EP0000122A1 - Cell for ultracentrifuge in interferometric optical analyses - Google Patents
Cell for ultracentrifuge in interferometric optical analyses Download PDFInfo
- Publication number
- EP0000122A1 EP0000122A1 EP78100101A EP78100101A EP0000122A1 EP 0000122 A1 EP0000122 A1 EP 0000122A1 EP 78100101 A EP78100101 A EP 78100101A EP 78100101 A EP78100101 A EP 78100101A EP 0000122 A1 EP0000122 A1 EP 0000122A1
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- EP
- European Patent Office
- Prior art keywords
- cell
- ultracentrifuge
- cells
- rotor
- plane
- 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.)
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
- B04B—CENTRIFUGES
- B04B5/00—Other centrifuges
- B04B5/04—Radial chamber apparatus for separating predominantly liquid mixtures, e.g. butyrometers
- B04B5/0407—Radial chamber apparatus for separating predominantly liquid mixtures, e.g. butyrometers for liquids contained in receptacles
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/41—Refractivity; Phase-affecting properties, e.g. optical path length
- G01N21/45—Refractivity; Phase-affecting properties, e.g. optical path length using interferometric methods; using Schlieren methods
Definitions
- the invention relates to an ultracentrifuge cell for interference-optical investigations on liquids in ultracentrifuges with a rotor for holding a plurality of ultracentrifuge cells, containing a cell housing with a cell center piece in the form of a plane-parallel disk with two or more continuous channels, these channels being sealed by sealing the cell center piece with windows form suitable chambers for holding the liquid to be examined.
- Analytical ultracentrifuges with interference optics are mainly required for the determination of the molecular weight and the molecular weight distribution of synthetic polymers and of biopolymer in liquids from the sedimentation-diffusion equilibrium.
- the time to reach equilibrium in the centrifugal field can be 10 hours and more. Tried because of the relatively long test duration and the high price of an ultracentrifuge one to operate an ultracentrifuge so that several samples can be examined simultaneously.
- ultracentrifuge cells with several chambers are used, which are arranged in the radial direction to the axis of rotation of the rotor. For manufacturing and geometrical reasons, this design is limited to 2 or 3 x 2 chambers (channels); the expansion of the measuring capacity remains limited to a factor of 3.
- ultracentrifuge rotor Another possibility to expand the capacity of an ultracentrifuge is to provide several possibilities for holding ultracentrifuge cells in the ultracentrifuge rotor. For geometric and strength reasons, up to 8 ultracentrifuge cells can be taken up by one rotor at the same distance from the rotor axis. In order to be able to observe each cell individually, in a known embodiment the cell center parts are different, prismatic. As a result, the light bundles passing through the cells are deflected to different distances from the axis of rotation and the images of the individual cells are separated at the observation site. Molecular weight and molecular weight distribution are determined by interference optics (E. Knözinger, H. Renz, Chemiker-Zeitung 98 (1974) 194 / 2O2).
- a particular problem with the ultracentrifuge cell is the material problem. Due to their strength and lightness, only a few fabrics are considered as cell centerpieces; in addition to aluminum, only aluminum and animal charcoal-filled epoxy resin and an aluminum coated with trifluorochlorethylene are known. A cell centerpiece made of aluminum is also suitable for examinations at higher temperatures, but the pH of the solution to be examined must be 7. Centerpieces made of filled epoxy resin (known as filled epon (R) ) are in resistant to a pH range of 3 to 10, but not resistant to most organic solvents. Centerpieces made of aluminum (known as Kel F (R) ) coated with trifluorochloro-polyethylene cannot be prismatic for processing reasons.
- the windows are ground differently prismatic, the prism edge being perpendicular to the radius vector of the rotor to the center of the ultracentrifuge concerned.
- the angle of inclination of the prism hardly exceeds 1 °, since otherwise the interference patterns would no longer fall within the limited field of view.
- the window brackets must be adapted to the prismatic windows according to the angle and direction of inclination.
- a particular advantage of the device according to the invention is that the cell centerpieces do not have to be prismatic, i.e. they can consist of a material that can only be processed into plane-parallel spacers, and the cells can still measure the concentration profile in such cells, even if they are in a rotor with several ultracentrifuge cells.
- the time saved is very considerable because liquids, which were previously only in rotors with one measuring cell, are now examined together with other measuring cells in a rotor which can accommodate 4 or 6 cells, for example can be. It is particularly advantageous to use a center piece provided with 3 x 2 chambers, with which up to 15 samples can be measured in an ultracentrifuge run.
- the cell center piece 2 In the case of interference-optical investigations, the cell center piece 2 must be designed in two sectors so that the rays from the sample and the reference sample are coherent.
- the shape of the chamber 3 in the cell center piece 2 is trapezoidal perpendicular to the beam direction; however, the shape differs only a few degrees from a rectangle.
- the thickness of the intermediate piece is usually between 1 and 30 mm.
- the cell center piece 2. is a plane-parallel disk made of trifluorochlorethylene in a version with 2 chambers (channels) 3.
- the chambers 3 in the intermediate piece 2 are delimited at the top by a window 4 made of quartz glass and at the bottom by a window 5 made of industrial sapphire.
- Intermediate rings 6, 7 made of plastic serve for sealing.
- FIG. 1 further individual parts of the ultracentrifuge cell, such as window frames 8, seals 9, upper 10 and lower 11 window holders, spacers 12 and pre-screw 13 are shown.
- a plane-parallel 6-channel cell center piece 2 is shown in FIG. 2. Each of the two sectors is divided into 3 channels. The volume is ⁇ 0.2 ml.
- the cell center piece is installed in the centrifuge so that the sectors run radially.
- one of the windows 4, 5 is preferably not plane-parallel but prismatic, the prism edge being perpendicular to the radius vector of the rotor to the center of the ultracentrifuge concerned. If you extrapolate the upper and lower window area up to the cutting line, the angle at the prism edge is less than 1 degree.
- 2 types of prismatic window for example, of 0.5 ° and 1 0 and with plane-parallel windows one already 5 different cells can build up, so that the observation plane in 5 separate fields of observation result. The examination time is only a fifth.
- 6-channel cell centerpieces instead of the 2-sector centerpieces.
- 6-channel cells made of Kel-F (R) with a plane-parallel center piece are known.
- the measuring capacity is increased again by a factor of 3 by using 6-channel cells in a rotor that can accommodate several ultracentrifuge cells.
- the beam path in the region of the upper window is shown schematically in FIG.
- the middle piece 2 is plane-parallel and preferably consists of aluminum coated with trifluorochloro-polyethylene.
- the prismatic upper window 4 made of quartz glass is excessively strongly inclined.
- the upper window holder 10 must be adapted to the prismatic window.
- the rotor axis of the ultracentrifuge lies in the plane of the drawing parallel to the guide groove 14.
Abstract
Description
Die Erfindung richtet sich auf eine Ultrazentrifugenzelle für interferenzoptische Untersuchungen an Flüssigkeiten in Ultrazentrifugen mit einem Rotor zur Aufnahme mehrerer Ultrazentrifugenzellen, enthaltend ein Zellengehäuse mit einem Zellenmittelstück in Form einer planparallelen Scheibe mit zwei oder mehreren durchgehenden Kanälen, wobei diese Kanäle durch dichten Abschluß des Zellenmittelstücks mit Fenstern geeignete Kammern zur Aufnahme der zu untersuchenden Flüssigkeit bilden.The invention relates to an ultracentrifuge cell for interference-optical investigations on liquids in ultracentrifuges with a rotor for holding a plurality of ultracentrifuge cells, containing a cell housing with a cell center piece in the form of a plane-parallel disk with two or more continuous channels, these channels being sealed by sealing the cell center piece with windows form suitable chambers for holding the liquid to be examined.
Analytische Ultrazentrifugen mit Interferenzoptik.werden hauptsächlich zur Bestimmung des Molekulargewichts und der Molekulargewichtsverteilung von synthetischen Polymeren und von Biopolymeran in Flüssigkeiten aus dem Sedimentationa-Diffusions-Gleichgewicht benötigt. Die Zeit bis zur Gleichgewichtseinstellung im Zentrifugalfeld kann 10 Stun-3en und mehr betragen. Wegen der relativ langen Versuchsdauer und des hohen Preises einer Ultrazentrifuge versucht man, eine Ultrazentrituge so zu betreiben, daß gleichzeitig mehrere Proben untersucht werden können. Man verwendet beispielsweise Ultrazentrifugenzellen mit mehreren Kammern, die in radialer Richtung zur Rotationsachse des Rotors angeordnet sind. Diese Bauweise ist aus Herstellungs- und geometrischen Gründen auf 2 oder 3 x 2 kammern (Kanäle) be-, grenzt; die Erweiterung der MeBkapazität bleibt auf einen Faktor 3 beschränkt. Eine andere Möglichkeit, die Kapazität einer Ultrazentrifuge zu erweitern, besteht darin, daß man im Ultrazentrifugenrotor mehrere Möglichkeiten zur Aufnahme von Ultrazentrifugenzellen vorsieht. Aus geometrischen und Festigkeitsgründen können heute bis zu 8 Ultrazentrifugenzellen in gleichem Abstand von der Rotorachse von einem Rotor aufgenommen werden. Um jede Zelle einzeln beobachten zu können, sind in einer bekannten Ausführung die Zellenmittelatücke unterschiedlich, prismatisch ausgebildet. Dadurch werden die durch die Zellen gehenden Lichtbündel verschieden weit von der Rotationsachse abgelenkt und die Bilder der einzelnen Zellen am Beobachtungsort getrennt. Molekulargewicht und Molekulargewichtsverteilung werden interferenzoptisch bestimmt (E. Knözinger, H. Renz, Chemiker-Zeitung 98 (1974) 194/2O2).Analytical ultracentrifuges with interference optics are mainly required for the determination of the molecular weight and the molecular weight distribution of synthetic polymers and of biopolymer in liquids from the sedimentation-diffusion equilibrium. The time to reach equilibrium in the centrifugal field can be 10 hours and more. Tried because of the relatively long test duration and the high price of an ultracentrifuge one to operate an ultracentrifuge so that several samples can be examined simultaneously. For example, ultracentrifuge cells with several chambers are used, which are arranged in the radial direction to the axis of rotation of the rotor. For manufacturing and geometrical reasons, this design is limited to 2 or 3 x 2 chambers (channels); the expansion of the measuring capacity remains limited to a factor of 3. Another possibility to expand the capacity of an ultracentrifuge is to provide several possibilities for holding ultracentrifuge cells in the ultracentrifuge rotor. For geometric and strength reasons, up to 8 ultracentrifuge cells can be taken up by one rotor at the same distance from the rotor axis. In order to be able to observe each cell individually, in a known embodiment the cell center parts are different, prismatic. As a result, the light bundles passing through the cells are deflected to different distances from the axis of rotation and the images of the individual cells are separated at the observation site. Molecular weight and molecular weight distribution are determined by interference optics (E. Knözinger, H. Renz, Chemiker-Zeitung 98 (1974) 194 / 2O2).
Ein besonderes Problem bei der Ultrazentrifugenzelle.ist das Werkstoffproblem. Nur wenige Stoffe kommen aufgrund ihrer Festigkeit und Leichtigkeit als Zellenmittelstücke in Frage; neben Aluminium sind nur aluminium- und tierkohlegefülltes Epoxidharz und ein mit Trifluorchlorpolyäthylen beschichtetes Aluminium bekannt. Ein Zellenmittelstück aus Aluminium ist zwar auch für Untersuchungen bei höheren Temperaturen geeignet, jedoch muß der pH-Wert der zu untersuchenden Lösung bei 7 liegen. Mittelstücke aus gefülltem Epoxidharz (bekannt als filled epon(R)) sind in einem pH-Bereich von 3 bis 10 beständig, jedoch unbeständig gegenüber den meisten organischen Lösungsmitteln. Mit Trifluorchlorpolyäthylen beschichtete Mittelstücke aus Aluminium (bekannt als Kel F(R)) können aus bearbeitungstechnischen Gründen nicht prismatisch hergestellt werden.A particular problem with the ultracentrifuge cell is the material problem. Due to their strength and lightness, only a few fabrics are considered as cell centerpieces; in addition to aluminum, only aluminum and animal charcoal-filled epoxy resin and an aluminum coated with trifluorochlorethylene are known. A cell centerpiece made of aluminum is also suitable for examinations at higher temperatures, but the pH of the solution to be examined must be 7. Centerpieces made of filled epoxy resin (known as filled epon (R) ) are in resistant to a pH range of 3 to 10, but not resistant to most organic solvents. Centerpieces made of aluminum (known as Kel F (R) ) coated with trifluorochloro-polyethylene cannot be prismatic for processing reasons.
Diese Aufgabe wird dadurch gelöst, daß die Fenster unterschiedlich prismatisch geschliffen sind, wobei die Prismenkante senkrecht auf dem Radiusvektor des Rotors zu dem betreffenden Ultrazentrifugenzellenmittelpunkt steht.This object is achieved in that the windows are ground differently prismatic, the prism edge being perpendicular to the radius vector of the rotor to the center of the ultracentrifuge concerned.
Der Neigungswinkel des Prismas übersteigt kaum 1° , da sonst die Interferenzmuster nicht mehr in das begrenzte Sichtfeld fallen würden. Die Fensterhalter müssen den prismatischen Fenstern nach Winkel und Neigungsrichtung angepaßt sein.The angle of inclination of the prism hardly exceeds 1 °, since otherwise the interference patterns would no longer fall within the limited field of view. The window brackets must be adapted to the prismatic windows according to the angle and direction of inclination.
Von besonderem Vorteil der erfindungsgemäßen Vorrichtung ist, daß die Zellenmittelstücke nicht prismatisch sein müssen, also aus einem Stoff bestehen können, der nur zu planparallelen Zwischenstücken verarbeitet werden kann, und mit solchen Zellen trotzdem der Konzentrationsverlauf in jeder Zelle gemessen werden kann, auch wenn sie in einem Rotor mit mehreren Ultrazentrifugenzellen eingebaut sind. Die Zeitersparnis ist sehr erheblich, weil Flüssigkeiten, die bisher nur in Rotoren mit einer Meßzelle jetzt zusammen mit anderen Meßzellen in einem Rotor, der beispielsweise 4 oder 6 Zellen aufnehmen kann, untersucht werden können. Besonders vorteilhaft ist die Verwendung eines mit 3 x 2 kammern versehenen Mittelstückes, mit dem in einem Ultrazentrifugenlauf bis zu 15 Proben vermessen werden können. Ein weiterer wirtschaftlicher Vorteil entsteht bereits da, wo das prismatische Zellenmittelstück aus filled epon (R) durch ein planparalleles Zellenmittelstück aus mit KEL-F(R) beschichtetem Aluminium ersetzt wird, da die Haltbarkeit des Zellenmittelstückes aus Trifluorchloräthylenpolymer wesentlich größer ist. Einen weiteren Vorteil bietet die Vereinheitlichung der Zellenmittelstücke. Planparallele Zellenmittelstücke können universell benutzt werden, während prismatische hautpsächlich in der Interferenzoptik Verwendung finden. Spezielle Fensterhalter sind für beide Fälle notwendig.A particular advantage of the device according to the invention is that the cell centerpieces do not have to be prismatic, i.e. they can consist of a material that can only be processed into plane-parallel spacers, and the cells can still measure the concentration profile in such cells, even if they are in a rotor with several ultracentrifuge cells. The time saved is very considerable because liquids, which were previously only in rotors with one measuring cell, are now examined together with other measuring cells in a rotor which can accommodate 4 or 6 cells, for example can be. It is particularly advantageous to use a center piece provided with 3 x 2 chambers, with which up to 15 samples can be measured in an ultracentrifuge run. Another economic advantage arises where the prismatic cell centerpiece made of filled epon (R) is replaced by a plane-parallel cell centerpiece made of aluminum coated with KEL-F (R) , since the durability of the cell centerpiece made of trifluorochloroethylene polymer is significantly greater. The standardization of the cell centerpieces offers a further advantage. Plane-parallel cell centerpieces can be used universally, while prismatic cells are mainly used in interference optics. Special window holders are necessary for both cases.
Die Erfindung ist beispielhaft in der Zeichnung dargestellt und im folgenden näher beschrieben. Es zeigen:
- Figur 1 eine Ultrazentrifugenzelle für interferenzoptische Versuche.
Figur 2 ein Sechskanalmittelstück.- Figur 3 einen Ausschnitt aus dem Strahlengang am oberen prismatischen Fenster.
- Figure 1 shows an ultracentrifuge cell for interference optical experiments.
- Figure 2 shows a six-channel centerpiece.
- 3 shows a section of the beam path at the upper prismatic window.
In Figur 1 sind die Einzelteile einer Ultrazentrifugenzelle übereinander gezeichnet, die in dem Zellengehäuse 1 sind.In Figure 1, the individual parts of an ultracentrifuge cell are drawn one above the other, which are in the cell housing 1.
Bei interferenzoptischen Untersuchungen muß das Zellenmittelstück 2 zweisektoral ausgebildet sein, damit die Strahlen durch Probe und Referenzprobe kohärent sind. Die Form der Kammer 3 im Zellenmittelstück 2 ist senkrecht zur Strahlenrichtung trapezförmig; jedoch weicht die Form nur um wenige Grad von einem Rechteck ab. Die Dicke des Zwischenstücks liegt üblicherweise zwischen 1 und 30 mm. Das Zellenmittelstück 2.ist eine planparallele Scheibe aus Trifluorchlorpolyäthylen in einer Fassung mit 2 Kammern (Kanäle) 3. Die Kammern 3 im Zwischenstück 2 werden oben durch ein Fenster 4 aus Quarzglas und unten durch ein Fenster 5 aus Industriesaphir begrenzt. Zur Abdichtung dienen Zwischenringe 6, 7 aus Kunststoff. In der Figur 1 sind noch weitere Einzelteile der Ultrazentrifugenzelle, wie Fensterfassungen 8, Dichtungen 9, oberer 10 und unterer 11 Fensterhalter, Abstandhalter 12 und vorschraubung 13 dargestellt.In the case of interference-optical investigations, the
Ein planparalleles 6-Kanalzellenmittelstück 2 ist in Figur 2 dargestellt. Jeder der beiden Sektoren ist in 3 Kanäle unterteilt. Der Rauminhalt beträgt ~ 0,2 ml. Das Zellenmittelstück wird in die Zentrifuge so eingebaut, daß die Sektoren radial verlaufen.A plane-parallel 6-channel
Erfindungsgemäß ist vorzugsweise eines der Fenster 4, 5 nicht planparallel sondern prismatisch, wobei die Prismenkante senkrecht auf dem Radiusvektor des Rotors zu den betreffenden Ultrazentrifugenzellenmittelpunkt steht. Extrapoliert man die obere und untere Fensterfläche bis zur Schnittlinie, so beträgt der Winkel an der Prismenkante weniger als 1 Grad. Mit 2 Sorten prismatischer Fenster beispielsweise von 0,5° und 10 und mit planparallelen Fenstern kann man bereits 5 verschiedene Zellen aufbauen, so daß sich 5 in der Beobachtungsebene getrennte Beobachtungsfelder ergeben. Die Untersuchungszeit beträgt nur noch ein Fünftel.According to the invention, one of the
Es besteht daneben aber grundsätzlich die Möglichkeit weiter, statt der 2-Sektor-Mittelstücke auch beispielsweise 6-Kanal-Zellenmittelstücke einzubauen. 6-Kanalzellen aus Kel-F (R) mit planparallelem Mittelstück sind bekannt. Die Meßkapazität wird durch Verwendung von 6-Kanalzellen bei einem Rotor, der mehrere Ultrazentrifugenzellen aufnehmen kann, noch einmal um einen Faktor 3 erhöht.In addition, there is always the option of installing 6-channel cell centerpieces instead of the 2-sector centerpieces. 6-channel cells made of Kel-F (R) with a plane-parallel center piece are known. The measuring capacity is increased again by a factor of 3 by using 6-channel cells in a rotor that can accommodate several ultracentrifuge cells.
In Figur 3 ist der Strahlengang im Bereich des oberen Fensters schematisch dargestellt. Das Mittelstück 2 ist planparallel und besteht bevorzugt aus mit Trifluorchlorpolyäthylen-beschichtetem Aluminium. Das prismatisch ausgebildete obere Fenster 4 aus Quarzglas ist übertrieben stark geneigt. Der obere Fensterhalter 10 muß an das prismatische Fenster angepaßt sein. Die Rotorachse der Ultrazentrifuqe liegt in der Zeichenebene parallel zur Führungsnut 14.The beam path in the region of the upper window is shown schematically in FIG. The
Claims (1)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19772726920 DE2726920A1 (en) | 1977-06-15 | 1977-06-15 | ULTRACENTRIFUGAL CELL |
DE2726920 | 1977-06-15 |
Publications (1)
Publication Number | Publication Date |
---|---|
EP0000122A1 true EP0000122A1 (en) | 1979-01-10 |
Family
ID=6011554
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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EP78100101A Withdrawn EP0000122A1 (en) | 1977-06-15 | 1978-06-06 | Cell for ultracentrifuge in interferometric optical analyses |
Country Status (2)
Country | Link |
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EP (1) | EP0000122A1 (en) |
DE (1) | DE2726920A1 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3833974A1 (en) * | 1988-10-06 | 1990-04-12 | Bayer Ag | ULTRACENTRIFUGE FOR DETERMINING PARTICLE SIZE DISTRIBUTIONS |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3391597A (en) * | 1956-03-14 | 1968-07-09 | Beckman Instruments Inc | Centrifuge apparatus having a two sector sample holder |
US3778171A (en) * | 1972-11-09 | 1973-12-11 | Beckman Instruments Inc | Sample cell for ultracentrifuge utilizing-multiple-beam interference optics |
US3937581A (en) * | 1973-05-17 | 1976-02-10 | Heraeus-Christ Gmbh | Analytic cell for use in high-speed ultra centrifuges |
-
1977
- 1977-06-15 DE DE19772726920 patent/DE2726920A1/en active Pending
-
1978
- 1978-06-06 EP EP78100101A patent/EP0000122A1/en not_active Withdrawn
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3391597A (en) * | 1956-03-14 | 1968-07-09 | Beckman Instruments Inc | Centrifuge apparatus having a two sector sample holder |
US3778171A (en) * | 1972-11-09 | 1973-12-11 | Beckman Instruments Inc | Sample cell for ultracentrifuge utilizing-multiple-beam interference optics |
US3937581A (en) * | 1973-05-17 | 1976-02-10 | Heraeus-Christ Gmbh | Analytic cell for use in high-speed ultra centrifuges |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3833974A1 (en) * | 1988-10-06 | 1990-04-12 | Bayer Ag | ULTRACENTRIFUGE FOR DETERMINING PARTICLE SIZE DISTRIBUTIONS |
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Publication number | Publication date |
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DE2726920A1 (en) | 1978-12-21 |
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