Express-chromatron

FIELD: the invention refers to laboratory chromatographic devices for conducting high-speed chromatographic analysis.

SUBSTANCE: the express-chromatron has an injector, a chromatographic column located in a thermostat, a detector, an amplifier of the signal of the detector, an analog-digital converter, a control system, a pneumatic system. The column is fulfilled either in the shape of a short capillary column or either in the shape of a polycapillary column. The injector is fulfilled with possibility of introduction of the test for the time of 5-50 ms. The detector and the amplifier of its signal are fulfilled with possibility of ensuring constant time of no worse then 10-3 sec. The analog-digital converter is fulfilled with possibility of ensuring speed of no less then 200 measurements in a second.

EFFECT: ensures conducting high-speed chromatographic analysis.

11 cl, 2 dwg

 

The invention relates to chromatography, in particular for laboratory chromatographic instruments for conducting high-speed chromatographic analysis.

Known gas chromatograph, comprising injector input sample in a chromatographic column for separation, thermostat to maintain desired temperature analysis or programming temperature at a given speed, the pneumatic circuit, to generate the required differential pressure at the inlet of the chromatographic column, a detector for the registration of substances coming out of the speakers and amplifier electrical signal from the detector, analog-to-digital Converter for digitizing the signal from the detector control system for the collection, processing chromatographic data, management of the physical parameters chromatograph (pressure on the column, the temperature of thermostat), necessary for the separation process in the device that is selected as a prototype (the chromatograph Crystal - 2000M, Manual, Special design Bureau "chromatic", 1995).

The disadvantage of this chromatograph is that it does not allow the separation of a mixture of several components, for 5-20 times with and work with short capillary and polycapillary columns. This restriction is due the ANO with the what elements of the chromatograph are not adapted to the modes, providing both rapid sample introduction into the column and the detection of small time (20-200 MS) chromatographic peaks.

The authors sought to develop a chromatograph for rapid analysis, allowing the separation of a mixture of several components, for 5-20 times with and work with short capillary and polycapillary columns.

The problem is solved in that in the Express chromatograph, including the injector, chromatographic column, thermostat, pneumatic circuit, the detector, the amplifier signal detector, an analog-to-digital Converter, the control system, the chromatographic column is made in the form of a short capillary column diameter capillary 10-100 μm, or in the form of a polycapillary column length of 5-100 see the Injector in it is made with the possibility of introduction of the sample during 5-50 MS. The detector is arranged to provide a time constant of not less than 10-3with the opportunity to work with the flow of carrier gas from 30 to 150 cm3/min. Amplifier signal detector configured to provide a time constant of not less than 10-3with made in the form of electrometric amplifier with low input capacitances. Analog-to-digital Converter is implemented with a chance to view the Yu ensuring speed digitizing at least 200 measurements per second, made containing either a scaler signal, or an electronic switch amplifiers with different gain. thermostat is configured to implement the regime, temperature programming of the column in the area of values from 1 to 150°C/min Pneumatic circuit is designed with programmable pressure of carrier gas at the inlet into the column in the field values from 0.1 to 10 ATM surplus for times from 1 to 300 C. thermostat and pneumatic circuit is made with possibility of simultaneous programming during the analysis of temperature and pressure. The control system is configured to monitor the efficiency of pneumatic elements, which include pressure regulators, flow regulators, gas regulators reset gas valves, gas lines, by setting between the pneumatic circuit elements of the pressure sensors and monitoring, remote network monitoring its pneumatic and electronic components, as well as for ongoing and completed tests.

The technical effect of the invention is to provide opportunities to work with columns for rapid chromatography - short capillary and polycapillary mode as gas-liquid, and getaccountinfo chromatography in Tahlequah, when you need rapid separation of mixtures of chemical compounds, for example, in energy, industry, environment, medicine, as well as when conducting chemical analyses in a wide range of activities related to chemistry. In multiple analyses for a short time, which improves the accuracy of chromatographic analysis. And the possibility of remote maintenance and network diagnostics.

The invention is illustrated by figure 1, which presents a block diagram of the chromatograph, and figure 2, which shows the chromatogram of light hydrocarbons on polycapillary column polytrimethylene (PTMSP) as chromatographic material.

Declare chromatograph consists of the following elements: 1 - injector, 2 - chromatographic column, 3 - thermostat 4 - detector, 5 - e amplifier signal detector, 6 - analog-to-digital Converter (ADC), 7 - management system, 8 - programming device inlet pressure column 9 - unit temperature control thermostat.

To implement high-speed chromatography required speed input sample 5-50 MS. If the length of the input is larger, then it determines the width of the final peak, leaving a column that does not allow to realize all the possibilities of the column. So I known chromatograph taken as the e prototype focused on manual entry allows you to enter the sample for a time of about 200-300 MS, and this time depends on the skill of the operator. Automatic dispensers (autosampler) can reduce this time to 100 MS, which is not always suitable speed injection.

In the case when the detector has a large time constant (as in the prototype), it has a slow response to the flowing substance from the column, it leads to a distortion of the peak shape, the deterioration observed efficiency of the column and, consequently, deterioration of the observed separation properties.

Electronic amplifier, amplifying the signal detector also has its own time constant. In that case, if the value of this time constant is large, it will also contribute to the observed increase of the width of the peak and, consequently, deterioration of the separation efficiency component of the sample.

After the signal from the detector is amplified by an electronic amplifier, it is converted by analog-to-digital Converter (ADC) in a digital form for further computer processing. The most important characteristic of the ADC for high-speed signal processing is the number of measurements per second. If during the output of the chromatographic peak will be conducted 1-10 measurements, calculated on the basis of these data the value of pasadita would be a big mistake for to be used for quantitative measurements. Thus, there are several reasons that affect the ability of the instrument to conduct a rapid chromatographic separation.

Work claimed chromatograph based on the fact that the chromatograph has a set of elements that do not distort the shape of the chromatographic peaks: the Sample is introduced into the column at the time of 5-50 MS using a specially designed injector. The injector 1 is made automatic with the possibility of input samples during 5-50 MS, or in a short capillary column diameter capillary 10-100 μm, or polycapillary column length of 5-100 see the Detector 4 may be based on different physical principles and has a time constant not worse in 0.001 sec. It may work if the flow of carrier gas from 30-150 cm3/min. Electronic amplifier 5 that amplifies the signal from the detector is made with small input capacitances, providing the opportunity to have the time constant is not worse than 0,001 C. Amplifier 5 may be made in the form of electrometric amplifier with low input capacitances. The control system is arranged so that the rate of the digitized signal from the detector through an analog-to-digital Converter (ADC) 6 occurs at a rate of 500-1000 measurements per second, which allows for multiple ozimok the chromatographic peak with a small duration. To increase dynamic range while maintaining its performance ADC is made or containing a block scale signal, or is equipped with an electronic switch amplifiers with different gains. However, when processing small-time peaks, there is a feature that is not possible to apply standard techniques of signal processing. Namely, when working electrometric amplifiers are used to amplify the signal from ionization detectors, the main source of interference is a network aiming to avoid in which the installation place of the chromatograph is almost impossible. The usual way to tackle it is to use filters based on the presence of the RC-circuit in the amplifier circuit. But this way of reducing network interference leads to an increase in the time constant of the amplifier and, consequently, to a distortion of the peak shape. Of course, that such a method of suppressing noise is not reasonable in the processing of chromatographic peaks of short duration. Therefore, when working with rapid chromatographic columns, the signal is filtered not hardware methods, and special mathematical processing implemented by numerical methods, which allows you to filter signal from noise. To ensure reliable filtering of the signal, the speed Egiazarov should be as high as possible. Besides the function of signal processing, ADC 6 is arranged in such a way that its launch simultaneously generates an electrical signal at the start input device samples. This gives the possibility of increasing the accuracy and reproducibility in the measurement of the time of the separated components from the column.

For the analysis of the mixture of substances injected into the injector 1, where it evaporates and is located in the volume, which is connected by capillary column 2, but in column misses. While the carrier gas flows through a short capillary or polycapillary column 2, located in thermostat 3. In the beginning of the analysis cycle, the control system switches the gas flows so that the flow of carrier gas ceases to be fed to the column begins to pass through the volume with the sample and makes the sample into the column. In this position the flow of carrier gas is maintained for a certain time, which is necessary for the input samples. After sample injection, the flow of carrier gas returns to its original position, and the sample introduced into the column and is separated into individual components emerging from the column and enters the detector 4. The detector 4 converts the concentration received him the substance into an electric signal, which, in turn, enhanced electronic (in the case of ionization detectors - electrometric) amplifier 5. Standing in the time of the amplifier 5 and the detector 4 are what they do not change the width of the chromatographic peak of more than 1%. Simultaneously, the amplifier 5 produces a strengthening of the current detector 4 and converts it into a voltage value required for the ADC 6. ADC 6 converts the analog signal 500-1000 times per second digital value, and transmits the control computer, and then using a program processing digital filtering of noise (for example, network interference), removes noise, and using the program processing the chromatographic data is the representation of the separation in the form of a chromatogram and its numerical characteristics.

In the process of separation, that is, while the sample in the column from the input sample to the output of the last component is the programming of the temperature of the column (i.e. the temperature increase from the initial, lower to higher). Programming of the temperature is performed at a speed ranging from 1 to 150°C/min depending on the problem being solved. This mode of carrying out the separation process increases the rate of elution of the components of the mixture. At the same time, to further increase the speed of separation is programming the inlet pressure in the column, i.e. the increase in the pressure in the pressure range from 0.1 to 10 ATM redundant during the separation process with lying to the us from 1 to 300 C. Two types of programming - pressure and temperature can occur simultaneously, or separately programming the temperature at constant pressure at the inlet into the column and programming of pressure at constant temperature. There is also the ability to carry out the separation process at constant temperature and pressure.

To control the pneumatic system of the device, on all gas communications installed pressure sensors that allows you to record the state of the chromatograph and make a conclusion about the fault without disconnecting the communication. The testimony of all pressure sensors are visualized on the computer monitor management system that enables quick diagnosis of the state of the device.

The system control device is constructed in such a way that when the computer is connected, is included in the control system, computer network, there is the possibility of remote communication, that is, work with it and control it from another, remote computer.

An advantage of the claimed device in comparison with the prototype is the ability to work not only with traditional types of chromatographic columns mode as gas-liquid, and getaccountinfo chromatography, but with Express-column - short small diameter capillary and polycapillaries opens the possibility to solve in addition to the traditional tasks of gas chromatography, related to the separation of different classes of chemical compounds in petrochemical, energy, food industry and medicine, but also in those industries where the use of chromatography was not possible. For example, in the analysis of thermolabile compounds that emerge from Express columns for the reason that do not have time to decompose due to the low time presence in the chromatographic column for rapid analysis. Using the claimed device, you receive the possibility of multiple analyses for a limited time, which increases as the accuracy of chromatographic analysis, and improve the metrological characteristics of the methods in which gas chromatography is the ultimate method definitions. An example of the advantages claimed chromatograph is illustrated in figure 2 separation of a mixture of hydrocarbons, C1-C4on GAC length of 30 cm with polytrimethylene (PTMSP) as stationary phase. Stream media, nitrogen is 70 ml/min, column temperature 45°C. a Detector - ionization-flaming. The mixture of hydrocarbons figure 2 is a 1 - methane + ethylene; 2 - propene; 3 - propane; 4 - isobutane; 5 - butane. At the same Express terms of input samples, and use a high-speed ADC (1000 per second) for signal amplification high-speed ionization-flaming det is ktora used two different electronic signal amplifier: BID-36, which staff chromatograph equipped with a COLOR-500 (figa), and the amplifier with a time constant of 2 MS (figb). The observed separation R of butane and isobutane shown on the chromatogram when using the amplifier BID-36 is 1.2, whereas the degree of separation using an amplifier with a time constant of 2 MS is 2.9, which is more than twice as high. This example clearly shows the effect of the time constant of the electronic amplifier to the type of performance that will be obtained. Similarly affects the appearance of the chromatogram speed input sample into the column and the time constant of the detector.

Another advantage of the proposed device is a network control of its gas scheme and the result of the division, which opens up entirely new possibilities for remote maintenance, network diagnostics and methodological consulting, which is important in the absence of specialists in the field of chromatography for users of the device.

1. Express chromatograph, including the injector, chromatographic column, thermostat, pneumatic system, detector, amplifier signal detector, an analog-to-digital Converter, control system, characterized in that the chromatographic column is made in the form of either a short capillary column, or polycapillary the column, an injector configured to introduce the sample during 5-50 MS, the detector configured to provide a time constant of not less than 10-3with the amplifier of the signal detector is arranged to provide a time constant of not less than 10-3with an analog-to-digital Converter configured to provide speed digitizing at least 200 measurements per second.

2. Chromatograph according to claim 1, characterized in that the short capillary column made with the diameter of the capillary 10-100 microns.

3. Chromatograph according to claim 1, wherein the polycapillary column made of length 5-100 see

4. Chromatograph according to claim 1, characterized in that the detector is designed to operate at flows of carrier gas 30-150 cm3/min

5. Chromatograph according to claim 1, characterized in that the amplifier is made in the form of electrometric amplifier with low input capacitances.

6. Chromatograph according to claim 1, characterized in that the analog-to-digital Converter is implemented with a scaler signal, or an electronic switch amplifiers with different gain.

7. Chromatograph according to claim 1, wherein thermostat is configured to implement regime change temperature of the column in the field values 1-150°C/min

8. Chromatograph according to claim 1, characterized in that the pneumatic system is configured to increase the pressure of carrier gas at the inlet into the column in the field values of 0.1-10 ATM at times 1-300 C.

9. Chromatograph according to claim 1, characterized in that the chromatograph is made with possibility of simultaneous changes during the analysis of temperature and pressure.

10. Chromatograph according to claim 1, characterized in that the control system is configured to monitor the efficiency of pneumatic elements by setting all of its gas communication between the pneumatic circuit elements of the pressure sensors and control their condition.

11. Chromatograph according to claim 1, characterized in that the control system is capable of remote network monitoring its pneumatic and electronic components, as well as for ongoing and completed tests.



 

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Express-chromatron // 2300764

FIELD: the invention refers to laboratory chromatographic devices for conducting high-speed chromatographic analysis.

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