CN206601333U - A kind of ultraviolet dual wave-band fast detector separated for normal pressure, medium pressure column chromatography - Google Patents

Abstract

The utility model discloses a kind of ultraviolet dual wave-band fast detector separated for normal pressure, medium pressure column chromatography, it is characterised in that including sampling system, light-source system, data handling system；Described sampling system is made up of polyfluortetraethylene pipe and flow cell, and the polyfluortetraethylene pipe is connected with the flow cell, and sample liquid flows through flow cell by polyfluortetraethylene pipe；Described light-source system is made up of 365nm uviol lamps, 254nm uviol lamps, rectifier and transformer；The data handling system is by the first Ultraviolet sensor, the second Ultraviolet sensor, 8 single-chip microcomputers, the first group of four figures pipe, the second group of four figures pipe and serial data wire terminal, host computer composition；The utility model has relative low price, safety, practical, easy to operate, the features such as, have and promote well and practical value, good economic and social benefit can be produced after extensive promotion and application.

Description

A kind of ultraviolet dual wave-band fast detector separated for normal pressure, medium pressure column chromatography

Technical field

The utility model is related to a kind of for ultraviolet rapid detection apparatus during column chromatography for separation, more particularly to a kind of use The ultraviolet dual wave-band fast detector separated in normal pressure, medium pressure column chromatography.

Background technology

In the extracting and developing and purge process of organic synthesis and natural drug, column chromatography for separation is using the most Universal and extensive separation and purification technique.And its detection typically uses manual method：First deployed with thin-layer chromatography, then with purple Outer analysis instrument is observed, or is observed again with uv analyzer after sprinkling developer.

The problem of the method is present be：1. workload is big, and every batch of sample is required for detection；2. detection sensitivity is than relatively low： In process of the test, thin-layer chromatography detection method needs to merge the sample liquid of collection the intersection for so resulting in compound, makes Secondary separation will be carried out by obtaining the compound for being able to separate originally, thus significantly increase the cumbersome and difficulty of experimentation, And further loss will be caused to isolate；3. thin layer detection synchronous with experiment can not be carried out, and there is certain hysteresis quality, Need to carry out expansion detection after sampling, and duration of run is long, it is difficult to realize to testing and producing efficient requirement.Especially It is that pressure column chromatography is not difficult that a small amount of multiple collection is carried out to liquid stream in the middle pressure separation process of natural products, typically, This allows for thin-layer chromatography can not being used to detect in a large amount of preparation process, can only carry out it is without basis beat section, then divided again From, may so cause script initial gross separation compound intersect it is serious.

Ultraviolet Detector of the prior art uses single band measuring method (CN 2553374Y), the light warp that light source is sent Cross and monochromatic light formed after optical filter, by after sample cell with sample effect, be partly absorbed by the sample, partly through flow cell, shine Electrooptical device is mapped to, electric signal is converted to, will be simulated by D/A converter module again after amplifying circuit amplified signal Signal is converted to the data signal proportional with concentration.Curve is drawn out through numeral method or output to specific register instrument Figure, then carry out post-processing.

But, compound it is complicated, species is various, and the wave band of its UV absorption is also incomplete same, only with The compound that other do not possess wave band absorption is inevitably omitted in the absorption of single wave band detection compound.Some single ripples Although the UV-detector of section can select 2 wave bands, compound can not be monitored using 2 wave bands simultaneously, lost Leakage is still inevitable.Meanwhile, instrument directly can not be connected with computer, it is necessary to a recorder record data.Instrument is heavy, operation Trouble.

Utility model content

The purpose of this utility model is that a kind of ultraviolet dual wave-band for normal pressure, medium pressure column chromatography separation of offer is fast Fast detector, can detect to the wavelength of 254nm and 365nm wave bands, greatly extend the inspection of different compounds simultaneously Scope is surveyed, by upper computer software, more directly perceived column chromatography for separation situation will be accurately grasped, by observing real-time absorption curve The separation situation of compound can more intuitively be grasped.

To achieve the above object, the technical solution of the utility model is as follows：

A kind of ultraviolet dual wave-band fast detector separated for normal pressure, medium pressure column chromatography, including sampling system, light source system System, data handling system；Described sampling system is made up of polyfluortetraethylene pipe and flow cell, the polyfluortetraethylene pipe and institute State flow cell to be connected, sample liquid flows through flow cell by polyfluortetraethylene pipe；Described light-source system is by 365nm uviol lamps, 254nm Uviol lamp, rectifier and transformer composition；The data handling system is by the first Ultraviolet sensor, the second Ultraviolet sensor, 8 Position single-chip microcomputer, the first group of four figures pipe, the second group of four figures pipe and serial data wire terminal, host computer composition；The circulation The side in pond is provided with the 365nm uviol lamps and 254nm uviol lamps, opposite side and the 365nm uviol lamps and 254nm uviol lamps Corresponding position is provided with the first Ultraviolet sensor and the second Ultraviolet sensor, first Ultraviolet sensor and the second ultraviolet biography Sensor is connected with 8 single-chip microcomputers；8 single-chip microcomputers respectively with the first group of four figures pipe, the second group of four figures pipe phase Even；8 single-chip microcomputers are connected by serial data wire terminal with the host computer.

Preferably, the ultraviolet dual wave-band fast detector also includes amplification module and analog-to-digital converting module, described First Ultraviolet sensor and the second Ultraviolet sensor are connected with an amplification module respectively, and the amplification module passes through a mould respectively Plan/data-converting block is connected with 8 single-chip microcomputers.

Compared with prior art, the utility model has the advantage that：During sample liquid flows through flow cell, pass through Single-chip microcomputer not only transmits the display of light absorption value while different-waveband Ultraviolet sensor is read to charactron, and is sent out to serial ports One group of two-parameter data is sent, after host computer receiving, can change with time and draw out the photon absorbing intensity of two waveband；Thus may be used Realize the line real time monitoring and analyzing to efflux.The utility model has relative low price, safety, practical, easy to operate, The features such as, have and promote well and practical value, good economic and social benefit can be produced after extensive promotion and application.

Brief description of the drawings

Fig. 1 is structural representation of the present utility model

Fig. 2 is utility model works modular structure schematic diagram

Fig. 3 is the utility model testing result oscillogram

Wherein, 1- rectifiers, 2- polyfluortetraethylene pipes, 3- flow cells, 4- first group of four figures pipes, the groups of four figures of 5- second Pipe, the Ultraviolet sensors of 6- first, 7-254nm uviol lamps, the Ultraviolet sensors of 8- second, 9-365nm uviol lamps, 10- transformers, 11-8 single-chip microcomputers, 12- serial data wire terminals.

Embodiment

The technical scheme to this patent is described in more detail below in conjunction with the accompanying drawings.

A kind of ultraviolet dual wave-band fast detector separated for normal pressure, medium pressure column chromatography, including sampling system, light source system System, data handling system；Described sampling system is made up of polyfluortetraethylene pipe 2 and flow cell 3, the polyfluortetraethylene pipe 2 It is connected with the flow cell 3, sample liquid flows through flow cell 3 by polyfluortetraethylene pipe 2；Described light-source system is ultraviolet by 365nm Lamp 9,254nm uviol lamps 7, rectifier 1 and transformer 10 are constituted；The data handling system is by the first Ultraviolet sensor 6, Two Ultraviolet sensors 8,8 single-chip microcomputers 11, the first group of four figures pipe 4, the second group of four figures pipe 5 and serial data wire terminal 12nd, host computer is constituted；The side of the flow cell 3 is provided with the 365nm uviol lamps 9 and 254nm uviol lamps 7, opposite side and institute State 365nm uviol lamps 9 and the corresponding position of 254nm uviol lamps 7 be provided with the first Ultraviolet sensor 6 and the second Ultraviolet sensor 8, The Ultraviolet sensor 8 of first Ultraviolet sensor 6 and second is connected with 8 single-chip microcomputers 11；11 points of 8 single-chip microcomputers It is not connected with the first group of four figures pipe 4, the second group of four figures pipe 5；8 single-chip microcomputers 11 by serial data wire terminal 12 with The host computer connection.

Meanwhile, in order that the detection of this instrument is more accurate, in addition to amplification module and analog-to-digital converting module, described the One Ultraviolet sensor 4 and the second Ultraviolet sensor 5 are connected with an amplification module respectively, and the amplification module passes through a mould respectively Plan/data-converting block is connected with 8 single-chip microcomputers 11.

Detection experiment：

In under normal pressure, sample 1 is separated：Ethyl (E) -3-4- fluorobenzene base esters, sample 2：The tert-butyl group (E) -3- (2- hydroxyls -3- Methoxyl group) acrylate, chromatographic column is silicagel column, and filler is 100 mesh, and applied sample amount is 200mg；

Prior to installing inspection software in calculating, and install after CH340 drivings, by USB line by computer and ultraviolet detection Instrument is connected；Now, the first charactron 4 is shown as " BULB ", represents that uviol lamp is closed；By instrument access column chromatography system After uniting and ensureing that liquid stream flows through instrument, column chromatography valve is closed, instrument is opened and simultaneously switchs.Now, the charactron of instrument first shows It is shown as " CHEC ", represents that instrument carries out ultraviolet calibration.Current light absorption value is shown when calibrating and completing, while clicking on computer Software carries out serial ports scanning.Obtain after Serial Port Information, it is the real-time monitoring that computer software can be achieved to click on and open serial ports.

Detection and analysis result such as 3,8 single-chip microcomputers 11 of accompanying drawing send data to computer software by serial ports, to double ginsengs Number carries out hyperbola drawing, while detecting ethyl (E) -3-4- fluorobenzene base ester and the tert-butyl group (E) -3- (2- hydroxyl -3- methoxies Base) acrylate.

Above-listed detailed description is illustrating for the utility model possible embodiments, and the embodiment is simultaneously not used to limitation The scope of the claims of the present utility model, all equivalence enforcements or change without departing from carried out by the utility model are intended to be limited solely by this case In the scope of the claims.

Claims (2)

1. a kind of ultraviolet dual wave-band fast detector separated for normal pressure, medium pressure column chromatography, it is characterised in that including sample introduction system System, light-source system, data handling system；Described sampling system is made up of polyfluortetraethylene pipe and flow cell, the polytetrafluoro Ethylene tube is connected with the flow cell, and sample liquid flows through flow cell by polyfluortetraethylene pipe；Described light-source system is purple by 365nm Outer lamp, 254nm uviol lamps, rectifier and transformer composition；The data handling system is by the first Ultraviolet sensor, the second purple Outer sensor, 8 single-chip microcomputers, the first group of four figures pipe, the second group of four figures pipe and serial data wire terminal, upper unit Into；The side of the flow cell is provided with the 365nm uviol lamps and 254nm uviol lamps, opposite side and the 365nm uviol lamps and The corresponding position of 254nm uviol lamps is provided with the first Ultraviolet sensor and the second Ultraviolet sensor, first Ultraviolet sensor It is connected with the second Ultraviolet sensor with 8 single-chip microcomputers；8 single-chip microcomputers respectively with the first group of four figures pipe, second Group of four figures pipe is connected；8 single-chip microcomputers are connected by serial data wire terminal with the host computer.

2. the ultraviolet dual wave-band fast detector according to claim 1 separated for normal pressure, medium pressure column chromatography, its feature It is, the ultraviolet dual wave-band fast detector also includes amplification module and analog-to-digital converting module, the first ultraviolet biography Sensor and the second Ultraviolet sensor are connected with an amplification module respectively, and the amplification module passes through an analog/digital conversion respectively Module is connected with 8 single-chip microcomputers.