JPS585247Y2 - Sample introduction device - Google Patents

Description

[Detailed Description of the Invention] This invention relates to a sample introduction device in a gas analyzer such as a gas chromatograph or a gas chromatograph mass spectrometer.

When introducing a sample into a gas analyzer, it is necessary for analysis efficiency to remove the solvent in the sample and introduce the entire amount of target components into the analysis system.For this reason, carrier gas is usually used at the stage before vaporizing the sample. The solvent gas is temporarily reversed and only the solvent gas is discharged to the outside.

However, there are various types of samples, such as high-boiling point samples and low-boiling point samples, and the above-described solvent separation means that always relies only on the difference in volatility between the solute and solvent of the sample at room temperature is not efficient.

In addition, from the perspective of introducing samples into efficient analysis systems,
When the vaporized bone is discharged at room temperature, the loss of the sample is large when the boiling point of the sample is low.

This idea was devised in view of the above-mentioned drawbacks of the conventional methods.When a sample is introduced into an analysis system, the solvent is efficiently separated and discharged from the system, and the solvent is not discharged from the system together with the sample solvent. This is intended to improve sample introduction efficiency.

Next, embodiments will be described with reference to the drawings. FIG. 1 is a partially sectional side view of the sample introduction device of this invention, showing the position at the time of sample introduction.

In the figure, reference numeral 1 indicates a microsyringe, which is used to inject a sample into a sample introduction section 3 having a sealing rubber 2.

Reference numeral 4 denotes a sample loading frame, which has a glass needle portion 4' at its tip, and a magnet 5, for example, is attached to the other end, and is held in this position by cooperating with an electromagnetic mechanism 6 outside the pipe, or a Go down to the sample vaporization position shown in Figure 2.

A heating device 7 is provided outside the tube at the lower limit position where the tip of the glass needle 4' at the tip of the sample loading frame 4 has descended inside the tube.
The sample loaded onto the tip 4' of the glass needle is heated and vaporized at this position and sent to the analysis system, for example a column 9, via the analysis system connection port 8.

10 indicates a carrier gas introduction hole. An exhaust hole to the outside air, that is, a solvent outlet 11 in this case, is provided above the sample introduction section 3 .

The above parts in the figure show existing technical parts.

In the figure, reference numeral 12 denotes a temperature control jacket that covers the outside of the sample introduction section 3 and adjusts and maintains the temperature inside the sample introduction section 3 at a desired temperature.

As the fluid for heating or cooling, in addition to tap water, cold water, and high-temperature gas, liquid nitrogen, dry ice, etc. are used for cooling, depending on the desired temperature.

Depending on the case, it is also possible to jacket the cooling body or heating body with a solid material.

By providing this temperature control jacket 12, the temperature of the sample introduction part 3 can be adjusted as desired, and for example, for low boiling point samples, it is possible to prevent the sample loaded into the sample loading frame 4 from being vaporized and discharged together with the solvent. Cooling with a jacket restricts vaporization at that position, and for high boiling point samples, unnecessary low boiling point samples are vaporized and removed along with the solvent by heating with a jacket, and all date and time solvents are efficiently exhausted. This allows a large amount of only the high boiling point sample to be efficiently introduced into the analysis system while being discharged to the outlet.

Next, in the figure, numerals 13 and 14 respectively indicate on-off valves.

It is convenient to use electromagnetic on-off valves for these.
and the carrier gas introduction hole 10 as well as at the solvent outlet section 11.

The on-off valve 14 is preferably for a throttle valve lid.

Optionally in this embodiment it is possible to insert 15 vacuum suction devices as shown in the figure.

Next, the operation of the sample introduction device having the above configuration will be explained.

First, the operation when the vacuum suction device 15 is not used will be described.

First, a heating or cooling fluid is caused to flow through the temperature control jacket 12 so that the temperature of the temperature control jacket 12 meets the conditions described later, and the electromagnetic mechanism 6 attracts the magnet 5 to the sample loading frame 4. Glass needle at the tip of 4'
set so that the part is located at the center of the sample introduction part 3.

The on-off valves 13 and 14 are left open so that the carrier gas flows in through the inlet 10 and flows toward the analysis system 9 and the solvent outlet 11.

Next, a sample is inserted through the sealing rubber 2 using a microsurgical needle 1, and the sample is attached to the tip of the glass needle 4' of the sample load 4.

Once the sample has been deposited, the microsyringe 1 is removed.

In this state, the solvent contained in the sample is vaporized by the temperature of the sample introduction part 3 set by the temperature control jacket 12, and is absorbed into the carrier gas which is also flowing in the direction of the solvent outlet part 11 as described above. is discharged outside.

Next, after waiting for the solvent gas to be discharged, the on-off valve 14 is closed, the electromagnetic mechanism 6 is operated, the sample loading frame 4 is dropped, and the glass needle portion at the tip thereof is positioned within the heating device 7.

Figure 2 shows this position.

At this position, the sample is vaporized and introduced into the analysis system 9 on a carrier gas.

The temperature set by the temperature control jacket 12 of the sample introduction section 3 is set to a value lower than the boiling point of the sample and higher than the boiling point of the solvent and unnecessary low-boiling point samples.

For example, when the sample is cholesterol (boiling point 280°C) and the solvent is acetone (boiling point 56.5°C), the controlled temperature is set within the range of 150°C to 200°C.

In this device, the temperature of the sample introduction part is arbitrarily controlled and set by the temperature control jacket as described above, so when selectively discharging the solvent, the solvent is actively vaporized and the solvent discharge efficiency is high. Since a set temperature lower than the boiling point of the solute can be selected, there is no fear that the sample will be vaporized and discharged together with the solvent, and the entire amount of the sample can be sent to the analysis system.

Next, the operation when using the vacuum suction device 15 will be explained.

With the on-off valve 13 in the closed position, a sample is loaded from the sealing rubber 2 onto the tip of the sample loading frame 4 using the microsyringe 1 as described above.

When the load is completed, the on-off valve 14 is opened and exhausted by the vacuum suction device 15, and the vaporized gas of the refrigerant is discharged to the outside of the pipe.

After completing exhaustion, close the on-off valve 14, open the on-off valve 13,
After waiting for the flow of the carrier gas to stabilize, the tip of the sample loading frame 4 is lowered to the heating device 7 section and analysis is performed.

Since the sample loading frame 4 passes through the opening/closing valve 13 during descent, the opening/closing valve is of a type that opens at the center.

By using a vacuum suction device, the time required to exhaust the solvent can be shortened compared to the conventional method, and by lowering the atmospheric pressure, the boiling point of the solvent can be lowered and the suction and exhaust efficiency can be increased.

Since the sample introduction device of this invention is constructed as described above, the temperature of the sample introduction part can be adjusted to an intermediate temperature between the temperature of the solvent and the sample solute when selectively discharging the solvent due to the difference in volatility of the solvent. By being able to set it at any position, it can be carried out efficiently, and if the sample has a low boiling point, the temperature at that part can be set low to reduce the loss of the sample solute being discharged to the outside together with the solvent, i.e., the loss of introduction into the analysis system. This has the effect of making it possible to introduce it into a full-volume branching system.

[Brief explanation of drawings]

The figures show an embodiment of the sample introduction device of this invention, in which FIG. 1 is a partially sectional side view at the sample introduction position, and FIG. 2 is a similar view during sample vaporization analysis. 1...Microsyringe, 2...Sealing rubber, 3...Sample introduction part, 4...Sample loading frame, 5... Magnet, 6... Electromagnetic mechanism, 7... Heating device, 8... Analysis system connection port, 9... Analysis system (column), 10...
... Carrier gas inlet, 11 ... Solvent discharge port, 12 ... Temperature control jacket, 13 ...
...Opening/closing valve, 15...Vacuum suction device.

Claims (1)

[Scope of utility model registration request] 1. A sample introduction section in which a sample is introduced by penetrating the sealing rubber with a microsyringe, a sample heating section, and a discharge section for discharging the solvent contained in the sample to the outside; these parts are connected, and A carrier gas introduction hole is provided between the sample introduction section and the sample heating section, and a conduit with a connection port to the analysis system is provided at the rear end, and is moved between the sample introduction section 1 and the sample heating section. In an apparatus that allows the sample to be introduced and vaporized into the analysis system using a sample loading frame, the sample introduction section is equipped with a temperature adjustment jacket that adjusts the temperature of that part from the outside to a desired temperature. What is claimed is: 1. A sample introduction device, further comprising a first on-off valve in a conduit between a sample introduction part and a carrier gas introduction hole, and a second on-off valve in a solvent discharge conduit. 2. The sample introduction device according to claim 1, wherein a vacuum suction device is connected to the solvent discharge pipe.