Patent Publication Number: US-11387089-B2

Title: Direct sample introduction device and method for cooling sample introduction probe

Description:
INCORPORATION BY REFERENCE 
     The disclosure of the following priority application is herein incorporated by reference: Japanese Patent Application No. 2019-234813 filed Dec. 25, 2019 
     TECHNICAL FIELD 
     The present invention relates to a direct sample introduction device and a method for cooling a sample introduction probe 
     BACKGROUND ART 
     In a mass spectrometer, other than a method for introducing a sample to be analyzed which has passed through a preliminary analyzer such as a gas chromatograph, a direct sample introduction method (direct introduction probe method or direct exposure probe method) in which a sample to be analyzed is introduced directly into an ion source without passing through the preliminary analyzer is also utilized. In the direct sample introduction method, a probe with a solid or liquid sample to be analyzed inserted in or coated at the tip is introduced into the mass spectrometer, and the probe is heated to vaporize the sample to be analyzed (See Patent Literature 1). 
     CITATION LIST 
     Patent Literature 
     Patent Literature 1: Japanese Laid-Open Patent Publication No. 2009-264950 
     SUMMARY OF INVENTION 
     Technical Problem 
     In the direct sample introduction method, a probe is heated to around 500° C. in order to vaporize a sample. Therefore, in order to take out the probe used for introducing the sample from a direct sample introducing device or a mass spectrometer, it is necessary to wait for the temperature of the probe to drop to around room temperature for safety. Therefore, because of a waiting time required for cooling the probe during the analysis of a plurality of samples, it is difficult to sufficiently improve the analysis throughput. 
     Solution to Problem 
     According to the first aspect, a direct sample introduction device includes: a pre-evacuating chamber that has an internal space extending in a first direction through which a sample introduction probe extends in the first direction; a first ventilation unit that is allowed to be opened and closed, with a first end thereof being connected to the pre-evacuating chamber; and a second ventilation unit a first end of which is connected to the pre-evacuating chamber and a second end of which is connected to a low pressure source. 
     According to the second aspect, a method of cooling a sample introduction probe includes: arranging a sample introduction probe in the pre-evacuating chamber having an internal space extending in a first direction; supplying gas to an inside of the pre-evacuating chamber through a first ventilation unit a first end of which is connected to the pre-evacuating chamber; and evacuating gas of the inside of the pre-evacuating chamber through a second ventilation unit a first end of which is connected to the pre-evacuating chamber. 
     Advantageous Effects of Invention 
     According to the present invention, the heated sample introduction probe can be cooled in a short time, and the waiting time for taking out the sample introduction probe can be shortened. 
    
    
     
       BRIEF DESCRIPTION OF DRAWINGS 
         FIG. 1  is a cross-sectional view showing a state in which a sample introduction probe is being pre-evacuated or a sample introduction probe is being cooled in a mass spectrometer equipped with a direct sample introduction device according to one embodiment. 
         FIG. 2  is a cross-sectional view showing a state in which a sample is being introduced from a sample introduction probe into the mass spectrometer equipped with a direct sample introduction device according to one embodiment. 
         FIG. 3  is a diagram showing an example of a sample introduction probe. 
         FIG. 4  is a diagram showing a first embodiment of a method for cooling a sample introduction probe. 
         FIG. 5  is a diagram showing a second embodiment of a method for cooling a sample introduction probe. 
     
    
    
     DESCRIPTION OF EMBODIMENTS 
     One Embodiment of Direct Sample Introduction Device 
     Hereinafter, a direct sample introduction device  1  according to one embodiment will be described with reference to  FIGS. 1 and 2 . 
       FIG. 1  is a cross-sectional view showing a mass spectrometer  20  equipped with the direct sample introduction device  1  which is shown in a region surrounded by a broken line according to one embodiment.  FIG. 1  shows a state in which a sample introduction probe  10  is being pre-evacuated or the sample introduction probe  10  is being cooled in the direct sample introduction device  1 . 
       FIG. 2  is a cross-sectional view showing a state in which a sample is being introduced from the sample introduction probe  10  to the mass spectrometer  20  equipped with the direct sample introduction device  1  according to one embodiment which is shown in a region surrounded by a broken line. 
     The mass spectrometer  20  is, for example, a quadrupole mass spectrometer including an ionization chamber  22 , a skimmer  23 , an ion guide  24 , a partition electrode  25 , a quadrupole mass filter  26 , and an ion detector  27  in a housing  21 . 
     The sample to be analyzed is ionized in the ionization chamber  22 , and then proceeds in the +Z direction, passes through the skimmer  23 , is guided by the ion guide  24  to pass through the partition electrode  25 , is selected by the quadrupole mass filter  26  according to m/z, and is incident to the ion detector  27 . 
     The inside of the housing  21  is depressurized by a vacuum pump  28 . 
     The direct sample introduction device  1  includes a pre-evacuating chamber  2  having an internal space  3  extending in the X direction shown by an arrow in  FIGS. 1 and 2 , and the internal space  3  of the pre-evacuating chamber  2  is configured such that the sample introduction probe  10  can run through the internal space in the X direction. 
     A gate valve  17  is provided between the pre-evacuating chamber  2  of the direct sample introduction device  1  and the housing  21  of the mass spectrometer  20 . The gate valve  17  includes, as an example, an outer frame  17   s  and a rotary valve  17   r  having a through hole  17   p  therein. The rotary valve  17   r  is rotatable with respect to the outer frame  17   s  about a rotation axis in the Y direction which is orthogonal to the X direction and to the Z direction. 
     As shown in  FIG. 1 , depending on the rotation angle of the rotary valve  17   r , when the direction of the through hole  17   p  does not coincide with the X direction, the gate valve  17  is in a closed state so that the inside of the housing  21  is sealed from the pre-evacuating chamber  2 . 
     On the other hand, depending on the rotation angle of the rotary valve  17   r , when the direction of the through hole  17   p  coincides with the X direction, the gate valve  17  shifts to an open state, and then the sample introduction probe  10  can be inserted into the housing  21  via the through hole  17   p  from the pre-evacuating chamber  2 . 
     The gate valve  17  is not limited to the one having the rotary valve  17   r  described above, but may be one having a valve that is movable linearly. 
     A gas supply/evacuate unit  4 , a gas evacuate unit  5 , and a gas supply unit  6  are connected to the internal space  3  of the pre-evacuating chamber  2 , and the gas in the pre-evacuating chamber  2  is supplied or evacuated through the gas supply/evacuate unit  4 , the gas evacuate unit  5 , or the gas supply unit  6 . 
     The gas supply/evacuate unit  4  includes a valve  4   v , and one end (first end)  4   a  extended from the valve  4   v  is connected to the pre-evacuating chamber  2  and the other end (second end)  4   b  extended from the valve  4   v  is open to the atmosphere (or other than the internal space  3  of the pre-evacuating chamber  2 ). 
     The gas evacuate unit  5  includes a valve  5   v , and one end (first end)  5   a  extended from the valve  5   v  is connected to the pre-evacuating chamber  2  and the other end (second end)  5   b  extended from the valve  5   v  is connected to a low pressure source  31 , such as a vacuum pump. The low-pressure source  31  is, for example, a vacuum pump, and may be a back pump of the vacuum pump  28  connected to the mass spectrometer  20 . 
     As an example, the first end  5   a  of the gas evacuate unit  5  and the first end  4   a  of the gas supply/evacuate unit  4  are arranged at different positions in the pre-evacuating chamber  2  in the X direction. 
     The gas supply unit  6  includes a valve  6   v , and one end (first end)  6   a  extended from the valve  6   v  is integrated with the first end  5   a  of the gas evacuate unit  54  and connected to the pre-evacuating chamber  2 , and the other end (second end)  6   b  extended from valve  6   v  is connected to a gas supply source  32  that supplies a gas having pressure equal to or higher than atmospheric pressure. As an example, the first end  6   a  of the gas supply unit  6  and the first end  4   a  of the gas supply/evacuate unit  4  are arranged at different positions in the pre-evacuating chamber  2  in the X direction. 
     The gas supply source  32  may be, for example, a compressor or the like, and if the low pressure source  31  or the vacuum pump  28  connected to the mass spectrometer  20  is capable of supplying a predetermined pressure, the low pressure source  31  or the vacuum pump  28  may be used as the gas supply source  32 . The gas supplied from the gas supply source  32  may be air or a gas other than air such as nitrogen. 
     For improving the airtightness of the internal space  3  of the pre-evacuating chamber  2  in a state where the sample introduction probe  10  is inserted, seal members  9  such as O-rings are provided near both ends in the X direction of the pre-evacuating chamber  2 . 
     The pre-evacuating chamber  2  is provided with a contact type or non-contact type temperature sensor  7  for measuring information about the temperature of the sample introduction probe  10  which is to be inserted into the pre-evacuating chamber  2 . The temperature information measured by the temperature sensor  7  is input to a control unit  8  as a signal St 1 . 
     The control unit  8 , as an example, transmits control signals Sa, Sb 1  and Sc respectively to the valves  4   v  of the gas supply/evacuate unit  4 , the valve  5   v  of the gas evacuate unit  5 , and the valve  6   v  of the gas supply unit  6  to control the opening/closing operation of each valve. 
     Further, the control unit  8  may send a control signal Sd to the gate valve  17  to control opening/closing operation of the gate valve  17 . 
     In one embodiment of the direct sample introduction device  1 , the gas supply/evacuate unit  4  may be referred to as a first ventilation unit, the gas evacuate unit  5  may be referred to as a second ventilation unit, and the gas supply unit  6  may be referred to as a third ventilation unit. 
     In one embodiment as described above, the first end  5   a  of the gas evacuate unit  5  and the first end  6   a  of the gas supply unit  6  are integrated together and connected to the pre-evacuating chamber  2 . However, the first end  5   a  of the gas evacuate unit  5  and the first end  6   a  of the gas supply unit  6  may be individually connected to the pre-evacuating chamber  2 . 
     As will be explained in an embodiment of the method for cooling the sample introduction probe  10 , the direct sample introduction device  1  can cool the sample introduction probe  10  without necessarily including the evacuate unit  6 . Therefore, the direct sample introduction device  1  does not necessarily have the evacuate unit  6 . 
     The control unit  8  may control the pressure (low pressure) itself generated by the low pressure source  31  by transmitting a control signal Sb 2  to the low pressure source  31  instead of controlling the opening/closing operation of the valve  5   v  of the gas evacuate unit  5 . In this case, the valve  5   v  of the gas evacuate unit  5  may be always in an open state, or the valve  5   v  of the gas evacuate unit  5  may not be provided. 
     Method of Mass Spectrometry Using Direct Sample Introduction Device of One Embodiment 
     Hereinafter, a method of mass spectrometry using the direct sample introduction device  1  and the mass spectrometer  20  will be described with reference to  FIGS. 1 to 3 . 
       FIG. 3  is a cross-sectional view showing an example of the sample introduction probe  10  used in the direct sample introduction device  1  of the embodiment. The sample introduction probe  10  is provided with a heater  12  for heating a sample cup  11  and a wiring  13  for supplying electric power for heating the heater  12 . Further, a temperature sensor  14  may be provided for measuring information about the temperature in the vicinity of a tip portion  10   a  including the sample cup  11  of the sample introduction probe  10 . The temperature sensor  14  outputs a signal St 2  including information about temperature via a signal line  15 . 
     For analysis, an operator puts a sample to be analyzed in the sample cup  11  arranged near the tip portion  10   a  of the sample introduction probe  10 . Alternatively, the sample to be analyzed may be coated on the heater  12 . 
     The operator inserts the sample introduction probe  10  which the sample is put in or coated on into the internal space  3  of the pre-evacuating chamber  2  of the sample introduction device  1  from the tip portion  10   a . When the sample introduction probe  10  is inserted, the seal members  9  contact with the sample introduction probe  10 , so that the internal space  3  is substantially airtight to the outside. 
     It is noted that, the internal space  3  of the pre-evacuating chamber  2  is open to the atmosphere until the sample introduction probe  10  is inserted. Therefore, until the sample introduction probe  10  is inserted, the control unit  8  transmits the control signal Sb 1  to the valve  5   v  to make the valve  5   v  in a closed state so as to block the flow of gas via the gas evacuate unit  5  from the pre-evacuating chamber  2  to the low pressure source  31 . Further, the control unit  8  transmits the control signal Sc to the valve  6   v  to make the valve  6   v  in a closed state so as to block the flow of gas via the gas supply unit  6  from the gas supply source  32  to the pre-evacuating chamber  2 . Further, the control unit  8  makes the gate valve  17  also in a closed state. 
     When the sample introduction probe  10  is inserted into the internal space  3  of the pre-evacuating chamber  2 , the control unit  8  transmits the control signal Sb 1  to the valve  5   v  to make the valve  5   v  in an open state. And the control unit  8  transmits the control signal Sa to the valve  4   v  to make the valve  4   v  in a closed state so as to block the flow of gas via the gas supply/evacuate unit  4  from the outside to the pre-evacuating chamber  2 . As a result, the gas in the internal space  3  of the pre-evacuating chamber  2  is evacuated via the gas evacuate unit  5 , and the internal space  3  is depressurized. 
     After the internal space  3  of the pre-evacuating chamber  2  is sufficiently depressurized, the operator makes the gate valve  17  in an open state and inserts the tip portion  10   a  of the sample introduction probe  10  into the ionization chamber  22  in the mass spectrometer  20  through the gate valve  17 . Then, electric power is supplied through the wiring  13  in the sample introduction probe  10  to heat the heater  12  (see  FIG. 3 ), so that the sample put in the sample cup  11  or coated on the heater  12  is vaporized and released from the tip portion  10   a . As described above,  FIG. 2  shows this state. 
     The sample introduced into the ionization chamber  22  is ionized in the ionization chamber  22  and, as described above, mass-analyzed by the mass spectrometer  20 . 
     After completion of the sample analysis, the sample introduction probe  10  is taken out from the mass spectrometer  20  and the direct sample introduction device  1 . However, since the sample introduction probe  10  is being heated to, for example, around 500° C. for vaporizing the sample, it is necessary to cool the sample introduction probe  10  to around room temperature before taking it out in order to ensure safety. 
     First Embodiment of Method for Cooling Sample Introduction Probe 
     Hereinafter, with reference to  FIG. 4 , a first embodiment of a method for taking out the sample introduction probe  10  and cooling the sample introduction probe  10  will be described. Note that the following description also describes a part of effects of the direct sample introduction device  1  of the above-described one embodiment. 
       FIG. 4  is a diagram showing a sequence of a method for cooling the sample introduction probe  10  in the first embodiment. 
     In step S 10  in the initial state, the tip portion  10   a  of the sample introduction probe  10  is inserted in the mass spectrometer  20 . At this stage, as described above, the valve  4   v  is in the closed state (Close), the valve  5   v  is in the open state (Open), and the valve  6   v  is in the closed state (Close). 
     In the subsequent step S 11 , the sample introduction probe  10  is retracted until the tip portion  10   a  enters the pre-evacuating chamber  2 . 
     Then, in step S 12 , the gate valve  17  is moved to be in the closed state (Close). 
     In the following step S 13 , the control unit  8  transmits the control signal Sa to the valve  4   v  to make the valve  4   v  in the open state (Open). By shifting the valve  4   v  to the open state (Open), the external gas (air) flows into the inside of the pre-evacuating chamber  2  from the second end  4   b  of the gas supply/evacuate unit  4  through the valve  4   v  and the first end  4   a  of the gas supply/evacuate unit  4 . 
     In step S 13 , the valve  5   v  is still in the open state (Open), and the evacuation of the pre-evacuating chamber  2  by the low pressure source  31  through the gas evacuate unit  5  is continuously performed. Therefore, the gas that has flowed into the pre-evacuating chamber  2  through the first end  4   a  of the gas supply/evacuate unit  4  passes around the side surface of the sample introduction probe  10  and flows along the X direction in the pre-evacuating chamber  2  towards the first end  5   a  of the gas evacuate unit  5 . Due to this gas flow, the sample introduction probe  10  can be cooled in a short time. 
     In the cooling method of the sample introduction probe  10  according to the first embodiment, the gas supply/evacuate unit  4  can be referred to as the first ventilation unit and the gas evacuate unit  5  can be referred to as the second ventilation unit. 
     In step S 14 , the control unit  8  determines as to whether or not the temperature T indicated in the temperature sensor  7  is lower than a predetermined temperature T 0  based on the signal St 1  indicative of the information about the temperature measured by the temperature sensor  7  installed in the pre-evacuating chamber  2 . The predetermined temperature T 0  is, for example, temperature at which there is no risk of burns even if the sample introduction probe  10  is touched, and is, for example, around 50° C. to 70° C. 
     If the determination in step S 14  is Yes, the process proceeds to step S 15 , and if it is No, the process returns to step S 13 . 
     In step S 15 , the control unit  8  stops the cooling of the sample introduction probe  10 . That is, the control unit  8  transmits the control signal Sb 1  to the valve  5   v  to shift it to the closed state (Close). The valve  6   v  is maintained in the closed state (Close). 
     The valve  4   v  may be either in the open state (Open) or in the closed state (Close). 
     In step S 15 , both the valve  5   v  and the valve  6   v  are in the closed state (Close) so as to avoid unnecessary evacuation from the gas evacuate unit  5  and unnecessary gas supply from the gas supply unit  6  to reduce an operating cost of the direct sample introduction device  1 . Therefore, if only the cooling of the sample introduction probe  10  is concerned, the valve  5   v  or the valve  6   v  may be set to be in the open state (Open) in step S 15 . 
     In subsequent step S 16 , the operator takes out the sample introduction probe  10  from the pre-evacuating chamber  2 . Since the sample introduction probe  10  has been sufficiently cooled through steps  13  to  15 , there is no risk of suffering burns even if the operator touches the sample introduction probe  10 . 
     In the above example, the valve  4   v , the valve  5   v , and the valve  6   v  are automatic opening/closing valves, and opening/closing operations of the valves are controlled by the control signals Sa to Sc transmitted from the control unit  8 , respectively. However, at least one of the valve  4   v , the valve  5   v , and the valve  6   v  may be a manual operation valve, and in this case, the opening/closing operations of the manual operation valve in the above steps are performed by the operator. 
     Alternatively, the gate valve  17  may also be an automatic opening/closing valve, and in this case, the opening/closing operation is controlled by the control signal Sd transmitted from the control unit  8 . 
     Further, the insertion and removal of the sample introduction probe  10  into and from the pre-evacuating chamber  2  may be performed by an automatic carrying/unloading device controlled by the control unit  8 . 
     Second Embodiment of Method for Cooling Sample Introduction Probe 
     Hereinafter, a cooling method of the sample introduction probe  10  of a second embodiment will be described with reference to  FIG. 5 . The following cooling method of the second embodiment is basically the same as the cooling method of the above-described first embodiment, and therefore the differences will be described below, and the description of common parts will be omitted as appropriate. 
     With respect to the cooling method of the sample introduction probe  10  of the second embodiment, it is different from the first embodiment in that step  13  of the above-described first embodiment is replaced with step  13   a  described below. Other steps of the second embodiment are common to the above-described first embodiment. 
     In step  13   a  of the second embodiment, the control unit  8  transmits the control signal Sa to the valve  4   v  to shift it to the open state (Open), transmits the control signal Sb 1  to the valve  5   v  to shift it to the closed state (Close), and transmits the control signal Sc to the valve  6   v  to shift it to the open state (Open). 
     By setting the valve  6   v  in the open state (open), the gas having pressure higher than the atmospheric pressure supplied from the gas supply source  32  flows into the inside of the pre-evacuating chamber  2  via the second end  6   b , the valve  6   v  and the first end  6   a  of the gas supply unit  6 . As a result, the pressure inside the pre-evacuating chamber  2  becomes higher than the atmospheric pressure, so that part of the gas inside the pre-evacuating chamber  2  flows out to the outside (atmosphere) of the pre-evacuating chamber  2  through the gas supply/evacuate unit  4 . 
     Therefore, the gas having flowed into the inside of the pre-evacuating chamber  2  through the first end  6   a  of the gas supply unit  6  passes around the side surface of the sample introduction probe  10  and flows along the X direction in the pre-evacuating chamber  2  toward the first end  4   a  of the gas supply/evacuate unit  4 . In the cooling method according to the second embodiment, the sample introduction probe  10  can be cooled in a short time by this gas flow. 
     In the cooling method of the sample introduction probe  10  according to the second embodiment, the gas supply unit  6  can be referred to as the first ventilation unit and the gas supply/evacuate unit  4  can be referred to as the second ventilation unit. 
     In the cooling method according to the above-described first embodiment and the cooling method according to the above-described second embodiment, in step  14 , the control unit  8  makes determination based on the signal St 1  indicative of the information about the temperature measured by the temperature sensor  7  installed in the pre-evacuating chamber  2 . 
     However, the signal St 2  indicative of the information about the temperature measured by the temperature sensor  14  provided in the sample introduction probe  10  described above may be input to the control unit  8  and the control unit  8  may perform the above determination based on the signal St 2 . 
     Alternatively, the control unit  8  may determine, in Step  14 , whether or not to proceed to Step  15  based on the cooling duration time in Step  13  in place of the temperature information. 
     Alternatively, in step  14 , the control unit  8  may determine whether or not to proceed to step  15  based on an instruction input by the operator. 
     In the above description of the method of mass spectrometry and the method for cooling the sample introduction probe  10 , the gas evacuate unit  5  is equipped with the valve  5   v , and the control unit  8  controls the opening/closing operation of the valve  5   v  by the signal Sb 1 . However, as described above, the direct sample introduction device  1  may have an alternative construction in which the gas evacuate unit  5  does not have the valve  5   v  or the valve  5   v  is always in the open state, and the control unit  8  controls the pressure (low pressure) of the low pressure source  31  by the control signal Sb 2 . 
     In this case, in the above-described mass spectrometry method and the method for cooling the sample introduction probe  10 , instead of switching the open/closed state of the valve  5   v  by the control signal Sb 1 , the control unit  8  transmits the control signal Sb 2  to the low pressure source (or depressurization unit)  31  to control the pressure inside the low pressure source  31  to atmospheric pressure or to a low pressure state. Alternatively, the operator may operate the low pressure source  31  to control the pressure inside the low pressure source  31 . 
     Although various embodiments and modifications have been described above, the present invention is not limited to those contents. Moreover, each of the embodiments may be applied individually or in combination. Other aspects that are conceivable within the scope of the technical concept of the present invention are also included within the scope of the present invention. 
     Aspects 
     It will be understood by those skilled in the art that the above-described plurality of exemplary embodiments or variations thereof are specific examples of the following aspects. 
     Item 1 
     A direct sample introduction device according to one aspect includes: a pre-evacuating chamber that has an internal space extending in a first direction through which a sample introduction probe extends in the first direction; a first ventilation unit that is allowed to be opened and closed, with a first end thereof being connected to the pre-evacuating chamber; and a second ventilation unit a first end of which is connected to the pre-evacuating chamber and a second end of which is connected to a low pressure source. As a result, a gas flow from the first ventilation unit to the second ventilation unit is formed in the pre-evacuating chamber  2  so that the sample introduction probe can be efficiently cooled by this gas flow. Thereby, it is possible to realize a direct sample introduction device that reduces a cooling time of the sample introduction probe. 
     Item 2 
     According to another aspect of the direct sample introduction device, in the direct sample introduction device according to Item 1, the first end of the first ventilation unit and the first end of the second ventilation unit are arranged at different positions to each other in the pre-evacuating chamber in the first direction. As a result, the gas flow formed in the pre-evacuating chamber can move along the side surface of the sample introduction probe, increasing the contact area between the gas flow and the sample introduction probe. It is thereby possible to cool the sample introduction probe more efficiently. 
     Item 3 
     The direct sample introduction device according to another aspect, in the direct sample introduction device according to Item 1 or Item 2, further includes a temperature sensor that measures information related to temperature of the sample introduction probe in the pre-evacuating chamber. As a result, it is possible to measure whether or not the sample introduction probe in the pre-evacuating chamber  2  has been cooled. 
     Item 4 
     The direct sample introduction device according to another aspect, in the direct sample introduction device according to any one of Items 1 to 3, further includes a control unit that controls an open/closed state of the first ventilation unit or at least one of an open/closed state of the second ventilation unit and pressure of the low pressure source. As a result, the control unit can automatically perform opening/closing operation of the valves necessary for cooling the sample introduction probe or control of the pressure in the low pressure source. 
     Item 5 
     The direct sample introduction device according to another aspect, in the direct sample introduction device according to any one of Items 1 to 3, further includes a third ventilation unit that is allowed to be opened and closed, with a first end thereof being connected to the pre-evacuating chamber and a second end thereof being connected to a gas supply source, wherein: the first end of the first ventilation unit and the first end of the third ventilation unit are arranged at different positions to each other in the pre-evacuating chamber in the first direction. As a result, flow of gas flowing from the third ventilation unit to the first ventilation unit can be formed in the pre-evacuating chamber, and the sample introduction probe can be cooled by this flow of gas. 
     Item 6 
     The direct sample introduction device according to another aspect, in the direct sample introduction device according to Item 5, further includes a control unit that controls an open/closed state of at least one of the first ventilation unit, the second ventilation unit and the third ventilation unit or pressure of the low pressure source. As a result, the control unit can automatically perform the opening/closing operation of the valves necessary for cooling the sample introduction probe and control of the pressure inside the low pressure source. 
     Item 7 
     According to another aspect of the direct sample introduction device, in the direct sample introduction device according to Item 4 or Item 6, the control unit controls the open/closed state or the pressure of the low pressure source based on information related to temperature of the sample introduction probe in the pre-evacuating chamber. As a result, the sample introduction probe can be cooled in the minimum necessary time, and the cooling time of the sample introduction probe can be further shortened. 
     Item 8 
     A method for cooling a sample introduction probe according to one aspect includes: arranging a sample introduction probe in a pre-evacuating chamber having an internal space extending in a first direction; supplying gas to the inside of the pre-evacuating chamber through a first ventilation unit a first end of which is connected to the pre-evacuating chamber; and evacuating gas of the inside of the pre-evacuating chamber through a second ventilation unit a first end of which is connected to the pre-evacuating chamber. As a result, the sample introduction probe can be efficiently cooled by the gas flow from the first ventilation unit to the second ventilation unit formed in the pre-evacuating chamber, and the cooling time of the sample introduction probe can be shortened. 
     Item 9 
     According to another aspect of the method for cooling a sample introduction probe, in the method for cooling a sample introduction probe according to Item 8, the first end of the first ventilation unit and the first end of the second ventilation unit are arranged at different positions to each other in the first direction; and the sample introduction probe is cooled by flowing gas from the first ventilation unit toward the second ventilation unit along the first direction in the pre-evacuating chamber. As a result, gas flow formed in the pre-evacuating chamber can flow along the side surface of the sample introduction probe, increasing the contact area between the gas flow and the sample introduction probe, and thereby it is possible to cool the sample introduction probe more efficiently. 
     Item 10 
     According to another aspect of the method for cooling a sample introduction probe, in the method for cooling a sample introduction probe according to Item 9, by depressurizing the second ventilation unit by connecting the second end of the second ventilation unit to a low pressure source, gas is caused to flow from the first ventilation unit toward the second ventilation unit. As a result, the gas flow formed in the pre-evacuating chamber can be strengthened by the low pressure supplied from the low pressure source so that the sample introduction probe can be cooled more efficiently. 
     Item 11 
     According to another aspect of the method for cooling a sample introduction probe, in the method for cooling a sample introduction probe according to Item 9, by pressurizing the first ventilation unit by connecting the second end of the first ventilation unit to a gas supply source, gas is caused to flow from the first ventilation unit toward the second ventilation unit. As a result, the high pressure gas supplied from the gas supply source can strengthen the gas flow formed in the pre-evacuating chamber so that the sample introduction probe can be cooled more efficiently. 
     Item 12 
     According to the method for cooling a sample introduction probe, in the method for cooling a sample introduction probe according to any one of Items 9 to 11, gas supply from the first ventilation unit to the inside of the pre-evacuating chamber and gas evacuation from the pre-evacuating chamber through the second ventilation unit are controlled based on information related to temperature of the sample introduction probe. As a result, the sample introduction probe can be cooled in the minimum necessary time, and the cooling time of the sample introduction probe can be further shortened. 
     REFERENCE SIGNS LIST 
       1  . . . Direct Sample Introduction Device 
       2  . . . Pre-evacuating Chamber 
       3  . . . Internal Space 
       4  . . . Gas Supply/evacuate Unit 
       5  . . . Gas Evacuate Unit 
       6  . . . Gas Supply Unit 
       4   v ,  5   v ,  6   v  . . . Valve 
       7  . . . Temperature Sensor 
       8  . . . Control Unit 
       9  . . . Seal Member 
       10  . . . Sample Introduction Probe 
       11  . . . Sample Cup 
       12  . . . Heater 
       14  . . . Temperature Sensor 
       17  . . . Gate Valve 
       20  . . . Mass Spectrometer 
       21  . . . Housing 
       22  . . . Ionization Chamber 
       28  . . . Vacuum Pump 
       31  . . . Low Pressure Source 
       32  . . . Gas Supply Source