CN105891346A - Ion chromatography system for controlling double-conductance-cell series technology through virtual instrument - Google Patents

Ion chromatography system for controlling double-conductance-cell series technology through virtual instrument Download PDF

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Publication number
CN105891346A
CN105891346A CN201610120746.5A CN201610120746A CN105891346A CN 105891346 A CN105891346 A CN 105891346A CN 201610120746 A CN201610120746 A CN 201610120746A CN 105891346 A CN105891346 A CN 105891346A
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China
Prior art keywords
conductance
ion
signal
ion chromatography
conductance cell
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CN201610120746.5A
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Inventor
苏程远
赵云麒
张道敬
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Qingdao Lu Hai Electro-Optical Technology Inc (us) 62 Martin Road Concord Massachusetts 017
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Qingdao Lu Hai Electro-Optical Technology Inc (us) 62 Martin Road Concord Massachusetts 017
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Priority to CN201610120746.5A priority Critical patent/CN105891346A/en
Publication of CN105891346A publication Critical patent/CN105891346A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N2030/022Column chromatography characterised by the kind of separation mechanism
    • G01N2030/027Liquid chromatography

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)

Abstract

The invention discloses an ion chromatography system for controlling a double-conductance-cell series technology through a virtual instrument. The system comprises an ion chromatography separation module fixed to an ion chromatography instrument, a suppressor flow path module, a conductance cell series module, an ion chromatography interface equipment card inserted into a microcomputer PCI slot, and a software measurement and control module located in a microcomputer. A specific analog or digital circuit in a traditional ion chromatography instrument is obtained through a software program to complete measuring and testing functions, noise can be greatly lowered, the signal to noise ratio is increased, and the measuring result is more precise. Samples with large concentration differences are tested at a time through the double-conductance-cell series technology, the temperature is unified, and measuring precision is improved. It is not needed to carry out high-concentration ion pretreatment on the samples with the large concentration differences, analysis time is shortened, measuring efficiency is improved, and the detection and operation cost is reduced.

Description

A kind of ion chromatography system utilizing virtual instrument to control double conductance cell serial connection technology
Technical field
The present invention relates to ion chromatography system, be specifically related to a kind of utilize virtual instrument to control double conductance cell serial connection technology Ion chromatography system.
Background technology
Chromatography of ions is the novel liquid chromatograph grown up after 20 century 70s.This technology quickly grows, Become the powerful tool separating with detecting different anions and canons.At present, known ion chromatograph is by high-pressure pump, enters Sample valve, detached dowel, suppression unit, Conductivity detection unit and data processing units etc. six are most of to be constituted.At conventional ion color In analysis of spectrum, tested component is separated, flow out mutually with flowing after suppression, enters conductance detecting pool and is measured.Conductance detecting pool Continuously by the concentration of elution fraction in chromatographic column with flowing phase change detection out, and be changed into the signal of telecommunication continuously, defeated Enter in data processing equipment, obtain a chromatogram changing over separation component.One preferable detector is to different Sample, under the conditions of different sample concentrations and various leacheate, all energy is accurate, reflect the change of chromatographic peak in time continuously, and And under difficult environmental conditions same sample is had identical response signal, so, conductance detecting pool should possess higher spirit Sensitivity, the wider detection by quantitative range of linearity, selectivity and repeatability.
According to kohilraush law, electrical conductivity K=1/1000 A/L ∑ Ci λ i:A is that electrode sections is amassed, and L is the two poles of the earth Between distance, when an actual conductance pond is fabricated to, then A/L is a fixed value, and referred to as cell constant of conductometric vessel K, Ci is that ion is dense Degree, λ i is the authority molar conductance of ion.In the chromatography of ions, the ion concentration of system is less than 1mmol/L, at one enough In dilute solution, the molar conductance of ion reaches maximum, and electric conductivity value is proportional with ion concentration.Ion is utilized at us When chromatographic system carries out sample ions analysis and detection, sample contains the ion of a large amount of variable concentrations.When we utilize one Conductance detecting pool by the concentration of elution fraction in chromatographic column with flowing phase change detection out, and be transformed into the signal of telecommunication, finally The chromatogram changing over separation component obtained.Owing in sample, the concentration difference of different ions is relatively big, will go out The chromatography of ions peak of existing low concentration is covered by the chromatographic peak of high concentration ion completely or low concentration chromatography of ions peak shows, And high concentration ion is because of excessive concentration, the chromatographic peak generation peak shape shown or area distortion, and can not qualitative to it and Determine quantitative analysis.
At present, in order to avoid the interference of this situation, often pre-treatment pillar is used to remove the height in sample in sample Concentration ion or take first to determine sample low concentration ion, is then determined in sample further by dilute sample High concentration ion.But use its use cost of pretreatment process high, and be disposable consumptive material, life-time service, detects into Ben Taigao;And use two-step method to measure sample ions, along with the use ambient temperature of instrument is the most variant, inspection can be caused Survey the change of signal, such as, baseline drift can occur, once drift beyond certain numerical value, ion chromatograph detection knot will be affected Really.A kind of can eliminate the high concentration ion method to low concentration ion interference accordingly, it would be desirable to develop, both can ensure that sample from The accuracy that son measures, can reduce again testing cost simultaneously, and improve analysis efficiency.
Summary of the invention
It is an object of the invention to provide a kind of ion chromatography system utilizing virtual instrument to control double conductance cell serial connection technology, With the defect overcoming prior art to exist.
For achieving the above object, the technical solution used in the present invention is as follows:
A kind of ion chromatography system utilizing virtual instrument to control double conductance cell serial connection technology, including being fixed on ion chromatograph Ion chromatographic separation module, suppressor stream module, conductance cell serial module structure, insert the ion color in micro computer PCI slot Spectrum interface equipment card, be positioned at the measure and control software module within micro computer, it is characterised in that: described conductance cell serial module structure be by Two conductance cells are connected, when sample flows through generation two detection analogue signal;Described chromatography of ions interface equipment card rank Connect the communication of computer and ion chromatograph, by being inserted in pci card groove, the analogue signal that conductance cell produces can be acquired, It is transmitted to measure and control software module;Described measure and control software module includes that A/D conversion, Digital Signal Analysis process, D/A changes;
Described A/D conversion: two analogue signals are converted into digital signal;
Described Digital Signal Analysis processes: is analyzed digital signal, regards signal and noise thereof as stochastic signal, pass through Utilize its statistical nature, reduce noise and obtain signal itself and signal integration is obtained optimal digital signal,
Described D/A conversion: the optimal digital signal processed by analysis is changed into corresponding analog signal.
Furthermore, described conductance cell serial module structure is a Pyatyi conductance cell and two grades of conductance cells to be carried out Series connection;
Furthermore, it is to utilize digital filtering, fft analysis, single product extraction, single-frequency inspection that described Digital Signal Analysis processes Survey, Wavelet Denoising Method, autocorrelation analysis, weighted average value filtering, anti-impulse disturbances average value filtering, program judge filtering, adaptive Should filter, linear neural network de-noising, curve matching method to realize correlation function.
Owing to sample intermediate ion concentration difference is relatively big, Pyatyi conductance cell and two grades of conductance cells are connected by the present invention, Owing to Pyatyi conductance cell electric conductivity value is big, highly sensitive, for measuring the ion that concentration in sample is low, and two grades of conductance cell electric conductivity values Relatively small, sensitivity decrease, may be used for measuring the ion of sample middle and high concentration, conductance cell serial module structure exports two simulation letters Number, utilize measure and control software module to be analyzed processing, in conjunction with the mensuration advantage of two kinds of conductance cells, retain Pyatyi conductance cell and measure low Concentration signal and two grades of conductance cells measure high concentration signal, thus realize the optimum integration of signal.
Traditional ion chromatograph is the measurement test merit realizing instrument by designing concrete analog or digital circuit Can, the present invention utilizes software program this virtual instrument form to complete these functions.The mould that conductance cell serial module structure is exported Intend signal to be extracted by the chromatography of ions interface equipment card being inserted on computer PCI draw-in groove, be input to software control module, come Complete the measurement test of sample further.
The analogue signal that measure and control software module processes inputting by starting Digital Signal Analysis carries out A/D conversion, often adopts Collection to one data are fed to Digital Signal Analysis process and are filtered computing, and operation result send D/A to be converted to analog quantity. Being repeated continuously said process, the outfan in D/A conversion just obtains filtered analogue signal.In calculating process, not only Signal is carried out denoising, and by two analogue signals of conductance cell serial module structure output, has been converted into by A/D Two digital signals, and analyse and compare further, two digital signals are optimized combination, ultimately form an optimal digital Signal, delivers to D/A and is converted to analog quantity, and then further form preferable chromatographic peak collection of illustrative plates.
Beneficial effects of the present invention:
(1) a kind of ion chromatography system utilizing virtual instrument to control double conductance cell serial connection technology of the present invention, utilizes software Program realizes the measurement test function that analog or digital circuit concrete in conventional ion chromatograph completes, and can be substantially reduced Noise, improves signal to noise ratio, makes measurement result more accurate;
(2) a kind of ion chromatography system utilizing virtual instrument to control double conductance cell serial connection technology of the present invention, by double electricity Leading pond serial connection technology and the sample that concentration difference is big is disposably completed test, temperature is unified, improves measuring accuracy;
(3) a kind of ion chromatography system utilizing virtual instrument to control double conductance cell serial connection technology of the present invention, to concentration difference Different big sample, without carrying out high concentration ion pretreatment, decreases analysis time, improves determination efficiency, reduces detection fortune Row cost.
Accompanying drawing explanation
Accompanying drawing is used for providing a further understanding of the present invention, constitutes the part of the application, and the present invention's is schematic real Execute example and illustrate for explaining the present invention, being not intended that inappropriate limitation of the present invention.In the accompanying drawings:
Fig. 1 is the flow process connection figure of the ion chromatography system utilizing the double conductance cell serial connection technology of virtual instrument control
Fig. 2 is through the color of conventional ion chromatographic system by the dilute sample containing high-concentration chlorine ion and low concentration nitrite anions Spectrogram
Fig. 3 is that through virtual instrument, the sample containing high-concentration chlorine ion and low concentration nitrite anions is controlled double conductance cell series connection The chromatograph of the ion chromatography system of technology
Detailed description of the invention
Below in conjunction with accompanying drawing, embodiments of the invention are described in detail, but the present invention can be defined by the claims and cover The various different modes of lid are implemented.
Embodiment
1, system balancing
Will be equipped with the present invention utilize virtual instrument control double conductance cell serial connection technology ion chromatography system chromatography of ions Instrument and ion chromatograph in the market carry out system balancing respectively.After leacheate enters ion isolation module, then access presses down Device stream module processed, inhibited device enters conductance cell serial module structure, and the analogue signal of generation passes through chromatography of ions interface equipment card Enter measure and control software module, to manifest the poised state of whole system.The system connection figure of the present invention is shown in Fig. 1.On market from Sub-chromatograph system balancing the most here repeats.After system balancing, by the same sample in the range of identical sex-limited test one Adding in ion chromatograph in the market after dilution, another is directly added into and utilizes virtual instrument control equipped with the present invention The ion chromatography system of double conductance cell serial connection technologies ion chromatograph in carry out sample introduction analysis.
2, dilute sample analysis in conventional ion chromatograph
Ion chromatograph commercially after the solution of nitrite anions containing low concentration in high-concentration chlorine ion is diluted In carry out sample introduction analysis, now sample is through detached dowel, after suppressor, finally enter conductance cell, on chromatographic software To the chromatogram (see figure 2) of sample detection, the chromatographic peak of nitrite anions is complete from chromatogram it can be seen that in this case Entirely covered by the chromatographic peak of high-concentration chlorine ion, need dilution further to measure chloride ion, and low concentration can not be obtained The data of nitrite anions, need to utilize pretreatment column to remove high-concentration chlorine ion and measure further, so say and cause data Inaccurate, thus it can not be carried out qualitative and quantitative analysis.
3, sample is in the ion chromatograph of the ion chromatography system of the double conductance cell serial connection technology of virtual instrument control Analyze
The solution containing low concentration nitrite anions in high-concentration chlorine ion is being controlled double conductance cell series connection skill through virtual instrument The ion chromatograph of the ion chromatography system of art carries out sample introduction analysis, and now sample is through ion isolation module, passes through suppressor After stream module, finally entering conductance cell serial module structure, the analogue signal of generation enters soft by chromatography of ions interface equipment card Part control module, obtains the chromatogram (see figure 3) of sample detection on chromatographic software, it can be seen that the present invention from chromatogram By Pyatyi conductance cell and two grades of conductance cells are connected, owing to Pyatyi conductance cell electric conductivity value is big, highly sensitive, it is used for surveying The ion that in random sample product, concentration is low, and two grades of conductance cell electric conductivity values are relatively small, sensitivity decrease, may be used for measuring in sample high The ion of concentration, conductance cell serial module structure two analogue signals of output, utilize measure and control software module to be analyzed processing, in conjunction with two Plant the mensuration advantage of conductance cell, retain Pyatyi conductance cell and measure low concentration signal and two grades of conductance cells mensuration high concentration signals, from And realize the optimum integration of signal, thus obtain the separating effect figure of nitrite anions and chloride ion, can to its carry out qualitative and Quantitative analysis.

Claims (3)

1. utilize virtual instrument to control an ion chromatography system for double conductance cell serial connection technology, including being fixed on ion chromatograph On ion chromatographic separation module, suppressor stream module, conductance cell serial module structure, insert the ion in micro computer PCI slot Chromatograph interface equipment card, is positioned at the measure and control software module within micro computer, it is characterised in that: described conductance cell serial module structure is Two conductance cells are connected, when sample flows through generation two detection analogue signal;Described chromatography of ions interface equipment card Linking computer and the communication of ion chromatograph, by being inserted in pci card groove, can adopt the analogue signal that conductance cell produces Collection, is transmitted to measure and control software module;Described measure and control software module includes that A/D conversion, Digital Signal Analysis process, D/A changes;
Described A/D conversion: two analogue signals are converted into digital signal;
Described Digital Signal Analysis processes: is analyzed digital signal, regards signal and noise thereof as stochastic signal, pass through Utilize its statistical nature, reduce noise and obtain signal itself and signal integration is obtained optimal digital signal,
Described D/A conversion: the optimal digital signal processed by analysis is changed into corresponding analog signal.
Conductance cell serial module structure the most according to claim 1 is a Pyatyi conductance cell and two grades of conductance cells to be carried out Series connection.
It is to utilize digital filtering, fft analysis, Dan Pinti that described Digital Signal Analysis the most according to claim 1 processes Take, single-frequency detection, Wavelet Denoising Method, autocorrelation analysis, weighted average value filtering, anti-impulse disturbances average value filtering, program judge Filtering, adaptive-filtering, linear neural network de-noising, the method for curve matching realize correlation function.
CN201610120746.5A 2016-03-03 2016-03-03 Ion chromatography system for controlling double-conductance-cell series technology through virtual instrument Pending CN105891346A (en)

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CN201610120746.5A CN105891346A (en) 2016-03-03 2016-03-03 Ion chromatography system for controlling double-conductance-cell series technology through virtual instrument

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109100441A (en) * 2018-08-23 2018-12-28 西南科技大学 A kind of method of liquid chromatogram curve removal impulse disturbances

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109100441A (en) * 2018-08-23 2018-12-28 西南科技大学 A kind of method of liquid chromatogram curve removal impulse disturbances
CN109100441B (en) * 2018-08-23 2021-05-07 西南科技大学 Method for removing pulse interference of liquid chromatography curve

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Application publication date: 20160824