US3585862A - Device for introducing samples into a chromatographic column - Google Patents

Device for introducing samples into a chromatographic column Download PDF

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Publication number
US3585862A
US3585862A US814375A US3585862DA US3585862A US 3585862 A US3585862 A US 3585862A US 814375 A US814375 A US 814375A US 3585862D A US3585862D A US 3585862DA US 3585862 A US3585862 A US 3585862A
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US
United States
Prior art keywords
sample
passage member
casings
samples
capillary
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Expired - Lifetime
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US814375A
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English (en)
Inventor
Jiri Hrdina
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Czech Academy of Sciences CAS
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Czech Academy of Sciences CAS
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    • 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
    • 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

Definitions

  • the invention relates to a device for introducing samples into a chromatographic column.
  • a device for introducing samples automatically or semiautomatjcally into a chromatographic column from one or several containers holding in a capillary the sample to be analyzed and sectionalized into adjacent liquidal columns for example by one or several bubble pistons.
  • the individual sample containers are successively connected by valve means into a hydraulic circuit leading to the chromatographic column either directly or through a pump. This type of apparatus is described in US. Patent No. 3,401,564.
  • Another device for introducing samples into a chromatographic column successively from more than one cartridge in which the individual samples are bonded for example by sorption on a small quantity of a porous possibly loose material such as an ion exchanger used as a separating charge of the chromatographic column.
  • the samples are placed beforehand into a number of cartridge-shaped casings which are clamped for example between two porous plates. Samples held in this manner in the cartridge-shaped container may be practically kept for any time in a wet or dry condition.
  • the casing is tightly supported between a pressure head and a frame body provided with a capillary duct leading to the chromatographic column.
  • the pressure head is provided with another duct connected to a pump which forces an eluent to flow therethrough and through the easing into the column.
  • the eluent carries along with it the sample held by sorption on the charge of the casing and introduces it into the chromatographic column. Desorption is achieved by suitable physical-chemical properties of the eluent. As the dimensions of the individual casings are small, a number of casings containing samples intended for progressive analyses can be prearranged on a suitable conveyor.
  • the individual cartridges are replaced from their operating position in the following manner: a cartridge containing a just analyzed sample is released from any connection by lifting the pressure head, then the conveyor means lifts to a certain extent all cartridges placed on it and frees them from any contact, and in this lifted condition the conveyor means is moved, that is shifted or rotated to bring the next nearest cart'ridge into the abandoned operating position between the pressure head and the duct leading to the chromatographic column. The conveyor means is then lower and a new cartridge is brought into the operating position thus securing close hydraulic communication between the central duct in the pressure head and the cartridge, and also a close communication between the lower end of the cartridge and a continuing capillary duct leading to the chromatographic column.
  • This type of sample introducing device is described in US. Pat. No.
  • Bubble pistons prove to be a very effective means for preventing undesirable mixing between the individual sections of the liquidal column moving through its capillary.
  • the bubbles may be so small that no difficulties arise from the presence of a very small quantity of gas which they introduce into the column, more particularly in cases where the eluent and the sample both pass through a closure with a porous body.
  • the bubbles become fragmented and the resulting very small parts do not interfere any longer becoming quickly dissolved in the adjacent liquid.
  • the second required demand made on the analyses is to achieve maximum separation efficiency of the analyzer even in semiautomatic cycles.
  • At least one cartridgelike casing holding samples intended for treatment is replaced by a passage member at a place where the sample is transferred into the chromatographic column, the capillary outlet of the passage member being tightly connected to the capillary duct leading to the column.
  • H68. 1 and 2 illustrate substantially in sectional views two embodiments, respectively, of a device in accordance with the invention
  • FIG. 1 a plurality of known exchangeable cartridgelike casings 1 is located in a transportation means such as shiftable disc 2' each casing 1 provided with a duct 1' holding a sample.
  • a transportation means such as shiftable disc 2' each casing 1 provided with a duct 1' holding a sample.
  • One casing 1 is replaced by a passage member 2 outwardly shaped substantial identical with the casing 1.
  • the passage member 2 is shown in a position where the sample can be transferred from a capillary duct 15 therein into the column 20 the pressure head 3 and the sealing rings 25, 25 securing the receiver 2 in a hydraulic circuit leading to the column 20.
  • a pump 4 forces eluent through pipe 5, duct 6, the cranked duct 9 in rotary valve 8 thin the frame body 7 and through the adjoining pipe 10 into the three-way valve 11.
  • This valve 11 in the position shown in FIG. k permits the eluent to flow through pipe 12 over a known adjustable loop dosing device 13 into pipe 14 and into L-shaped duct 15 in passage member 2.
  • the pressure of adjusting screw 3' upon pressure head 3 secures in view of pressure rings 25, 25' a tight connection between duct 15 and duct 16 from where the eluent flows through the adjustable duct 17 of valve 8 into the supply duct 19 leading to column 20.
  • FIG. 2 illustrates schematically another embodiment of the device in accordance with my invention.
  • Passage member 2 which replaces an individual casing l in carrier 2 is provided with two angular ducts K5 and lb, separated from each other.
  • Duct l is equivalent with the identically numbered duct of HG. l, the only difi'erence being that it may lead into pipe M with a smaller angular bend which is advantageous for the transfer of bubble pistons.
  • the second angular duct lb opens with one leg into the top face of passage member 2 and is tightly joined by a sealing ring 25 to duct 22 in the pressure body 3. This duct 22 is directly connected to eluent pump 4 by the pipe 2H.
  • frame body 7 does not comprise hydraulic switching means such as valve b, the duct 16 being directly connected to column 20.
  • the sample is here transferred from the loop 23 of the dosing device to the column 20 in the same manner as in the embodiment of FIG. 11.
  • the advantage of the embodiment illustrated in FIG. 2 resides in the elimination of the three-way valve ill.
  • the loop dosing device 13 together with the passage member 2 connected thereto may permit to carry out individual analyses with increased separation power by replacing passage member 2 in carrier 2' by a normal cartridge l.
  • a conventional cartridge-type machine has a movable disc 2' which is typically in the form of a turntable that supports a plurality of casings ll containing samples to be analyzed.
  • the casings i move sequentially between the movable clamp 3 and the socket in the base '7 of the machine.
  • the passage l6 conducts liquid from the casing to the column 20. Fluid is conducted from the pump 43 through the conduit 21 and through the clamp 33 from which it flows through the interior passage in the casing l to transfer the sample into the column.
  • the apparatus of this invention permits the conventional turntable apparatus to be converted for use with a loop dosing device.
  • the passage member 2 has the same shape as the conventional casing 1 so that it is received in one of the openings in the disc 2'.
  • the capillary 23 receives a sample to be tested by operation of the dosing device 113. in accordance with conventional practice, the sample is separated by air bubbles, which are shown in dotted lines in the tube 23.
  • the apparatus and technique for introducing the samples into the capillary 23 and for controlling flow into and out of the capillary are well known in the art.
  • the valve ill controls flow of fluid from the pump and may be a conventional manual valve. Fluid under ressure flows throu h the conduit E2 to the closing device 1 or through the con uit 21 to the clamping head 3. lf the valve is in the position shown in FIG. ll, samples are introduced into the column from the capillary 23 and when the valve is rotated clockwise fluid under pressure is introduced into the casing 11 to wash the sample into the column in accordance with conventional techniques.
  • passage member 2 may have a shape different from that of the individual cartridges 1 permitting a more convenient stabilization.
  • capillary means for temporarily retaining a liquid sample to be analyzed
  • connecting means providing fluid communication between said capillary means and said passage member, said pge member having therein a passage communicating between said connecting means and said outlet conduit means, and i means for controlling flow of liquid through said connecting means from said capillary means to said passage member whereby samples may be introduced into a chromotographic column selectively from said sample casings and said capillary means.
  • inlet and outlet means include means for selectively clamping said casings and said passage member between said inlet means and outlet means, and including valve means for selectively conducting fluid under pressure alternately to said inlet means and said capillary means.

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  • 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)
US814375A 1968-04-09 1969-04-08 Device for introducing samples into a chromatographic column Expired - Lifetime US3585862A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CS262768 1968-04-09

Publications (1)

Publication Number Publication Date
US3585862A true US3585862A (en) 1971-06-22

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US814375A Expired - Lifetime US3585862A (en) 1968-04-09 1969-04-08 Device for introducing samples into a chromatographic column

Country Status (7)

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US (1) US3585862A (ko)
AT (1) AT297666B (ko)
BE (1) BE731146A (ko)
CH (1) CH489793A (ko)
DE (1) DE1917723B2 (ko)
FR (1) FR2005871A1 (ko)
GB (1) GB1258825A (ko)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112272772A (zh) * 2018-06-14 2021-01-26 沃特世科技公司 样品组织器、托盘、系统和方法
CN112362794A (zh) * 2020-11-10 2021-02-12 山东悟空仪器有限公司 进样机和满环进样方法、液体分析方法和液相色谱系统

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3916692A (en) * 1973-11-14 1975-11-04 Waters Associates Inc Novel injector mechanism
DE3735814A1 (de) * 1987-10-22 1989-05-11 Siemens Ag Einrichtung und verfahren zum dosieren von proben fuer die gaschromatographische analyse
JP2845909B2 (ja) * 1988-12-09 1999-01-13 株式会社日立製作所 液体クロマトグラフおよびそれを用いる方法
DE20020555U1 (de) * 2000-12-05 2001-05-17 LC Tech GmbH, 84405 Dorfen Vorrichtung zur Erzeugung eines vorbestimmten Volumens vorgereinigter Bestandteile von Lösungsgemischen

Citations (6)

* Cited by examiner, † Cited by third party
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
US3192969A (en) * 1962-07-02 1965-07-06 Warner Lambert Pharmaceutical Automatic sample handling apparatus
US3192968A (en) * 1962-07-02 1965-07-06 Warner Lambert Pharmaceutical Apparatus for performing analytical procedures
FR1452572A (fr) * 1964-11-06 1966-02-25 Ceskoslovenska Akademie Ved Procédé et installation pour introduire des échantillons dans des colonnes chromatographiques
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

Patent Citations (6)

* Cited by examiner, † Cited by third party
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
US3192969A (en) * 1962-07-02 1965-07-06 Warner Lambert Pharmaceutical Automatic sample handling apparatus
US3192968A (en) * 1962-07-02 1965-07-06 Warner Lambert Pharmaceutical Apparatus for performing analytical procedures
US3282651A (en) * 1963-07-12 1966-11-01 Technicon Instr Sample and reagent and/or wash liquid supply apparatus
FR1452572A (fr) * 1964-11-06 1966-02-25 Ceskoslovenska Akademie Ved Procédé et installation pour introduire des échantillons dans des colonnes chromatographiques
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 (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112272772A (zh) * 2018-06-14 2021-01-26 沃特世科技公司 样品组织器、托盘、系统和方法
CN112272772B (zh) * 2018-06-14 2024-07-12 沃特世科技公司 样品组织器、托盘、系统和方法
CN112362794A (zh) * 2020-11-10 2021-02-12 山东悟空仪器有限公司 进样机和满环进样方法、液体分析方法和液相色谱系统

Also Published As

Publication number Publication date
DE1917723B2 (de) 1971-07-15
DE1917723A1 (de) 1969-10-16
AT297666B (de) 1972-04-10
BE731146A (ko) 1969-09-15
CH489793A (de) 1970-04-30
GB1258825A (ko) 1971-12-30
FR2005871A1 (ko) 1969-12-19

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