AUTOMATED PURGE SYSTEM BY GAS INJECTION

Abstract

The present invention addresses to an automated gas injection system in vials with rubber septa, for simultaneous injection of gas in 24 or more positions, with injection pressure control and/or overpressure detection, applied to mass spectrometry analyses and/or gas chromatography. The present invention can be used, for example, in isotopic analyses of geological materials in equipment with carbonate extraction units, in the cleaning and decontamination of tubes to be used in isotopic or chromatographic analyses, and in the removal of contaminants from steam drag or by continuous flow, or coming from the free space of vials or tubes in the analyses of organic and inorganic materials.

The application of this invention allows reducing the current times of routine purge (flush) of at very least 3 minutes for every 2 positions (72 positions in total and final time of 108 minutes, in a batch of samples) to a total of 96 positions in 3 minutes, with a reduction of 12 times or more in the flush time, which implies greater analytical capacity to the laboratory, lower external costs of sending samples, less time to obtain results, with technology that is easy to implement in universities and research centers in general, in addition to increasing the lifespan of rubber septa.

Claims

1- AN AUTOMATED PURGE SYSTEM BY GAS INJECTION, characterized in that it comprises a block containing needles (10) for simultaneous perforation of rubber septa (11), fixed on a platform (7) coupled to an adjustable arm elevator (5), provided with a flow rate meter (1) and a pressure meter (2), with a drag gas injection point (9) and a gas outlet point (8), in addition to a lift control system (6) of the needle block (10) that perforates the septa (11) and a heating block (3) with a temperature gauge and controller (4).

2- THE AUTOMATED PURGE SYSTEM BY GAS INJECTION according to claim 1, characterized in that the block contains needles (10) for simultaneous perforation of 24, 25, 36, 48, 50, 72, 80, or 96 positions.

3- THE AUTOMATED PURGE SYSTEM BY GAS INJECTION according to claim 1, characterized in that the inlet (9) and outlet (8) of the gases occur through the same needle, or through distinct needles.

4- THE AUTOMATED PURGE SYSTEM BY GAS INJECTION according to claim 3, characterized in that in all cases the gas injection and outlet lines are independent.

5- THE AUTOMATED PURGE SYSTEM BY GAS INJECTION according to claim 1, characterized in that it has a buttonhole (6) to lift and control the height and perforation point of the rubber septa (11) by means of a tower or elevator (5) of the platform (7) of needle support (10).

6- THE AUTOMATED PURGE SYSTEM BY GAS INJECTION according to claim 1, characterized in that it has an overpressure control (2) of the outlet gases and flow rate (1) of the injection gas.

7- THE AUTOMATED PURGE SYSTEM BY GAS INJECTION according to claim 1, characterized in that the heating block (3) is a ceramic, aluminum or stainless steel digester block, with heating by controller and sensor of temperature (4).

8- THE AUTOMATED PURGE SYSTEM BY GAS INJECTION according to claim 7, characterized in that the temperature sensor can be of the Pt100, T, J, or K type.

9- THE AUTOMATED PURGE SYSTEM BY GAS INJECTION according to claim 1, characterized in that it maintains the temperature of the block between 55° C. and 90° C.

10- THE AUTOMATED PURGE SYSTEM BY GAS INJECTION according to claim 1, characterized in that it works by dragging gases indicated by the operator before the start of the process, either by means of a manual selection box, or by automatic switching.

11- THE AUTOMATED PURGE SYSTEM BY GAS INJECTION according to claim 1, characterized in that the gas injection cleaning operation time is at very least, but not limited to, 3 minutes, in a total of 72 or more positions.

12- THE AUTOMATED PURGE SYSTEM BY GAS INJECTION according to claim 1, characterized in that it can be applied, for example, in isotopic analyses of geological materials in equipment with carbonate extraction units, in the cleaning and decontamination of tubes to be used in isotopic or chromatographic analyses, and in the removal of contaminants from steam dragging or by continuous flow, or from the free space of vials or tubes, in the analyses of organic and inorganic materials.

Description

BRIEF DESCRIPTION OF DRAWINGS

[0015] The present invention will be described in more detail below, with reference to the attached figures which, in a schematic form and not limiting the inventive scope, represent examples of its embodiment. In the drawings, there are:

[0016] FIG. 1 illustrating Thermo Fischer commercial two-position automated system for gas injection with two simultaneous needles.

[0017] FIG. 2 illustrating the Thermo Fischer purge system. This describes a method of transferring CO.sub.2 using helium as a cleaning drag gas through a Thermo Fisher twin needle, showing the inlet and outlet of gas in the flush process. There are shown: a helium gas stream (A), helium gas and helium+air streams (B), a transfer needle (C), a rubber septum (D), a drag gas (helium) outlet to the sample tube (E), a sample tube (F), a sample (G), and an outlet hole (H) of contaminants by (B).

[0018] FIG. 3 illustrating the manual manifold-type system for placing needles for injecting drag gas into tubes, used in some laboratories.

[0019] FIG. 4 illustrating the commercial evaporation or drying system, or sample concentrator by gas injection, with manual elevator system.

[0020] FIG. 5 illustrating a schematic drawing of the automated gas injection system in vials with septum, object of the present invention. There are represented: a flow meter (1) for injection gas, a pressure meter (2) for outlet gases, a digester block (3) for test tubes, a temperature meter or controller (4), a tower or platform elevator (5), a lift control actuator button (6), a needle support platform (7), a gas outlet hole (8), a drag gas injection hole (9), and a gas inlet needle (10)).

[0021] FIG. 6 illustrating a detail of the system of twin needles that pass through the rubber septum, in screw closures or crimp closures, allowing the use of standard needles with gauge 15 AWG to 28 AWG of stainless steel, common, easily available on the market, not requiring special cannulas. There are represented: streams of outlet gas and contaminant mixture (example: air, water vapor, etc.) (8), inlet gas stream (9), gas inlet needle (10), rubber septum (11), needle (12) where the drag gas (e.g., helium) exits from the sample tube (13), sample tube (13), and sample (14).

DETAILED DESCRIPTION OF THE INVENTION

[0022] The automated gas injection system that is object of this invention and illustrated in FIG. 5 comprises a block containing needles (10), fixed on a platform (7), for the simultaneous perforation of, but not limited to, 24, 25, 36, 48, 50, 72, 80, or 96 positions, in septa of butyl rubber or similar, with a buttonhole (6) to lift and control the height and the point of perforation of the septa, by means of a tower or elevator (5) of the platform (7), with overpressure control (2) of the outlet gases and of the flow rate (1) of injection of the drag gas.

[0023] The inlet (9) and outlet (8) of the gases can occur through the same needle (10), or through distinct needles. A digester block (3) in ceramic, aluminum or stainless steel, with resistances for heating by the controller and thermocouple sensor (4) type Pt100, T, J, or K, which allows heating and maintaining the temperature of the set between 55 and 90° C., with an accuracy of 0.2° C. or better. Details of the system of this invention can be seen in FIG. 6, for the case of two distinct needles, where the drag gas exits the sample tube (13) through the needle (12).

[0024] The simultaneous perforation reduces the time of the gas injection cleaning operation, with a simultaneous perforation of 24, 25, 36, 48, 50, 72, 80, 96 vials with septum and caps, or precisely of septa of these vials with septum and caps.

[0025] The system of the invention is not a concentrator, but can function as one. It works by dragging gases indicated by the operator before the start of the process, or by means of a manual selection box, or by automatic switching.

[0026] The system of this invention allows the reduction of the current total cleaning routine times in a batch of samples by gas injection of 3 minutes for every 2 positions, 72 positions in total and final time of 108 minutes, for a total of 72 positions in 3 minutes; that is, a 36 times reduction in cleaning time by gas injection, considering the same number of positions. This allows a reduction of almost two hours in cleaning time by gas injection, allowing the analysis of 5 to 6 batches per week, instead of just 3, as is normally practiced.

[0027] A system that perforates and injects gas simultaneously in 72 positions, like the one of this invention, not only allows reducing the total time of all injection positions to 3 minutes; that is 108/3=36 times faster than the conventional system, but also it does not add the time of moving the robotic arm from the equipment to the new position to the initial time of 108 minutes. In addition, if a longer purge time is required, going from 3 minutes to 10 minutes, the impact on the result of the times would be even greater (72*10/2=360 minutes), but still 36 times faster than the conventional system (360/10=36). Currently, with a total cleaning time of 108 minutes by helium injection, which takes place within administrative hours, it will allow a reduction between analysis runs of almost 2 hours, considering the cleaning time by gas injection.

[0028] A weekly calculation (5 days) indicates a loss of 10 hours with the cleaning procedure; that is, more than hours of the administrative regime. For each batch of analyses, 18 hours of analysis are effectively spent after the cleaning procedure (72 positions or samples at a time). These analysis hours cannot yet be reduced due to instrumental and software limitations, as there are no two analysis channels. On average, the time spent for each batch between preparation steps and analysis is between 2 and 4 hours. In case of system adjustments, this prevents more than 3 weekly batches, as the tubes must be freshly cleaned before the start of the analysis.

[0029] With the reduction of cleaning (purge) time by gas injection to 3 minutes, by using the present invention, it is possible to add two more weekly batches of 72 (1 hour and 48 minutes) or 80 samples (120 minutes), which can increase productivity by approximately 72 positions×2 additional batches×4 weeks in samples per month (576 to 648 samples/month).

[0030] It should be emphasized that additional samples can be fed to the reaction and analysis system of the invention, but depend on the elimination of air in the new sample tubes. However, when the analysis equipment enters “reaction and data acquisition” mode, it is not possible to inject gas to clean the new tubes added.

[0031] The example cited above was used in order to illustrate some particular embodiments of the present invention, and should not, however, be interpreted as limiting the same.

[0032] The system of the invention allows the quick cleaning of several tubes, increasing the productivity of the analysis system in administrative hours and allowing a faster routine of preparation for analysis, having a direct impact on the number of samples to be analyzed per block and per day, resulting in a reduction in the number of samples to be sent to external laboratories. This represents a better use of the hour/machine time, a reduction of external shipping costs, a reduction of expenses with contracts and expenses with external analysis, less time to obtain results, faster customer service. The application of the present invention leads to greater analytical capacity in the laboratory, with the use of a technology that is easy to implement in research centers in general.

[0033] The reduction of current routine purge (flush) times allows the analysis of more weekly batches, in addition to the reduction of analytical costs with shorter shutdowns between analyses, local flush in the preparation equipment itself for analyses, or externally, in a separate module.

[0034] Furthermore, the invention allows the injection and dragging in vials with septum and caps, closed, with control of the pressure and flow of the injected gas, without risks for the operators, with direct displacement to a gas outlet, or to the exhaust, without opening the system. This is an advantage if there is the presence of toxic gases, such as H.sub.2S, inside the vials, generated during sample preservation and after collection. These generated gases are not of interest to analysis and could also be displaced by inert gas injection prior to analysis.

[0035] The application of the invention also allows reducing the disposal of rubber septa, which would be constantly perforated in the same position by the conventional flush system. With the invention, the perforations in points in positions adjusted by the user, but random, results in the increase of the useful life of the rubber septa.

[0036] It should be noted that, although the present invention has been described in relation to the attached drawings, it may undergo modifications and adaptations for configuration adjustments, depending on the specific situation, but provided that it is within the inventive scope defined herein.