U.S. patent number 3,633,027 [Application Number 05/023,715] was granted by the patent office on 1972-01-04 for mass spectrometer connected to a gap chromatograph through a valved molecule separator.
This patent grant is currently assigned to LKB-Produkter AB. Invention is credited to Erik Ragnar Ryhage.
United States Patent |
3,633,027 |
Ryhage |
January 4, 1972 |
MASS SPECTROMETER CONNECTED TO A GAP CHROMATOGRAPH THROUGH A VALVED
MOLECULE SEPARATOR
Abstract
An instrument for analyzing organic chemical compounds is
provided. The instrument comprises a gas chromatograph which via a
molecule separator is connected to the ion source of a mass
spectrometer. The separator consists of a number of series
connected evacuating stages, each stage being connected to a vacuum
pump. Each stage is provided with an input jet nozzle and a coaxial
output nozzle, a slide being insertable between these nozzles in
the first stage so as to make it possible to switch off the flow
through the separator.
Inventors: |
Ryhage; Erik Ragnar (Stockholm,
SW) |
Assignee: |
LKB-Produkter AB (Bromma,
SW)
|
Family
ID: |
20266851 |
Appl.
No.: |
05/023,715 |
Filed: |
March 30, 1970 |
Foreign Application Priority Data
|
|
|
|
|
Apr 21, 1969 [SW] |
|
|
5621/69 |
|
Current U.S.
Class: |
250/288 |
Current CPC
Class: |
G01N
30/7293 (20130101); H01J 49/0422 (20130101) |
Current International
Class: |
H01J
49/02 (20060101); G01N 30/00 (20060101); H01J
49/04 (20060101); G01N 30/72 (20060101); H01j
039/34 (); B01d 059/44 () |
Field of
Search: |
;250/41.9S,41.9G |
References Cited
[Referenced By]
U.S. Patent Documents
Foreign Patent Documents
Primary Examiner: Lawrence; James W.
Assistant Examiner: Church; C. E.
Claims
1. An instrument for analyzing organic-chemical compounds, the
instrument comprising a gas chromatograph, a molecule separator and
a mass spectrometer having a housing, the molecule separator being
connected between the output of the gas chromatograph and the input
of the ion source of the mass spectrometer, the molecule separator
including at least one separating stage consisting of an evacuation
chamber connected to a vacuum pump, a jet input nozzle from which
molecules in gas phase are supplied from the gas chromatograph and
an output nozzle coaxial with the jet nozzle, characterized in that
the molecule separator comprises a slide element, and means
mounting said slide element for movement in a direction transverse
to the axis of said input and output nozzles so as to be inserted
between the jet nozzle and the output nozzle to close the space
therebetween and cut off the gas flow through the molecule
separator and
2. An instrument according to claim 1, characterized in that the
surface of said slide element is shaped to seal the output nozzle
and to provide space for leakage at the jet input nozzle when the
slide element is in an
3. An instrument according to claim 1, characterized in, that the
number of stages is at least two, the last stage being combined
with the housing of the ion source.
Description
The present invention relates to an instrument for analyzing
organic chemical compounds, the instrument comprising a gas
chromatograph, a molecule separator and a mass spectrometer, the
molecule separator being connected between the output of the gas
chromatograph and the input of the ion source of the mass
spectrometer, the separator including at least one separating stage
consisting of an evacuation chamber connected to a vacuum pump, a
jet input nozzle via which molecules in gas phase are supplied from
the gas chromatograph and an output nozzle coaxial with the jet
nozzle.
In a combination instrument as defined above, so called molecule
separators are used for separating a carrier gas, usually helium,
from the specimen to be analyzed and for reducing the pressure in
the ion source of the mass spectrometer.
Different kinds of separators are used for this purpose, the so
called Becker-Ryhage-Separator however having several advantages in
comparison to the others. In this separator the enrichment is high,
the loss of specimen is small, the dead volume is small and the
memory effect is negligible. The Becker-Ryhage-Separator is
generally made in two stages. In the first stage the pressure is
reduced to 0.001 mm. Hg by an oil diffusion pump. In this way
approximately 99 percent of the carrier gas is evacuated while at
least 75 percent of the specimen remains. The pressure will then be
further reduced at the ion source of the mass spectrometer.
The above described separator is described in detail by the
inventor for instance in Analytical Chemistry vol. 36., No 4, Apr.
1964 pages 759-764. The principle of the separator is described in
the German Pat. No. 105 2,955 (See FIG. 1).
By using a conventional molecule separator several problems do
however arise. For changing the gas chromatograph column the
following steps have to be performed: (a) The connection between
the separator and the ion source of the mass spectrometer has to be
switched off or otherwise the current to the filament of the ion
source has to be switched off. It is however not desirable to
change the ionization conditions and thus a tap is generally
mounted between the separator and the ion source; (b) The oil
diffusion pump connected to the second separator stage is switched
off; (c) The mechanical vacuum pump connected to the first
separator stage is switched off; (d) The pressure in the separator
is raised by means of a blow cock connected between the mechanical
vacuum pump and the first separator stage; (e) Then the gas
chromatograph column is exchanged; (f) The system is evacuated by
connecting first the mechanical vacuum pump and then the oil
diffusion pump; (g) When the pressure has been reduced sufficiently
the tap of the ion source is opened. The above described procedure
is very lengthy, especially the evacuation. The insertion of a tap
between the separator and the ion source does further imply and
increase of the dead volume of the system which in turn affects the
separation obtained in the gas chromatograph. Furthermore the
separator and the connection to the ion source has to be heated and
it is of course desirable that the heated part is as small as
possible. Although the pressure after the separator is very low and
the velocity of the molecules is high a certain risk for
degradation in the tap and the connecting pipes arises because of
thermic and catalytic effects.
The above discussed drawbacks can be avoided by using an instrument
designed in accordance with the present invention, the essential
features of which are defined in the attached claims.
The invention will now be described in detail with reference to the
enclosed drawings in which:
FIG. 1 shows a two-stage separator according to the invention
provided with a switching-off arrangement in the form of a
slide;
FIG. 2 shows another embodiment of a two-stage separator according
to the invention in which the second separator stage has been
combined with the ion source.
In FIG. 1 reference 1 denotes a mounting flange for connection of a
gas chromatograph G, reference 2 denotes the first separator stage,
reference 3 denotes the second separator stage and reference 4
denotes the mounting flange of the ion source of the mass
spectrometer M. The input jet nozzle of the separator stages are
denoted 5a and 5b respectively and the output nozzles are denoted
6a and 6b respectively. Reference 7 denotes the slide by means of
which the gas flow can be switched off or at least be prevented
from passing into the second separator stage. Reference 8 denotes a
bellows which controls the position of the slide 7 and reference 9
denotes a knob for moving the bellows. The slide can be set into
two positions 11a and 11b, which positions are adjusted by means of
a screw 10. References 12 and 13 denote connections leading to a
mechanical vacuum pump and an oil diffusion pump respectively.
When the column of the gas chromatograph should be changed or if it
for some other reason is desirable to switch off the gas flow
through the separator, the slide 7 is inserted between the nozzles
5a and 6a. The distance between these nozzles is about 0.1 mm. and
thus the slide should have this dimension. The nozzle 5a does also
have a diameter of about 0.1 mm. The slide does not necessarily
have to seal this nozzle completely but a small leakage into the
separator housing can be permitted. It has turned out in practice
that in spite of this leakage the mechanical vacuum pump provides a
pressure which is sufficiently low for making the oil diffusion
pump work and for not making it necessary to have the ion source
switched off. Even if the pressure in the first separator stage 2
is as much as 1 mm. Hg, instead of the normal value 0.1 mm. Hg, the
system works satisfactory. Thus the pumps do not have to be
switched off.
As it is sometimes desirable to have a certain leakage into the
separator without having any gas flow into the ion source, the
slide 7 can be shaped so as to seal only the output nozzle 6a. In
this case the slide 7 could be provided with a slot in the surface
turned to the input nozzle 5a. This shaping of the slide is
suitable when a gas flow through only the gas chromatograph column
is wanted, for instance after mounting the column.
In the arrangement according to the present invention the dead
volume after the separator is reduced considerably. In the
previously used systems the volume of the tap between the separator
and the ion source is approximately 0.5 ml. and the connecting
pipes have a volume of approximately the same size. If these values
are compared with the area of the channel through the separator
(0.8 mm..sup.2) and the area of the nozzle (0.008 mm..sup.2) the
significance of the reduced dead volume is understood. Of course a
reduced volume after the separator means less than a reduced volume
before the separator, the pressure conditions being completely
different, but a reduced volume is still desirable. The insertion
of some sort of tap before the separator is not suitable as this
will increase the dead volume. Each person skilled within this
field is aware of the drawbacks of such an arrangement, especially
when capillary columns are used in the gas chromatograph.
A tap mounted before the separator further makes it more difficult
to remove the flange for cleaning the nozzle 5a. The other nozzles
do not have to be cleaned so often as the pressure and thus the
fouling is less at these nozzles.
In the above described embodiment of the invention the switching
off means consist of a slide. The slide can of course be shaped in
different ways and the insertion of the slide between the nozzles
of the separator can be arranged in different ways. If only a
sealing of the output nozzle is wanted it might thus be suitable to
make the top of the output nozzle radially movable.
In FIG. 2 a new way of connecting the separator to a mass
spectrometer is shown. This connection is made possible by using
the present invention. In this figure the references denote the
same members as in FIG. 1, the difference being that reference 15
denotes the connection leading to the ion source and references 14a
and 14b denote the nozzle of the second separator stage. Reference
16 denotes the connection of the high vacuum system which in this
case is the same for the second separator stage and the ion source
housing. In this embodiment the dead volume is considerably
decreased in comparison with the embodiment of FIG. 1. On the other
hand the flexibility will be somewhat reduced.
* * * * *