CN101303279A - On-line enriching apparatus for near-infrared testing low abundance components and use method thereof - Google Patents
On-line enriching apparatus for near-infrared testing low abundance components and use method thereof Download PDFInfo
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- CN101303279A CN101303279A CN 200810039550 CN200810039550A CN101303279A CN 101303279 A CN101303279 A CN 101303279A CN 200810039550 CN200810039550 CN 200810039550 CN 200810039550 A CN200810039550 A CN 200810039550A CN 101303279 A CN101303279 A CN 101303279A
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Abstract
The invention relates to an online enriching device applied to near infrared detection and use method thereof. The device comprises a near infrared diffuse device having a light beam window cling to the surface of an enriching column, wherein the enriching column is sleeved in a special detection accessory which is arranged to cover the light beam window, and the bottom of the enriching column is connected with a vacuum system. Sample solution is added into the enriching column in a constant vacuum for enrichment, and near infrared spectrum scan can be directly performed on the upper end of the enriching column for measurement. The enriching device of the invention can be used for completing enrichment and near infrared detection for a sample in only 5 minutes, the detection limit can reach ppm stage, the accuracy grade is high, the operation is simple and the requirements of trace analysis and in-situ analysis can be met. Besides, no samples are consumed in the analysis process, and almost no other consumptions exist except for a little electric energy consumed by the self, so detection cost can be reduced substantially compared with the common standards or reference methods.
Description
Technical field
The present invention relates to the detection range of near-infrared method to trace components, a kind of specifically specific adsorption effect enrichment low abundance components that utilizes enrichment material and low abundance components combines device that carries out analyzing and testing and using method thereof with nir instrument.
Background technology
Modern near-infrared spectrum analysis (NIR) organically combines near-infrared spectrum technique and computing machine, Chemical Measurement, is fast, the most noticeable spectral analysis technique of development in recent years.Compare with traditional quantitative analysis method, the outstanding advantage of near-infrared spectrum technique be can't harm, fast, low-cost, simple to operate, can be used for on-the site analysis, test favorable reproducibility etc.But also there is the lower shortcoming of detection sensitivity near infrared.
Heavy metal lead, farming low abundance components such as residual only need seldom that amount will cause serious harm to environment and human body, are very important analysis projects in environmental monitoring and the food security.Now Chang Yong analysis determining method has atomic spectrum, ICP-MS, spectrophotometric method, stripping voltammetry, HPLC etc., and these methods exist cost and running expense height, instrument complexity, complex operation, are unfavorable for problems such as on-the-spot real-time analysis.
The incorporate analytic system of enrichment-near infrared ray is for a new way is opened up in the near infrared spectrum express-analysis of low abundance material.Utilize enrichment material absorption low abundance components, realize the highly sensitive detection of its near infrared.In conjunction with chemometrics method, the analyzing detecting method of development low abundance components.On-line preconcentration detects advantages such as the low abundance components near infrared spectroscopy is fast with its analysis speed, analysis low cost, and wide application prospect is being arranged aspect the low abundance components on-the site analysis.
Summary of the invention
Be not suitable for the defective that low abundance components is analyzed at near-infrared spectrum technique, the invention provides a kind of on-line preconcentration device, realize the highly sensitive detection of near infrared, and its detection method is provided.
The present invention is achieved by the following technical solutions:
A kind of on-line preconcentration device that is used for near-infrared testing low abundance components, it is characterized in that described on-line preconcentration device is made up of near-infrared diffuse reflectance device 1, the enriching column 2 that enrichment material is housed, the test special accessories 3 that has ring groove 4 and vacuum system 5; Nearly the light beam window 6 of infrared diffuse device 1 is close to the surface of enriching column 2, enriching column 2 is set in the ring groove 4, ring groove 4 is carved mutually with enriching column 2 surfaces and is closed, and test special accessories 3 is positioned at ring groove 4 two side portions and plane, light beam window 6 place coincide, and cover light beam window 6, test special accessories 3 is supported on the level table of apparatus for placing, and its height h is more than or equal to the diameter of light beam window 6, and enriching column 2 bottoms connect vacuum system 5;
Wherein, the material of enriching column 2 is the optical material of no near infrared absorption, and is a kind of among preferred quartz, glass, fused quartz, the AgCl;
The material of test special accessories 3 is: the inner surface material of annex 3 is selected near infrared light is had reflection or reflective functions and do not absorb the material of near infrared light, as metallic aluminium, gold, glass etc., material that parasitic lights such as outer surface material selection visible light can't penetrate such as metallic aluminium etc.; Purpose is to prevent to diffuse loss, allows all diffuse lights all enter integrating sphere; Prevent that simultaneously parasitic light from entering the detecting device in the integrating sphere 9 of near-infrared diffuse reflectance device;
Enrichment material can select that low abundance components is had the absorption or the granular material or the integral material of exchange interaction, can select a kind of in resin, cross-linked chitosan, mesoporous material, the silica gel;
Near-infrared diffuse reflectance device 1 is the Cary500 of U.S. Varian company, the UV-Vis-NIR near infrared spectrometer, and light beam window 6 diameter 20mm face the upper end of enriching column, because concentration of component herein is the highest, can effectively improve detection sensitivity.
Test special accessories 3 can be a baffle plate 7 of being made up of ring groove 4 and plane, ring groove 4 both sides, and the baffle plate upper/lower terminal is respectively equipped with two rings 8, and ring groove 4 is closely buckled on the enriching column 2.
The present invention also provides a kind of using method of above-mentioned on-line preconcentration device, it is characterized in that, described method step is as follows:
1, makes the sample solution constant speed flow through enriching column, use enrichment material that sample is carried out enrichment;
2, use 1 pair of enriching column of near-infrared diffuse reflectance device to carry out near infrared spectrum scanning, obtain the correlation analysis data;
3, with the enrichment material in the washing fluid flushing enriching column, elution samples from the enrichment material.
Beneficial effect
Use on-line preconcentration device of the present invention only to need 1-5min just can finish enrichment and near infrared detection to the environmental sample of the complicated substrate of a duplicate samples, detection limit is low, and the accuracy height is easy and simple to handle, can satisfy trace analysis and on-the site analysis requirement.Analytic process does not consume sample, and self does not almost have other consumption except that consuming a bit electricity, compares with standard or reference method commonly used, and testing expense can reduce significantly.
Description of drawings
Fig. 1 is that the A-A of on-line preconcentration device is to sectional view.Wherein, 1-near-infrared diffuse reflectance device, the 2-enriching column, 3-tests special accessories, 5-vacuum system, 6-light beam window, 9-integrating sphere, 10-bottle,suction, 11-vacuum pump, 12-enrichment material, the height of h-test special accessories.
Fig. 2 is an on-line preconcentration device vertical view.Wherein, 1-near-infrared diffuse reflectance device, the 2-enriching column, 3-tests special accessories, 4-ring groove, 6-light beam window, 9-integrating sphere.
Fig. 3 is that the test special accessories is the on-line preconcentration device vertical view of baffle plate.Wherein, 1-near-infrared diffuse reflectance device, 2-enriching column, 4-ring groove, 6-light beam window, 7-baffle plate, 8-ring, 9-integrating sphere.
Fig. 4 is the original near infrared light spectrogram (a) of 11 samples and the spectrogram of proofreading and correct through MSC (b).
Fig. 5 is the linearly dependent coefficient R of each wavelength place concentration and spectral absorbance.
Fig. 6 sets up predicated error under the different hidden variable numbers of PLS model gained with the near infrared spectrum of all-wave long (a), 1020-1500nm wavelength coverage (b) respectively.
Embodiment
The present invention is further elaborated below by drawings and Examples.
Application example:
The invention will be further described below in conjunction with accompanying drawing and example.
Chelating resin D401 adopts the wet method uniform glass column of quality (internal diameter 10mm) of packing into after pre-service, use the glass fibre jam-pack at the bottom of the post, when cylinder shop layer of glass prevents liquid feeding the upper strata resin is evoked.Resin should be evenly closely knit in the high 70mm of resin column, post, do not have space and bubble.
Before then glass column being fixed on the detection window of diffuse device with spring clamp, at long 70mm of resin column upper end position outsourcing, the tinfoil of wide 35mm is made baffle plate, buckles a semicircular ring on the tinfoil, semicircular ring width 10mm.
With the plumbous standard solution (Pb of 1000 μ g/mL
2+) 11 parts of concentration ranges of dilution preparation are 0.00,1.00,2.00,3.00,4.00,5.00,6.00,7.00,8.00,9.00, each 100mL of sample solution of 10.00ppm, get 30.00mL solution and carry out enrichment with the enriching apparatus that is fixed on the near infrared spectrometer, vacuum tightness is fixed as 0.02MPa.
Just stop enrichment immediately when the lead solution liquid level arrives the resin column top, then directly measure the diffuse reflection near infrared spectrum in the enriching column upper end.Near infrared spectrometer is UV-Vis-NIR spectrometer (Cary500, a U.S. Varian company), and the spectroscopic assay wavelength coverage is 800-2500nm, and spectral resolution is 1nm, and sweep velocity is 600nm/min.
After every duplicate samples enrichment, mensuration finish, under 0.015MPa vacuum tightness, wash pillar, use the ultrapure water rinse resin of 20mL again with 20mL 2mol/L hydrochloric acid solution.
Use the chemometrics method deal with data.
Fig. 3 is the original near infrared light spectrogram (a) of 11 samples and the spectrogram of proofreading and correct through MSC (b).Handle through MSC, the spectrum that causes because of light scattering disperses obviously to reduce.
Fig. 4 is the linearly dependent coefficient R of each wavelength place concentration and spectral absorbance.The spectrum after MSC handles and the linearly dependent coefficient of concentration at most wave bands all greater than 0.8, particularly in wavelength 1020-1500nm and two SPECTRAL REGION of 1850-2500nm, linear dependence is better, and coefficient R is basically greater than 0.80, and maximum reaches 0.9588.
Fig. 5 sets up predicated error under the different hidden variable numbers of PLS model gained with the near infrared spectrum of all-wave long (a), 1020-1500nm wavelength coverage (b) respectively.With the long near infrared spectrum modeling of all-wave, be 2 o'clock at the hidden variable number, it is minimum that predicated error reaches, and is 0.8824 μ g/mL; Selecting the near infrared spectrum modeling of 1020-1500nm wavelength coverage for use, is 2 o'clock at the hidden variable number, and it is minimum that predicated error reaches, and is 0.8697 μ g/mL.As seen, better with the model of 1020-1500nm wavelength coverage foundation.
Claims (6)
1, a kind of on-line preconcentration device that is used for near-infrared testing low abundance components, it is characterized in that described on-line preconcentration device is made up of near-infrared diffuse reflectance device 1, the enriching column 2 that enrichment material is housed, the test special accessories 3 that has ring groove 4 and vacuum system 5; Nearly the light beam window 6 of infrared diffuse device 1 is close to the surface of enriching column 2, enriching column 2 is set in the ring groove 4, ring groove 4 is carved mutually with enriching column 2 surfaces and is closed, and the part that makes test special accessories 3 be positioned at ring groove 4 both sides is close to the plane at light beam window 6 places, and cover light beam window 6, the height h of test special accessories 3 is more than or equal to the diameter of light beam window 6, and enriching column 2 bottoms connect vacuum system 5;
Wherein, the material of enriching column 2 is the optical material of no near infrared absorption;
The material of test special accessories 3 is: the inner surface material of annex 3 is for having reflection or reflective functions and not absorbing the material of near infrared light near infrared light, outer surface material is the material that visible light or other parasitic lights can't penetrate;
Enrichment material is for having the granular material or the integral material of absorption or exchange interaction to low abundance components.
2, the on-line preconcentration device that is used for near-infrared testing low abundance components as claimed in claim 1 is characterized in that, the material of described enriching column 2 is a kind of among quartz, glass, fused quartz, the AgCl.
3, the on-line preconcentration device that is used for near-infrared testing low abundance components as claimed in claim 1, it is characterized in that, the material of said test special accessories 3 is: the inner surface material of annex 3 is a kind of in metallic aluminium, gold and the glass, and outer surface material is a metallic aluminium.
4, the on-line preconcentration device that is used for near-infrared testing low abundance components as claimed in claim 1 is characterized in that, enrichment material is a kind of in resin, cross-linked chitosan, mesoporous material, the silica gel.
5, the on-line preconcentration device that is used for near-infrared testing low abundance components as claimed in claim 1, it is characterized in that, test special accessories 3 is a baffle plate 7 of being made up of ring groove 4 and plane, ring groove 4 both sides, the baffle plate upper/lower terminal is respectively equipped with two rings 8, and ring groove 4 is closely buckled on the enriching column 2.
6, a kind of using method of on-line preconcentration device as claimed in claim 1 is characterized in that, described method step is as follows:
1) makes the sample solution constant speed flow through enriching column, use enrichment material that sample is carried out enrichment;
2) carry out near infrared spectrum scanning with 1 pair of enriching column of near-infrared diffuse reflectance device, obtain the correlation analysis data;
3) with the enrichment material in the washing fluid flushing enriching column, elution samples from the enrichment material.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200810039550 CN101303279B (en) | 2008-06-26 | 2008-06-26 | On-line enriching apparatus for near-infrared testing low abundance components and use method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101660999B (en) * | 2009-09-11 | 2011-01-19 | 华东理工大学 | Micro near-infrared spectral analytical method based on enrichment of integrated material |
| CN102313713A (en) * | 2011-07-14 | 2012-01-11 | 浙江大学 | Rapid detection method of abundance of tracer isotope <15>N in plant based on midinfrared spectrum |
| CN103472050A (en) * | 2013-09-20 | 2013-12-25 | 华东交通大学 | Portable enrichment device for Raman detection of heavy metals |
| CN103472050B (en) * | 2013-09-20 | 2016-11-30 | 华东交通大学 | A kind of enriching apparatus of portable Raman detection heavy metal |
| CN106872386A (en) * | 2017-01-19 | 2017-06-20 | 曹鹏 | A kind of solid-phase extraction device suitable for the measurement of online transmission mode |
| CN109916700A (en) * | 2019-03-26 | 2019-06-21 | 华东理工大学 | A kind of small-sized Solid Phase Extraction and solid phase spectra detect aggregate device |
| CN113340701A (en) * | 2021-06-08 | 2021-09-03 | 天津工业大学 | Enrichment detection device and enrichment detection method for scale inhibitor in water |
| CN113884465A (en) * | 2021-09-28 | 2022-01-04 | 武汉轻工大学 | Prediction model for detecting lead and cadmium concentrations in crayfish by combining resin with near infrared spectrum and establishment method and application thereof |
-
2008
- 2008-06-26 CN CN 200810039550 patent/CN101303279B/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101660999B (en) * | 2009-09-11 | 2011-01-19 | 华东理工大学 | Micro near-infrared spectral analytical method based on enrichment of integrated material |
| CN102313713A (en) * | 2011-07-14 | 2012-01-11 | 浙江大学 | Rapid detection method of abundance of tracer isotope <15>N in plant based on midinfrared spectrum |
| CN102313713B (en) * | 2011-07-14 | 2013-04-03 | 浙江大学 | Rapid detection method of abundance of tracer isotope <15>N in plant based on midinfrared spectrum |
| CN103472050A (en) * | 2013-09-20 | 2013-12-25 | 华东交通大学 | Portable enrichment device for Raman detection of heavy metals |
| CN103472050B (en) * | 2013-09-20 | 2016-11-30 | 华东交通大学 | A kind of enriching apparatus of portable Raman detection heavy metal |
| CN106872386A (en) * | 2017-01-19 | 2017-06-20 | 曹鹏 | A kind of solid-phase extraction device suitable for the measurement of online transmission mode |
| CN109916700A (en) * | 2019-03-26 | 2019-06-21 | 华东理工大学 | A kind of small-sized Solid Phase Extraction and solid phase spectra detect aggregate device |
| CN113340701A (en) * | 2021-06-08 | 2021-09-03 | 天津工业大学 | Enrichment detection device and enrichment detection method for scale inhibitor in water |
| CN113340701B (en) * | 2021-06-08 | 2023-02-21 | 天津工业大学 | Enrichment detection device and enrichment detection method for scale inhibitor in water |
| CN113884465A (en) * | 2021-09-28 | 2022-01-04 | 武汉轻工大学 | Prediction model for detecting lead and cadmium concentrations in crayfish by combining resin with near infrared spectrum and establishment method and application thereof |
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| CN101303279B (en) | 2010-12-08 |
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