CN1963472A - Method for examining deposit or organic matter content in soil by ozone oxidation - Google Patents
Method for examining deposit or organic matter content in soil by ozone oxidation Download PDFInfo
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- CN1963472A CN1963472A CN 200610069599 CN200610069599A CN1963472A CN 1963472 A CN1963472 A CN 1963472A CN 200610069599 CN200610069599 CN 200610069599 CN 200610069599 A CN200610069599 A CN 200610069599A CN 1963472 A CN1963472 A CN 1963472A
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Abstract
This invention provides one method to test deposition or earth organic content by use of ozone oxidation light, which comprises the following steps: a, using ozone generator for ozone sent to reaction chamber; b, processing water drying and grinding and filtering of sample to be tested sent to reaction chamber; c, mixing the zone and sample in the reaction chamber to detect light signal from detect window; d, using photoelectricity amplifying tube to collect light intensity signals for computing, correction, display and printing.
Description
Technical field
The present invention relates to environmental monitoring and agrotechnique, specifically utilize the method for ozone oxidation luminescence principle detection sediment or organic matter content in soil,
Background technology
Present domestic detection sediment, claim substrate again, or the method for organic matter content in soil mainly is to carry out in the laboratory, adopt the analytical approach of the potassium bichromate titrimetric method of standard GB 9834-88 " soil organism determination method " and the standard NY/T85-1988 of the Ministry of Agriculture " soil organism determination method " recommendation, this method length that expends time in, analytic process is numerous and diverse, to operating personnel require height, environmental baseline harshness, reagent consumption big, produce secondary pollution etc.For the occasion that requires on-the site analysis, for example: be subjected to the region of organic pollutants, the contaminated degree difference of diverse location, difference is bigger, when needing to monitor in time and in a large number, this method is very restricted and retrains at aspects such as personnel, time, expenses.Some simple alternative methods exist principle problem and systematic error, have labile factor, and its result's accuracy and representativeness can not get guaranteeing.For sediment and soil organic matter feature, be meant the content and the ratio of active organic matter, organic carbon, organic contaminant, detection method more lacks with inaccurate, simply distinguishes and judges do not have unified standard and scientific quantitative foundation with physics method, chemical method and bioanalysis.
In recent years, along with electronic technology, new material, new technology, the development of new optical device, especially computer technology makes rapid progress, the corresponding appearance of method of adopting the potassium bichromate titrimetric method automatic analyzer and measuring sediment and soil organic matter based on the analyser of automatic titration system, but owing to there is not the support of new principle, some shortcomings of lab analysis have been broken away from though use the instrument of these methods, but the pattern from work on the spot also has a segment distance, big as reagent consumption, personnel require height to Operation and Maintenance, poor stability, sensitivity and resolution are low, the defective that environmental interference etc. are difficult to overcome does not truly realize the pattern of on-the-spot real-time continuous work.
Summary of the invention
In order to solve the problem that prior art exists, the present invention proposes a kind of method of utilizing ozone oxidation luminescence to detect sediment or organic matter content in soil, it can be on-the-spot, in real time, fast detecting sediment or organic matter content in soil and related data, solve that existing method sense cycle is long, expense is high, reagent consumption big and problem such as pollution is arranged, and can carry out more deep research detected object.
In order to reach the purpose that solves the problems of the technologies described above, technical scheme of the present invention is that a kind of method of utilizing ozone oxidation luminescence to detect sediment or organic matter content in soil is characterized in that, testing process utilizes ozone oxidation sediment or organic matter content in soil detector to realize
(1). utilize ozone generator to produce ozone, the concentration of ozone is that 18～25mg/L and flow are 0.5～2l/min, and it is sent into reaction chamber;
(2). sample dehydrate with levigate sieving after, sample is sent into reaction chamber;
(3). ozone and sample carry out hybrid reaction at reaction chamber, guarantee can fully to contact between ozone and the sample, and reaction chamber is carried out the optics sealing, survey luminous signal from detection window;
(4). utilize photomultiplier that the light intensity signal that sent of reaction is gathered, and convert electric signal to and send into the data processing instrument and handle, to the signal of gathering quantize, calculating, correction, demonstration, printout.
In the present invention, also has following technical characterictic: instrument is demarcated, what photoelectric tube was exported is the Strength Changes of luminous signal, what collect is the rule that changes sample and ozone reaction luminous intensity variations in time, should convert the data of organic content to, integration is carried out in the number of the winning the confidence live part of change procedure in time, data as sediment or organic matter content in soil, and compare with the organic content data that national standard method detects with same sample, sample contrast test through a large amount of different organic content, the opening relationships curve is as the nominal data of instrument
Relation between the organic content that the integrated value of the curve that instrument draws and national standard method are measured is linear, configures conversion relation in instrument, directly draws the organic content of sample.
In the present invention, also have following technical characterictic: the ozone passage that reversal valve is formed, earlier ozone is carried out ozone before detecting and clear up, when beginning to detect ozone is imported reaction chamber.
In the present invention, also have following technical characterictic: reaction chamber adopts light-proof material, sample turnover structure takes rubber seal to carry out the sealing of gas and light, multilayer prevents that every the structure of light the light catadioptric from entering reaction chamber, carry out thereby make to be reflected in the dark environment, reach the optics sealing of reaction chamber.
In the present invention, also have following technical characterictic: photomultiplier adopts Japanese shore pine Photosensor Modules H5784 Series.
The contrast of this method and existing several method is as follows:
| The contrast feature | Laboratory method | Solid TOC/ U.S. | This method |
| Measurement range g/kg | 0.1-150 | 0.05-3 | 0.5-500 |
| Measure required time | 240 minutes | 8-31 minute | 15 minutes |
| Whether need reaction reagent | Need | Need | Do not need |
| Whether secondary pollution is arranged | Have | Have | No |
| Environment for use | Only for the laboratory | Laboratory environment | On-the-spot |
| To operating personnel's requirement | The professional | The professional | Simple training |
The method of detection sediment of the present invention or organic matter content in soil, it is the important component part in the environmental monitoring system, it is based on the ozone oxidation luminescence principle and carries out, being using ozone reacts as strong oxidizer and sediment (substrate) or pedotheque, by the low-light photoelectric conversion technique light signal that produces in the course of reaction is detected and to pick up, through amplify, quantize, and machine data correcting process as calculated, draw the data of sediment (substrate) or organic matter content in soil.
The present invention utilizes the ozone oxidation luminescence principle to detect the method for sediment or organic matter content in soil, need not add reagent, do not produce secondary pollution, avoided conventional method to require the high shortcoming of operating conditions, can detect sediment or organic matter content in soil and feature accurately and rapidly, can be at the medium-term and long-term reliably working of common outdoor environment, the portable occasions such as vehicle-mounted, boat-carrying, factory and laboratory that are suitable for are used, and can carry out scene, real-time measurement to the target that needs are monitored.This method has changed the index monitoring means of existing sediment or organic matter content in soil, promptly adopts on-site sampling, laboratory to carry out chemico-analytic conventional test methodologies for a long time, can form new detection principle and method.Deepen the understanding organic content and corresponding index ability and can carry out more deep research.
Description of drawings
Below in conjunction with drawings and Examples the present invention is described in detail.
Fig. 1 is the process flow diagram that utilizes the inventive method to detect;
Fig. 2 is the block diagram that utilizes the detection system of the inventive method;
Fig. 3 is critical piece structure principle charts such as reaction chamber;
In Fig. 3: 1-ozone gas; 2-reversal valve 1; 3-reaction chamber air intake opening; 4-reaction chamber; 5-sample; 6-detecting window; 7-photomultiplier; 8-reaction chamber gas outlet; 9-reversal valve B; 10-clear up the chamber to ozone.
Fig. 4 is the luminous curve map for example that ozone oxidation sediment or soil produce;
Fig. 5 is dissimilar soil testing result curve contrast figure;
Fig. 6 is the concentration and the integral area table of comparisons.
Embodiment
Referring to Fig. 1, utilize the ozone oxidation luminescence principle to detect the method for sediment or soil (hereinafter to be referred as sample) organic content, its principle flow chart is as shown in Figure 1.
Air produces ozone gas through filtering and drying device enters ozone generator, enters reversal valve 1 through air pump, and reversal valve does not lead to ozone and clears up the chamber when test begins, and receiving commutates behind the initiation command enters the example reaction chamber.Testing sample is put into instrument, instrument dehydrates, levigate sieve, take by weighing fixing weight after, send into the example reaction chamber.Ozone gas enters through reversal valve after receiving commencing signal, and ozone and sample react, and produces chemiluminescence.Photomultiplier is surveyed luminous signal, shows the information of test result through opto-electronic conversion and data processing.
Referring to Fig. 2, testing process realizes with ozone oxidation sediment or organic matter content in soil detector.The composition frame chart of instrument as shown in Figure 2.
Automatically the sampling system sends sample into the example reaction chamber, ozone and sample react, the light signal that produces sees through from the window of reaction chamber wall, (Japanese shore pine Photo sensor Modules H5784 Series) gathers amplification by optical detecting gear-photomultiplier, and converts electric signal to and send into the microcomputer data handling system; Utilize the microcomputer data handling system, realize Signal Processing by software programming, according to the signal power, the content of organic matter of judging sample in conjunction with other features such as area, maximal value etc. the line output of going forward side by side shows.Demarcate the update the system error with standard model.
Referring to Fig. 3, the ozone gas that ozone generator produces pressurizes through air pump, and sequence number 1 ozone gas enters reversal valve 1 from figure, and reversal valve is opened the direction to the figure bottom when sample is not ready for, directly enters ozone and clears up the chamber ozone gas is cleared up.After sample is ready to, send signal and make the reversal valve action, ozone gas is imported reaction chamber air intake opening, at this moment opening entry reaction signal.Sample 5 is evenly placed in reaction chamber 4, produces chemiluminescence after touching ozone gas.The light that sends is received by photomultiplier through behind the detecting window, converts electric signal to and handles.Reacted ozone gas is synchronization actions through reaction chamber 4 gas outlets to 2, two reversal valves of reversal valve, makes redundant ozone gas enter ozone and clears up the chamber and clear up.
The measure of optics sealing: during reaction chamber 4 designs, adopt light-proof material, sample turnover structure takes rubber seal to carry out the sealing of gas and light, multilayer prevents that every the structure of light the light catadioptric from entering reaction chamber, carry out thereby make to be reflected in the dark environment, reach the optics sealing of reaction chamber.
Light-proof material is the stainless steel metal plate among the present invention, and described multilayer adopts the stainless steel metal plate that staggers every the structure of light.
The curve horizontal ordinate is the time among Fig. 4, and unit is second, and ordinate is the photomultiplier output voltage, and unit is a millivolt, representative be the ozone oxidation sample time luminous intensity.From curve as can be seen, the characteristic factors such as area that surround of ascending velocity, maximal value, decline rate, duration and curve can corresponding sample in different content of material data.
As shown in Figure 4, the luminosity curve that ozone oxidation sediment or soil produce, can be divided into the stages such as beginning is luminous, ascending velocity, peak, decline rate, deadline, the feature of these different phases, as size, slope, perdurability, area, relative value etc., can represent organic content different in the sample or ratio respectively, thereby represent different organic features, further the component in the analytic sample.
Referring to Fig. 4, river bed, the Yellow River sand and city grassland soil are detected according to method of the present invention respectively, and contrast is carried out synchronous detection with national standard method in Shandong Province's ocean monitoring technologytechnologies key lab, experiment shows, luminosity curve integral area (millivolt * second) difference that the inventive method detects two kinds of samples that draw is obvious, the variation tendency that its variation tendency and national standard method detect the content of organic matter (%) that draws is identical, illustrates that method of the present invention can distinguish the sample of two kinds of different contents.It is as follows to detect the data list contrast:
| The contrast index | The area that the inventive method draws | The organic matter that standard method detects |
| River bed, the Yellow River sand | 118 millivolts * second | 3.0％ |
| The city grassland soil | 246 millivolts * second | 4.3％ |
Referring to Fig. 6, utilize the pedotheque of the different organic carbon contents of preparation to carry out the ozone oxidation luminescence test, draw the ozone oxidation luminescence curve of variable concentrations organic carbon, the area of curvilinear integral (millivolt * second) and organic carbon concentration (%) contrast relationship such as following table:
| Organic carbon concentration | 1.81 | 1.86 | 1.89 | 1.93 | 1.98 |
| The curvilinear integral area | 29.3 | 30.5 | 31.4 | 32.7 | 34.0 |
Draw out curve according to the table of comparisons as figure below, as can be seen, containing the concentration of organic carbon and the integral area of ozone oxidation sample luminosity curve in the pedotheque has good linear relationship, and the R2 value of its regression curve approaches 1, and two kinds of methods of this relation explanation can be good at correspondence and conversion.
The inventive method embodiment 1
(1). utilize ozone generator to produce ozone, the concentration of ozone is that 18mg/L and flow are 0.5l/min, and the ozone passage that reversal valve is formed carries out ozone with ozone earlier before detecting and clears up, and when beginning to detect ozone is imported reaction chamber.
(2). sample dehydrate with levigate sieving after, sample is sent into reaction chamber;
(3). ozone and sample carry out hybrid reaction at reaction chamber, guarantee can fully to contact between ozone and the sample, and reaction chamber is carried out the optics sealing, survey luminous signal from detection window;
(4). utilize photomultiplier that the light intensity signal that sent of reaction is gathered, and convert electric signal to and send into the data processing instrument and handle, to the signal of gathering quantize, calculating, correction, demonstration, printout.
Instrument is demarcated; What photoelectric tube was exported is the Strength Changes of luminous signal; What collect is the rule of temporal evolution sample and ozone reaction luminous intensity variations; Should convert the data of content of organics to; The live part of the number of winning the confidence temporal evolution process carries out integration; Data as deposit or organic matter content in soil; And compare with the content of organics data that national standard method detects with same sample; Sample contrast test through a large amount of different content of organics; The opening relationships curve is as the nominal data of instrument
Relation between the organic content that the integrated value of the curve that instrument draws and national standard method are measured is linear, configures conversion relation in instrument, directly draws the organic content of sample.
The inventive method embodiment 2
(1). utilize ozone generator to produce ozone, the concentration of ozone is that 25mg/L and flow are 2l/min, and the ozone passage that reversal valve is formed carries out ozone with ozone earlier before detecting and clears up, and when beginning to detect ozone is imported reaction chamber.
(2). sample dehydrate with levigate sieving after, sample is sent into reaction chamber;
(3). ozone and sample carry out hybrid reaction at reaction chamber, guarantee can fully to contact between ozone and the sample, and reaction chamber is carried out the optics sealing, survey luminous signal from detection window;
(4). utilize photomultiplier that the light intensity signal that sent of reaction is gathered, and convert electric signal to and send into the data processing instrument and handle, to the signal of gathering quantize, calculating, correction, demonstration, printout.
Instrument is demarcated; What photoelectric tube was exported is the Strength Changes of luminous signal; What collect is the rule of temporal evolution sample and ozone reaction luminous intensity variations; Should convert the data of content of organics to; The live part of the number of winning the confidence temporal evolution process carries out integration; Data as deposit or organic matter content in soil; And compare with the content of organics data that national standard method detects with same sample; Sample contrast test through a large amount of different content of organics; The opening relationships curve is as the nominal data of instrument
Relation between the organic content that the integrated value of the curve that instrument draws and national standard method are measured is linear, configures conversion relation in instrument, directly draws the organic content of sample.
The inventive method embodiment 3
(1). utilize ozone generator to produce ozone, the concentration of ozone is that 21mg/L and flow are 1.5l/min, and the ozone passage that reversal valve is formed carries out ozone with ozone earlier before detecting and clears up, and when beginning to detect ozone is imported reaction chamber.
(2). sample dehydrate with levigate sieving after, sample is sent into reaction chamber;
(3). ozone and sample carry out hybrid reaction at reaction chamber, guarantee can fully to contact between ozone and the sample, and reaction chamber is carried out the optics sealing, survey luminous signal from detection window;
(4). utilize photomultiplier that the light intensity signal that sent of reaction is gathered, and convert electric signal to and send into the data processing instrument and handle, to the signal of gathering quantize, calculating, correction, demonstration, printout.
Instrument is demarcated; What photoelectric tube was exported is the Strength Changes of luminous signal; What collect is the rule of temporal evolution sample and ozone reaction luminous intensity variations; Should convert the data of content of organics to; The live part of the number of winning the confidence temporal evolution process carries out integration; Data as deposit or organic matter content in soil; And compare with the content of organics data that national standard method detects with same sample; Sample contrast test through a large amount of different content of organics; The opening relationships curve is as the nominal data of instrument
Relation between the organic content that the integrated value of the curve that instrument draws and national standard method are measured is linear, configures conversion relation in instrument, directly draws the organic content of sample.
The above only is preferred embodiment of the present invention, is not to be the restriction of the present invention being made other form, and any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the equivalent embodiment of equivalent variations.But every technical solution of the present invention content that do not break away to any simple modification, equivalent variations and remodeling that above embodiment did, still belongs to the protection domain of technical solution of the present invention according to technical spirit of the present invention.
Claims (5)
1. a method of utilizing ozone oxidation luminescence to detect sediment or organic matter content in soil is characterized in that, testing process utilizes ozone oxidation sediment or organic matter content in soil detector to realize,
(1). utilize ozone generator to produce ozone, the concentration of ozone is that 18～25mg/L and flow are 0.5～21/min, and it is sent into reaction chamber;
(2). sample dehydrate with levigate sieving after, sample is sent into reaction chamber;
(3). ozone and sample carry out hybrid reaction at reaction chamber, guarantee can fully to contact between ozone and the sample, and reaction chamber is carried out the optics sealing, survey luminous signal from detection window;
(4). utilize photomultiplier that the light intensity signal that sent of reaction is gathered, and convert electric signal to and send into the data processing instrument and handle, to the signal of gathering quantize, calculating, correction, demonstration, printout.
2. method according to claim 1, it is characterized in that instrument is demarcated, what photoelectric tube was exported is the Strength Changes of luminous signal, what collect is the rule that changes sample and ozone reaction luminous intensity variations in time, should convert the data of organic content to, integration is carried out in the number of the winning the confidence live part of change procedure in time, data as sediment or organic matter content in soil, and compare with the organic content data that national standard method detects with same sample, sample contrast test through a large amount of different organic content, the opening relationships curve is as the nominal data of instrument
Relation between the organic content that the integrated value of the curve that instrument draws and national standard method are measured is linear, configures conversion relation in instrument, directly draws the organic content of sample.
3. method according to claim 2 is characterized in that the ozone passage that reversal valve is formed, and earlier ozone is carried out ozone before detecting and clears up, and when beginning to detect ozone is imported reaction chamber.
4. method according to claim 3, it is characterized in that reaction chamber adopts light-proof material, sample turnover structure takes rubber seal to carry out the sealing of gas and light, multilayer prevents that every the structure of light the light catadioptric from entering reaction chamber, carry out thereby make to be reflected in the dark environment, reach the optics sealing of reaction chamber.
5. method according to claim 4 is characterized in that photomultiplier adopts Japanese shore pine Photo sensor Modules H5784 Series.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101915723A (en) * | 2010-07-21 | 2010-12-15 | 山东省科学院海洋仪器仪表研究所 | Method and device for measuring total organic carbon in waterbody |
| CN102621046A (en) * | 2010-07-21 | 2012-08-01 | 山东省科学院海洋仪器仪表研究所 | Method for measuring total organic carbon in water body |
| CN104089932A (en) * | 2014-06-30 | 2014-10-08 | 山东省科学院海洋仪器仪表研究所 | Ozone oxidation luminescent spectrum-based in-situ rapid measurement method and device of soil nutrients |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102788783B (en) * | 2012-08-24 | 2015-04-01 | 山东省科学院海洋仪器仪表研究所 | Method for detecting organic matter composition by ozone oxidation luminescent method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5470754A (en) * | 1992-06-01 | 1995-11-28 | The Coca-Cola Company | Method and system for sampling and determining the presence of compounds |
| US6105416A (en) * | 1998-10-16 | 2000-08-22 | Geo-Centers, Inc. | Ethylene monitoring and control system |
| JP2002022662A (en) * | 2000-07-07 | 2002-01-23 | Hamamatsu Photonics Kk | Luminous-reaction measuring apparatus |
| EP1243918A3 (en) * | 2001-03-23 | 2004-10-06 | Instrumentarium Corporation | An improved chemiluminescent gas analyzer |
| CN2589971Y (en) * | 2002-12-25 | 2003-12-03 | 中国科学院安徽光学精密机械研究所 | Air quality nitrogen oxide automatic monitoring apparatus |
| CN1177216C (en) * | 2003-01-30 | 2004-11-24 | 山东省科学院海洋仪器仪表研究所 | Method for measuring chemistry oxygen consumption of sea water based on luminous intensity principle of ozone oxidation |
| CN100476409C (en) * | 2005-08-29 | 2009-04-08 | 山东省科学院海洋仪器仪表研究所 | Method for measuring total organic carbon in water body by chemiluminescence in ozone oxidizing process |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101915723A (en) * | 2010-07-21 | 2010-12-15 | 山东省科学院海洋仪器仪表研究所 | Method and device for measuring total organic carbon in waterbody |
| CN102621046A (en) * | 2010-07-21 | 2012-08-01 | 山东省科学院海洋仪器仪表研究所 | Method for measuring total organic carbon in water body |
| CN101915723B (en) * | 2010-07-21 | 2012-09-05 | 山东省科学院海洋仪器仪表研究所 | Method and device for measuring total organic carbon in waterbody |
| CN104089932A (en) * | 2014-06-30 | 2014-10-08 | 山东省科学院海洋仪器仪表研究所 | Ozone oxidation luminescent spectrum-based in-situ rapid measurement method and device of soil nutrients |
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