CN205157434U - Online metal analysis system - Google Patents
Online metal analysis system Download PDFInfo
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- CN205157434U CN205157434U CN201520863252.7U CN201520863252U CN205157434U CN 205157434 U CN205157434 U CN 205157434U CN 201520863252 U CN201520863252 U CN 201520863252U CN 205157434 U CN205157434 U CN 205157434U
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Abstract
The utility model discloses an online metal analysis system, online metal analysis system for metallic element's on -line measuring, including specimen cup, spectrum appearance and the air feeder who communicates in order, the spectrum appearance is connected with an industry control is electromechanical the await measuring digestion instrument of the chaff interference that metal element content detected that it is used for eliminating the effects of the act to be provided with on the middle route between specimen cup and the spectrum appearance, the specimen cup with it has and is used for await measuring metallic element's an enrichment device of enrichment to go back the parallel connection on the middle route between the digestion instrument, digestion instrument and enrichment device respectively with the industry control is electromechanical to be connected. Adopt the utility model discloses, can detect at all metallic element of wire pair, have low detecting limit's characteristics.
Description
Technical field
The utility model belongs to metallic element detection field, is specifically related to a kind of online metal analysis system.
Background technology
According to the difference of measuring principle, existing online heavy metal analyser is main comprises two kinds: one is colourimetry (or spectrophotometric method), it is the absorption utilizing the light of material to a certain specific wavelength in ultraviolet-visible light district to have, and absorbance (light of absorption) and the concentration of material are certain relation, thus quantitative test is carried out to material, but there is the higher problem of detection limit.Another kind is Anodic stripping, is to carry out quantitatively and qualitative analysis according to the redox property of material, and the detection limit of this quasi-instrument can be accomplished very low, be mainly used in the on-line monitoring of surface water, but instrument repeatability is poor, range of application is restricted simultaneously, can only analysis heavy metal element.
In addition, a small amount of online heavy metal analyser is also had to adopt Pressurized sample digestion and x-ray fluorescence method, but the instrument of Pressurized sample digestion can only be used for analyzing specific element, as mercury, and x-ray fluorescence method detects limit for height, cannot meet the requirement of surface water water quality monitoring, the application on site of this two quasi-instrument is all very limited, and quantity is few.
And the method that the Analysis of Heavy Metal instrument in laboratory uses, except aforesaid colourimetry and Anodic stripping, main also have atomic absorption spectrography (AAS) (AAS), microwave plasma atomic emission spectroscopy method (MP-AES), spectrographic technique and mass spectrum (MS) methods such as inductively coupled plasma emission spectrography (ICP-AES).This quasi-instrument generally has good stability, and can analyze the advantage of multiple metallic element simultaneously, but due to spectroscopic methodology instrument and the requirement of mass spectroscopy instrument to operator and sample all higher, generally adopt manual operation, therefore not easily realize in linearize.
Utility model content
In order to solve the problem, the purpose of this utility model is: provide a kind of online metal analysis system, both can detect all metallic elements online, and also have the feature that detection limit is low.
For achieving the above object, the utility model is achieved by following scheme:
Online metal analysis system described in the utility model, for the on-line checkingi of metallic element, comprises the sample cup, spectrometer and the feeder that are communicated with in turn; Described spectrometer is electrically connected with an industrial computer, the via intermedia between described sample cup and spectrometer is provided with a digestion instrument of the chaff interference detected for metal element content to be measured of eliminating the effects of the act; Via intermedia between described sample cup and described digestion instrument is gone back and is connected with the enriching apparatus for enrichment metallic element to be measured; Described digestion instrument and enriching apparatus are electrically connected with described industrial computer respectively.
Further, described feeder is electrically connected with described spectrometer.
Further, described feeder is electrically connected with described industrial computer.
Further, be provided with in described enriching apparatus for the exchange column of adsorbing metal element with for providing the elution mechanism of wash-out adsorbing metal element; The packing material adopted in described exchange column is ion exchange resin, chelating resin or synthesis modification resin.
Further, described sample cup front end is also communicated with for the pretreatment unit to testing sample coarse filtration.
Further, described pretreatment unit is electrically connected with described industrial computer.
Further, described feeder comprises nitrogen gas generator and argon gas steel cylinder.
Further, described spectrometer is microwave plasma atomic emission spectroscopy instrument.
Further, in described microwave plasma atomic emission spectroscopy instrument, be provided with microwave magnetron, formed in order to excite and maintain nitrogen plasma.
Further, described digestion instrument is high temperature acidolysis or ultraviolet acidolysis for eliminating the mode of clearing up of chaff interference.
Compared with existing, the beneficial effects of the utility model are:
Online metal analysis system described in the utility model, by setting up digestion instrument and enriching apparatus, and mate industrial computer control, wherein, industrial computer can control all devices or instrument performs detection according to pre-set programs, thus achieves in linearize; Described digestion instrument can remove the chaff interference in solution to be measured, the metallic element that described enriching apparatus requires to meet part high detection, to testing liquid through absorption, wash-out, to improve the content of metallic element to be measured to detection limit, analyze finally by spectrometer, both ensure that the impact from other chaff interferences in analytic process, also meet the requirement that detection limit is low.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, embodiment of the present utility model is described in further detail, wherein:
Fig. 1 is that in the described online metal analysis system of the utility model embodiment 1, pipeline connects schematic block diagram;
Fig. 2 is that in the described online metal analysis system of the utility model embodiment 1, circuit connects schematic block diagram;
Fig. 3, Fig. 4 and Fig. 5 are that described online metal analysis system of the present utility model carries out the detection statistics figure after monitoring continuously for 168 hours;
Fig. 6 is that in the described online metal analysis system of the utility model embodiment 2, circuit connects schematic block diagram.
In figure:
1: pretreatment unit 2: sample cup 3: enriching apparatus 4: digestion instrument 5: spectrometer 6, industrial computer 7: feeder 71: nitrogen gas generator 72: argon gas steel cylinder
Embodiment
Below in conjunction with accompanying drawing, preferred embodiment of the present utility model is described, should be appreciated that preferred embodiment described herein is only for instruction and explanation of the utility model, and be not used in restriction the utility model.
Embodiment 1:
Online metal analysis system described in the utility model, both achieved on-line checkingi, once can also can detect all metallic elements, be not only heavy metal element, also comprise alkali metal, alkali earth metal, metalloid element etc., and the low demand of detection limit can also be met.Wherein, described online metal analysis system includes sample cup 2, digestion instrument 4, spectrometer 5, feeder 7 and industrial computer 6, and wherein, described sample cup 2, digestion instrument 4, spectrometer 5 are communicated with in turn with feeder 7.
Described sample cup 2 gets sample (such as surface water etc.) to be detected for filling, and its volume is enough large, ensures the sample size needed for systems axiol-ogy; Described feeder 7 is for providing nitrogen needed for spectrometer 5 and argon gas.
Described spectrometer 5 is specifically designed to the content detecting metallic element to be measured; The chaff interference that described digestion instrument 4 detects for metal element content to be measured of eliminating the effects of the act, the organic interfering substance such as such as colloid, by adding dissimilar acid, and regulate different acidity, all kinds of heterogeneity water sample is cleared up, can take the mode of high temperature acidolysis, also can adopt the mode of ultraviolet acidolysis, object is to remove organic interfering substance.
From above structure, the via intermedia between described sample cup 2 and described digestion instrument 5 is gone back and is connected with an enriching apparatus 3; Described enriching apparatus 3 for improving more than metal element content value detection limit to be detected, thus achieves the requirement of lower detection limit.Described detection limit refers to Cmin or the minimum that a certain analytical approach can detect test substance in the given degree of reliability from sample.Therefore for some metallic element that content in sample is lower, require that the detection limit of instrument is lower with regard to it, in order to guarantee to reach this requirement, the object of enriching apparatus 3 is exactly first by absorption metallic element to be measured, then wash-out, the volume ratio of detected sample and this eluent is between 10-100 times.
The exchange column for adsorbing metal element and the wash-out mechanism (not shown) that eluent is provided is provided with in described enriching apparatus 3, wherein exchange column is for adsorbing metallic element to be measured, the material of filling in it can be ion exchange resin, also can be chelating resin or synthesis modification resin, above resin be used for having inrichment to the specific heavy metal element of some low contents in sample.Described wash-out mechanism is used for providing eluent.After digestion instrument 4 free time, extract to digestion instrument and clear up.Enriched sample after clearing up is sent to spectrometer 5 again and analyzes.
In actual use, type of detection, properties of samples and testing requirement are divided into two parts per sample, after a part is sent in enriching apparatus 3 and carried out enrichment process to sample, then send in digestion instrument 4 and clear up; Another part is then directly sent in digestion instrument 4 and is cleared up process to sample.
The above feeder 7, spectrometer 5, digestion instrument 4 are all connected with industrial computer 6 respectively with enriching apparatus 3, thus ensure that above device or equipment automatically can run in the control of industrial computer 6, achieve unattended line model.
For the ease of the sample analysis of whole system, the front end of described sample cup 2 is also communicated with pretreatment unit 1, and described pretreatment unit 1 is also connected with described industrial computer 6, and it is for carrying out coarse filtration to sample, remove some bulky grain thing and the foreign material in sample, in order to avoid the pipeline of block system.Sample after pretreatment unit 1 processes is transported in sample cup 2 and carries out subsequent treatment.
Described feeder 7 includes nitrogen gas generator 71 and argon gas steel cylinder 72, and wherein nitrogen gas generator 71 is for providing nitrogen, and it utilizes air to produce nitrogen; Argon gas steel cylinder 72 is for providing argon gas.Nitrogen and argon gas are all delivered to spectrometer 5.
What spectrometer 5 described in the utility model adopted is microwave plasma atomic emission spectroscopy instrument, is provided with microwave magnetron (not shown) in it.Nitrogen gas generator 71 carries the nitrogen of coming, through magnetic field and the electric field of microwave magnetron generation, excite and formed and maintain nitrogen plasma, and make the temperature of microwave plasma remain on more than 5000K, sample aerosol is imported in nitrogen plasma, when getting back to ground state according to the Elements Atom to be measured being in excited state, the characteristic spectral line of transmitting and intensity carry out qualitative and quantitative analysis to element to be measured, and then complete monitoring.
The microwave plasma source that described spectrometer 5 adopts excites generation by microwave magnetron, avoids the potential safety hazard that inflammable gases such as using acetylene brings.The nitrogen simultaneously used is obtained from surrounding air by nitrogen gas generator 71, greatly reduces the day-to-day operation cost of whole system.
The heavy metal detection limit of laboratory microwave plasma emission spectrometer and the detection limit of native system are listed in the table below one, can find out that the detection limit of native system can meet the testing requirement (with reference to " GB3838-2002 water environment quality standard ") of heavy metal in surface water completely thus.
Table one
Meanwhile, in order to better illustrate function and the principle of online technique analytic system described in the utility model, first standard model is analyzed.Wherein, copper: 0.642mg/l is contained in water quality standard sample (GSBZ50009-88); Plumbous: 0.882mg/l; Zinc: 2.19mg/l; Cadmium: 0.0747mg/l; Nickel: 0.395mg/l; Chromium: 0.383mg/l, when using native system to analyze, because testing concentration level is all higher than the detection limit of native system, sample only through pretreatment unit and digestion instrument, and need be analyzed without the need to using enriching apparatus can enter spectrometer 6.The result obtained through native system analysis is as shown in Table 2:
Table two
From the data of above table two analysis environments standard model, the assay value of native system is in nominal range.
Meanwhile, actual sample (actual water sample of employing takes from Guangzhou Zhujiang section) is analyzed:
Because contents of heavy metal elements most in the water sample of cross section of river is all lower, native system adopts Direct Analysis to Partial Elements, and Partial Elements is analyzed after enrichment again.Water sample collects in sample cup through pretreatment unit, small part sample is directly sent into digestion instrument by peristaltic pump, with clear up after reagent mixes, namely carry out High Temperature High Pressure according to the parameter of setting to clear up, after completing, sample is drawn into spectrometer 6, and now instrument is analyzed elements such as copper, chromium, zinc, iron, manganese, nickel.Meanwhile, most of sample (being generally 1000mL) in sample cup is drawn into enriching apparatus, when flowing through enriching column, filler wherein will adsorb specific heavy metal element, until 1000mL sample all after enriching column, extract 20mL eluent (can adjust according to enrichment times) heavy metal element be adsorbed on enriching column is eluted and collects, digestion instrument is cleared up after extracting eluent again and clearing up reagent mixing, clear up complete, sample is drawn into spectrometer 6, and now the element of instrument to low concentrations such as lead, cadmiums is analyzed.An instrument can be utilized so once to have analyzed the heavy metals such as copper, chromium, zinc, lead, cadmium, iron, manganese, nickel.Record concentration of element in this water sample as following table three:
It is to be noted that * is the analysis data after enrichment process, be enriched sample is analyzed data to convert back according to enrichment times (50 times) data of primary sample concentration.
The Comparative result surveyed with laboratory analysis methodologies (ICP-AES) is seen, online metal analysis system described in the utility model, the data surveyed and its coincide, data accurately, reliable, the requirement of the analysis of surface water quality heavy metal can be met.
Table three
In addition, when Real-Time Monitoring service data, by online metal analysis system described in the utility model, monitoring continuously in 168 hours is carried out to dissimilar heavy metal standard solution, three statistical graphs that separate of its test result as shown in Fig. 3, Fig. 4 and Fig. 5.
Can draw from Fig. 3, Fig. 4 and Fig. 5: from the continuous monitoring of this system of measuring stability to most of heavy metal, there is good stability, the continuous monitoring of all kinds of heavy metal in water quality can be met.
Embodiment 2:
As Fig. 6 the present embodiment is only with embodiment 2 difference: as described in feeder be electrically connected with spectrometer 5, be controlled by spectrometer 5.
Principle of work in actual use and effect of realization are the same.
The above, it is only preferred embodiment of the present utility model, not any pro forma restriction is done to the utility model, therefore everyly do not depart from the utility model plan content, the any amendment done above embodiment according to essence of the present utility model, equivalent variations and modification, all still belong in the scope of the utility model scheme.
Claims (10)
1. online metal analysis system, for the on-line checkingi of metallic element, comprises the sample cup, spectrometer and the feeder that are communicated with in turn; Described spectrometer is electrically connected with an industrial computer, it is characterized in that:
Via intermedia between described sample cup and spectrometer is provided with a digestion instrument of the chaff interference detected for metal element content to be measured of eliminating the effects of the act;
Via intermedia between described sample cup and described digestion instrument is gone back and is connected with the enriching apparatus for enrichment metallic element to be measured;
Described digestion instrument and enriching apparatus are electrically connected with described industrial computer respectively.
2. online metal analysis system according to claim 1, is characterized in that:
Described feeder is electrically connected with described spectrometer.
3. online metal analysis system according to claim 1, is characterized in that:
Described feeder is electrically connected with described industrial computer.
4. online metal analysis system according to claim 1, is characterized in that:
Be provided with for the exchange column of adsorbing metal element with for providing the elution mechanism of wash-out adsorbing metal element in described enriching apparatus;
The packing material adopted in described exchange column is ion exchange resin, chelating resin or synthesis modification resin.
5. online metal analysis system according to claim 1, is characterized in that:
Described sample cup front end is also communicated with for the pretreatment unit to testing sample coarse filtration.
6. online metal analysis system according to claim 5, is characterized in that:
Described pretreatment unit is electrically connected with described industrial computer.
7. the online metal analysis system according to claim 1 or 2 or 3, is characterized in that:
Described feeder comprises nitrogen gas generator and argon gas steel cylinder.
8. online metal analysis system according to claim 1, is characterized in that:
Described spectrometer is microwave plasma atomic emission spectroscopy instrument.
9. online metal analysis system according to claim 8, is characterized in that:
Be provided with in described microwave plasma atomic emission spectroscopy instrument and formed for exciting and maintain the microwave magnetron of nitrogen plasma.
10. online metal analysis system according to claim 1, is characterized in that:
Described digestion instrument is high temperature acidolysis or ultraviolet acidolysis for eliminating the mode of clearing up of chaff interference.
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| CN201520863252.7U CN205157434U (en) | 2015-10-29 | 2015-10-29 | Online metal analysis system |
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| CN201520863252.7U CN205157434U (en) | 2015-10-29 | 2015-10-29 | Online metal analysis system |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105223168A (en) * | 2015-10-29 | 2016-01-06 | 伊创仪器科技（广州）有限公司 | Online metal analysis system |
| CN106198441A (en) * | 2016-07-26 | 2016-12-07 | 中国科学院福建物质结构研究所 | A kind of can analog sample adsorption desorption process In situ spectroscopic test device |
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2015
- 2015-10-29 CN CN201520863252.7U patent/CN205157434U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105223168A (en) * | 2015-10-29 | 2016-01-06 | 伊创仪器科技（广州）有限公司 | Online metal analysis system |
| CN106198441A (en) * | 2016-07-26 | 2016-12-07 | 中国科学院福建物质结构研究所 | A kind of can analog sample adsorption desorption process In situ spectroscopic test device |
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