US3820660A - Fluid analytical instrument - Google Patents
Fluid analytical instrument Download PDFInfo
- Publication number
- US3820660A US3820660A US00329142A US32914273A US3820660A US 3820660 A US3820660 A US 3820660A US 00329142 A US00329142 A US 00329142A US 32914273 A US32914273 A US 32914273A US 3820660 A US3820660 A US 3820660A
- Authority
- US
- United States
- Prior art keywords
- tubing
- tube
- fluid
- chromatographic
- length
- 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
Links
- 239000012530 fluid Substances 0.000 title claims abstract description 28
- 230000005526 G1 to G0 transition Effects 0.000 claims description 3
- 239000000203 mixture Substances 0.000 abstract description 18
- 239000007788 liquid Substances 0.000 abstract description 5
- 230000009471 action Effects 0.000 description 12
- 241000237858 Gastropoda Species 0.000 description 9
- 239000007789 gas Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 238000009792 diffusion process Methods 0.000 description 4
- 238000000638 solvent extraction Methods 0.000 description 3
- 238000004804 winding Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000004075 alteration Effects 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 210000002966 serum Anatomy 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Images
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
- F16L11/00—Hoses, i.e. flexible pipes
- F16L11/04—Hoses, i.e. flexible pipes made of rubber or flexible plastics
- F16L11/12—Hoses, i.e. flexible pipes made of rubber or flexible plastics with arrangements for particular purposes, e.g. specially profiled, with protecting layer, heated, electrically conducting
- F16L11/121—Hoses, i.e. flexible pipes made of rubber or flexible plastics with arrangements for particular purposes, e.g. specially profiled, with protecting layer, heated, electrically conducting specially profiled cross sections
-
- 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
- B01L3/56—Labware specially adapted for transferring fluids
- B01L3/561—Tubes; Conduits
-
- 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
- G01N30/60—Construction of the column
- G01N30/6052—Construction of the column body
- G01N30/6086—Construction of the column body form designed to optimise dispersion
-
- 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
- G01N35/08—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor using a stream of discrete samples flowing along a tube system, e.g. flow injection analysis
-
- 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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/38—Flow patterns
Definitions
- the shape reduces overlapping of compositions.
- a tube of elliptical cross section is improved when major and minor axes of e1- lipse alternate along length of tube as by twisting the tube or providing offset pinches to a round tube. Additional efficiency is obtained when the tube with thealtemating positions of axes is wound into a helix of the order of 10 mm diameter.
- a fluid analyzing instrument including a tube conduit having a cross section of non-circular shape and the tube being acutely contorted.
- the problem outlined above is of special significance in chromatography, both gas and liquid, where a partitioningcolumn has a carrier medium flowing therethrough,into which medium a small slug of mixture is injected for separation into its components.
- the inner walls ofthe open tube are coated with a thin film acting as a stationary phase which reversibly interacts with the molecules ofthe mixture-under study e.g. by absorption and desorption.
- the several components of the mixture have different transit times through the interior of the column and hence are eluted from the column at different points of timefBecause the times of elution differ for the components, the latter can be determined by detectors based on heat conductivity or by differential refractometers. An important requirement for satisfactory measurement of the several components is that the different constituents ofthe mixture not overlap as they emerge or are eluted.
- the ideal condition would be, that the length of the injected slug remained constant throughout the entire movement in the instrument, so that the individual components would emerge as slugs equally spaced one after the other. This has been found not to be the case however, but instead the slug undergoes a lengthening deformation which can lead to overlapping of the individual emerging slugs of the components to be determined in the mixture.
- the lengthening increases with the flow-through speed dictated by the operating speed, which in turn is dictated by the duration of time in which an analysis must be made.
- the lengthening deformation is traceable to. mixing actions which occur at the separation between the slugs and the carrier medium upon its movement inside of round tubular conduits in apparatus having a column formed as an open tube.
- the invention shows a way to hold the above de scribed mixing action to an especially small amount in the longitudinal direction of the tube. It has been found if the clean cross section of the tube is not circular and the flow of the medium in the tube in the general direction of the tube is additionally altered or contorted or turned, the non-circular cross section and turning of the carrier flow each makes for greater efficiency and the two may be combined for still better results.
- An effective and easily produced form of the invention is a tube having a substantially elliptical inner cross section that is additionally wound about an axis representing the direction of general flow through the tube. Results are better if the major axis of the ellipse lies in an approximate plane of a turn.
- the tube is preferably formed from conventional capillary tube for columns having an inner diameter of about 1 mm by partially flattening such a tube to give an elliptical cross section having major and-minor axes in the ratio 3:1.
- the 1 mm tube is wound into a helix having a diameter of about 10 mm.
- the contorted flow may be obtained by twisting an elliptical tube formed in the manner mentioned above to give a full twist every 25 mm, and then winding the twisted tube into a helix of 10 mm diameter.
- Equally as satisfactory as the twisted tube is a form in'which successive sections of a round tube are partially flattened to elliptical cross sections and wherein alternate sections are at right angles to each other about the main longitudinal axis of the tube. If the sectional lengths are not more than 50 times the length of the major axis of the cross section the desired action is obtained. The resulting tube can be additionally woun'd helically to give even greater efficiency.
- FIG. 1 shows schematically a chromatographic apparatus including a source 1 of mobile phase or carrier medium, such as helium, providing a continuous stream of carrier gas.
- the source may be a storage tank provided with a regulating valve.
- the carrier medium is supplied small amounts of the sample to be analysed-by a syringe 3 through a serum cap, so that a small injected slug of the sample starts off inside the transfer medium stream at zone 2.
- This slug migrates through the partitioning column 4 which is in the form of an open capillary tube whose inner walls are coated, the coating acting and reacting with components to be determoned in the sample. Owing to the different characteristic properties of the components to be separated, they undergo a differential separatory delay during passage through the column so as to leave the column serially, one component after another.
- a detector 5 for example a measuring instrument based on heat conductivity, receives the separated fractions and indicates the amounts by registration on a recording chart 6.
- the composition may be determined by area-integration under the peaks of the chart curve in conventional manner after, for example, the column has been timecalibrated for operation of the system under fixed conditions. For good measurements it is essential that the peaks not overlap. They should be steep sided. This means that the slugs formed from the different components should not become so elongated inside the column that they may mix with each other. Since the column is of capillary dimensions and must be very long, the column is coiled helically to conserve space.
- FIG. 2 shows a column in one form of the invention.
- a capillary cylindrical tube of about I mm inside diameter has been squeezed to produce one of elliptical cross section.
- the major and minor axes of the cross sections are about in the ratio 3:1 and are denoted a and b.
- the squeezing of the tube, if of metal, may be carried out between rollers, but it may be carried out in the same manner at softening temperatures if glass or plastic tubing is used.
- the tube is moreover coiled to form a relatively tightly wound helix of about 8 to 30 mm in diameter preferably about 10 mm, which is in the general course of the tube.
- the novel feature is then not as to the general loose coiling which is as shown in FIG.
- FIG. 2 The construction in FIG. 2 is thus a tight winding according to FIG. 2 incorporated in the further loose coiling shown in FIG. 1.
- the conduit is first formed according to FIG. 2 and then the coiled tube is loosely wound according to FIG. I in order to reduce space requirements.
- FIG. 3 A modification of the invention is shown in FIG. 3.
- the same tube of elliptical cross section is used, but the tube is twisted so as to provide a full turn for each say, to 50 mm of length, preferably about mm, along its l ongitudinal axis.
- This twisting can be done by holding one end of a straight tube fast and turning the other about the tube axis.
- the lie of the different sectional portions is shown in FIG. 3a.
- Such a tube exhibits, in this very form, an increased effect in inhibition of overlapping. It can thus be coiled to conserve space as shown in FIG. I and used as a chromatographic column. An especially good effect is obtained if the twisted tube is first tightly wound as a helix similar to that in FIG. 2, and then the helical coil loosely looped in order to conserve space as shown in FIG. 1.
- FIG. 4 shows another modification of the invention.
- a straight cylinder (1 mm diameter).
- straight denotes a coiling into loops with the loop diameter of at least 50 mm in diameter to save space.
- Looping of the diameter was found to be essentially of the same effect as actually straight tubing.
- the total length of tubing used in a column was from I 20 to 30 meters for liquids and 45 meters for gas.
- FIGS. 5 and 6 the widening h of the slugs in cm is plotted against flow rate of the carrier medium in cm/sec. for the various forms of tubes A to F.
- FIG. 5 shows the results in the case of liquid chromatography.
- the values of h are less than those for the cylindrical tubing, whether tightly helically wound or not, at any given flow rate. It may be noted that the different forms vary in their effect.
- the curve F for the elliptical, twisted, and then helically wound tube This form of the tube gives a very low value for h and the action is nearly independent of flow rate.
- the action is independent from the action of the partitioning column.
- the slug lengthening is accordingly reduced when alternate action of the molecules does 1 not take place with the coating of the partitioning column.
- Chromatographic apparatus for examining fluids comprising a source of carrier fluid, means connected to said source adapted to define a stream for the carrier fluid, means for introducinga sample into a stream of the carrier fluid, a chromatographic column defining a path for the fluid stream following the point of introduction of the sample, a detector connected to said chromatographic column for measuring a characteristic parameter of the fluid stream emerging from said chromatographic column, said chromatographic column being formed of tubing which has been geometrically deformed along a substantial portion of its length so that the tubinghas a major and a minor diameter, said major and minor diameters being alternatively rotated along the deformed portion to produce a movement of the fluid transverse to the direction of flow, said major and minor diameters being of constant lengths throughout the length of said tubing whereby the volume of fluid flow is unchanged throughout the length of said tubing.
- Chromatographic apparatus according to claim 1 wherein said tubing is formed by successively pinching the tubing at spaced invervals along the length thereof with alternate pinchings disposed at 90 to each other.
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Pathology (AREA)
- General Engineering & Computer Science (AREA)
- Immunology (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Mechanical Engineering (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Clinical Laboratory Science (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Priority Applications (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19681675313 DE1675313C3 (de) | 1968-02-15 | 1968-02-15 | Rohr zur Führung sich in ihrer Zusammensetzung ändernder Medien für analytische Geräte |
NL6902180A NL6902180A (xx) | 1968-02-15 | 1969-02-12 | |
GB8101/69A GB1220552A (en) | 1968-02-15 | 1969-02-14 | Instruments for analysing or separating fluids |
FR6903628A FR2001967A1 (xx) | 1968-02-15 | 1969-02-14 | |
US00329142A US3820660A (en) | 1968-02-15 | 1973-02-02 | Fluid analytical instrument |
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DEH0065321 | 1968-02-15 | ||
DE19681675313 DE1675313C3 (de) | 1968-02-15 | 1968-02-15 | Rohr zur Führung sich in ihrer Zusammensetzung ändernder Medien für analytische Geräte |
US79835869A | 1969-02-11 | 1969-02-11 | |
US00329142A US3820660A (en) | 1968-02-15 | 1973-02-02 | Fluid analytical instrument |
Publications (1)
Publication Number | Publication Date |
---|---|
US3820660A true US3820660A (en) | 1974-06-28 |
Family
ID=34382053
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US00329142A Expired - Lifetime US3820660A (en) | 1968-02-15 | 1973-02-02 | Fluid analytical instrument |
Country Status (4)
Country | Link |
---|---|
US (1) | US3820660A (xx) |
FR (1) | FR2001967A1 (xx) |
GB (1) | GB1220552A (xx) |
NL (1) | NL6902180A (xx) |
Cited By (12)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
EP0416234A2 (en) * | 1989-09-05 | 1991-03-13 | Hewlett-Packard Company | Electrophoresis apparatus |
US5032283A (en) * | 1983-03-03 | 1991-07-16 | The Perkin Elmer Corporation | Low dispersion fluid conduit useful in chromatography systems |
US5273655A (en) * | 1989-10-10 | 1993-12-28 | The Regents Of The University Of California | Organic contaminant separator |
US5308493A (en) * | 1989-10-10 | 1994-05-03 | The Regents Of The University Of California | Organic contaminant separator |
US5391296A (en) * | 1994-01-05 | 1995-02-21 | Rotundo; David A. | Pool skimmer deflecting device |
EP0990133A1 (en) * | 1996-02-08 | 2000-04-05 | Lab Connections, Inc. | Nozzle arrangement for collecting components from a fluid for analysis |
US20090139934A1 (en) * | 2007-12-03 | 2009-06-04 | Schlumberger Technology Corporation | Differential acceleration chromatography |
EP2098284A2 (de) * | 2008-03-05 | 2009-09-09 | Dionex Softron GmbH | Kapillarartige Verbindung für die Flüssigkeitschromatographie, insbesondere für die Hochleistungsflüssigkeitschromatographie mit verminderter Dispersion und verbesserten thermischen Eigenschaften |
WO2011061769A1 (en) * | 2009-11-18 | 2011-05-26 | Avantech Group S.R.L. | Supporting devices for capillary and nano hplc columns |
CN102214491A (zh) * | 2010-04-07 | 2011-10-12 | 通用电气-日立核能美国有限责任公司 | 用于最大化钼-99洗提效率的塔几何结构 |
CN107149794A (zh) * | 2017-06-30 | 2017-09-12 | 西华大学 | 一种高效分离生物大分子的方法及所用碟片式螺旋管柱 |
WO2018150842A1 (ja) * | 2017-02-15 | 2018-08-23 | 株式会社島津製作所 | 分析装置用の配管デバイス及びその配管デバイスを用いた分析装置 |
-
1969
- 1969-02-12 NL NL6902180A patent/NL6902180A/xx unknown
- 1969-02-14 GB GB8101/69A patent/GB1220552A/en not_active Expired
- 1969-02-14 FR FR6903628A patent/FR2001967A1/fr not_active Withdrawn
-
1973
- 1973-02-02 US US00329142A patent/US3820660A/en not_active Expired - Lifetime
Cited By (24)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5032283A (en) * | 1983-03-03 | 1991-07-16 | The Perkin Elmer Corporation | Low dispersion fluid conduit useful in chromatography systems |
EP0416234A2 (en) * | 1989-09-05 | 1991-03-13 | Hewlett-Packard Company | Electrophoresis apparatus |
EP0416234A3 (en) * | 1989-09-05 | 1991-07-03 | Hewlett-Packard Company | Electrophoresis apparatus |
US5273655A (en) * | 1989-10-10 | 1993-12-28 | The Regents Of The University Of California | Organic contaminant separator |
US5308493A (en) * | 1989-10-10 | 1994-05-03 | The Regents Of The University Of California | Organic contaminant separator |
US5389251A (en) * | 1989-10-10 | 1995-02-14 | The Regents Of The University Of California | Organic contaminant separator |
US5403477A (en) * | 1989-10-10 | 1995-04-04 | The Regents Of The University Of California | Organic containment separator |
US5391296A (en) * | 1994-01-05 | 1995-02-21 | Rotundo; David A. | Pool skimmer deflecting device |
EP0990133A1 (en) * | 1996-02-08 | 2000-04-05 | Lab Connections, Inc. | Nozzle arrangement for collecting components from a fluid for analysis |
EP0990133A4 (en) * | 1996-02-08 | 2000-04-05 | Lab Connections Inc | NOZZLE ARRANGEMENT FOR THE COLLECTION OF COMPONENTS FROM A FLUID FOR THEIR ANALYSIS |
US8778059B2 (en) | 2007-12-03 | 2014-07-15 | Schlumberger Technology Corporation | Differential acceleration chromatography |
WO2009073270A1 (en) * | 2007-12-03 | 2009-06-11 | Services Petroliers Schlumberger | Differential acceleration chromatography |
US20090139934A1 (en) * | 2007-12-03 | 2009-06-04 | Schlumberger Technology Corporation | Differential acceleration chromatography |
US8512457B2 (en) | 2007-12-03 | 2013-08-20 | Schlumberger Technology Corporation | Differential acceleration chromatography |
EP2098284A3 (de) * | 2008-03-05 | 2009-11-11 | Dionex Softron GmbH | Kapillarartige Verbindung für die Flüssigkeitschromatographie, insbesondere für die Hochleistungsflüssigkeitschromatographie mit verminderter Dispersion und verbesserten thermischen Eigenschaften |
US20090266752A1 (en) * | 2008-03-05 | 2009-10-29 | Hermann Hochgraeber | Capillary-like connector for liquid chromatography, in particular, high-performance liquid chromatography with reduced dispersion and improved thermal characteristics |
EP2098284A2 (de) * | 2008-03-05 | 2009-09-09 | Dionex Softron GmbH | Kapillarartige Verbindung für die Flüssigkeitschromatographie, insbesondere für die Hochleistungsflüssigkeitschromatographie mit verminderter Dispersion und verbesserten thermischen Eigenschaften |
WO2011061769A1 (en) * | 2009-11-18 | 2011-05-26 | Avantech Group S.R.L. | Supporting devices for capillary and nano hplc columns |
CN102214491A (zh) * | 2010-04-07 | 2011-10-12 | 通用电气-日立核能美国有限责任公司 | 用于最大化钼-99洗提效率的塔几何结构 |
US9240253B2 (en) * | 2010-04-07 | 2016-01-19 | Ge-Hitachi Nuclear Energy Americas Llc | Column geometry to maximize elution efficiencies for molybdenum-99 |
WO2018150842A1 (ja) * | 2017-02-15 | 2018-08-23 | 株式会社島津製作所 | 分析装置用の配管デバイス及びその配管デバイスを用いた分析装置 |
JPWO2018150842A1 (ja) * | 2017-02-15 | 2019-11-07 | 株式会社島津製作所 | 分析装置用の配管デバイス及びその配管デバイスを用いた分析装置 |
CN107149794A (zh) * | 2017-06-30 | 2017-09-12 | 西华大学 | 一种高效分离生物大分子的方法及所用碟片式螺旋管柱 |
CN107149794B (zh) * | 2017-06-30 | 2019-11-08 | 西华大学 | 一种高效分离生物大分子的方法及所用碟片式螺旋管柱 |
Also Published As
Publication number | Publication date |
---|---|
DE1675313B2 (de) | 1975-05-28 |
FR2001967A1 (xx) | 1969-10-03 |
DE1675313A1 (de) | 1972-03-16 |
NL6902180A (xx) | 1969-08-19 |
GB1220552A (en) | 1971-01-27 |
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