Source: http://www.google.com/patents/US6393898?ie=ISO-8859-1&dq=%E2%80%9Cconfiguration+using+structure+and+rules+to+provide+a+user+interface.%E2%80%9D
Timestamp: 2014-12-25 07:28:08
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Patent US6393898 - High throughput viscometer and method of using same - Google PatentsSearch Images Maps Play YouTube News Gmail Drive More »Sign inAdvanced Patent SearchPatentsAn apparatus and method for measuring viscosity or related properties of fluid samples in parallel is disclosed. The apparatus includes a plurality of tubes and reservoirs in fluid communication with the tubes. The tubes provide flow paths for the fluid samples, which are initially contained within the...http://www.google.com/patents/US6393898?utm_source=gb-gplus-sharePatent US6393898 - High throughput viscometer and method of using sameAdvanced Patent SearchPublication numberUS6393898 B1Publication typeGrantApplication numberUS 09/578,997Publication dateMay 28, 2002Filing dateMay 25, 2000Priority dateMay 25, 2000Fee statusLapsedAlso published asUS6732574, US20020148282, US20040211247Publication number09578997, 578997, US 6393898 B1, US 6393898B1, US-B1-6393898, US6393898 B1, US6393898B1InventorsDamian Hajduk, Paul ManskyOriginal AssigneeSymyx Technologies, Inc.Export CitationBiBTeX, EndNote, RefManPatent Citations (115), Non-Patent Citations (40), Referenced by (31), Classifications (6), Legal Events (9) External Links: USPTO, USPTO Assignment, EspacenetHigh throughput viscometer and method of using sameUS 6393898 B1Abstract An apparatus and method for measuring viscosity or related properties of fluid samples in parallel is disclosed. The apparatus includes a plurality of tubes and reservoirs in fluid communication with the tubes. The tubes provide flow paths for the fluid samples, which are initially contained within the reservoirs. The apparatus also includes a mechanism for filling the reservoirs with the fluid samples, and a device for determining volumetric flow rates of fluid samples flowing from the reservoirs through the plurality of tubes simultaneously. The disclosed apparatus is capable of measuring viscosity or related properties of at least five fluid samples simultaneously. Useful reservoirs and tubes include syringes.
What is claimed is: 1. An apparatus for measuring viscosity or related properties of fluid samples in parallel, the apparatus comprising:
a frame; a plurality of tubes, each having a first end and second end, providing flow paths for the fluid samples, each of the tubes having a predefined length terminating at the first end with a tip adapted for aspirating a sample from a sample holder and a substantially uniform inner diameter over at least a portion of the pre-defined length; a plurality of reservoirs each in fluid communication with one of the plurality of tubes, and being connected therewith via a hub; an assembly attached to the frame adapted for receiving said tubes and securing them in place relative to the frame; a mechanism adapted for filling the reservoirs with the fluid samples; and a device adapted for determining volumetric flow rates of fluid samples flowing from the reservoirs and through the plurality of tubes simultaneously; wherein the apparatus is capable of measuring viscosity of related properties of at least five fluid samples simultaneously. 2. The apparatus of claim 1, wherein the mechanism for filling the reservoirs is a vacuum source in fluid communication with the reservoirs.
24. The apparatus of claim 23, wherein the preloaded block includes an 8�12 array of throughholes.
a three axis robot having at least one arm and at least one tip on the at least one arm; a tube providing a flow path for the plurality of fluid samples, the tube having a predefined length and a substantially uniform inner diameter over at least a portion of the pre-defined length; a syringe barrel defining a reservoir for receiving the fluid samples, the reservoir in fluid communication with the tube, the barrel and the tube attached to the at least one tip of the robot and the barrel including a vent hole providing fluid communication between the reservoir and the atmosphere outside the barrel; a plunger disposed within the barrel for aspirating the plurality of fluid samples into the reservoir, the plunger aspirating each the plurality of samples into the reservoir until the plunger passes the vent hole, which then allows each of the plurality of samples to flow out of the reservoir; and an upstream detector and a downstream detector for detecting the plurality of samples as the plurality of samples flows out of the reservoir such that a volumetric flow rate of each of the plurality of fluid samples can be determined; wherein the apparatus is capable of measuring the viscosity or related properties of the plurality of fluid samples by relating the volumetric flow rate of each of the plurality of samples to the viscosity or related properties as the robot moves the tube from sample to sample to aspirate each of the plurality of samples followed by allowing each of the plurality of samples to flow out of the reservoir. 29. An apparatus for measuring viscosity or related properties of a at least four fluid samples, the apparatus comprising;
a three axis robot having at least one arm and at least two tips on the at least one arm; at least two tubes providing a at least two flow paths for the at least four fluid samples, the at least two tubes having a predefined length and a substantially uniform inner diameter over at least a portion of the pre-defined length; at least two syringe barrels defining at least two reservoirs for receiving the at least four fluid samples, the at least two reservoirs in fluid communication with the at least two tubes, the at least two barrels and the at least two tubes attached to the at least two tips of the robot and the at least two barrels including at least two vent holes for providing fluid communication between the at least two reservoirs and the atmosphere outside the at least two barrels; at least two plungers disposed within the at least two barrels for aspirating the at least four fluid samples into the at least two reservoirs, the at least two plungers aspirating the at least four samples into the at least two reservoirs until the at least two plungers pass the at least two vent holes, which then allows each of the at least four samples to flow out of the at least two reservoirs; and a plunger plate connect to the at least two plungers, the plunger plate providing uniform translation of the at least two plungers for aspirating the at least four samples an upstream detector and a downstream detector associated with the at least two reservoirs for detecting the at least four samples as the at least four samples flow out of the at least two reservoirs such that a volumetric flow rate of each of the at least four samples can be determined; wherein the apparatus is capable of measuring the viscosity or related properties of the at least four fluid samples by relating the volumetric flow rate of each of the at least four samples to the viscosity or related properties as the robot moves the at least two tubes from sample to sample to aspirate each of the at least four samples followed by allowing each of the at least four samples to flow out of the reservoir. 30. A method of screening fluid samples comprising:
providing a plurality of fluid samples to a plurality of wells; providing a plurality of reservoirs in fluid communication with the plurality of fluid samples, the reservoirs defined by a plurality of barrels, the barrels attached to a plurality of capillary tubes via a plurality of hubs; aspirating the plurality of fluid samples into the plurality of reservoirs using vacuum pressure to induce flow of the plurality of samples through the plurality of capillary tubes and through the plurality of hubs; allowing the plurality of fluid samples to flow from the reservoirs through the plurality of tubes, the tubes having known diameter and length, the tubes secured in place by an assembly that is adapted to receive the tubes, the assembly being attached to a frame; and detecting the volumetric flow rates of the plurality of fluid samples through each of the tubes simultaneously; and relating the volumetric flow rates to a rheological property of the plurality of fluid samples. 31. The method of claim 30, wherein providing fluid samples to the plurality of reservoirs comprises aspirating the fluid samples into the reservoirs.
a three axis robot having at least one arm and at least one tip on said at least one arm; a tube providing a flow path for the plurality of fluid samples, the tube having a predefined length and a substantially uniform inner diameter over at least a portion of the pre-defined length; a reservoir for containing the fluid samples, the reservoir in fluid communication with the tube via a hub and said reservoir attached to said at least one tip of said robot; an array of fluid samples from wells of a substrate housing; a mechanism for aspirating the plurality of fluid samples into the reservoir from the array of fluid samples; and a pair of detectors for determining volumetric flow rates of the plurality of fluid samples flowing from the reservoir and through the tube, the pair of detectors determining the volumetric flow rates by detecting the plurality of fluid samples at the plurality of samples flow out of the reservoir after aspiration; wherein the 3 axis robot arm is adapted for translation between the wells of the substrate for measuring viscosity or related properties of the plurality of fluid samples by said robot moving said tube from sample to sample in the array of samples. 40. The apparatus of claim 29, wherein said robot comprises at least 2 tips with a reservoir attached to each of said at least 2 tips.
an array of syringes, each of the syringes comprising a barrel for containing the fluid samples, a plunger located within the barrel for aspirating the fluid samples into the barrel, and a hypodermic needle in fluid communication with the barrel, the hypodermic needle providing a flow path for the fluid samples and having a substantially uniform inner diameter over a majority of its length; and upstream and downstream detector arrays located along the barrel of each syringe for monitoring volumetric flow rates of the fluid samples through each hypodermic needle simultaneously; wherein the apparatus is capable of measuring viscosity or related properties of at least five fluid samples simultaneously. 48. The apparatus of claim 47, further comprising a plunger plate attached to each plunger, the plunger plate providing uniform translation of each plunger in a direction parallel to its longitudinal axis.
Combinatorial chemistry generally refers to methods and materials for creating collections of diverse materials or compounds�commonly known as libraries�and to techniques and instruments for evaluating or screening libraries for desirable properties. Combinatorial chemistry has revolutionized the process of drug discovery, and has enabled researchers to rapidly discover and optimize useful materials.
SUMMARY OF THE INVENTION The present invention provides an apparatus for measuring viscosity or related properties of fluid samples in parallel. In some embodiments, the apparatus includes a plurality of tubes and reservoirs in fluid communication with the tubes. Each of the tubes has a predetermined length and a uniform inner diameter over at least a portion of the tube's length. In addition, the tubes provide flow paths for the fluid samples, which are initially contained within the reservoirs. The apparatus also includes a mechanism for filling the reservoirs with the fluid samples, and a device for determining volumetric flow rates of fluid samples flowing from the reservoirs through the plurality of tubes simultaneously. The disclosed apparatus is capable of measuring viscosity or related properties of at least five fluid samples simultaneously.
BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a perspective front view of a parallel viscometer.
FIG. 18 shows a plot of relative viscosity�1 versus concentration of polyisobutylene in hexane for six narrow molecular weight distribution polyisobutylene standards.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Overview of Parallel Viscometer
A parallel viscometer made in accordance with the present invention generally includes two or more tubes. The tubes can be constructed of any material, but stainless steel is particularly useful because of its mechanical strength, high thermal conductivity, and excellent dimensional stability and control. Each of the tubes has a substantially uniform inner diameter, d, over at least a portion of its length, l, which defines a viscosity measurement region. Typically, this region is the same for each of the tubes and coincides with their total lengths, but one can vary the inner diameter and length of individual tubes to account for differences in sample viscosity. In addition, the inner diameter of the tubes may assume any value as long as the Reynolds Number, R, which provides a measure of inertial forces to viscous forces within a liquid sample is less than about 103�i.e., liquid flow within the tubes is laminar. From a practical standpoint, d and l are usually minimized to allow viscosity measurements using as little of the samples as possible. This is often the case when screening combinatorial libraries because the amount of any particular sample or library member can be as small as about 102 μl.
Generally, the parallel viscometer also includes a device for monitoring the volumetric flow rate, Q, of the samples flowing through the tubes. As described below, once the volumetric flow rate is known, one may calculate the viscosity of the samples from the Hagen-Poiseulle equation, which relates fluid viscosity to the volumetric flow rate and the pressure drop, ΔP, across the viscosity measurement region of an individual tube. For gravity-driven flows, the pressure drop comprises the product of the sample density, the gravitational acceleration, and the length of the viscosity measurement region. When gravity is insufficient to induce flow�i.e., when sample viscosity or capillary forces are large�the parallel viscometer includes a mechanism for applying and monitoring a force (pressure) that drives the liquid samples through the tubes. Typically, the parallel viscometer employs rams or pistons within the reservoirs to drive the fluid samples through the tubes.
FIG. 10 and FIG. 11 show top and cross sectional views, respectively, of the preload block 252. The preload block 252, like the Luer hub capture plate 250, is typically fabricated from a rigid material such as aluminum. The preload block 252 includes through-holes 300 that extend from an upper surface 302 of the block 252 to a lower surface 304 of the block 252. The through-holes 300 are arrayed on nine-mm center�corresponding to the well spacing of a standard ninety-six well microtiter plate�and include counter bores 306 that extend from the upper surface 302 part way into the preload block 252. The preload block 252 includes a second group of through-holes 310 for aligning the preload block 252 and the Luer-hub capture plate 250, and a third group of through-holes 312 for attaching the preload block 252 to the Luer hub capture plate 250.
As noted in the description of FIG. 1, the upstream 136 and downstream 138 detector arrays monitor the volumetric flow rate of fluid samples. The detector arrays 136, 138 measure the time necessary for a liquid meniscus within the syringe barrel 112 to travel between the detector arrays 136, 138, which can be accomplished by noting changes in voltages generated by the detector arrays 136, 138 in response to fluid characteristics. For example, in the absence of liquid in the barrel 112, infrared light from the emitter 390 exits the second aperture 394 of the detector block module 370, travels through the syringe barrel 112, enters the first aperture 392, and strikes the infrared detector 388. This results in a voltage, VS, at the output of the detector 388. When the boundary between the fluid sample and air within the syringe barrel 112 passes the detector array element 386, VS changes relative to some reference voltage, VREF. If the fluid sample is substantially transparent to infrared light, the change is brief and results from disruption of the infrared light beam by the sample meniscus. If, however, the fluid sample is opaque, VS exhibits a step change�an increase or decrease relative to VREF�upon passage of the meniscus depending on the electrical response of the detector 388 to an increase in light level.
Although one can detect the transition in VS directly, the viscometer 100 typically employs either a standard comparator circuit or a Schmitt trigger circuit to detect a rise (or fall) in VS. With a standard comparator, the comparator output, VO, saturates at VCC for VS greater than VREF and saturates at −VEE for VS less than VREF. Thus, when using the standard comparator, the momentary drop in VS results in a sharp decrease in VO from VCC to −VEE and a sharp increase in VO from −VEE to VCC as the meniscus passes the detector array element 386. The standard comparator usually works well unless VS is �noisy.� Sources of noise include gas occlusions, voids, and other impurities in the fluid sample, which can perturb the IR light and result in spurious beam interruptions.
The Schmitt trigger circuit can detect the transition even for �noisy� VS. It uses a comparator whose reference voltage, VREF, is derived from a voltage divider across the output (i.e., positive feedback). VREF changes when the output switches state: VREF=βVCC for VO>0 and −βVEE for VO<0, where β is called the feedback factor and is a positive number less than unity. Thus, when VS rises through VREF=βVCC, VO is at VCC and switches to −VEE, and when VS falls through VREF=−βVEE, VO is at −VEE and switches to VCC. As a result, the Schmitt trigger will not respond to input noise having a magnitude less than the differences between the two threshold voltages, VN<β(VCC+VEE). Note that one may implement the standard comparator and Schmitt trigger circuits in hardware or software.
As noted in the overview section, one can calculate viscosity, η, from the volumetric flow rate, Q. of samples flowing through the capillary tubes 114 using the Hagen-Poiseulle equation: Q = π   d 4  Δ   P 128   l   η I where d and l are the inner diameter and length of the capillary tube 114, and ΔP is the pressure drop across l. For gravity-driven flows, the pressure drop is the product of the fluid sample density, the gravitational acceleration, and l. Q can be calculated from the expression: Q = π   D 2  L / 4 Δ   t II where D is the inner diameter of the syringe barrel 112, L is the distance between the upstream 136 and downstream 138 detector arrays and At is the measured drop time.
η/ηS=1+C[η] III In equation III, [η] is the intrinsic viscosity, which exhibits a power-law dependence on polymer molecular weight given by the Mark-Houwink-Sakurada (MHS) relation,
[η]=[ηO ]M a IV where the constants [ηO] and α depend on the polymer, solvent, and temperature. Correction factors are available in the literature for solutions containing a distribution of polymer molecular weights.
If the concentration of the polymer solution is initially unknown, both the molecular weight and the concentration can be estimated by measuring the ratio of drop times in two different solvents. The first solvent is a good solvent for the polymer, and typically has a constant α of 0.7 or greater. The second solvent is a marginal solvent for the polymer, and is usually prepared by adding a known amount of a poor solvent to the first solvent. Ordinarily, one should maximize the difference in a between the first (good) and second (marginal) solvents by adding as much of the poor solvent as possible to the first solvent without causing the polymer to precipitate. In such cases, the marginal solvent typically has an α of about 0.5. If we then define μ=η/ηS−1, where η/ηS is the ratio of drop times as described above, then μ 1 μ 2 = C 1  [ η 1 ] C 2  [ η 2 ] = ( C 1 C 2 )  ( η O , 1 η O , 1 )  M α1 - α2 V where subscripts 1 and 2 denote measurements of polymer solutions made using the first and second solvents, respectively, and the second solvent is prepared by adding a known amount of a poor solvent to the first solvent.
Example 1 Variation in Drop Time Between Syringes
A parallel viscometer similar to the apparatus depicted in FIG. 1 was used to measure drop time, Δt, for tetrahydrofuran (THF) samples at 20� C. The drop time was measured for ninety-six samples simultaneously, and was repeated four times for each sample. FIG. 16 plots drop time (in seconds) versus sample number (1-4) that were obtained for three different syringes (channels 3, 4 and 5). Although some variation exists between syringes (channels), drop time measurements for individual channels are highly repeatable.
Example 2 Single Channel (Syringe) Reproducibility
The parallel viscometer of Example 1 was used to measure drop time for toluene samples at 20� C. The drop time was measured for a series of twenty-three samples using a single syringe (channel) having a 20-gauge hypodermic needle. FIG. 17 plots drop time (in seconds) versus sample number (1-23) for the single channel. The average drop time for the twenty-three samples was 3.690 s, and the standard deviation was 0.006 seconds. Note that a filter could be used to eliminate disordant data (sample 9, 17).
Example 3 Measurement of Intrinsic Viscosity
The parallel viscometer of Example 1 and 2 was used to determine the intrinsic viscosities of a set of commercially available polyisobutylene standards at concentrations in hexane from 1 to 20 mg/ml at 25� C. The molecular weights of these materials as reported by the supplier (Polymer Standards Service USA, Silver Springs, Md.) appear in Table 1. FIG. 18 shows Δt/ΔtS−1 or η/ηS−1 versus polyisobutylene concentration, where Δt and ΔtS are the drop times for the polymer solution and for pure hexane, respectively, and where the ratio η/ηS is the relative viscosity. Each data point represents an average of at least five measurements. A linear least-squares fit each of these curves yields the intrinsic viscosity, [η], for each standard of differing molecular weight. These data are summarized in Table 1 and plotted in FIG. 19. The resulting power law relation, [η]�M0.611, indicates that hexane is a reasonable (though not good ) solvent for this polymer.
�103 2470
134000 117000 89.0
1110000 862000 201
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