US3585863A - Method and device for introducing samples into a chromatographic column - Google Patents
Method and device for introducing samples into a chromatographic column Download PDFInfo
- Publication number
- US3585863A US3585863A US814324A US3585863DA US3585863A US 3585863 A US3585863 A US 3585863A US 814324 A US814324 A US 814324A US 3585863D A US3585863D A US 3585863DA US 3585863 A US3585863 A US 3585863A
- Authority
- US
- United States
- Prior art keywords
- cartridge
- liquid
- column
- pumping
- sample
- 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 - Lifetime
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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
- G01N1/405—Concentrating samples by adsorption or absorption
-
- 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
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
-
- 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
- G01N30/20—Injection using a sampling valve
-
- 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
- G01N30/20—Injection using a sampling valve
- G01N2030/201—Injection using a sampling valve multiport valves, i.e. having more than two ports
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8881—Modular construction, specially adapted therefor
-
- 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
- G01N30/24—Automatic injection systems
Definitions
- a plurality of cartridges are transported sequentially into fluid communication with the column.
- Each cartridge contains a solid porous sorption material retained between perforated plates.
- the cartridge is clamped in a fluid circuit and deaeration of the sorption material is carried out by pumping a liquid through the cartridge. After deaeration of the porous material, eluent liquid is pumped through the cartridge and into the column and the danger of the inclusion of air bubbles in the stream is eliminated.
- the samples to be analyzed are introduced before being analyzed into individual cartridges wherein they are held by sorption on a small amount of an ion exchanger gripped between two porous plates.
- This method has the disadvantage that the samples to be analyzed are bonded to the ion exchanger mostly in dried form, particularly if the samples are introduced into the respective cartridges as early as for example one month prior to the analysis.
- a relatively large amount of air is contained either in microscopic holes between ion exchanger grains or other microscopic spaces in the cartridge and when the liquid eluent fiows through the cartridge, the air is entrained in the liquid stream which flows into the chromatographic column. This is not too harmful in analytical processes of medium effectivity in which one analysis may last about two hours. But in highly effective modern methods this disadvantage becomes damaging substantially reducing the total efficiency of the method and device.
- each of the cartridges is freed of an undesirable quantity of air before being put into a position in which the sample is transposed from the cartridge into the chromatographic column.
- To free the cartridge of air it is introduced into a hydraulic circuit close to the place at which the sample is to be transposed from the cartridge into the chromatographic column. In this position a suitable liquid is pumped through it either pennanently or temporarily. This liquid fills up all spaces which heretofor have been occupied by air or by a gas.
- FIG. 2 shows a'sectional view of a detail of FIG. I
- FIG. 3 is a partial top view of a transportation disc for the cartridges.
- FIG. 4 is a schematic view of one modified form of the pump and conduit apparatus of FIG. I.
- FIG. is a schematic view of another modified form of the pump and conduit apparatus of FIG. 1.
- the cartridges 1, 2 are transposed stepwise by a carrier 3 such as a transportation disc which turns step-by-step in the direction of arrow 4 and which also liftably frees cartridges 1, 2 from the positions shown in FIG. I where they are clamped between the pressure bodies and 18 and the discharge channels 13 and 19, respectively.
- a carrier 3 such as a transportation disc which turns step-by-step in the direction of arrow 4 and which also liftably frees cartridges 1, 2 from the positions shown in FIG. I where they are clamped between the pressure bodies and 18 and the discharge channels 13 and 19, respectively.
- Each of the cartridges 1, 2 is provided with a longitudinally extending central boring which contains a certain amount of for example a cation exchange resin 5 held between plates 6 and 7 made from a porous material.
- cartridge 1 by means of sealing rings 11, 12 is tightly clamped between the spring-loaded pressure body 10 actuated by pressure element 9 and the mouth of channel 13 leading the eluent into column 8 through channel 24 in the rotary valve member 14.
- Another channel 25 in said valve member 14 connects pipe 15 with duct 15 and guides the elution solution from pump 14 through conduits 16,17 into the cartridge I from where said solution continues through ducts 13 and 24 into column 8.
- the cartridge 2 Prior to transposing a cartridge from position 2 into position 1 and to the performance of the analysis the cartridge 2 is clamped similar to cartridge 1 between the pressure body 18 and the mouth of duct 19 and liquid of proper qualities is pumped from container 23 by pump 22 through conduits 21, 20 into and through cartridge 2 into conduits 19',19 leading into waste. Thereby any gaseous content is removed from cartridge 2 before it is moved into position 1 and before analysis is performed.
- the liquid fed by pump 22 need not be accurately dosed and pump 22 may be of any proper type such as a peristaltic pump because the hydraulic resistances of cartridges 1, 2 or of their porous charge 5 and of the porous plates 6, 7 are very small.
- the sample bonded by sorption or otherwise to the carrier material in the cartridge is not carried away from the cartridge even to a small extent.
- This can be achieved by filling the cartridges with a small quantity for example of thesame cation exchange resin with which the columns are also filled.
- the liquid used for expelling air or gas forms for example a citrate or another bufier which is substantially identical with elution buffers intended not only to carry the sample into the column but also to perform chromatography in the column.
- the pH value is so low that no untolerable quantity of the sample will be carried away into waste when the liquid flows through the cartridge, and the entire quantity of the sample remains bonded to the material in the cartridge.
- FIG. 2 illustrates the rotary valve member 14 turned approximately by 60 clockwise to directly connect the pipe 15 through the channel 25 in the rotary valve member 14 with column 8; the eluent is thus fed directly into the column 8 and the cartridges 1, 2 can be freely manipulated as they are not introduced into the hydraulic circuit between pump 14 and column 8.
- FIG. 3 shows a conventional transportation disc 3 supporting a plurality of cartridges 1, 2 arranged in two concentric placements. This arrangement is advantageous for automatic introduction of samples into more than one column.
- the disc 3 rotates at predetermined time intervals to advance the cartridges from one position to the next.
- the cartridges are unclamped by raising the clamping heads 10 and 18, while raising the disc 3 to engage the collar at the upper end of each cartridge 1 and 2.
- the cartridges are disengaged from the conduits l7 and 13; and the conduits 21 and 19' and are free to move from the position indicated at 2 in FIG. 1 to the position indicated at 1 in FIG. 1.
- the cartridge previously in position indicated 1 advances toward the right, as viewed in FIG. 1 and as indicated by the arrow 4.
- the cartridges are thus transported step by step into and out of engagement with the clamping heads 10 and 18.
- the pump 22 draws liquid from the container 23 for deaeration.
- the valve 14 is in the position shown in FIG. 2 while the cartridge is being transported from one position to the other.
- the pump 14' operates continuously and the eluent liquid fiows through the conduit 15 and through the valve passage 25 to the column 8.
- the valve 14 is rotated to the position shown in FIG. 1 to conduct eluent through the passage 17, through the cartridge containing the sample, and into the column 8.
- the valve 14 is then returned to the position shown in FIG. 1 to stop the flow of eluent liquid to the cartridge, thereby allowing the cartridge to be transported by the disc 3.
- the deaerating step that is performed at FIG. 2 and the elution step that is performed at position 1 occur substantially simultaneously.
- FlG. 3 shows a modified form of the pump and apparatus at the pump and conduit apparatus of FIG. 1.
- the liquid container 23a supplies liquid to the pump 22a and a valve 24a selectively controls flow through the conduit 21a which corresponds to the conduit 21 in H6. l, or with the waste conduit 1%, corresponding to the waste conduit 19 in IF 16.
- MG. discloses a pump 22b for supplying liquid from a container 23b to the conduit 21b or 19b, as controlled by the operation of the valves 26 and 27.
- a method for introducing liquid samples into a chromatrographic column in the absence of air bubbles comprising: adsorbing a quantity of a sample liquid on a porous material within a cartridge, connecting said cartridge in a first fluid circuit, pumping a first liquid stream through said cartridge, subsequently disconnecting said cartridge from said first circuit and connecting said cartridge with a second fluid circuit, and pumping a second liquid stream through said cartridge and into said column, whereby said first liquid stream deaerates said cartridge.
- a method for introducing liquid samples into a chromatographic column in the absence of air bubbles comprising: adsorbing a quantity of a sample liquid on a porous material within a cartridge, supporting a plurality of said cartridges for sequential movement through a first position and through a second position, pumping a first liquid stream through said cartridge at said first position, and subsequently pumping a second liquid stream through said cartridge at said second position and into said column, whereby said first liquid stream deaerates said cartridge.
- Apparatus for introducing samples into a chromatographic column comprising: a plurality of cartridges, means mounting said cartridges for sequential movement between a deaerating position and a sample introduction porition, first means for pumping liquid through said cartridge while in said deaerating position to displace air from the interior of said cartridge, and second means for pumping eluent liquid through said cartridge while in said sample introduction position, said eluent pumping means including a conduit communicating between said cartridge and said chromatographic column while said cartridge is in said sample introducing position.
- the apparatus according to claim 5 including means for clam ing said cartridges in said deaerating position and in said samp e introduction position, said clamping means including fluid passages in fluid circuits with said first and second pumping means, respectively and sealing means between said clamping means and said cartridge, whereby said cartridges are effectively transported from one position to the other and connected in the respective fluid pumping circuits.
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CS262968 | 1968-04-09 |
Publications (1)
Publication Number | Publication Date |
---|---|
US3585863A true US3585863A (en) | 1971-06-22 |
Family
ID=5363947
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US814324A Expired - Lifetime US3585863A (en) | 1968-04-09 | 1969-04-08 | Method and device for introducing samples into a chromatographic column |
Country Status (7)
Country | Link |
---|---|
US (1) | US3585863A (xx) |
AT (1) | AT298420B (xx) |
BE (1) | BE731148A (xx) |
CH (1) | CH500484A (xx) |
DE (1) | DE1916930A1 (xx) |
FR (1) | FR2005873A1 (xx) |
GB (1) | GB1258827A (xx) |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4084440A (en) * | 1976-03-31 | 1978-04-18 | Her Majesty In Right Of Canada As Represented By The Minister Of National Defence | Chromatograph injection system |
US4203817A (en) * | 1979-03-06 | 1980-05-20 | Jenoptik Jena G.M.B.H. | Method of and device for moving liquid samples |
US4444066A (en) * | 1981-06-29 | 1984-04-24 | Beckman Instruments, Inc. | High pressure sample injector valve |
US20080149869A1 (en) * | 2005-07-27 | 2008-06-26 | Shannon Mark A | Bi-direction rapid action electrostatically actuated microvalve |
US20090131643A1 (en) * | 2006-04-14 | 2009-05-21 | Zheng Ni | Rapid metal organic framework molecule synthesis method |
US20090211452A1 (en) * | 2008-01-16 | 2009-08-27 | The Regents Of The University Of Illinois | Micromachined Gas Chromatography Columns For Fast Separation of Organophosphonate and Organosulfur Compounds and Methods for Deactivating Same |
US20100075123A1 (en) * | 2008-04-08 | 2010-03-25 | University of Illinois - Office of Technology Management | Water repellent metal-organic frameworks, process for making and uses regarding same |
US20100132547A1 (en) * | 2005-10-06 | 2010-06-03 | Masel Richard I | High gain selective metal organic framework preconcentrators |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3220853A1 (de) * | 1981-06-11 | 1982-12-30 | Sandoz-Patent-GmbH, 7850 Lörrach | Probenwechsler fuer gaschromatographische analysenapparate |
DE3242214C2 (de) * | 1982-11-15 | 1986-09-25 | Panayotis Dipl.-Ing. Dr.-Ing. 6100 Darmstadt Roumeliotis | Verfahren und Vorrichtung zum Analysieren eines in einer Hochdruckextraktionsvorrichtung gewonnenen Extraktes |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2833151A (en) * | 1954-04-09 | 1958-05-06 | Ici Ltd | Device for delivering measured quantities of gases or vapours |
US3119251A (en) * | 1960-05-20 | 1964-01-28 | Standard Oil Co | Multiple column gas chromatography valve |
US3192968A (en) * | 1962-07-02 | 1965-07-06 | Warner Lambert Pharmaceutical | Apparatus for performing analytical procedures |
US3249403A (en) * | 1962-11-02 | 1966-05-03 | Beckman Instruments Inc | Liquid sample reactor and evolved gas detector |
US3282651A (en) * | 1963-07-12 | 1966-11-01 | Technicon Instr | Sample and reagent and/or wash liquid supply apparatus |
FR1507455A (fr) * | 1966-03-25 | 1967-12-29 | Atomic Energy Authority Uk | Appareil pour charger automatiquement des échantillons en vue d'une analyse sur unecolonne chromatographique |
-
1969
- 1969-04-02 DE DE19691916930 patent/DE1916930A1/de active Pending
- 1969-04-02 CH CH510369A patent/CH500484A/de not_active IP Right Cessation
- 1969-04-08 AT AT338869A patent/AT298420B/de not_active IP Right Cessation
- 1969-04-08 GB GB1258827D patent/GB1258827A/en not_active Expired
- 1969-04-08 US US814324A patent/US3585863A/en not_active Expired - Lifetime
- 1969-04-08 BE BE731148D patent/BE731148A/xx unknown
- 1969-04-09 FR FR6910885A patent/FR2005873A1/fr not_active Withdrawn
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2833151A (en) * | 1954-04-09 | 1958-05-06 | Ici Ltd | Device for delivering measured quantities of gases or vapours |
US3119251A (en) * | 1960-05-20 | 1964-01-28 | Standard Oil Co | Multiple column gas chromatography valve |
US3192968A (en) * | 1962-07-02 | 1965-07-06 | Warner Lambert Pharmaceutical | Apparatus for performing analytical procedures |
US3249403A (en) * | 1962-11-02 | 1966-05-03 | Beckman Instruments Inc | Liquid sample reactor and evolved gas detector |
US3282651A (en) * | 1963-07-12 | 1966-11-01 | Technicon Instr | Sample and reagent and/or wash liquid supply apparatus |
FR1507455A (fr) * | 1966-03-25 | 1967-12-29 | Atomic Energy Authority Uk | Appareil pour charger automatiquement des échantillons en vue d'une analyse sur unecolonne chromatographique |
Cited By (13)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4084440A (en) * | 1976-03-31 | 1978-04-18 | Her Majesty In Right Of Canada As Represented By The Minister Of National Defence | Chromatograph injection system |
US4203817A (en) * | 1979-03-06 | 1980-05-20 | Jenoptik Jena G.M.B.H. | Method of and device for moving liquid samples |
US4444066A (en) * | 1981-06-29 | 1984-04-24 | Beckman Instruments, Inc. | High pressure sample injector valve |
US20080149869A1 (en) * | 2005-07-27 | 2008-06-26 | Shannon Mark A | Bi-direction rapid action electrostatically actuated microvalve |
US8123834B2 (en) | 2005-10-06 | 2012-02-28 | The Board Of Trustees Of The University Of Illinois | High gain selective metal organic framework preconcentrators |
US20100132547A1 (en) * | 2005-10-06 | 2010-06-03 | Masel Richard I | High gain selective metal organic framework preconcentrators |
US7880026B2 (en) | 2006-04-14 | 2011-02-01 | The Board Of Trustees Of The University Of Illinois | MOF synthesis method |
US20090131643A1 (en) * | 2006-04-14 | 2009-05-21 | Zheng Ni | Rapid metal organic framework molecule synthesis method |
US20090211452A1 (en) * | 2008-01-16 | 2009-08-27 | The Regents Of The University Of Illinois | Micromachined Gas Chromatography Columns For Fast Separation of Organophosphonate and Organosulfur Compounds and Methods for Deactivating Same |
US8123841B2 (en) | 2008-01-16 | 2012-02-28 | The Board Of Trustees Of The University Of Illinois | Column design for micro gas chromatograph |
US8152908B2 (en) | 2008-01-16 | 2012-04-10 | The Board Of Trustees Of The University Of Illinois | Micromachined gas chromatography columns for fast separation of Organophosphonate and Organosulfur compounds and methods for deactivating same |
US20100075123A1 (en) * | 2008-04-08 | 2010-03-25 | University of Illinois - Office of Technology Management | Water repellent metal-organic frameworks, process for making and uses regarding same |
US8269029B2 (en) | 2008-04-08 | 2012-09-18 | The Board Of Trustees Of The University Of Illinois | Water repellent metal-organic frameworks, process for making and uses regarding same |
Also Published As
Publication number | Publication date |
---|---|
GB1258827A (xx) | 1971-12-30 |
DE1916930A1 (de) | 1969-12-04 |
CH500484A (de) | 1970-12-15 |
AT298420B (de) | 1972-05-10 |
BE731148A (xx) | 1969-09-15 |
FR2005873A1 (xx) | 1969-12-19 |
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