CN105372238A - Automated discrete analyzer - Google Patents
Automated discrete analyzer Download PDFInfo
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- CN105372238A CN105372238A CN201510909717.2A CN201510909717A CN105372238A CN 105372238 A CN105372238 A CN 105372238A CN 201510909717 A CN201510909717 A CN 201510909717A CN 105372238 A CN105372238 A CN 105372238A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/00584—Control arrangements for automatic analysers
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Abstract
An automated discrete analyzer comprises a sample holder system, a cleaning system and a detection system. The sample holder system is used for holding a reaction cup which is used for pretreating a sample to be detected. The cleaning system is used for cleaning a container for holding the pretreated sample to be detected. The detection system is used for detecting the sample to be detected in the container. The automated discrete analyzer is characterized in that the cleaning system includes two cleaning lines using different cleaning fluids and the different cleaning fluids are selected through valve control to carry out cleaning operation. According to the automated discrete analyzer, a sample reagent bottle, a sample holder, an instrument cleaning system, a method program library and other parts are improved, automatic analytical ability and testing range of the system are promoted, and analytical testing capability of instruments in a lab are fully performed. The invention is a technological innovation of existing instruments and expands application fields of instrument and equipment.
Description
Technical field
The present invention relates to instrument analysis technology field, relate more specifically to one and be automatically interrupted chemical analyzer.
Background technology
Nitrogen and phosphorus are most important biological elements on the earth, in the research of ecosystem geochemical cycle, there is critical role, in Environmental Analytical Chemistry, the research of more than 75% relates to nitrogen and phosphorus yield, and the content of nitrogen and phosphorous or reserves index have become the important component in environmental monitoring and Environmental Health assessment indicator system.
The problem that nitrogen and phosphorus element content must be considered in measuring comprises: (1) nitrogen, P elements are extensive in distributed in nature, occurrence form abundant, content range is wide, requires nitrogen, testing requirement that the detectability of phosphorus element content assay method meets determined element; (2) there is various ways in nitrogen, P elements, and can change (as nitrified nitrogen in soil and ammoniacal nitrogen with the change of environment between each existence form, can change with the time of soil moisture content, soil microbial activity ability and sample storage), therefore nitrogen, the method for quick of phosphorus element content or instrument is required, to meet the Accurate Determining of multi-form nitrogen, phosphorus element content; (3) nitrogen, P elements are the conventional indexs in environmental chemical analysis, and working sample amount is many, need assay method can be convenient to batch and measure.
Along with making rapid progress of science and technology, the method of traditional labor measurement nitrogen and phosphorus content can not meet the demand of modern scientific research and time, therefore Modern Analytical Chemistry almost employs all technological means, to improve the ageing of nitrogen and phosphorus detection, the sensitivity of measurement result and accuracy.According to solid-liquid gaseous state occurrence form and the estimating precision demand of nitrogen, phosphorus, the instrument of representative has gas chromatography, elemental analyser, mass spectrometer, full-automatic azotometer, chromatography of ions, Continuous Flow Analysis instrument, is interrupted chemical analyzer etc.Wherein gas chromatography is generally used for the nitrogen of mensurated gas composition form, as N
2o etc.; Elemental analyser is generally mainly used in the full nitrogen measuring solid form and liquid form, but its detectability is often higher than the detectability of Environmental Trace element; Chromatography of ions can measure other nitrogen of trace level and phosphorus content, but the requirement of this instrument to sample introduction fluid matrix is stricter, comparatively the destruction of sample introduction liquid to separating column of complex matrices is large, and the introducing of high concentration background value easily causes chromatographic peak to trail, and affects the mensuration of the low ion concentration of other concentration; Full-automatic azotometer instrument detectability is higher, is unfavorable for the sample determination of low content, and can only measure nitrogen, can not measure phosphorus; Mass spectrometer can measure the sample of the various liquid matrix of trace element, but its cost consumption is very large, is comparatively applicable to batch and multi objective mensuration, a small amount of index and a small amount of sample determination high cost.Therefore current to nitrogen, phosphorus element content measure in, with Continuous Flow Analysis instrument and discontinuity chemical analyzer comparatively applicable.The advantage of Continuous Flow Analysis instrument is multi objective Simultaneously test, mensuration robotization is strong, estimating precision is high, and shortcoming is that all reaction systems are in same closed system, and because liquid communication pipeline is long, system is once contaminated cleaning is difficult; Continuous Flow Analysis instrument bubble segmentation sample and reactant liquor, and all reagent and sample are in same closed duct, easily cause baseline wander.
Full-automatic interruption chemical analyzer (AutoDiscreteAnalyzers) is the new breakthrough of current ion domain analysis technology.In this technical development process, experienced by 1st generation circulation technology, be progressively developed to 2nd generation reading technology now.Features such as it has that analysis efficiency is high, analytical precision is large, automatic capability is strong, reagent consumption is few, and can the chemical analyzer of the variform content such as Simultaneously test nitrogen phosphorus, to become in like product letter valency than the highest a nitrogen and phosphorus content analytical instrument.
But there are following technical matters in actual use: (1) is when expanding the mensuration of the elements such as soil nitrogen phosphorus to by sensing range, measure nitrogen and measure phosphorus cuvette cleaning fluid inconsistent, cause once assay method changes must carry out cleaning fluid system conversion, complex operation; (2) when basic soil rapid available phosphorus measures, leaching liquor is alkalescence, and nitrite ion is acid, and in adjustment reacting liquid pH value process, reactant liquor will produce bubble, and reaction liquid, once overflow, will affect test result; (3) instrument does not configure the soil liquid and comprises the constituent content method for measuring programs such as nitrogen phosphorus.Below what time become this instrument of restriction and expanded the important bottleneck factor becoming environmental chemical analysis instrument by Water Test Kits.
Summary of the invention
In view of this, one is the object of the present invention is to provide automatically to be interrupted chemical analyzer.
To achieve these goals, the invention provides one and be automatically interrupted chemical analyzer, comprising:
Specimen holder system, for placing response cup, described reaction cup is used for carrying out pre-service to detected sample;
Purging system, for hold through pre-service, etc. the container of detected sample to be detected clean;
Detection system, for detecting the detected sample in described container;
It is characterized in that, described purging system comprises the two cover detergent lines adopting different cleaning fluid, selects to adopt different cleaning fluid to carry out cleaning operation by Valve controlling.
Wherein, described valve is four-way valve, is communicated with respectively with another two for two of controlling in described four-way valve four outlet.
Wherein, described specimen holder system comprises back and forth shakes functional module, for increasing reaction cup reciprocating frequency to eliminate bubble.
Wherein, the outer wall shape of described reaction cup is the pipe that stage casing is circumscribed with spherical, caliber and expands gradually.
Wherein, in described full-automatic interruption chemical analyzer containing being applicable to method program nitrogen in the soil liquid or leaching liquor, P elements being carried out to assay.
Known based on technique scheme, full-automatic intermittent analysis instrument of the present invention solves affects several key factors that this instrument realizes automation process, comprise: (1) cleaning fluid is incompatible between different testing index, cause affecting its multi-method Simultaneously test; (2) in reactant liquor to nitrite ion process cannot the row's of completing bubble and and pH value adjustment etc.; (3) the analytical approach program disappearance or the problem such as imperfection that are applicable to instrument are improved, full-automatic intermittent analysis instrument automatic analysis ability and test specification are promoted, to give full play to the analytical test ability of instrument from the angle of improvement sample reagent bottle, specimen holder, instrument purging system method for building up routine library.The present invention improves experimental technique and pertinent instruments simultaneously, is not only the technological innovation to existing instrument, can expand again the application of instrument and equipment.Significantly can promote the nitrogen and phosphorus content quality measurement under the different occurrence form such as soil, water body and service efficiency, for further investigated nitrogen phosphorus ecosystem biogeochemical cycle feature and process, the sustainable development of maintenance agricultural high-effiency, improve the correlative studys such as evaluation on Ecosystem Health technical support service be provided.
Accompanying drawing explanation
Fig. 1 is the Technology Roadmap of the improvement project of the full-automatic intermittent analysis instrument of the present invention;
Fig. 2 is the pipeline design figure of cuvette purging system of the present invention;
Fig. 3 is the change schematic diagram that reaction cup structure of the present invention is improved.
Embodiment
For making the object, technical solutions and advantages of the present invention clearly understand, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in further detail.
Full-automatic interruption chemical analyzer is by a kind of analytical test means of colorimetric analysis robotization, it simulates manpower comparing color method completely, sample, reagent and developer are added in cuvette and produces color reaction, its concentration and color proportional, penetrating light intensity is detected through tintmeter, obtain corresponding absorbance, more automatically calculate corresponding concentration by typical curve.Pass through sample introduction arm and conputer controlled in steps, fully realize mechanization and intellectuality.
Full-automatic interruption chemical analyzer tool has the following advantages: (1) is short for analysis time, and each sample determination needs time about 2min; (2) maneuverability, is applicable to batch sample mensuration and is also applicable to a small amount of sample determination; (3) each sample is all in one independently in reaction system, and sample cup, reaction tank etc. be easy to cleaning, be convenient for changing and can prevent cross pollution, avoid baseline wander; (4) can to design program the multiple Testing index of sequentially determining; (5) control program is open, can require design according to user and select diverse ways program, complete fast accurate and measure; (6) sample used, reagent and cleaning liquid measure are few, economy, environmental protection, cost-saving; (7) adopt instrumental analysis, avoid manual operation error, measurement result favorable reproducibility.
But by be automatically interrupted chemical analyzer be applied to the mensuration of the elements such as Nitrogen In Soils phosphorus time, wherein also there are some technical matterss as described above, namely the present invention makes, full-automatic interruption chemical analyzer of the present invention particularly for described technical matters, comprising:
Specimen holder system, for placing response cup, reaction cup is used for carrying out pre-service to detected sample;
Purging system, for hold through pre-service, etc. the container of detected sample to be detected clean;
Detection system, for detecting the detected sample in container;
Wherein, purging system comprises the two cover detergent lines adopting different cleaning fluid, selects to adopt different cleaning fluid to carry out cleaning operation by Valve controlling.
As preferably, valve is four-way valve, is communicated with respectively with another two for two of controlling in four-way valve four outlet.
As preferably, specimen holder system comprises back and forth shakes functional module, for increasing reaction cup reciprocating frequency to eliminate bubble.
As preferably, purging system is threaded a pipe by washer bottle, wash liquid stream, peristaltic pump, four-way valve, purge pipe etc. form, its principle of work is under the effect of peristaltic pump, produce negative pressure, by cleaning fluid in washer bottle by washer bottle pump to pipe blow-through, and along stationary pipes in the container flowing to detected sample place, cleaning container is clean, and by cleaning fluid collect, from another pipe to be discharged in waste liquid cylinder; Described four-way valve is made up of four outlets and a unicom pipeline, it is characterized in that cleaning fluid forms path when a and b is exported UNICOM by unicom pipeline, c and d exports self-closed, formed closed circuit, cleaning fluid can only be passed to assigned address in path, and does not flow in closed circuit; When cross over pipe is to when turning c and d two outlet, c and d two goes out interruption-forming path, and it is closed circuit that a and b two goes out interruption-forming, unicom pipeline UNICOM another one cleaning fluid bottle, and instrument realizes automatically not completing binary purging system via manual operation and automatically switches.
As preferably, the side profile of reaction cup is the isosceles trapezoid that polygon or the arc convex outwards expanded is contained in hypotenuse stage casing; Further preferably, the outer wall shape of reaction cup is the pipe that stage casing is circumscribed with spherical, caliber and expands gradually.
As preferably, this is automatically interrupted in chemical analyzer containing the method program being applicable to carrying out nitrogen in the soil liquid or leaching liquor, P elements assay.
As preferably, this is automatically interrupted chemical analyzer and also comprises sampling apparatus, for automatically taking out detected sample and transferred in the container detected sample to be detected such as holding from reaction cup.
Transform example as below with the full-automatic interruption chemical analyzer of Smartchem140 model, explanation is further elaborated to technical scheme of the present invention.
1, the transformation of cleaning station module
Smartchem140 unitary purging system is converted to binary purging system, realizes the Simultaneous Determination of nitrogen P elements, improve instrumental detection efficiency.
Smartchem140 discontinuous chemical analysis instrument cleaning station has four passages, can only run a set of purging system.Its structure is two sample pin cleaning fluids, a cuvette cleaning fluid and a deionized water, be respectively used to cleaning suction needle and cuvette, they correspond to four cleaning needles on cleaning station respectively, if if add a passage, and do not need cleaning station to add a cleaning needle, just need to add a three-way pipe and four-way valve on flushing channel, by the closedown of software control three-way pipe and four way valve, to control, final what draw is any cuvette cleaning fluid.Concrete resolving ideas of the present invention is: three-way pipe and four-way valve will be placed on suitable position by (1), and the hardware of minimum change instrument is wanted in this position; (2) switching of setting up cuvette cleaning has software automatically to complete, and reduces over many artificial inputs, to reduce labour cost.
As shown in Figure 2, in the present invention, with the addition of a set of pipe blow-through, add four-way valve and complete pipeline enclosure switching, add alternate modular in control software design program to control the switching between the pipeline module of new interpolation and grand master pattern block.In Fig. 2, V is cleaning fluid (cleaningsolution), IV is lauryl sodium sulfate; No. 1 is cuvette to be cleaned.When a and b hole is connected by four-way valve UNICOM position, IV washer bottle is connected in system, and in IV washer bottle, liquid can enter corresponding pipeline under the effect of peristaltic pump, and plays cleanup action; Now V washer bottle is in off state in systems in which, does not have liquid and enter instrument in the V washer bottle of its correspondence.When c and d hole is connected, be connected in system in V washer bottle, the liquid in now V washer bottle can enter system under the effect of peristaltic pump; And the liquid in IV washer bottle is in off state in systems in which, system can not be entered.
2, the transformation of specimen holder system
The leaching liquor that full-automatic interruption chemical analyzer measures or the Acidity Range that boils liquid of disappearing often inconsistent with the Acidity Range of assay method, therefore often adjust ph is adopted in conventional determining, make leaching liquor or disappear to boil liquid pH value and be just in color range, add developer again, but may be along with in adjust ph process, as produced the chemical reactions such as bubble, therefore, sample is after pre-treatment, can not directly go up machine process, also need further to add medicine adjust ph, if this process can process on the enterprising line of instrument, significantly can reduce the test duration, increase work efficiency.But also do not have a instrument can complete above-mentioned work at present.
Resolving ideas of the present invention is, by improving reaction cup structure and reaction cup shelf structure, increases space in reaction cup, prevent bubble from overflowing, increase reaction glass stand reciprocating frequency and eliminate bubble, thus reach without the need to manual operation, automatically complete the work that reactant liquor adds.
Thus, main improvement of the present invention is: increase in (1) specimen holder and back and forth shake functional module; (2) sample bottle form is transformed, side profile contains the trapezoidal of circular protrusions by the original trapezoidal hypotenuse central part that becomes, increase sample bottle reaction compartment, make reactant liquor in sample bottle be unlikely to overflow under the violent chemical reaction conditions such as generation bubble and affect measurement result.Thus the intelligent adaptibility to response that instrument reacts special chemical can be improved, improve the work efficiency of sample determination.
3, sample evaluation procedures storehouse is set up
In environmental chemical analysis, because test sample content range is wide, test sample complex shape, for different sample features, that disposal route formulates the experimental technique routine library being applicable to instrumental analysis is very necessary.Method base mainly comprises following components: sample tests method program under (1) low content height background condition; (2) the assay method program of nitrogen phosphorus working sample under different occurrence patterns.Method base Establishing process: the establishment being completed a kind of method by testing index pretreatment process, experimental technique program composition and test method control experiment.
The present invention designs and with the addition of the control program storehouse of the multi-form nitrogen and phosphorus content mensuration meeting GB or industry standard, meets content in carrier deposited by instrument in different occurrence form and tax mensuration requirement to nitrogen phosphorus, expands automatic detectability and the scope of instrument.
Following table is the technical indicator contrast that project completes front and back instrument and equipment function:
As can be seen here, innovation point of the present invention is mainly:
1. on the basis not increasing test module, increase the ability that instrument measures different index simultaneously;
2. the chemical reaction produced in elimination sample pipetting volume process is on the impact of test result.
Above-described specific embodiment; object of the present invention, technical scheme and beneficial effect are further described; be understood that; the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. be automatically interrupted a chemical analyzer, comprise:
Specimen holder system, for placing response cup, described reaction cup is used for carrying out pre-service to detected sample;
Purging system, for hold through pre-service, etc. the container of detected sample to be detected clean;
Detection system, for detecting the detected sample in described container;
It is characterized in that, described purging system comprises the two cover detergent lines adopting different cleaning fluid, selects to adopt different cleaning fluid to carry out cleaning operation by Valve controlling.
2. be automatically interrupted chemical analyzer as claimed in claim 1, it is characterized in that, described valve is four-way valve, is communicated with respectively with another two for two of controlling in described four-way valve four outlet.
3. be automatically interrupted chemical analyzer as claimed in claim 1, it is characterized in that, described specimen holder system comprises back and forth shakes functional module, for increasing reaction cup reciprocating frequency to eliminate bubble.
4. be automatically interrupted chemical analyzer as claimed in claim 1, it is characterized in that, the side profile of described reaction cup is the isosceles trapezoid that polygon or the arc convex outwards expanded is contained in hypotenuse stage casing.
5. be automatically interrupted chemical analyzer as claimed in claim 4, it is characterized in that, the outer wall shape of described reaction cup is the pipe that stage casing is circumscribed with spherical, caliber and expands gradually.
6. be automatically interrupted chemical analyzer as claimed in claim 1, it is characterized in that, containing being applicable to method program nitrogen in the soil liquid or leaching liquor, P elements being carried out to assay in described full-automatic interruption chemical analyzer.
7. be automatically interrupted chemical analyzer as claimed in claim 1, it is characterized in that, described full-automatic interruption chemical analyzer also comprises sampling apparatus, for automatically taking out detected sample and to hold described in being transferred to etc. in the container of detected sample to be detected from described reaction cup.
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| CN201510909717.2A CN105372238B (en) | 2015-12-10 | 2015-12-10 | Full-automatic interruption chemical analyzer |
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| CN201510909717.2A CN105372238B (en) | 2015-12-10 | 2015-12-10 | Full-automatic interruption chemical analyzer |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114965845A (en) * | 2022-05-13 | 2022-08-30 | 上海赫冠仪器有限公司 | Kjeldahl apparatus capable of eliminating error caused by long time interval in continuous detection |
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| CN105372238B (en) | 2018-08-03 |
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