CA1223461A - Method and apparatus for the introduction of a vapourized sample into an analytical test apparatus - Google Patents
Method and apparatus for the introduction of a vapourized sample into an analytical test apparatusInfo
- Publication number
- CA1223461A CA1223461A CA000473884A CA473884A CA1223461A CA 1223461 A CA1223461 A CA 1223461A CA 000473884 A CA000473884 A CA 000473884A CA 473884 A CA473884 A CA 473884A CA 1223461 A CA1223461 A CA 1223461A
- Authority
- CA
- Canada
- Prior art keywords
- sample
- needle
- vapourized
- tube
- sample tube
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
- G01N30/18—Injection using a septum or microsyringe
Abstract
TITLE
A METHOD AND APPARATUS FOR THE INTRODUCTION
OF A VAPOURIZED SAMPLE
INTO AN ANALYTICAL TEST APPARATUS
INVENTORS
André H. Lawrence Lorne Elias ABSTRACT OF DISCLOSURE
This invention is concerned with an apparatus and a method for the introduction of vapourized samples into an apparatus for the analysis of such samples, such as a gas chromatograph, and especially a capillary gas chromatograph and ion mobility spectrometer. A
sample is vapourized or desorbed from a sample tube by heating the sample tube and then transferred by a carrier gas to the analytical apparatus by being withdrawn from the sample tube along and condensed on the inner surface of a heat conductive metal walled needle of a hypodermic syringe from which it is then vapourized and introduced into the analytical apparatus.
Suitable samples may also be introduced into an ion mobility spectrometer directly by placing a sample-charged sample tube into a sample-introduction port thereto.
A METHOD AND APPARATUS FOR THE INTRODUCTION
OF A VAPOURIZED SAMPLE
INTO AN ANALYTICAL TEST APPARATUS
INVENTORS
André H. Lawrence Lorne Elias ABSTRACT OF DISCLOSURE
This invention is concerned with an apparatus and a method for the introduction of vapourized samples into an apparatus for the analysis of such samples, such as a gas chromatograph, and especially a capillary gas chromatograph and ion mobility spectrometer. A
sample is vapourized or desorbed from a sample tube by heating the sample tube and then transferred by a carrier gas to the analytical apparatus by being withdrawn from the sample tube along and condensed on the inner surface of a heat conductive metal walled needle of a hypodermic syringe from which it is then vapourized and introduced into the analytical apparatus.
Suitable samples may also be introduced into an ion mobility spectrometer directly by placing a sample-charged sample tube into a sample-introduction port thereto.
Description
~.~2346~
1 BACKGROUND OF TI~E INVENTION
Methods for introducing samples into an apparatus for the analysis of vapours and vapour-entrained materials, such as gas chromatographs and ion mobility spectrometers, have hitherto been (1) mainly limited to handling liquids, for example, a syringe carrying a liquid sample is introduced into many conventional gas chromatographs through a rubber septum, or (2) of the type that allows vapour-entrained samples to be introduced from sample tubes. However, the sample introduction means used in these methods must be designed specifically for the particular purpose of analysis. An example of this type of means is the Perkin Elmer Model ATD 50 [TM] system, two-stage adsorber type gas chromatograph in which a sample is adsorbed onto an adsorbent material such as para-polyphenylene-oxide in the form of TENAX
[TM] contained in a sample tube and then the sample is transferred to an adsorbent material in a second sample tube of different (usually smaller) dimensions from those of the first sample tube. A particular variant of this procedure is described by F. Raschdorf in Chimia 32, 1978. Raschdorf employs a needle method for the introduction of compounds into gas chromatographs.
A 100 ml gas syringe is described by Raschdorf and ~ ~ .
12X34~1 l is employed to draw a known volume of sample gas through a thiek needle containing an adsorbent such as TENAX.
This needle, which functions as a sample tube, is dis-conneeted from the barrel of the syringe and then eonnected to a supply o'c carrier gas before being introduced into the gas chromatograph. ~hile the needle of Raschdorf is useful there are drawbacks in that (a) it requires a large barrellecl syringe and adsorbent loaded needle as opposed to the more convenient and conventional sample tubes, (b) a carrier gas entrained sample flow rate of 14 cc/min which is required to transfer the sample from the syringe to the gas ehromatograph and this is an order of magnitude too great to be handled by eapillary chromatography eolumns of the type preferred lS for mieroanalysis, and (e) hardware modifieations may be neeessary in the sample introduetion port of the ehromatograph to aeeommodate the large needle that is used.
There is a need for a method and an apparatus for the introduetion of a vapourized sample into an analytieal test apparatus whieh uses sample tubes of the eonventional type, with the attendant advantages of ehoiee of ac1sorption material that they allow, but whieh is also eapable of matehing the ideal flow for proper desorption through eonventional sample tubes ~. ", 1~23~61 1 of about 30 cc/min., with the optimum flow for capillary gas chromatograph operati.ons of 1-5 cc/min.
SUMMARY OF T~IE INVENTION:
According to the present invention there is provided an apparatus for the introduction of a vapour-ized sample into an analytical test apparatus, compris-ing:
- a sample tube for the collection of a condensed sample and from which, when heated, the sample may be vapourized and eluted - means at an upstream end of the sample tube for passing a carrier gas to the sample tube interior;
- a hypodermic syringe having a heat dissipating metal walled, hollow needle for the condensation of the vapourized sample, from the sample tube on an inner surface of the needle, and transfer of the condensed sample in a vapourized, concentrated form therefrom to the analytical test apparatus;
- a valve attached to the hypodermic syringe, at a position adjacent the needle, for venting carrier gas therefrom from which the vapourized sample has been condensed in the needle; and - a plug closing the downstream end of the sample tube and, in operation, sealing said needle in a perforation for the transfer of an eluted sample from the sample tube to the hypodermic syringe.
:122~4~;1 l The apparatus may include heating means for heating the sample tube.
The sample tube may contain sample adsorbent material, such as, for example, a polymeric sample-adsorbent material based on the monomer 2,6-diphenyl-p-phenylene oxide e.g. TENAX-GC [TM] or material such as platinum gauze, for the entrapment of sample vapours.
The syringe may comprise a barrel and a plunger.
The valve for ver,ting the hypodermic syringe may be in the side of the barrel thereof and comprise a pipe containing a closable valve.
The apparatus according to the present invention may be used in combination with cooling means for cooling at least a part of the metal walled, hollow needle.
The apparatus according to the present invention may also be used in combination with a carousel for introduc-ing and removing successive sample tubes for the with-drawal of a sample therefrom into the hollow needle with automatic means for the introduction of the hollow metallic needle into the analytical test apparatus.
Further according to the present invention there is provided a method for the introduction of a vapourized sample into an analytical test apparatus, comprising:
,~:
12~
1 a) collectill~ said sample in a condensed form in a sample tube;
b) closing a downstream end of the sample tube with a plug;
c) inserting a heat dissipati.ng metal walled needle of a hypoclermic syringe through the plug;
d) heating said sample in the tube to render the sample in vapour form;
e) feedi.ng a carrier gas through the tube to entrain the vapourized same and transport it into the needl.e;
f) condensing the sample from the carrier gas onto the inner surface of the needle;
g) venting carrier gas from which the sample has been condensed, from the hypodermic syringe at a position adjacent the needle, whereby h) said needle may be introduced into a heated sample intake port of the analytical apparatus, for injection of the sample in a vapourized, concentrated form therein for analysis.
The method according to the present invention may be used with a capillary gas chromatograph or an ion mobility spectrometer.
346~
1 BRIEF DESCRIPTION OF THE DRAWING:
In the accompanying drawing which illustrates, by way of example, an embodiment of the present inven-tion, Figure 1 is a partly sectional side view of an apparatus for the introduction of a sample into an analytical test apparatus.
DETAILED DESCRIPTION OF THE INVENTION:
In Figure 1 there is shown a sample tube 1 containing platinum gauze 3, which may be placed in heater 2, and connected at an upstream end via a TEFLON
[TM] type polytetrafluorethylene pressure plate 4 to a source of carrier gas 5. At the downstream end of sample tube 1 there is shown a TEFLON plug 6 perforated in sealing engagement by a heat dissipating metal walled, hollow needle 7, said needle 7 forming part of a hypo-dermic syringe 8 with barrel 9 and plunger 10. A one-way valve 11, connected to a vent 12, is set in the side of barrel 9.
This embodiment is preferably operated as follows.
Sample tube 1 is exposed to a source (not shown) of vapourized sample which is deposited in a condensed form upon the platinum gauze 3. The sample tube 1 is then connected to a source of carrier gas (not shown) by means of a pipe 5 and a TEFLON pressure plate 4.
A TEFLON plug 6 is then inserted in the other end of 12:23~
1 sample tube 1 in a vapour tight manner, the needle 7 is inserted in the plug 6 as illustrated in Figure 1, and then the one way valve 11 is opened. The heater
1 BACKGROUND OF TI~E INVENTION
Methods for introducing samples into an apparatus for the analysis of vapours and vapour-entrained materials, such as gas chromatographs and ion mobility spectrometers, have hitherto been (1) mainly limited to handling liquids, for example, a syringe carrying a liquid sample is introduced into many conventional gas chromatographs through a rubber septum, or (2) of the type that allows vapour-entrained samples to be introduced from sample tubes. However, the sample introduction means used in these methods must be designed specifically for the particular purpose of analysis. An example of this type of means is the Perkin Elmer Model ATD 50 [TM] system, two-stage adsorber type gas chromatograph in which a sample is adsorbed onto an adsorbent material such as para-polyphenylene-oxide in the form of TENAX
[TM] contained in a sample tube and then the sample is transferred to an adsorbent material in a second sample tube of different (usually smaller) dimensions from those of the first sample tube. A particular variant of this procedure is described by F. Raschdorf in Chimia 32, 1978. Raschdorf employs a needle method for the introduction of compounds into gas chromatographs.
A 100 ml gas syringe is described by Raschdorf and ~ ~ .
12X34~1 l is employed to draw a known volume of sample gas through a thiek needle containing an adsorbent such as TENAX.
This needle, which functions as a sample tube, is dis-conneeted from the barrel of the syringe and then eonnected to a supply o'c carrier gas before being introduced into the gas chromatograph. ~hile the needle of Raschdorf is useful there are drawbacks in that (a) it requires a large barrellecl syringe and adsorbent loaded needle as opposed to the more convenient and conventional sample tubes, (b) a carrier gas entrained sample flow rate of 14 cc/min which is required to transfer the sample from the syringe to the gas ehromatograph and this is an order of magnitude too great to be handled by eapillary chromatography eolumns of the type preferred lS for mieroanalysis, and (e) hardware modifieations may be neeessary in the sample introduetion port of the ehromatograph to aeeommodate the large needle that is used.
There is a need for a method and an apparatus for the introduetion of a vapourized sample into an analytieal test apparatus whieh uses sample tubes of the eonventional type, with the attendant advantages of ehoiee of ac1sorption material that they allow, but whieh is also eapable of matehing the ideal flow for proper desorption through eonventional sample tubes ~. ", 1~23~61 1 of about 30 cc/min., with the optimum flow for capillary gas chromatograph operati.ons of 1-5 cc/min.
SUMMARY OF T~IE INVENTION:
According to the present invention there is provided an apparatus for the introduction of a vapour-ized sample into an analytical test apparatus, compris-ing:
- a sample tube for the collection of a condensed sample and from which, when heated, the sample may be vapourized and eluted - means at an upstream end of the sample tube for passing a carrier gas to the sample tube interior;
- a hypodermic syringe having a heat dissipating metal walled, hollow needle for the condensation of the vapourized sample, from the sample tube on an inner surface of the needle, and transfer of the condensed sample in a vapourized, concentrated form therefrom to the analytical test apparatus;
- a valve attached to the hypodermic syringe, at a position adjacent the needle, for venting carrier gas therefrom from which the vapourized sample has been condensed in the needle; and - a plug closing the downstream end of the sample tube and, in operation, sealing said needle in a perforation for the transfer of an eluted sample from the sample tube to the hypodermic syringe.
:122~4~;1 l The apparatus may include heating means for heating the sample tube.
The sample tube may contain sample adsorbent material, such as, for example, a polymeric sample-adsorbent material based on the monomer 2,6-diphenyl-p-phenylene oxide e.g. TENAX-GC [TM] or material such as platinum gauze, for the entrapment of sample vapours.
The syringe may comprise a barrel and a plunger.
The valve for ver,ting the hypodermic syringe may be in the side of the barrel thereof and comprise a pipe containing a closable valve.
The apparatus according to the present invention may be used in combination with cooling means for cooling at least a part of the metal walled, hollow needle.
The apparatus according to the present invention may also be used in combination with a carousel for introduc-ing and removing successive sample tubes for the with-drawal of a sample therefrom into the hollow needle with automatic means for the introduction of the hollow metallic needle into the analytical test apparatus.
Further according to the present invention there is provided a method for the introduction of a vapourized sample into an analytical test apparatus, comprising:
,~:
12~
1 a) collectill~ said sample in a condensed form in a sample tube;
b) closing a downstream end of the sample tube with a plug;
c) inserting a heat dissipati.ng metal walled needle of a hypoclermic syringe through the plug;
d) heating said sample in the tube to render the sample in vapour form;
e) feedi.ng a carrier gas through the tube to entrain the vapourized same and transport it into the needl.e;
f) condensing the sample from the carrier gas onto the inner surface of the needle;
g) venting carrier gas from which the sample has been condensed, from the hypodermic syringe at a position adjacent the needle, whereby h) said needle may be introduced into a heated sample intake port of the analytical apparatus, for injection of the sample in a vapourized, concentrated form therein for analysis.
The method according to the present invention may be used with a capillary gas chromatograph or an ion mobility spectrometer.
346~
1 BRIEF DESCRIPTION OF THE DRAWING:
In the accompanying drawing which illustrates, by way of example, an embodiment of the present inven-tion, Figure 1 is a partly sectional side view of an apparatus for the introduction of a sample into an analytical test apparatus.
DETAILED DESCRIPTION OF THE INVENTION:
In Figure 1 there is shown a sample tube 1 containing platinum gauze 3, which may be placed in heater 2, and connected at an upstream end via a TEFLON
[TM] type polytetrafluorethylene pressure plate 4 to a source of carrier gas 5. At the downstream end of sample tube 1 there is shown a TEFLON plug 6 perforated in sealing engagement by a heat dissipating metal walled, hollow needle 7, said needle 7 forming part of a hypo-dermic syringe 8 with barrel 9 and plunger 10. A one-way valve 11, connected to a vent 12, is set in the side of barrel 9.
This embodiment is preferably operated as follows.
Sample tube 1 is exposed to a source (not shown) of vapourized sample which is deposited in a condensed form upon the platinum gauze 3. The sample tube 1 is then connected to a source of carrier gas (not shown) by means of a pipe 5 and a TEFLON pressure plate 4.
A TEFLON plug 6 is then inserted in the other end of 12:23~
1 sample tube 1 in a vapour tight manner, the needle 7 is inserted in the plug 6 as illustrated in Figure 1, and then the one way valve 11 is opened. The heater
2, which may be an aluminum heating block, is then used to heat the samplc tube 1 and vapourize the sample.
A valve (not shown) controlling the supply of carrier gas to pipe 5 is opened so that the carrier gas and vapourized sample are carried into the needle 7, where the sample is condensed and collected on the inner surface of the needle, while the carrier gas is vented through the one-way valve 11 to the vent 12. With the one-way valve of the syringe 8 closed, the needle containing the condensed sample is withdrawn from plug 6 and introduced into a heated injector port of an analytical apparatus (not shown). The condensed sample in the needle 7 vapourizes rapidly on the introduction of needle 7 into the heated injector port of the analyt-ical apparatus. The plunger 10 is then depressed to drive the sample vapours from the needle 7 into the carrier gas stream of the analytical apparatus, typically flowing at a rate of 1-5 cc/min.
If desired, a carousel of the sample tubes may be used, each capped with a TEFLON or rubber plug 6, and provision made for a stream of carrier gas to transfer vapourized samples from successive tubes 1 to the needle 7 of the hypodermic syringe 8. The syringe 1~234~1.
1 8 may be acti a-ted by a servo--mechanism to inject success-ive samples into the heated injector port of the analyt-ical apparatus.
Desirable ~eatures of the present invention are (a) conventional sample tubes may be used; (b) laminar flow rate cluring ejection of the vapourized sample from the needle allows the apparatus to be used with capillary ~as chromatographs; (c) the needle may be significantly sma]ler than needles of the type employed in known apparatus; (d) the needle does not require an adsorbent packing which is used in known apparatus;
and (e) no modifications to the analytical apparatus (e.g. gas chromatograph, ion mobility spectrometer) are necessary.
Mixtures of chlorinated biphenyls have been extracted from an air stream into a sample tube of the type shown in Figure 1. The samples were then transferred to syringe needles and these used to transfer the samples into suitable analytical test apparatus such as a capillary gas chromatograph or ion mobility spectrometer, in the manner described with reference to Figure 1.
Using the apparatus of the type described with reference to Figure 1, very satisfactory chromatographic results have been obtained. The apparatus can yield excellent peak sharpness and reproducibility. Given below are some results for six compounds tested using the apparatus shown in Figure 1.
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l It should be noted that the carrier gas flow through the sample tube l, when transferring the sample from a sample tube l to the needle 7, was found to be of the order of 15-25 cc/min while the gas flow for conveying the vapourized sample from the needle 7 to the gas chromatograph was found to be of the order of l-1.5 cc/min. From this it will be seen that condensing the vapourized sample in the needle and exhausting carrier gas from the syringe has the effectof delivering a much higher concentration of the sample in the carrier gas that is delivered to the gas chromatograph. For low boiling point compounds such as 2-dimethylaniline (Example 2) the needle should preferably be cooled to below ambient temperatures to improve condensation of the condensed sample in the needle 7. The apparatus according to the present invention has proved particularly useful in the analysis of polychlorinated biphenyls.
.
A valve (not shown) controlling the supply of carrier gas to pipe 5 is opened so that the carrier gas and vapourized sample are carried into the needle 7, where the sample is condensed and collected on the inner surface of the needle, while the carrier gas is vented through the one-way valve 11 to the vent 12. With the one-way valve of the syringe 8 closed, the needle containing the condensed sample is withdrawn from plug 6 and introduced into a heated injector port of an analytical apparatus (not shown). The condensed sample in the needle 7 vapourizes rapidly on the introduction of needle 7 into the heated injector port of the analyt-ical apparatus. The plunger 10 is then depressed to drive the sample vapours from the needle 7 into the carrier gas stream of the analytical apparatus, typically flowing at a rate of 1-5 cc/min.
If desired, a carousel of the sample tubes may be used, each capped with a TEFLON or rubber plug 6, and provision made for a stream of carrier gas to transfer vapourized samples from successive tubes 1 to the needle 7 of the hypodermic syringe 8. The syringe 1~234~1.
1 8 may be acti a-ted by a servo--mechanism to inject success-ive samples into the heated injector port of the analyt-ical apparatus.
Desirable ~eatures of the present invention are (a) conventional sample tubes may be used; (b) laminar flow rate cluring ejection of the vapourized sample from the needle allows the apparatus to be used with capillary ~as chromatographs; (c) the needle may be significantly sma]ler than needles of the type employed in known apparatus; (d) the needle does not require an adsorbent packing which is used in known apparatus;
and (e) no modifications to the analytical apparatus (e.g. gas chromatograph, ion mobility spectrometer) are necessary.
Mixtures of chlorinated biphenyls have been extracted from an air stream into a sample tube of the type shown in Figure 1. The samples were then transferred to syringe needles and these used to transfer the samples into suitable analytical test apparatus such as a capillary gas chromatograph or ion mobility spectrometer, in the manner described with reference to Figure 1.
Using the apparatus of the type described with reference to Figure 1, very satisfactory chromatographic results have been obtained. The apparatus can yield excellent peak sharpness and reproducibility. Given below are some results for six compounds tested using the apparatus shown in Figure 1.
~3~` ~
12~:~46~
_ a " ~ ~ SS
" o ,3 ~ ~ a ~ ;~
~7s ~, ~, ~ ~J X
~ C ~ ¦
C ~ Y ~) C ~ .
L _ .
_9_ ~2~3461 b t, .... '~ ~ V
~ D ~ b ~; g ~ ~
, ~Yg ~' ~9~ ~
. .
o ~ ~ ~,: o ;
q _ V~ ~ i ~2234~;1 .
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r i~ ._ _ a e ~, e ~
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F~; ¦
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.
o " ~ ~ ~, '~
a ~ a ~3~ ~
,~3~ ~
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9~ :.
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'' t 122~
l It should be noted that the carrier gas flow through the sample tube l, when transferring the sample from a sample tube l to the needle 7, was found to be of the order of 15-25 cc/min while the gas flow for conveying the vapourized sample from the needle 7 to the gas chromatograph was found to be of the order of l-1.5 cc/min. From this it will be seen that condensing the vapourized sample in the needle and exhausting carrier gas from the syringe has the effectof delivering a much higher concentration of the sample in the carrier gas that is delivered to the gas chromatograph. For low boiling point compounds such as 2-dimethylaniline (Example 2) the needle should preferably be cooled to below ambient temperatures to improve condensation of the condensed sample in the needle 7. The apparatus according to the present invention has proved particularly useful in the analysis of polychlorinated biphenyls.
.
Claims (5)
1. An apparatus for the introduction of a vapourized sample into an analytical test apparatus, comprising:
- a sample tube for the collection of a condensed sample and from which, when heated, the sample may be vapourized and eluted - means at an upstream end of the sample tube for passing a carrier gas to the sample tube interior;
- a hypodermic syringe having a heat dissipating metal walled, hollow needle for the condensation of the vapourized sample, from the sample tube on an inner surface of the needle, and transfer of the condensed sample in a vapourized, concentrated form therefrom to the analytical test apparatus;
- a valve attached to the hypodermic syringe, at a position adjacent the needle, for venting carrier gas therefrom from which the vapourized sample has been condensed in the needle; and - a plug closing the downstream end of the sample tube and, in operation, sealing said needle in a perforation for the transfer of an eluted sample from the sample tube to the hypodermic syringe.
- a sample tube for the collection of a condensed sample and from which, when heated, the sample may be vapourized and eluted - means at an upstream end of the sample tube for passing a carrier gas to the sample tube interior;
- a hypodermic syringe having a heat dissipating metal walled, hollow needle for the condensation of the vapourized sample, from the sample tube on an inner surface of the needle, and transfer of the condensed sample in a vapourized, concentrated form therefrom to the analytical test apparatus;
- a valve attached to the hypodermic syringe, at a position adjacent the needle, for venting carrier gas therefrom from which the vapourized sample has been condensed in the needle; and - a plug closing the downstream end of the sample tube and, in operation, sealing said needle in a perforation for the transfer of an eluted sample from the sample tube to the hypodermic syringe.
2. An apparatus according to claim 1, further comprising heating means for vapourizing a sample in the sample tube.
3. An apparatus according to claim 1, further comprising sample adsorbent material in the sample tube.
CLAIMS (Continued)
CLAIMS (Continued)
4. An apparatus according to claim 1, wherein the hypodermic syringe further comprises a barrel and a plunger.
5. A method for the introduction of a vapourized sample into an analytical test apparatus, comprising:
a) collecting said sample in a condensed form in a sample tube;
b) closing a downstream end of the sample tube with a plug;
c) inserting a heat dissipating metal walled needle of a hypodermic syringe through the plug;
d) heating said sample in the tube to render the sample in vapour form;
e) feeding a carrier gas through the tube to entrain the vapourized same and transport it into the needle;
f) condensing the sample from the carrier gas onto the inner surface of the needle;
g) venting carrier gas from which the sample has been condensed, from the hypodermic syringe at a position adjacent the needle, whereby h) said needle may be introduced into a heated sample intake port of the analytical apparatus, for injection of the sample in a vapourized, concentrated form therein for analysis.
a) collecting said sample in a condensed form in a sample tube;
b) closing a downstream end of the sample tube with a plug;
c) inserting a heat dissipating metal walled needle of a hypodermic syringe through the plug;
d) heating said sample in the tube to render the sample in vapour form;
e) feeding a carrier gas through the tube to entrain the vapourized same and transport it into the needle;
f) condensing the sample from the carrier gas onto the inner surface of the needle;
g) venting carrier gas from which the sample has been condensed, from the hypodermic syringe at a position adjacent the needle, whereby h) said needle may be introduced into a heated sample intake port of the analytical apparatus, for injection of the sample in a vapourized, concentrated form therein for analysis.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA000473884A CA1223461A (en) | 1985-02-08 | 1985-02-08 | Method and apparatus for the introduction of a vapourized sample into an analytical test apparatus |
| US07/025,060 US4732046A (en) | 1985-02-08 | 1987-03-12 | Method and apparatus for the introduction of a vaporizable sample into an analytical test apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA000473884A CA1223461A (en) | 1985-02-08 | 1985-02-08 | Method and apparatus for the introduction of a vapourized sample into an analytical test apparatus |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1223461A true CA1223461A (en) | 1987-06-30 |
Family
ID=4129790
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000473884A Expired CA1223461A (en) | 1985-02-08 | 1985-02-08 | Method and apparatus for the introduction of a vapourized sample into an analytical test apparatus |
Country Status (2)
| Country | Link |
|---|---|
| US (1) | US4732046A (en) |
| CA (1) | CA1223461A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5646334A (en) * | 1995-09-12 | 1997-07-08 | Seagate Technology, Inc. | Multisample dynamic headspace sampler |
Families Citing this family (27)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| US6871556B2 (en) * | 2001-07-27 | 2005-03-29 | The Regents Of The University Of California | Porous protective solid phase micro-extractor sheath |
| JP3917052B2 (en) * | 2002-10-16 | 2007-05-23 | 信和化工株式会社 | Copolymer, adsorbent or concentration medium using the same, injection needle for solid-phase microextraction |
| DE602004003220D1 (en) * | 2004-04-06 | 2006-12-28 | Mass Spec Analytical Ltd | desorber |
| DE102005026585A1 (en) * | 2005-05-03 | 2006-11-09 | Forschungszentrum Jülich GmbH | Method for sample introduction into modules as well as adapters |
| CN104749389B (en) * | 2013-12-30 | 2017-07-14 | 同方威视技术股份有限公司 | Universal injector, gas chromatograph and combination spectrometer |
| US10514365B2 (en) * | 2015-09-24 | 2019-12-24 | Alireza Ghiasvand | Cooling-assisted inside needle capillary adsorption trap device for analyzing complex solid samples using nano-sorbent |
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| US11754478B2 (en) | 2018-08-16 | 2023-09-12 | Abb Schweiz Ag | Rapid equilibrator for water isotope analysis |
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| US3733908A (en) * | 1970-08-19 | 1973-05-22 | Hydronautics | Sampling valve and compound detection system |
| US4003257A (en) * | 1974-03-12 | 1977-01-18 | Nasa | Analysis of volatile organic compounds |
| US3918913A (en) * | 1974-12-02 | 1975-11-11 | Lilly Co Eli | Sampler-injector for liquid chromatography |
| US4046014A (en) * | 1975-06-20 | 1977-09-06 | Boehringer John R | Sealable activated charcoal gas sampler |
| US4128008A (en) * | 1977-05-04 | 1978-12-05 | Xonics, Inc. | Concentration valve for a gas detecting apparatus, or the like |
| DE2818251C2 (en) * | 1978-04-26 | 1981-10-08 | Bodenseewerk Perkin-Elmer & Co GmbH, 7770 Überlingen | Sampler for gas chromatographs |
| US4378499A (en) * | 1981-03-31 | 1983-03-29 | The Bendix Corporation | Chemical conversion for ion mobility detectors using surface interactions |
| US4476734A (en) * | 1983-03-07 | 1984-10-16 | International Business Machines Corporation | Wet needle sampler for use with a gas chromatograph |
| US4551624A (en) * | 1983-09-23 | 1985-11-05 | Allied Corporation | Ion mobility spectrometer system with improved specificity |
| US4527438A (en) * | 1983-09-28 | 1985-07-09 | Cortex Research Corporation | Automatic feed system for sampling apparatus |
| US4584887A (en) * | 1984-10-10 | 1986-04-29 | The United States Of America As Represented By The Administrator Of The National Aeronautics & Space Administration | Solid sorbent air sampler |
-
1985
- 1985-02-08 CA CA000473884A patent/CA1223461A/en not_active Expired
-
1987
- 1987-03-12 US US07/025,060 patent/US4732046A/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5646334A (en) * | 1995-09-12 | 1997-07-08 | Seagate Technology, Inc. | Multisample dynamic headspace sampler |
| US5753791A (en) * | 1995-09-12 | 1998-05-19 | Seagate Technology, Inc. | Multisample dynamic headspace sampler |
| US5773707A (en) * | 1995-09-12 | 1998-06-30 | Seagate Technology, Inc. | Calibration method for multisample dynamic headspace sampler |
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| Publication number | Publication date |
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| US4732046A (en) | 1988-03-22 |
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