U.S. patent number 3,797,318 [Application Number 05/278,338] was granted by the patent office on 1974-03-19 for method and apparatus for collecting and introducing a sample into an analytical instrument.
This patent grant is currently assigned to Bodenseewerk Perkin-Elmer Co., GmbH. Invention is credited to Ernst Palm.
United States Patent |
3,797,318 |
Palm |
March 19, 1974 |
METHOD AND APPARATUS FOR COLLECTING AND INTRODUCING A SAMPLE INTO
AN ANALYTICAL INSTRUMENT
Abstract
A sample is collected and introduced into an analytical
instrument by sorbing the sample with a sorption material which is
arranged as a surface of a sampling transportable body, positioning
the sampling body in an inlet chamber of the instrument, heating
the sampling body for causing desorption of the sample material,
and conveying the desorbed material in a carrier stream to an
analysis station of the instrument. A sampling collecting device
comprises a sampling body including a sorption segment thereof
having a surface arranged for sorption of sample material. The
sampling body further includes an elongated segment which is
coupled to the sorption segment, an annular seal extending about a
circumference of the elongated segment and a sealing plug and
handle located at an end of the body opposite to that of the
sorption surface segment. An apparatus for receiving the sampling
device and for introducing the sample therein includes an inlet
chamber which is positioned near a guide channel and through which
channel the sorption segment of the sampling body is introduced.
The elongated segment is guided in the channel and a chamber
closure member is provided which is actuated by the device when the
annular seal on the elongated segment establishes a leak-proof seal
between the guide channel and chamber. The chamber closure member
is actuated by the sampling body for causing a carrier gas stream
to flow over the sampling body and to convey a desorbed material to
the instrument.
Inventors: |
Palm; Ernst (Uberlingen,
Bodensee, DT) |
Assignee: |
Bodenseewerk Perkin-Elmer Co.,
GmbH (Uberlingen/Bodensee, DT)
|
Family
ID: |
5816329 |
Appl.
No.: |
05/278,338 |
Filed: |
August 7, 1972 |
Foreign Application Priority Data
|
|
|
|
|
Aug 10, 1971 [DT] |
|
|
2139992 |
|
Current U.S.
Class: |
73/863.21;
73/864.83 |
Current CPC
Class: |
G01N
30/08 (20130101); G01N 30/00 (20130101); G01N
1/2247 (20130101); G01N 1/2214 (20130101); G01N
1/405 (20130101) |
Current International
Class: |
G01N
1/00 (20060101); G01N 1/22 (20060101); G01N
30/00 (20060101); G01N 30/08 (20060101); G01N
1/40 (20060101); G01n 001/10 () |
Field of
Search: |
;73/422GC,23.1 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Swisher; S. Clement
Attorney, Agent or Firm: Levinson; Daniel R.
Claims
What is claimed is:
1. A method of collecting and injecting a sample material into an
analytical apparatus comprising the steps of:
sorbing the sample material on the surface of a sorption segment of
a generally transportable sampling device by positioning said
segment of said device in a space above a liquid sample which space
is occupied by the vaporized liquid sample;
introducing the sorption segment bearing the sorbed sample material
into an inlet chamber of an analytical apparatus;
causing the desorption of the material from the sorption segment of
the sampling device within said chamber; and,
conveying the desorbed sample material to an analysis station of
the apparatus.
2. A method of collecting and injecting a sample material into an
analytical apparatus comprising the steps of:
sorbing the sample material on the surface of a sorption segment of
a generally transportable sampling device by positioning said
sorption segment of said device in an environment for exposing said
segment to the sample material;
positioning said sorption segment within a gas-tight vessel after
sample sorption and then transporting the sample device to an
analytical apparatus;
introducing the sorption segment bearing the sorbed sample material
into an inlet chamber of an analytical apparatus;
causing the desorption of the material from the sorption segment of
the sampling device within said chamber; and,
conveying the desorbed sample material to an analysis station of
the apparatus.
3. The method of claim 1 wherein said sample material is desorbed
by heating said sorption segment of said sampling device.
4. A method of collecting and injecting a sample material into an
analytical apparatus comprising the steps of:
sorbing the sample material on the surface of the sorption segment
of a generally elongated transportable sampling device;
introducing the sorption segment bearing the sorbed sample material
into an inlet chamber of an analytical apparatus;
causing the desorption of the material from the sorption segment of
the sampling device within said chamber; and,
conveying the desorbed sample material to an analysis station of
the apparatus;
said apparatus including an inlet chamber and valving means for
controlling the flow of a carrier gas from a source thereof through
said inlet chamber to the analysis station of the apparatus, and
said sampling device actuating said valving means during insertion
of said sorption segment into said inlet chamber.
5. An improved arrangement for introducing a sample material into
an analytical apparatus comprising:
an inlet chamber;
means for supplying a carrier gas to said inlet chamber;
means for conveying said carrier gas from said inlet chamber to
said analysis station of said apparatus;
a sampling device including a sorption segment adapted for sorbing
a sample material on a surface thereof; and,
means for introducing said sorption segment into said inlet
chamber, said means including a valve for inhibiting the flow of
carrier gas through said latter means to atmosphere, said valve
arranged for actuation by said sampling device.
6. The apparatus of claim 5 including a carrier gas transfer flow
channel communicating between said inlet chamber and a first outlet
aperture of said chamber and said valve is arranged for diverting
the flow of carrier gas about said sorption segment when said
sorption segment is positioned within said chamber and through said
transfer flow channel to the apparatus.
7. The apparatus of claim 6 wherein said inlet chamber is formed as
a cylinder and said valving means comprises a piston which is
reciprocated between first and second positions by the introduction
and removal of said sorption segment from said chamber.
8. The apparatus of claim 7 wherein said piston is arranged for
enabling the flow of carrier gas through said chamber directly to
said instrument when said piston is located in said first position
and for inhibiting the direct flow of carrier gas to said
instrument and causing said carrier gas to flow over said sorption
segment and through said transfer channel when said piston is
located in said second position.
9. The apparatus of claim 8 wherein said piston inhibits the flow
of carrier gas through said transfer channel when said piston is
located in said first position.
10. The apparatus of claim 5 wherein said valving means comprises a
sluice chamber positioned adjacent said inlet chamber, a normally
seated sluice valve which seals said sluice chamber from an inlet
aperture thereto and which is arranged to be actuated by the
sampling device when said sampling device is introduced through
said inlet aperture, means forming a passage between said sluice
chamber and said inlet chamber for introducing said sorption
segment into said inlet chamber, means for directing the flow of
carrier gas over said sorption segment, and means for inhibiting
the leakage of carrier gas from said inlet chamber through said
sluice valve.
11. The apparatus of claim 5 wherein said sampling device includes
means positioned thereon for establishing the gas-tight seal for
inhibiting leakage of carrier gas from said inlet chamber.
12. The apparatus of claim 10 wherein said sampling device includes
means positioned thereon for establishing the gas-tight seal for
inhibiting leakage of carrier gas from said inlet chamber, and said
gas leakage inhibiting means comprises means for inhibiting leakage
of gas from said inlet chamber to said sluice chamber and for
inhibiting leakage of gas from said sluice chamber to said inlet
aperture.
13. The apparatus of claim 5 wherein said valving means includes an
annular valve seat which is positioned within said inlet chamber
and through which said sorption segment extends upon entering said
chamber, said valve comprises a body which is normally seated at
said valve seat for inhibiting flow of carrier gas from said
chamber to a probe inlet to said chamber, said valve is arranged
for displacement in the direction parallel to a longitudinal axis
of said sampling device and said valve includes recesses formed on
an outer surface thereof for providing a carrier gas flow passage
between the outer surface of the valve and said inlet chamber when
said valve is unseated.
14. The sampling arrangement of claim 5 wherein said sorption
segment comprises a plurality of concentrically arranged tubes
extending over a predetermined length and spaced apart radially,
each of said tubes providing a sorption surface for sorbing and
adsorbing a sample material.
15. The sampling arrangement of claim 5 wherein said sorption
segment comprises a body having a surface portion thereof elevated
with respect to other portions of the body.
16. The sampling arrangement of claim 15 wherein said sorption
segment is formed by a plurality of lands and grooves formed in
said sorption segment.
17. The sampling arrangement according to claim 5, in which:
said sampling device comprises, in addition to said sorption
segment, a relatively elongated support segment attached
thereto;
and means are positioned on said support segment for establishing a
gas-tight seal between said segment at a wall of a body within
which said segment is positioned.
18. A sampling device comprising:
a generally cylindrically shaped body having a relatively elongated
support segment thereof and a relatively shorter sorption segment
extending from said support segment;
said sorption segment having a surface thereof adapted for sorbing
a sample material and for desorbing said sample material when said
sorption segment is heated;
the surface of said sorption segment being coated with a film of a
high-boiling liquid.
19. A sampling device comprising:
a generally cylindrically shaped body having a relatively elongated
support segment thereof and a relatively shorter sorption segment
extending from said support segment;
said sorption segment having a surface thereof adapted for sorbing
a sample material and for desorbing said sample material when said
sorption segment is heated;
the surface of said sorption segment being coated with a film of a
high-boiling liquid.
Description
This invention relates to analytical instruments. The invention
relates more particularly to an improved method and apparatus for
collecting a sample and for injecting the sample into an analytical
instrument.
Various arrangements have been employed for collecting a sample for
analysis and for introducing the sample into an analytical
instrument. In one collecting and injection technique, the sample
is drawn into a syringe and is then discharged into a flowing
carrier gas stream of a chromatographic instrument. One form of
separating column employed with a gas chromatographic instrument
comprises a capillary tube of small diameter, but relatively large
length. In this type of column, a separating substance is coated on
an inner surface of the tube and defines the wall of a free-passage
channel. The surface of such a column may be coated with a liquid
acting as a separating substance. Although separating columns of
this type are relatively sensitive, they have a relatively small
sample capacity and are only suited for processing relatively small
sample volumes. Handling of sample quantities of this small size is
generally impractical and unreliable. Thus, when a liquid sample is
introduced into the inlet section of a gas chromatograph employing
a capillary column by means of a syringe, a stream splitting means
is provided for dividing the sample and carrier gas stream in a
defined ratio for providing that only a fraction of the mixture of
sample and carrier gas is supplied to the separating column. This
requirement for stream splitting results in an undesirable loss of
carrier gas. Furthermore, the collection of dosed quantities of a
sample by means of an injection syringe can be unreliable since
during the sample taking and dosing, errors can be introduced as a
result of manual handling. In addition, the sample composition can
be altered by sorption, by fractionated evaporation, or by the flow
division.
Another technique provides for collection of the sample by
adsorption. In gas chromatographic analyses, for example, sample
introduction columns have been employed which are packed with an
adsorbent granular material through which a relatively large dosed
volume of a gas under analysis is conveyed at relatively low
temperature. This column is coupled to a gas chromatograph and is
connected into the flow stream of the carrier gas. The sample
introduction column is then heated and the sample gas which was
adsorbed by the column material is then exhausted and is conveyed
by the carrier gas to a separating column of the gas chromatograph
where analysis takes place. Sample collection is provided with this
arrangement through the use of means which convey a sample gas
stream through the sample introduction column. This technique,
however, undesirably enlarges the cost, size and space requirements
of the apparatus.
Accordingly, it is an object of this invention to provide an
improved method and apparatus for collecting and introducing a
sample to an analytical instrument.
Another object of the invention is to provide a method of sample
collection and injection in which errors due to different manual
handling during sample taking and dosing and alterations in the
sample composition are subsequently reduced.
Another object of the invention is to provide a relatively
noncomplex means for collecting a sample by sorption.
A further object of the invention is to provide an improved means
for collecting relatively small dosed sample quantities.
In accordance with the general features of the method of this
invention, a sample is collected and introduced into an analytical
instrument by sorbing the sample in a sorption material which is
arranged as a surface of a sampling transportable body, positioning
the sampling body in an inlet chamber of the instrument and heating
the sampling body for causing desorption of the sample material.
The sampling body is transferred in a gas-tight vessel to the inlet
chamber of the analytical apparatus. In collecting gaseous samples,
the surface of the sampling body is exposed to a sample gas for a
predetermined period of time. For example, the sample gas may
comprise the atmosphere at a specific location at which the air is
to be examined for pollutants. In collecting liquid samples, the
sample comprises the vaporized portion which occupies the vapor
space above the liquid sample. An adsorption occurs in the sampling
body in accordance with the vapor pressures of the individual
components of the liquid above the liquid level. The method is
further advantageous in that liquid samples may also be collected
by wetting the sampling body in the liquid sample, and permitting
adhering surplus sample to drip off the body. Powder type samples
can be collected with this method by the use of ceramic dosing rods
whose surface adhesion is increased by the application thereto of
electric charge. In the collection of solid samples, it is
necessary that the solid exist in fine-powdered or particulate form
so that the particles will adhere uniformly to the surface of the
sampling body and that they evaporate in the heated inlet chamber
of the analytical apparatus without residue.
In accordance with another feature of the method of the invention,
a reference sample is collected with a like sampling body, but upon
which sorption of a sample material does not take place. In this
manner, interfering components can be sensed and accounted for in
the analysis.
The invention further permits the analytical apparatus to comprise
a gas chromatograph having a capillary column to which all of the
sample desorbed by the molded body in the inlet chamber is
conducted, without flow division. This possibility not only
involves simplification and a saving of carrier gas but also
provides for the dosing of extremely small samples without
difficulties of handling.
A sample collecting device in accordance with the invention
comprises a sampling body including a segment thereof having a
surface arranged for sorption of sample material. In accordance
with more particular features of the invention, the sampling body
further includes an elongated segment and an annular seal extending
about a circumference of this segment, a sealing plug and a handle
located at an end opposite to that of sorption surface segment. An
instrument for receiving the device and for introducing the sample
therein includes an inlet chamber which is positioned near a guide
channel and through which the sorption surface segment of the
sampling body is introduced. The elongated segment is guided in the
channel and a chamber closure member is provided which is actuated
by the device when the annular seal on the elongated segment
establishes a leakproof seal between the guide channel and chamber.
A sorption surface segment, in one embodiment comprises a molded
body of generally cylindrical shape. This body is provided with
raised portions for elevating the sorption surface above the
supporting body. A recess is provided between this cylindrically
shaped segment and the elongated segment which comprises a rod, for
example. The sorption segment alternatively comprises a plurality
of coaxially arranged tubes.
In a particular embodiment of an apparatus in accordance with the
invention, the inlet chamber includes a first inlet aperture
communicating with the guide channel and a second inlet aperture
through which a carrier gas flows to the chamber. A first outlet
aperture is provided which communicates with an outlet channel for
conveying carrier gas from the chamber to the analytical
instrument. A transfer channel is also provided which communicates
between the chamber and the outlet channel. The closure member
comprises a sliding piston valve which is reciprocally actuated in
an inlet chamber of generally cylindrical configuration. The
chamber is coaxially positioned with respect to the guide channel.
The piston is translated by the device from a first position near
the guide channel to a second opposite position. A flow path
through the transfer gas channel is established when the piston is
located at the second position while the flow path between the
first inlet and first outlet of the chamber is interrupted. When
the piston is translated to the first position, the flow path
through the transfer channel is interrupted while a flow path
between the first inlet and outlet apertures is established.
In operation, the piston valve is initially located at the first
position in the inlet chamber and the transfer gas inlet is
maintained in communication with the outlet channel. When the
sampling device is introduced, the piston is moved past the
transfer channel in the chamber so that the carrier gas continues
to flow between the first inlet and outlet apertures to the outlet
channel. When the sorption segment is positioned substantially
within the inlet chamber, the piston has then been translated past
the transfer chamber inlet and now blocks communication between
carrier gas inlet and outlet channels to the chamber. The carrier
gas then flows over the sorption segment from the first aperture to
the transfer channel inlet and through the latter towards the
outlet channel. A desorbed sample from the sorption segment is
picked up, is carried along by the carrier gas, and is transferred
into the outlet channel.
The sampling device includes a coupling means which, upon
introduction into the guide channel, automatically engages a
coupling means of the piston valve. The coupling means is
automatically disengageable upon withdrawal of the device from the
chamber, when the piston valve reaches the first end of the inlet
chamber. With this arrangement it is ensured that, upon withdrawal
of the device after sample introduction, the piston will be
translated from the second to the first end of the inlet chamber
and the initial valve conditions are reestablished.
Alternative to a piston valve arrangement, the apparatus includes a
sluice chamber and an inlet chamber. The sampling device extends
initially through the sluice chamber and then into the inlet
chamber. Two annular seals are positioned on the elongated segment
and are disposed on both sides of the sluice chamber, when the
sorption segment is positioned substantially in the inlet chamber.
In one embodiment, the inlet chamber is coaxial with the guide
channel; it conforms in general shape and dimensions to the
sorption segment of the sampling device; and it is only slightly
larger than the latter. A carrier gas inlet extends into an annular
space defined by a recess formed between the sorption segment and
elongated segment and an outlet channel is provided to the
instrument through the inlet chamber which is disposed opposite the
guide channel. A relatively small inlet chamber dead space is
thereof obtained. The carrier gas which flows from the annular
space flows uniformly across the total surface of the sorption
segment to the outlet channel. In this manner, a relatively rapid
and concentrated injection of the desorbed sample material into the
analytical apparatus is achieved.
In accordance with an alternative embodiment, the closure member
comprises a valve body which is guided in a cylindrical inlet
chamber. The inlet chamber is arranged coaxially with the guide
channel. The valve body coacts with a valve seat from which it is
unseated by the sorption segment. Grooves extending in an axial
direction on the body of the valve provide a carrier gas passage
between the valve body and inlet chamber walls. A carrier gas inlet
aperture is positioned downstream from the valve seat and an outlet
channel is provided at an opposite end of the inlet chamber.
In accordance with another feature of the invention, the sampling
device is transportable with a sealed vessel which receives the
sorption segment for transfer. This vessel is sealed by a plug
means positioned on the elongated segment and this sorption segment
is suspended in the vessel by the elongated segment. The plug means
additionally provides for sealing a vessel containing a liquid
sample and for supporting the sorption segment above the liquid
surface in the vapor space.
These and other objects and features of the invention will become
apparent with reference to the following specification and to the
drawings wherein:
FIG. 1 is a sectional view of one embodiment of an inlet of an
analytical apparatus for use with the method of the present
invention;
FIG. 2 is a side view of a sampling device for use with the inlet
of FIG. 1;
FIG. 3 is an enlarged view, partially in section of one embodiment
of a sorption segment of the sampling device;
FIG. 4 is a sectional view taken along lines IV--IV of FIG. 3;
FIG. 5 is a sectional view of an alternative of the inlet for
carrying out the method of the invention;
FIG. 6 is a side view of a sampling device for use with the inlet
of FIG. 5;
FIG. 7 is an enlarged view of an alternative embodiment of a
sorption segment of the sampling device of FIG. 6;
FIG. 8 is a sectional view of a further embodiment of an inlet for
carrying out the method according to the invention; and,
FIG. 9 is a side elevation view, partially in section, illustrating
a sampling device and transfer vessel.
Referring now to FIG. 1, an inlet section of an analytical
instrument as for example, a gas chromatograph, includes a heated
block 10 in which there is formed an inlet chamber 12. The chamber,
for example, has a generally cylindrical shape. A tubular
projection 14 is integrally formed with the block 10 and includes a
guide channel 16 for receiving an elongated segment or member 18 of
the sampling device 20 (FIG. 2). The guide channel 16 is positioned
coaxially with the inlet chamber 12. A sliding piston valve 22 is
positioned in the chamber 12 and is reciprocally translated between
a first right end of the chamber 12, as viewed in FIG. 1, and a
second left end. The chamber 12 includes a first outlet aperture
and channel 24 leading to a gas chromatographic separating column.
A first carrier gas inlet aperture and channel 26 is provided and
terminates in the chamber 12 near the left end of the chamber. This
aperture is positioned with regard to the aperture 24 so that when
the piston 22 is located in its left end position and interrupts
the flow to aperture 24, the carrier gas flows from channel 26
towards a carrier gas transfer channel 28 which is formed in the
block 10 and which communicates with the outlet channel.
The sampling device 20 includes a sorption segment or member 30
which comprises a molded body having the shape of a stud as
illustrated in the embodiment of FIG. 2. This molded body has a
surface adapted for sorption of a sample material. The materials
from which a sorption surface of the molded body is formed is
dependent on the type of analysis sample being handled. The
sorption surface of the molded body is formed, for example, of
metal, of glass, of quartz or of a ceramic material. The surface of
the sorption segment of the molded body may be coated with a film
of high-boiling liquid. Furthermore, the surface of the sorption
zone of the molded body may be coated with an oxide layer adapted
for sorption. This surface capable of sorption has the length a as
illustrated in FIG. 2. In order to increase the effective sorption
surface area of the body, the sorption segment may be arranged as a
plurality of tubular pieces or segments 42, 44, and 46 (FIG. 3)
which are mounted coaxially with respect to each other.
Additionally, in order to eliminate the possibility of interaction
between metallic surfaces and the sample, the inlet chamber 12 is
provided with a lining of ceramic material. A pair of annular seals
32, such as "O" rings are positioned on the segment 18 and engage
the walls of the guide channel 16. A sealing plug 34 as well as a
handle 36 are mounted on an opposite end of the segment 18.
In accordance with the method of the invention, the sorption
segment 30 and its surface adapted for sorption is exposed to a gas
sample. This is accomplished, for example, in a manner for
providing that the sampling device 20 is immersed in a vessel 70
(FIG. 9) containing a sample liquid. The plug 34 provides a seal
for this vessel and the segment 18 supports the sorption segment 30
above the surface of the sample liquid in the vapor space. The
sorption segment with a surface thereof adapted for sorption is
exposed to the sample gases for a predetermined period of time.
Sorption of sample gases above the liquid surface occurs in
accordance with the vapor pressures of the constituent gases. The
sampling device 20 is then introduced into the guide channel 16 of
the inlet section of an analytical instrument. A leading segment of
the device engages and translates the piston 22 toward the left
from a first to a second position. The device 30 includes a
coupling member 38 for engaging the piston 22. The piston 22, when
located at the first position, enables the flow of carrier gas from
the inlet 26 to the outlet channel 24 both directly through the
chamber and through the transfer channel 28 as illustrated in FIG.
1. The first position of the piston 22 can alternatively be
selected for inhibiting the flow of carrier gas through the channel
28 and causing the carrier gas to flow directly through the chamber
to the outlet aperture 24. When the molded body 30 has been
advanced into the inlet chamber 12 by a distance for providing that
its sorption surface is positioned completely within the inlet
chamber 12, i.e., by the distance a (FIG. 1), then the piston 22,
as is shown in dotted lines, will inhibit the flow of the carrier
directly from the inlet 26 to the outlet channel 24. The carrier
gas then flows over the molded body 30 to the transfer channel 28
and through this channel into the outlet channel 24. Heating of the
inlet chamber causes a desorption of the sample substance from the
molded body 30. The substance is then transferred by the carrier
gas stream into the gas chromatographic separating column.
The piston 22 includes a coupling member in the form of a U-shaped
expansion spring 40 which is automatically engaged by the coupling
member 38 upon advancement of the sampling device 20 in the guide
channel 16. As the sampling device 20 is withdrawn from the guide
channel 16, it translates the engaged piston 22 to the first
position at which the piston abuts the right end of the inlet
chamber 12. The coupling means 38 and 40 are arranged for
disengagement by exerting a pulling force on the knob 36. The
initial condition of the piston 22, prior to introduction of the
sampling device 20, is then restored.
FIG. 5 illustrates an alternative embodiment of the inlet section
of an analytical instrument. Those components of FIG. 5 which
perform functions similar to components of FIG. 1 bear the same
reference numerals. In the embodiment of FIG. 5 a sluice chamber 48
is provided adjacent the guide channel 16. A pivotally mounted
sluice valve 50 is provided. In an unactuated position, this valve
seals the guide channel 16 from the sluice chamber 48 and from the
inlet chamber 12. The valve is rotatable in a clockwise direction
when actuated. An annular groove 52 is formed on the sampling
device between sorption segment 30 and elongated segment 18. Upon
introduction of the sampling device 20 into the guide channel 16,
the molded body 30 forces the sluice valve 50 in a clockwise
unseated position. When the molded body 30 is disposed completely
within the inlet chamber 12, the annular seals 32 are located on
both sides of the sluice chamber thereby sealing the sluice chamber
against leakage to the channel 16 and sealing the inlet chamber 12,
against leakage into the sluice chamber 48. Carrier gas is
introduced through gas inlets 54 and 55 into the annular space
provided by the annular groove 52. The inlet chamber 12 has a size
and shape which is adapted for receiving the molded body 30. More
particularly, it has a size only slightly larger than this body.
When the molded body 30 is positioned in the inlet chamber 12,
carrier gas flows through the inlets 54 and 55 into the annular
space defined by the annular groove 52 and along the surface of the
molded body 30 to the outlet channel 24. With this construction, a
particularly small dead volume in the inlet chamber 12 is obtained
so that the sample material is supplied rapidly and in concentrated
form to the separating column when the molded body 30 enters the
inlet chamber 12 and is heated. The inlet chamber 12 is
advantageously provided with a lining 56 of glass, quartz or
ceramic material.
An alternative embodiment of the inlet system is illustrated in
FIG. 8. Those components of FIG. 8 which perform functions similar
to components of FIGS. 1 and 5 bear the same reference numerals.
The inlet chamber 12 of FIG. 8 includes a valve seat 60 and a valve
body 62 which is guided for movement in an axial direction in the
inlet chamber 12. The valve body 62 includes grooves 64 extending
in a generally axial direction which permit a carrier gas flow
between the valve body 62 and the inlet chamber walls towards the
outlet channel 24. The carrier gas enters the inlet chamber 12
through a carrier gas inlet 66 which terminates near the valve seat
60. In order to maintain the projection 14 and the guide channel 16
relatively cool when heating the block 10, cooling ribs 68 are
provided on the projection 14.
FIG. 9 illustrates the mounting of the sampling device 20 in the
cylindrical transfer vessel 70. The plug 34 tightly seals the
transfer vessel 70 and the elongated segment 18 supports and
suspends the sorption segment 30 in the transfer vessel 70.
FIG. 7 illustrates a further embodiment of the sorption segment 30.
In order to raise the surface of the segment 30, the molded body
is, as illustrated in FIG. 7, provided with lands and valleys, or,
for example, a threaded groove 58 on its surface. Alternatively,
laterally spaced annular grooves or axial grooves are provided.
The described method and device according to the invention offer
various advantages. The sampling device 20 is relatively
insensitive to rough handling, in contrast, for example, to
sampling devices of the microliter syringe type. The dosed volume
and analytical result are substantially independent of individual
differences in handling which are common problems in syringe dosing
by different persons and which leads both to different total sample
volumes and to different analytical results. Reading errors are
avoided by the sample collection technique. In an arrangement
according to this invention, the chemical interaction of the sample
with metal such as it might occur when using microliter syringes,
can be avoided through the use of both a ceramic inlet chamber, or
an inlet chamber having a ceramic lining, and a ceramic sorption
segment 30. In addition, it is possible to conveniently and
accurately dose relatively small sample volumes. Therefore,
capillary columns can be used in gas chromatographs without the
need for flow division. This results in a considerable saving in
carrier gas and eliminates other sources of error. The relatively
small dead volume in the inlet section is of particular advantage.
By the selection of particular material for the surface of the
sorption segment, selective sample collection can be achieved In
many instances, an enrichment of traces without the use of any
auxiliary equipment is thus provided. Gas samples, particularly air
samples can be taken on site without the need for auxiliary
equipment such as pumps, etc. Therefore, sampling errors and
variations are precluded.
While there have been described herein particular embodiments of
the present invention, it will be apparent that various
modifications can be made by those skilled in the art without
departing from the spirit of the invention and the scope of the
appended claims.
* * * * *