US20050217393A1 - Auto-sampler - Google Patents

Auto-sampler Download PDF

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Publication number
US20050217393A1
US20050217393A1 US11/082,908 US8290805A US2005217393A1 US 20050217393 A1 US20050217393 A1 US 20050217393A1 US 8290805 A US8290805 A US 8290805A US 2005217393 A1 US2005217393 A1 US 2005217393A1
Authority
US
United States
Prior art keywords
needle
auto
coating material
sampler
coated
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.)
Abandoned
Application number
US11/082,908
Other languages
English (en)
Inventor
Masami Tomita
Yoshiaki Maeda
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shimadzu Corp
Original Assignee
Shimadzu Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Shimadzu Corp filed Critical Shimadzu Corp
Assigned to SHIMADZU CORPORATION reassignment SHIMADZU CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: MAEDA, YOSHIAKI, TOMITA, MASAMI
Publication of US20050217393A1 publication Critical patent/US20050217393A1/en
Priority to US11/648,640 priority Critical patent/US7337654B2/en
Abandoned legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
    • G01N35/1095—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices for supplying the samples to flow-through analysers
    • G01N35/1097—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices for supplying the samples to flow-through analysers characterised by the valves
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B01L3/02—Burettes; Pipettes
    • B01L3/0275—Interchangeable or disposable dispensing tips
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2300/00—Additional constructional details
    • B01L2300/16—Surface properties and coatings
    • B01L2300/161—Control and use of surface tension forces, e.g. hydrophobic, hydrophilic
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N2035/00178—Special arrangements of analysers
    • G01N2035/00277—Special precautions to avoid contamination (e.g. enclosures, glove- boxes, sealed sample carriers, disposal of contaminated material)
    • 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
    • G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
    • G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
    • G01N35/1004—Cleaning sample transfer devices
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T29/00—Metal working
    • Y10T29/49—Method of mechanical manufacture
    • Y10T29/4935—Heat exchanger or boiler making
    • Y10T29/49391—Tube making or reforming
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T29/00—Metal working
    • Y10T29/49—Method of mechanical manufacture
    • Y10T29/4998—Combined manufacture including applying or shaping of fluent material
    • Y10T29/49982—Coating

Definitions

  • the present invention relates to an auto-sampler of an analytical device such as a liquid chromatograph for analyzing liquid as an analytical subject.
  • the present invention relates to an auto-sampler with a needle for sampling.
  • the needle is typically made of stainless steel, i.e., an alloy consisting mainly of iron. Accordingly, iron is microscopically exposed on a surface of the needle, and a certain ingredient in a sample may preferably adhere to iron due to a chemical property of iron. For example, an alkaline substance easily adheres chemically due to a hydroxyl group thereof attracted to iron on a surface of stainless steel. Once an ingredient of a sample adheres chemically, it is difficult to remove the ingredient even through physical cleaning with a cleanser of organic solvent. A trace amount of the ingredient may adhere to a surface of the needle even after cleaning. Accordingly, it is possible that the ingredient mixes into a next sample when the next sample is collected, thereby causing cross-contamination.
  • the needle is coated with a layer of precious metal, synthetic resin, quartz, or the like, thereby preventing the chemical adsorption phenomenon (see Patent Document 1).
  • Patent Document 1 Japanese Patent Publication (Kokai) No. 2002-228668
  • the needle is coated with metal or resin for preventing the chemical adsorption phenomenon, it is possible that the needle has a rough surface depending on a process of metal plating or resin coating. As a result, small bumps and cavities may be formed on the surface of the needle. In this case, liquid may penetrate into a pleat of the bump or cavity and remain on the surface of the needle, thereby causing cross-contamination.
  • an object of the present invention is to provide an auto-sampler having a needle with a coated surface and capable of preventing cross-contamination.
  • an auto-sampler successively collects liquid samples from plural sample containers through a metallic needle.
  • a surface of the needle is coated with a coating material having a chemical activity smaller than that of a parent metal material of the needle, and the coated surface is polished to have an average roughness of 10 to 20 nm.
  • the coating material on the needle surface may include a precious metal or synthetic resin plated or deposited on the parent metal material, or a quartz thin film formed by chemical vapor deposition on the parent metal material.
  • the coating film on the needle is polished with a mechanical or chemical polishing method.
  • the needle is coated with the coating material having a chemical activity smaller than that of the parent metal material.
  • the coating film is polished to have a small surface roughness. Accordingly, it is possible to prevent cross-contamination caused by liquid remaining in bumps and cavities on the surface.
  • a liquid chromatograph may use the needle of the present invention, so that it is possible to eliminate interference due to cross-contamination, thereby obtaining high sensitivity of analysis.
  • FIGS. 1 (A) and 1 (B) are sectional views showing needles of an auto-sampler according to an embodiment of the present invention, wherein FIG. 1 (A) is a needle having a surface coated with platinum plating and polished, and FIG. 1 (B) is a needle having a surface coated with a synthetic resin and polished;
  • FIG. 2 is a schematic diagram showing an auto-sampler of a liquid chromatograph according to an embodiment of the present invention
  • FIGS. 3 (A) to 3 (C) are charts showing an effect of reducing cross-contamination in a case of a needle having a surface coated with platinum plating.
  • FIGS. 4 (A) to 4 (C) are charts showing an effect of reducing cross-contamination in a case of a needle having a surface coated with platinum plating and polished.
  • FIG. 2 is a schematic diagram showing an auto-sampler of a liquid chromatograph according to an embodiment of the present invention.
  • reference numeral 3 denotes a plunger moving reciprocally with a mechanical force.
  • Sample solutions to be analyzed are sealed in plural vials (small-capacity sample bottles) 8 in advance, and are placed on a rack 81 .
  • a needle 7 for collecting the samples from the vials 8 is connected to an injector valve 1 with a flexible loop tube 6 (loop).
  • the needle 7 is also supported by a drive mechanism (not shown), and is capable of moving freely between the vials 8 , a cleaning port 9 , and an injection port 5 in accordance with a program.
  • a valve 2 is a rotary six-position valve for switching the flow channels of the liquids to be attracted and ejected by the plunger 3 .
  • Reference numeral 4 denotes a bottle of cleaning solution.
  • the injector valve 1 is connected through piping to a liquid chromatograph apparatus 10 , and introduces a sample solution into mobile phase liquid.
  • the injector valve 1 is adjusted so that ports e to d communicate.
  • the valve 2 is adjusted so that ports 0 to b communicate as shown in the drawing.
  • the needle 7 is inserted into the vial 8 , and the plunger 3 is pulled to collect a prescribed quantity of the sample solution.
  • the sample solution stays inside the loop 6 , and does not reach the valve 2 or the plunger 3 .
  • the injector valve 1 is operated into a state shown in the figure.
  • the sample inside the loop 6 is introduced into the flow channel of the mobile phase liquid, thereby initiating liquid chromatographic analysis.
  • FIGS. 1 (A) and 1 (B) are sectional views showing needles of an auto-sampler according to an embodiment of the present invention.
  • FIG. 1 (A) is a needle having a surface coated with platinum plating and polished
  • FIG. 1 (B) is a needle having a surface coated with a synthetic resin and polished.
  • the needle 7 shown in FIG. 1 (A), for example, is a flat-head type needle having an outer diameter of 1.2 mm, an inner diameter of 0.5 mm, and a flat tip with a diameter of 0.65 mm.
  • a parent material B is made of stainless steel, and has a surface coated with a platinum plating layer T having a thickness of several ⁇ m to several tens of ⁇ m. The surface after plating is polished so that the surface roughness becomes smaller.
  • An average roughness Ra is 10.14 nm, and an average roughness Rtm of 10 points of maximum roughness is 101.43 nm.
  • the polishing process may be a mechanical process using abrasive grains, or a chemical polishing of treating the needle chemically.
  • the needle may be polished by hand with abrasive grains affixed to a polishing cloth.
  • the needle is immersed in an acid-based liquid to be chemically dissolved.
  • the parent material B is coated with a coating film P (thickness about 300 ⁇ m) of a synthetic resin, i.e., PEEK (polyetheretherketone) having excellent chemical resistance and mechanical strength.
  • a powder coating method can be applied.
  • PEEK is an organic material, and exhibits substantially no chemical adsorption.
  • PEEK is used as a piping material for liquid chromatographs, and is suitable for coating the needle 7 of the auto-sampler of liquid chromatograph.
  • the needle is polished by hand with abrasive grains affixed to a polishing cloth, and the surface roughness same as that in the embodiment shown in FIG. 1 (A) is obtained.
  • FIGS. 3 (A) to 3 (C) are charts showing an effect of reducing cross-contamination in a case of the needle having the surface coated with platinum plating (comparative example).
  • the needle is coated with platinum plating with the method disclosed in Patent Document 1.
  • FIGS. 4 (A) to 4 (C) are charts showing an effect of reducing, cross-contamination in a case that the surface of the needle 7 shown in FIGS. 3 (A) to 3 (C) is polished with the mechanical polishing (embodiment).
  • the comparative example had the average roughness Ra of 45.42 nm and the average roughness Rtm of the ten points of maximum roughness of 278.89 nm.
  • the embodiment had the average roughness Ra of 10.14 nm and the average roughness Rtm of the ten points of maximum roughness of 101.43 nm.
  • the needle surface is coated with the coating material having a chemical activity smaller than the parent material and polished to reduce the surface roughness, it is possible to suppress the cross-contamination as compared with the case that the surface is coated only.
  • the surface of the needle 7 was plated with platinum.
  • a substantially same effect can be obtained by applying the present invention in a case that the needle is coated with PEEK or a synthetic resin film, and the needle is formed of a parent material other than stainless steel.
  • the parent material and coating material are not limited to the embodiments.
  • a substantially same effect as with platinum can be obtained when the needle is plated with precious metals such as other platinum family elements or gold instead of platinum.
  • the dimensions of the needle 7 in the embodiments are just one example, and the present invention is not limited thereto.
  • the surface roughness is not limited to that in the embodiment, and the average roughness Ra may be about 10 to 20 nm.
  • the present invention is generally applicable to auto-samplers in which liquid samples are successively collected from plural vials through a needle.
  • the present invention is also applicable to auto-samplers of various analytical devices for analyzing liquid samples as well as the auto-sampler of liquid chromatograph.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Clinical Laboratory Science (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Automatic Analysis And Handling Materials Therefor (AREA)
US11/082,908 2004-03-30 2005-03-18 Auto-sampler Abandoned US20050217393A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US11/648,640 US7337654B2 (en) 2004-03-30 2007-01-03 Method of forming a needle for auto-sampler

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2004100328A JP4155218B2 (ja) 2004-03-30 2004-03-30 オートサンプラ
JP2004-100328 2004-03-30

Related Child Applications (1)

Application Number Title Priority Date Filing Date
US11/648,640 Continuation US7337654B2 (en) 2004-03-30 2007-01-03 Method of forming a needle for auto-sampler

Publications (1)

Publication Number Publication Date
US20050217393A1 true US20050217393A1 (en) 2005-10-06

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Family Applications (2)

Application Number Title Priority Date Filing Date
US11/082,908 Abandoned US20050217393A1 (en) 2004-03-30 2005-03-18 Auto-sampler
US11/648,640 Expired - Lifetime US7337654B2 (en) 2004-03-30 2007-01-03 Method of forming a needle for auto-sampler

Family Applications After (1)

Application Number Title Priority Date Filing Date
US11/648,640 Expired - Lifetime US7337654B2 (en) 2004-03-30 2007-01-03 Method of forming a needle for auto-sampler

Country Status (3)

Country Link
US (2) US20050217393A1 (enExample)
JP (1) JP4155218B2 (enExample)
CN (1) CN1677110A (enExample)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020102185A1 (en) * 2001-01-31 2002-08-01 Shimadzu Corporation Automatic sampler and needle for the same
EP1795264A1 (en) 2006-07-06 2007-06-13 Agilent Technologies, Inc. Fluid repellant needle
US20080172023A1 (en) * 2006-06-14 2008-07-17 Dionex Corporation Sampling needle and methods of forming and using same
US20100107783A1 (en) * 2008-10-30 2010-05-06 Shimadzu Corporation Auto-sampler
US9238226B2 (en) 2009-12-10 2016-01-19 Roche Molecular Systems, Inc. Combo-tip rack
US9579625B2 (en) 2012-09-21 2017-02-28 Total Synthesis Ltd. Fluid processing apparatus
US11774327B2 (en) 2020-12-29 2023-10-03 Dionex Corporation Bioinert sampling needle

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2433122B (en) 2005-12-10 2008-07-23 Endet Ltd Gas sampling probe
JP2007322148A (ja) * 2006-05-30 2007-12-13 Hitachi High-Tech Science Systems Corp 分注管およびそれを用いた分析装置
JP2008134154A (ja) * 2006-11-28 2008-06-12 Hitachi High-Tech Science Systems Corp 自動分析装置の分注管
DE102010031240A1 (de) * 2010-07-12 2012-01-12 Hamilton Bonaduz Ag Pipettierspitze mit hydrophober Oberflächenausbildung
GB2527169B (en) 2014-02-28 2018-10-24 Waters Technologies Corp Dispensing needle for a fraction collector
US10859541B2 (en) * 2018-03-06 2020-12-08 Waters Technologies Corporation Textured needle for improved piercing performance in liquid chromatography applications
CN108982785A (zh) * 2018-08-17 2018-12-11 重庆光大集团乳业股份有限公司 用于乳制品生产的智能检验检测系统及方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020102185A1 (en) * 2001-01-31 2002-08-01 Shimadzu Corporation Automatic sampler and needle for the same
US20030189053A1 (en) * 2002-04-04 2003-10-09 Felbaum John W. Inert-metal lined steel-bodied vessel end-closure device
US20060049056A1 (en) * 2002-04-12 2006-03-09 Acm Research, Inc. Electropolishing and electroplating methods

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020102185A1 (en) * 2001-01-31 2002-08-01 Shimadzu Corporation Automatic sampler and needle for the same
US20030189053A1 (en) * 2002-04-04 2003-10-09 Felbaum John W. Inert-metal lined steel-bodied vessel end-closure device
US20060049056A1 (en) * 2002-04-12 2006-03-09 Acm Research, Inc. Electropolishing and electroplating methods

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20020102185A1 (en) * 2001-01-31 2002-08-01 Shimadzu Corporation Automatic sampler and needle for the same
US7175812B2 (en) * 2001-01-31 2007-02-13 Shimadzu Corporation Automatic sampler and needle for the same
US20080172023A1 (en) * 2006-06-14 2008-07-17 Dionex Corporation Sampling needle and methods of forming and using same
US8313476B2 (en) * 2006-06-14 2012-11-20 Dionex Corporation Sampling needle and methods of forming and using same
EP1795264A1 (en) 2006-07-06 2007-06-13 Agilent Technologies, Inc. Fluid repellant needle
US20100107783A1 (en) * 2008-10-30 2010-05-06 Shimadzu Corporation Auto-sampler
US9238226B2 (en) 2009-12-10 2016-01-19 Roche Molecular Systems, Inc. Combo-tip rack
US9579625B2 (en) 2012-09-21 2017-02-28 Total Synthesis Ltd. Fluid processing apparatus
US11774327B2 (en) 2020-12-29 2023-10-03 Dionex Corporation Bioinert sampling needle

Also Published As

Publication number Publication date
US7337654B2 (en) 2008-03-04
JP4155218B2 (ja) 2008-09-24
CN1677110A (zh) 2005-10-05
JP2005283453A (ja) 2005-10-13
US20070130748A1 (en) 2007-06-14

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AS Assignment

Owner name: SHIMADZU CORPORATION, JAPAN

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:TOMITA, MASAMI;MAEDA, YOSHIAKI;REEL/FRAME:016398/0103

Effective date: 20050317

STCB Information on status: application discontinuation

Free format text: ABANDONED -- FAILURE TO RESPOND TO AN OFFICE ACTION