U.S. patent number 3,842,266 [Application Number 05/350,259] was granted by the patent office on 1974-10-15 for atmospheric sampling probe for a mass spectrometer.
This patent grant is currently assigned to The United States of America as represented by the Secretary of the Air. Invention is credited to Robert W. Thomas.
United States Patent |
3,842,266 |
Thomas |
October 15, 1974 |
ATMOSPHERIC SAMPLING PROBE FOR A MASS SPECTROMETER
Abstract
An atmospheric sampling probe capable of generating a molecular
beam for mass spectrometer analyzation including a quartz gas inlet
orifice adjustable in any plane with a first vacuum stage; a quartz
skimmer orifice adjustable in one plane having a second vacuum
stage and a collimating orifice and ionizing chamber adapted to be
connected to a quadrupole mass spectrometer with a third vacuum
stage.
Inventors: |
Thomas; Robert W. (Rome,
NY) |
Assignee: |
The United States of America as
represented by the Secretary of the Air (Washington,
DC)
|
Family
ID: |
23375919 |
Appl.
No.: |
05/350,259 |
Filed: |
April 11, 1973 |
Current U.S.
Class: |
250/288;
250/289 |
Current CPC
Class: |
G01N
1/2273 (20130101); H01J 49/24 (20130101); G01N
33/497 (20130101) |
Current International
Class: |
H01J
49/02 (20060101); H01J 49/04 (20060101); G01N
1/22 (20060101); G01N 33/483 (20060101); G01N
33/497 (20060101); B01d 059/44 () |
Field of
Search: |
;250/283,288,289,428,430,489 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Lawrence; James W.
Assistant Examiner: Nelms; D. C.
Attorney, Agent or Firm: Herbert, Jr.; Harry A. Miller, Jr.;
Henry S.
Claims
Having thus described my invention, I submit the following claims
thereon:
1. A system for continuously sampling gases at atmospheric pressure
comprising: a sample probe means, including a first microorifice
mounted on a frame and movable in any plane, a second microorifice
positioned in line with said first microorifice, adjacent thereto
and movable in one plane and a third orifice positioned in line
with said first and second microorifices and spaced therefrom; a
first stage vacuum system for creating a vacuum; a first vacuum
chamber, connected between said first microorifice and said first
stage vacuum system; a second stage vacuum system for creating a
vacuum of greater magnitude than the first stage vacuum system; a
second vacuum chamber positioned within said first vacuum chamber
connecting the second stage vacuum system and said second
microorifice; a third stage vacuum system for creating a vacuum of
greater magnitude than said second stage vacuum system; a third
vacuum chamber, connected between said third stage vacuum system
and said third orifice, in juxtaposition to said second vacuum
chamber and a mass spectrometer detector means connected to the
said third vacuum chamber whereby gases entering the sampling probe
means pass therethrough forming an uncontaminated molecular beam
for detection in the mass spectrometer.
2. A system for sampling gases according to claim 1 wherein said
first and second orifices are formed of quartz.
3. A system for sampling gases according to claim 2 wherein said
first stage vacuum system includes a pump, means for removing
condensibles from said stage, and ballast means between the pump
and condensibles removing means to prevent overload to the pump
when the probe means is open to atmosphereic pressure.
4. A system for sampling gases according to claim 3 wherein said
second stage vacuum system includes a turbomolecular pump.
5. A system for sampling gases according to claim 4 wherein said
third stage include an ion pump.
Description
BACKGROUND OF THE INVENTION
This invention relates generally to gas sampling probes and in
particular to a probe adapted to sample gases at atmospheric
pressure by means of a molecular beam generator combined with a
mass spectrometer.
The evolution of solid state electronics has created formidable
problems relating to the manufacture of solid state devices. Cost
necessitates that there be a minimum of waste, reliability and
accuracy require more stringent controls in the assembly process,
supply and demand call for more speed in the manufacturing process.
Generally, in the production of an article these requirements
become ultimately mutually exclusive, in that an increase in one
requirement necessarily produces a decrease in an other.
In the field of solid state electronics manufacture, it has been
found that the analytical tools available lack sufficient
sensitivity to maintain direct and absolute control over a
semiconductor processing environment, such as the epitaxial growth
process. It is readily apparent that the only satisfactory
technique to substitute for the presently used cut and try
procedure, is a real-time monitoring of the epitaxial reaction,
which would drastically reduce the time required to achieve optimum
epitaxial growth.
The same real time monitoring system could serve equally as well as
a means for studying the mechanisms of chemical vapor
decomposition; for sampling localized laser evaporations; for
measuring exhaled human breath as a disease diagnostic tool and for
quantatively measuring condensible air pollutants.
SUMMARY OF THE INVENTION
In order to solve the problems of inefficiencies in the prior art,
and to provide a new and improved method for sampling gases at
atmospheric pressure, this invention offers a sampling probe which,
when coupled with a mass spectrometer allows a chemically reactive
or condensible species of gas to be transported from atmospheric
pressure to 10.sup.-.sup.8 torr without collision with other
molecules or walls of the probe. The unique design of this system
allows adjustment of a first orifice in any plane and a second or
skimmer orifice in one plane while the system is operating under
vacuum. Another unique feature is the utilization of materials such
as stainless steel and quartz which will allow a 400.degree.C
bakeout of the unit while operating.
The system consists of two quartz microorifices, the first orifice
is used to generate a pure molecular beam by free expansion of the
sample at atmospheric pressure into a vacuum of 10.sup.-.sup.5
torr. The beam of particles generated by the orifice is skimmed by
the second orifice to form a pure beam of the sampled gas. The
skimmer effectively removes gas molecules which have reacted with
the walls of the first orifice to form unwanted secondary
combinations of atoms. The beam, after entering the second orifice,
is traveling at Mach. 5. At a vacuum of 10.sup.-.sup.5 torr the
molecules in the beam have a mean free path of sufficient length to
be detected by the quadrapole mass filter before suffering a
collision with another molecule. The design therefore, insures the
purity of the sampling beam. The beam enters the third collimating
orifice before it is detected by the mass filter and electron
multiplier.
The system was designed completely from stainless steel and quartz
to allow bakeout at 400.degree. C. This provides an effective
control over contamination which might arise from the probe
assembly itself. A particularly difficult problem arose where both
orifices must be adjustable for beam alignment. The successful
fabrication of the microorifices and the design of the bakeable
stainless probe assembly are the major innovative achievements in
the design of the probe system.
It is therefore an object of the invention to provide a new and
improved sampling probe that is more accurate than those of the
prior art.
It is a further object of the invention to provide a new and
improved sampling probe that is capable of providing a molecular
beam input to a mass spectrometer.
It is still another object of the invention to provide a new and
improved sampling probe that allows adjustment of the orifices
while the system is in operation.
It is still a further object of the invention to provide a new and
improved sampling probe that will allow uneffected operation of the
unit at 400.degree.C.
It is another object of the invention to provide a new and improved
sampling probe that is simple in design and more reliable than
those known in the art.
It is another object of the invention to provide a new and improved
sampling probe which is economical to produce.
These and other advantages, features and objects of the invention
will become more apparent from the following description taken in
connection with the illustrated embodiment in the accompanying
drawing.
DESCRIPTION OF THE DRAWING
FIG. 1 is a schematic representation of a system utilizing the
invention.
FIG. 2 is a crossectional view of the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENT
Referring now to FIG. 1, a typical application of the invention is
shown with an appropriate vacuum system for atmospheric sampling.
The probe is shown at 10 in combination with a quadrapole mass
spectrometer 12. The probe is shown with a gas inlet orifice 14 and
a skimmer orifice 16. A vacuum differential is maintained between
the first stage chamber generally indicated as 18 (10.sup.-.sup.3
torr) and the second stage chamber generally shown as 20
(10.sup.-.sup.5 torr). The probe is connected to the mass
spectrometer through an adapter 22 which contains a collimating
orifice 23 and serves as an ionizing chamber for molecules entering
through the probe. The mass spectrometer is a third stage vacuum
chamber and is maintained at 10.sup.-.sup.8 torr.
The pumping system for the first stage utilizes a six inch
diffusion pump 24 to achieve 10.sup.-.sup.3 torr. Due to the large
throughput of the first stage, a high capacity pump is required to
protect the system from such extraneous matter, as for example
readily condensible material. Flow from the first or inlet orifice
is fed into two open liquid nitrogen dewars 26 (only one of which
is shown) where condensation built-up can be then observed during
system operation, as well as the level of the liquid nitrogen.
After operation, the dewars can be isolated by closing the gate
valve 30 and the butterfly valves 28. A stopcock 32 is provided for
purging the dewars with dry nitrogen via inlet valve 31 into a fume
exhause system. Hence, a large percentage of the condensibles are
not allowed to enter the diffusion pump 24. Similarly, a water
baffle 34 and liquid nitrogen trap 36 at the diffusion pump
decreases the amount of hydrocarbons backstreaming into the first
stage of the probe. A bakeable molecular sieve foreline trap 38 is
used to isolate mechanical pump oil from the diffusion pump and
protect the mechanical pump 40 from condensation contamination. In
the event of a power loss, a solenoid valve 42 isolates the
diffusion pump from the mechanical pump. A glass bell jar 44 is
utilized as ballast to prevent overload of the diffusion pump when
the orifice is first open.
The second stage requires a higher degree of cleanliness as well as
a moderately high pumping speed. A turbo-molecular pump 46
connected through valve 41, performs this function and has
negligable memory effect and prevents the back-streaming of the
mechanical pump oil.
The second stage is connected to the turbo pump by means of
stainless steel tubing butterfly valves 27, and bellows 47 to
insure low outgassing rates into a molecular flow region. Under
load, the turbomolecular pump has the capacity to maintain a
pressure of 10.sup.-.sup.5 torr, thus insuring a mean from path of
sufficient length to allow molecules in the beam to travel from the
skimmer to the third collimating orifice 23 without collision. This
is necessary to maintain beam integrity from skimmer to
detector.
The collimating orifice 23 immediately in front of the quadrupole
12 separates the second and third stage vacuum systems. The third
vacuum stage maintains an ultra-clean vacuum in the detector by
means of a high capacity ion pump 50 valved at 48. During operation
of the beam, this pump maintains an ultra-high vacuum of
10.sup.-.sup.8 torr. This section of the system is maintained at
100.degree.C during probe operation to prevent buildup
contamination of the walls of the quadrupole mass spectrometer.
Concerning FIG. 2, there is shown an enlarged crossectional view of
the sampling probe. The gas inlet orifice is shown at 51 and is
formed of quartz material which is bonded to pyrex glass 52 and the
stainless steel 53. The stainless steel portion of the orifice
structure by friction engages the first adjustment plate 54 in a
friction fit. The adjustment screws 55 move both the plate and
orifice structure in any plane to insure proper alignment of the
various apertures. The first orifice structure is welded to the
frame 56 by a metal bellows 57. Pumping ports 58 allow a vacuum to
be created in that region of the apparatus.
A skimmer orifice 60 is positioned internally of and adjacent to
the gas inlet orifice 51. The skimmer in a manner similar to the
gas inlet orifice is formed of fused quartz 62; pyrex glass 64 and
a stainless steel base 66. The base is mounted in the flange
portion 68 which is in turn mounted on an extender 70 protruding
from the second adjustment plate 72. The adjustment screws 74
relative to the frame members 56 provide orthogonal movement of the
skimmer orifice. Second orifice adjustment plate 72 is sealed by
gold O-Ring 73 to frame member 76 by head sealing screws 75. O-Ring
73 and gasket 69 isolate chamber 1 and chamber 2. Copper gasket 71
seals chamber 1 from atmosphere.
Pumping parts 78 connect through bellows 80 to a vacuum pumping
system to allow control of the pressure in the skimmer chamber.
An adapter 80 is connected to the frame 76 and provided with a
collimating aperature 82. A vacuum pumping port is provided at 84.
The adapter is connected to a quadrapole mass spectrometer at the
flange 86 and sealed at 88.
In operation, referring to FIG. 1, gas at atmospheric pressure
enters the orifice 14 where it is expanded and a quantity of gas is
removed from the system via the first stage vacuum system. The
remaining gas passes through the skimmer orifice 16 where high
velocity molecules travel along the axis of the chamber and enter
the collimating orifice 23 after which the molecules are ionized
and analyzed in the quadrupole mass spectrometer 12. The orifices
are aligned by monitoring the intensity of a nitrogen molecular
beam and adjusting the orifices until maximum intensity is reached
as indicated by the mass spectrometer.
* * * * *