 202.
In the present embodiment, condensation reflux device 3 comprises condensation chamber 301 and condensate water spacer 302, this condensate water spacer 302 is wrapped on the outside surface of condensation chamber 301, offers water inlet 303 and water delivering orifice 304 on the condensate water spacer 302, is used for leading to chilled water in the condensate water spacer 302.The lower end of condensation chamber 301 links to each other with digestion pool 202, and the upper end of condensation chamber 301 is provided with upper head plate 305, is equiped with reduction valve assembly 306 on the upper head plate 305.Open upper head plate 305 during sample introduction so that go up logical atmosphere, close when clearing up so that sealed digestion.
Fig. 3 is the signal collection of illustrative plates of the nitrogen pool detection and the usefulness of surveying, when light beam passes through pilot hole 4011, a pulse appears in the collection of illustrative plates, the zero-time ta that indication is measured, subsequently, successively pass through respectively when detecting hole 4012 and reference hole 4013, form in succession in tb and tc position and detect crest Wb and reference crest Wc when detecting light beam and reference beam, according to the difference of peak value, concentration and nitrogen pool that can conversion place nitrate ion.
Principle of work: be to measure nitrogen pool, at first should make to contain nitrogen solution and clear up.When clearing up, normal pressure will cause down the boiling and the evaporation of test solution, and boiling point has only 100 ℃, is difficult to reach digestion condition.If with traditional pressure sealing container, not only there is potential safety hazard in complex structure, but also be difficult to carry out on-line operation, the condensation reflux unit that the present invention proposes is simple in structure, compact, make facility, can effectively solve this difficult problem, and creates conditions for the on-line measurement of nitrogen.
Make up after injection port 204 is introduced the digestion pools 202 at sample and oxygenant, heating wire 201 heats, temperature in the digestion pool 202 rises to 120 ℃, clear up reaction this moment, fierce nitration reaction takes place in sample and oxygenant, and the nitrogen that various forms in the sample is existed is converted into nitrate radical; Meanwhile, sample solution at high temperature seethes with excitement, and forms the steam volatilization.In condensation reflux device 3, the steam of rising is met cold, forms water droplet and returns, and forms the reparation circulation of solution-steam-water droplet-backflow and solution thus.Pass to cooling circulating water in the condensate water spacer 302 of condensation reflux device 3 peripheries, its flow velocity should guarantee that the temperature in the condensation reflux device 3 is lower than the required temperature of condensation, carries out smoothly to guarantee whole evaporation, condensation process.The set reduction valve assembly 306 in condensation reflux device 3 upper ends is the safety practices for preventing that mishap from designing, and with when pressure is higher than certain threshold values, opens pressure release, wholely clears up reaction and needs 30 minutes consuming time.
Clear up the reaction finish after, can carry out the nitrogen pool on-line measurement, at light source 1 place by the operation requirement launch ultraviolet light beam, through lamp guide transmitter unit 501, the sample solution through having cleared up enters lamp guide receiving element 502 again.The light beam of being drawn by lamp guide receiving element 502 enters sample detecting mechanism 4, and detection dish 401 is the constant speed rotation under the driving of drive motor 403.When light beam passes through pilot hole 4011, detection trigger mechanism, start detection, the detection light beam that leaches 220nm passes through from detecting hole 4012; The reference beam that leaches 275nm passes through from reference hole 4013.Because λ=220nm is a maximum absorption wavelength, it is by the sample solution after clearing up the time, to NO
3 -Form maximum absorption band, and the light beam of λ=275nm is not NO substantially
3 -Absorb, corresponding absorption peak is made the usefulness of reference, two-beam is converted to digital signal through photoelectric conversion unit 402, through data processing, provides NO
3 -The real-time numerical value of concentration.Can finish dual wavelength thus in single job detects.
The mountain is in having adopted the many technical measures that comprise These characteristics, and instrument has all obtained satisfied result according to the instrument that the present invention manufactured experimently in the occasion that numerous need carry out the on-line measurement nitrogen pool.
The technology applicating example:
Be assemblied on the homemade total nitrogen on-line monitoring instrument by this device, it is as follows that nitrogen content is that 2.64mg/L alanine and ammonium chloride mixed standard solution carry out the determination and analysis result:
| The 1st time | The 2nd time | The 3rd time | The 4th | The 5th | The 6th time |
| 2.83 | 2.58 | 2.69 | 2.72 | 2.89 | 2.55 |
Mean value=2.71, relative standard deviation=4.9%;
The standard solution that above-mentioned sample is added KNO3 makes nitrogen content increase 2mg/L measured value as follows:
| The 1st time | The 2nd time | The 3rd time |
| 4.79 | 4.83 | 4.68 |
Mean value=4.77, the recovery=102.8%,
Respond well.
The above only is a preferred implementation of the present invention, and protection scope of the present invention also not only is confined to the foregoing description, and all technical schemes that belongs under the thinking of the present invention all belong to protection scope of the present invention.Should be pointed out that for those skilled in the art in the some improvements and modifications that do not break away under the principle of the invention prerequisite, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (5)
1. the in-line digestion and the pick-up unit of total nitrogen content in the solution, it is characterized in that: it comprises light source (1), digestion instrument (2), condensation reflux device (3), sample detecting mechanism (4) and lamp guide, the top of described digestion instrument (2) links to each other with condensation reflux device (3), be equiped with heating arrangement on the outside surface of digestion instrument (2), lamp guide is inserted in digestion instrument (2) and the condensation reflux device (3), the upper end of lamp guide is corresponding with the detection dish (401) of sample detecting mechanism (4), and the lower end of lamp guide is corresponding with light source (1); Described condensation reflux device (3) comprises condensation chamber (301) and condensate water spacer (302), described condensate water spacer (302) is wrapped on the outside surface of condensation chamber (301), be used for offering water inlet (303) and water delivering orifice (304) on the condensate water spacer (302) of logical chilled water, the lower end of condensation chamber (301) links to each other with digestion instrument (2).
2. the in-line digestion and the pick-up unit of total nitrogen content in the solution according to claim 1, it is characterized in that: described sample detecting mechanism (4) comprises detects control box (405), detection dish (401), drive motor (403) and photoelectric conversion unit (402), detection dish (401) is installed in the detection control box (405) and is fixed on the driving shaft (404) of drive motor (403), photoelectric conversion unit (402) is installed in detection dish (401) and go up detects the top in hole and detected light signal is converted into electric signal and send to and detect control box (405) and handle, and lamp guide is positioned at the below of detection dish (401).
3. the in-line digestion and the pick-up unit of total nitrogen content in the solution according to claim 2, it is characterized in that: offer pilot hole (4011) on the described detection dish (401), detect hole (4012) and reference hole (4013), detect hole (4012) and locate to place the optical filter of 220nm, reference hole (4013) locate to place the optical filter of 275nm.
4. the in-line digestion and the pick-up unit of total nitrogen content in the solution according to claim 1 is characterized in that: the upper end of described condensation chamber (301) is provided with upper head plate (305), is equiped with reduction valve assembly (306) on the upper head plate (305).
5. according to the in-line digestion and the pick-up unit of total nitrogen content in claim 1 or 2 or the 3 or 4 described solution, it is characterized in that: described lamp guide comprises lamp guide transmitter unit (501) and lamp guide receiving element (502), lamp guide transmitter unit (501) be installed in digestion instrument (2) bottom and with the corresponding position of light source (1) on, lamp guide receiving element (502) be installed in digestion pool (202) the top and with sample detecting mechanism (4) corresponding position on.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101105440A (en) * | 2007-08-01 | 2008-01-16 | 山东省科学院海洋仪器仪表研究所 | Method for measuring water body total nitrogen and total phosphorous by digestion spectrophotometry of ultraviolet cooperating with ozone |
| CN101290276A (en) * | 2008-06-13 | 2008-10-22 | 南京工业大学 | Total nitrogen total phosphorus minisize light-catalyzed reaction device |
| CN201335809Y (en) * | 2009-01-13 | 2009-10-28 | 长沙华时捷环保科技发展有限公司 | Device for on-line digesting and detecting total nitrogen content in solution |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101105440A (en) * | 2007-08-01 | 2008-01-16 | 山东省科学院海洋仪器仪表研究所 | Method for measuring water body total nitrogen and total phosphorous by digestion spectrophotometry of ultraviolet cooperating with ozone |
| CN101290276A (en) * | 2008-06-13 | 2008-10-22 | 南京工业大学 | Total nitrogen total phosphorus minisize light-catalyzed reaction device |
| CN201335809Y (en) * | 2009-01-13 | 2009-10-28 | 长沙华时捷环保科技发展有限公司 | Device for on-line digesting and detecting total nitrogen content in solution |
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