U.S. patent application number 14/044472 was filed with the patent office on 2014-04-10 for apparatuses and methods for wireless monitoring and control of environmental sampling and chromatographic apparatuses.
This patent application is currently assigned to Teledyne Instruments, Inc.. The applicant listed for this patent is Teledyne Instruments, Inc.. Invention is credited to Jon L. Curran, Dale A. Davison, Daniel G. Jameson, Dale L. Meyer, Ruth A. Pipes, Jack E. Silver.
Application Number | 20140096597 14/044472 |
Document ID | / |
Family ID | 39666741 |
Filed Date | 2014-04-10 |
United States Patent
Application |
20140096597 |
Kind Code |
A1 |
Davison; Dale A. ; et
al. |
April 10, 2014 |
Apparatuses and Methods for Wireless Monitoring and Control of
Environmental Sampling and Chromatographic Apparatuses
Abstract
A liquid chromatographic system includes columns, column
mounting fixtures to which the columns are mounted, a detector, a
collector, a controller and a plurality of RFIDs. A first RFID
communicates with the controller and cooperating RFIDs mounted to
other components provide information such as the history of
components, parameters and the like. They also receive information
from sensors relating to the operation of the liquid chromatograph,
store the information and transmit it. Moreover, the RFIDs may
substitute for hard wiring in many applications and may enable a
central computer to control several liquid chromatographic and
environmental sample collectors.
Inventors: |
Davison; Dale A.;
(Greenwood, NE) ; Meyer; Dale L.; (Lincoln,
NE) ; Jameson; Daniel G.; (Roca, NE) ; Silver;
Jack E.; (Lincoln, NE) ; Curran; Jon L.;
(Lincoln, NE) ; Pipes; Ruth A.; (Odell,
NE) |
|
Applicant: |
Name |
City |
State |
Country |
Type |
Teledyne Instruments, Inc. |
Thousand Oaks |
CA |
US |
|
|
Assignee: |
Teledyne Instruments, Inc.
Thousand Oaks
CA
|
Family ID: |
39666741 |
Appl. No.: |
14/044472 |
Filed: |
October 2, 2013 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
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11980024 |
Oct 30, 2007 |
8555709 |
|
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14044472 |
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11699169 |
Jan 29, 2007 |
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11980024 |
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Current U.S.
Class: |
73/61.55 |
Current CPC
Class: |
Y10T 436/2575 20150115;
G01N 30/16 20130101; G01N 2030/0095 20130101; G01N 30/02 20130101;
B01D 15/10 20130101 |
Class at
Publication: |
73/61.55 |
International
Class: |
G01N 30/02 20060101
G01N030/02 |
Claims
1. A portable instrument comprising: at least one chromatographic
column; said at least one chromatographic column having a plurality
of sensors spaced along its length; at least one wireless
communication device on said portable instrument; at least some of
said plurality of sensors being configured to communicate with the
at least one wireless communication device; an input for the
chromatographic column; a readout device coupled to said portable
instrument, said readout device operably connected to said wireless
communication device, wherein readings from the plurality of
sensors may be displayed.
2. A portable instrument in accordance with claim 1 further
including a positioning device configured to provide a location of
an operation of said portable instrument; said positioning system
being able to record a position of said at least one
chromatographic column.
3. A portable instrument in accordance with claim 2 in which said
positioning device is a global positioning system.
4. A portable instrument comprising: a sample collector for
collecting a plurality of liquid samples, said sample collector
configured for receiving a plurality of sizes of containers; at
least one container of said plurality of sizes of containers having
a mounted nonvolatile memory, said mounted nonvolatile memory
configured for receiving and storing information; a wireless
communication device mounted on said at least one container, said
wireless communication device configured to receive an information
signal and transmit said information signal to said mounted
nonvolatile memory; a positioning system mounted within said
portable instrument, said positioning system configured for
receiving a positioning signal and determining a position of said
portable instrument; wherein said sample collector is configured
for receiving said plurality of liquid samples over time;
depositing at least one sample of said plurality of liquid samples
in said at least one container; transmitting said information
signal to said wireless communication device; said information
signal including at least said position of said portable
instrument; and rendering said mounted nonvolatile memory tamper
proof.
5. The portable instrument in accordance with claim 4, wherein said
sample collector is further configured for operation within an
environment comprising a portion of a liquid from which said
plurality of liquid samples is collected, said environment being
external to said sample collector.
6. The portable instrument in accordance with claim 4, wherein said
plurality of sizes of containers further includes at least one size
of test tube container.
7. The portable instrument in accordance with claim 4, wherein said
information signal further includes at least one of: a history of
at least one sample of said plurality of liquid samples and
instructions for processing said at least one sample of said
plurality of liquid samples.
8. The portable instrument in accordance with claim 4, wherein said
positioning system is further configured to receive and interpret
signals from a plurality of global positioning systems.
9. The portable instrument in accordance with claim 4, wherein said
information signal further comprises at least one of: a time said
at least one sample was collected, a customer for which said at
least one sample was collected, a source identification of the at
least one sample and a test step to be performed on said at least
one sample.
Description
RELATED APPLICATIONS
[0001] This application is a continuation application of U.S.
patent application Ser. No. 11/980,024, entitled APPARATUSES AND
METHODS FOR WIRELESS MONITORING AND CONTROL OF ENVIRONMENTAL
SAMPLING AND CHROMATOGRAPHIC APPARATUSES, filed on Oct. 30, 2007,
currently pending, which is a divisional application of U.S.
application Ser. No. 11/699,169 filed Jan. 29, 2007, entitled
APPARATUSES AND METHODS FOR WIRELESS MONITORING AND CONTROL OF
ENVIRONMENTAL SAMPLING AND CHROMATOGRAPHIC APPARATUSES, now
abandoned, by inventors Dale A. Davison, Dale L. Meyer, Daniel G.
Jameson, Jack E. Silver, Jon L. Curran and Ruth A. Pipes, all of
which are hereby incorporated by reference in their entirety.
FIELD OF THE INVENTION
[0002] This invention relates to apparatuses and methods for the
wireless monitoring, identification and control of environmental
and chromatographic apparatuses and synthetic chemistry and more
particularly for control of supplies used by the environmental and
chromatographic apparatuses.
BACKGROUND OF THE INVENTION
[0003] Wireless communication for the purpose of monitoring,
identifying and controlling devices and apparatus are known. For
example RFID devices and Bluetooth devices are in widespread use to
identify devices and transfer information to a receiver.
[0004] One prior art apparatus and method for identifying and
providing information about a chromatographic column to a receiver
is disclosed in U.S. Pat. No. 5,690,893 to Ozawa, et al., U.S. Pat.
No. 6,971,506 to Hassinen and U.S. Pat. No. 6,458,273 to Krakover.
U.S. Pat. No. 5,690,893 discloses a semi-conductor having a
non-volatile memory embedded within it and storing information such
as changes in the specification of the column, mixing ratios of
eluent flow rate, theoretical plates and other information. The
semi-conductor device is used for wireless communication to permit
a data processor to receive the information stored in the
semi-conductor U.S. Pat. No. 6,971,506 and U.S. Pat. No. 6,458,273
disclose a test tube carrier with an RFID tag on test tubes and a
micro titer plate that is bar coded.
[0005] However, prior art wireless identification and communication
techniques have not satisfactorily resolved many of the
identification and communication problems that occur in liquid
chromatography and environmental sampling.
SUMMARY OF THE INVENTION
[0006] Accordingly, it is an object of the invention to provide a
novel wireless multiple fraction instrument and process such as for
example, an instrument for wireless monitoring and control of
environmental sampling apparatuses or chromatographic
apparatuses.
[0007] It is a further object of the invention to provide a system
for permitting chromatographic apparatuses to communicate with
other chromatographic apparatuses.
[0008] It is a still further object of the invention to provide a
system by which environmental apparatuses may communicate with
other environmental apparatuses.
[0009] It is a still further object of the invention to provide a
novel system for recording the past history of a chromatographic
column on the column.
[0010] It is a still further object of the invention to provide a
novel system for the wireless communication of environmental
sampling apparatuses with other apparatuses.
[0011] It is a still further object of the invention to provide a
novel system that enables a central microprocessor to control
components on several chromatographic systems to coordinate or run
them.
[0012] It is a still further object of the invention to provide a
novel system which enables a microprocessor to control components
of several environmental sample collectors.
[0013] It is a still further object of the invention to provide a
novel system for providing to a controller a map or plan indicating
the position of one or more sample containers.
[0014] It is a still further object of the invention to provide a
novel system for indicating the position of an environmental sample
container holder or a chromatographic tube rack or micro titer
plate or the like.
[0015] It is a still further object of the invention to provide a
novel system for indicating information on chromatographic columns
intended to cooperate with both liquid chromatographic systems and
other sample separating systems such as a mass spectrometer or gas
chromatograph.
[0016] It is a still further object of the invention to provide a
novel system for controlling robotic transport arrangements for
moving a column from one separation system such as a liquid
chromatographic system to another such as a mass spectrometer.
[0017] It is a still further object of the invention for providing
a novel system for recording information on columns such as a
calibration curve, retention times, packing, history, lot numbers,
chromatograms, past separation conditions and the like.
[0018] It is a still further object of the invention to provide a
novel system of inventory control in which a wireless communication
system on chromatographic parts such as columns cooperate with a
database recorded in a microprocessor system to provide inventory
control.
[0019] It is a still further object of the invention to provide a
novel system in which reordering is triggered by information
maintained in columns or other chromatographic components or
environmental sampler components which wirelessly cooperate with
databases recorded in a separate microprocessor.
[0020] It is a still further object of the invention to provide a
quality control system in which the precision of characteristics
such as retention times of columns is recorded on the component
such as a column to enable automatic fitting of columns that have
characteristics operating within predetermined ranges to
applications requiring those predetermined ranges.
[0021] It is a still further object of the invention to provide a
novel system for tracing the efficiency of certain chromatographic
columns for pre-selected chemistries and runs or the times of
runs.
[0022] It is a still further object of the invention to provide a
novel system for automating combinatorial research using libraries
of compounds accessed wirelessly by components of the system.
[0023] It is a still further object of the invention to provide a
novel system for use in separation instruments such as
chromatographs for recording data automatically in electronic
notebooks.
[0024] It is a still further object of the invention to provide a
system permitting on-line communication with security between
chromatographic components and a central computer.
[0025] It is a still further object of the invention to provide a
novel communication system for chromatographic and environmental
apparatuses that is compatible with Wi-Fi or Bluetooth.
[0026] It is a still further object of the invention to provide a
novel system for recording the characteristics of columns such as
the column lining, the polar nature of solvents, the types of
chromatography and the like.
[0027] It is a still further object of the invention to provide a
novel system for recording information on chromatographic or
environmental components useful in servicing the environmental or
chromatographic components or identifying the end use or
determining when the components are out of date.
[0028] It is a still further object of the invention to provide a
system that renders chromatographic systems tamper proof in
accordance with Part 11 of the Code of Federal Regulations.
[0029] It is a still further object of the invention to provide a
novel system for recording all information needed to produce a drug
in accordance with Part 9 of the Code of Federal Regulations.
[0030] It is a still further object of the invention to provide a
novel system for transmitting billing information to a central
station.
[0031] It is a still further object of the invention to provide a
novel system for transmitting reliability information to a central
system.
[0032] It is a still further object of the invention to provide
information on columns for aiding and stacking the columns and
avoiding mistakes such as information about proper length and types
of columns for the stack.
[0033] It is a still further object of the invention to provide a
novel column or other container that may sense characteristics such
as temperature, conductivity, pH, pressure and the like with
sensors built into a column and connected to a transmitter.
[0034] It is a still further object of the invention to provide a
novel column, container or reactor that includes a sensor for
sensing physical characteristics of a reactant, feedstock or fluid
mixture and use the sensed characteristics for feedback.
[0035] It is a still further object of the invention to provide a
novel system for identifying columns in a rack by triangulation,
phase or the like.
[0036] It is a still further object of the invention to provide a
novel system for transmitting data from one instrument to
another.
[0037] It is a still further object of the invention to provide a
novel system for recording specific information such as default
conditions to customers or manufacturers.
[0038] It is a still further object of the invention to provide
standard data such as good laboratory practice or good
manufacturing practice on the components being manufactured.
[0039] It is a still further object of the invention to provide
information useful for quality control for sorting columns by grade
or cost or the like on a column.
[0040] It is a still further object of the invention to provide a
novel system for recording steps in manufacturing or testing for
quality control purposes.
[0041] It is a still further object of the invention to provide a
novel system for recording flow rate, pressure, solvent mixture,
pH, conductivity, dissolved oxygen, IQ OQ, PQ and the like on a
component of a separation system or environmental sampling
system.
[0042] It is a still further object of the invention to provide a
novel portable liquid chromatographic system with functions
performed on the column in communication with external devices.
[0043] It is a still further object of the invention to provide
recording-transmitting devices for communication with global
positioning systems to record conditions at certain locations where
a measurement is to be made by an environmental device.
[0044] It is a still further object of the invention to provide a
novel system for tracking values of consumables such as solvent
height in solvent containers in liquid chromatographic systems.
[0045] It is a still further object of the invention to provide
stacking systems such as a scavenger column with separation
columns.
[0046] In accordance with the above and further objects of the
invention, a multiple fraction instrument includes at least one
pumping system, at least one flow path, a flow path mounting
fixture, a container mounting fixture adapted for receiving at
least one container and a controller. The at least one pumping
system has a first wireless communication device and the controller
has a second wireless communication device. There is at least one
other component of the multiple fraction instrument that has a
third wireless communication device. The second wireless
communication device is positioned to communicate wirelessly with
at least the first and third wireless communication devices.
Advantageously, at least one other analytical instrument is
connected to receive a fraction from the flow path.
[0047] In this specification the words, "multiple fraction
instrument or process" means instruments or processes used in
scientific or investigative work such as in the separation sciences
or environment studies that process multiple fractions or samples
or component parts in a manner that requires identification or
control of individual fractions or component parts or samples or
the recall of information about individual ones of the fractions or
component parts or samples. The words "wireless communication
device" means a device that can either receive and/or transmit
information wirelessly and may or may not have a non-volatile
memory for storing information such as data or programs that can be
transmitted, altered or sequenced or received. A wireless
communication device may be either a transmitter, or a reader, a
transceiver or any combination of these. In the preferred
embodiment, they are RFID devices but may be Bluetooth or Wi-Fi or
Zigbee or any other wireless system.
[0048] More specifically, a liquid chromatographic system includes
at least one column, at least one column mounting fixture adapted
for receiving the at least one column, at least one detector
positioned to receive effluent from the at least one column, at
least one controller, and at least one other component of a liquid
chromatographic system. The at least one column has a first
wireless communication device and at least one other component of a
liquid chromatographic system has a second wireless communication
device. The at least one controller has a third wireless
communication device connected to communicate with the at least one
controller and at least one of the first, second and third wireless
communication devices is positioned to communicate with at least
another of first, second and third wireless communication devices.
There is at least one detector connected to a fourth wireless
communication device and positioned to receive effluent from the
column.
[0049] The fourth wireless communication device transmits
information about detected species to the third wireless
communication device. Moreover, a fraction collector and at least
one collection vessel rack is positioned to receive effluent from
the at least one detector and includes a fifth wireless
communication device in communication with the fraction collector
and at least a sixth wireless communication device in communication
with one of the third and the fifth wireless communication devices.
A personal computer has a wireless communication device that
communicates with a wireless communication device on the at least
one controller. The personal computer has an electronic notebook in
memory and records customized data therein.
[0050] In the operation of the liquid chromatograph, data
representing a chromatographic curve for a chromatographic column
is recorded in a first wireless communication device attached to
the chromatographic column. This curve is read when the
chromatographic column is inserted into a column mounting fixture
on a liquid chromatographic system. The data representing a
chromatogram is received on a second wireless communication device
communicating with a controller for the liquid chromatographic
system. Data representing the sequence of solvent conditions for
the chromatographic curve is transmitted from the second wireless
communication device to a third wireless communication device
communicating with a pumping system within the liquid
chromatographic system. The data is used to pump the solvents to
the chromatographic column in accordance with the sequence of
solvent conditions transmitted to the third wireless communication
device.
[0051] Data is wirelessly transmitted to the second wireless
communication device from a fourth wireless communication device
communicating with at least one detector positioned to receive
effluent from the chromatographic column and data is transmitted
from the second wireless communication device to a readout device
to indicate peaks detected by the at least one detector and to a
fraction collector to activate collection of bands. In another
embodiment, there is a controller having a gradient program stored
within it and a first wireless communication device electrically
connected to and communicating with the controller to transmit
information to a pumping system. The pumping system in a preferred
embodiment includes at least two syringe pumps and at least two
sources of liquid. The pumps may include at least one wireless
communication device which receives data from a wireless
communication device on the controller to control pumping rates. In
the alternative, the chromatographic system may include at least
one time proportioning electronically controllable liquid gradient
switching valve and a second wireless communication device
communicating with the at least one time proportioning
electronically controllable liquid gradient switching valve.
[0052] The switching valve is connected to switch liquid flow from
one or the other of the at least two sources of liquid to an inlet
of at least one of the at least two syringe pumps. The first and
second wireless communication devices are wired to transmit
switching times of the at least one time proportioning
electronically controllable liquid gradient switching valve to form
gradient stored in the controller. One of the at least two syringe
pumps is used for each one of multiple channels. Each of the at
least two syringe pumps has a displacement of at least five
milliliters and one of the at least two syringe pumps has a
discharge outlet connected to a sample injection device and thence
to a chromatographic column. The at least one wireless
communication device includes a memory. The memory has data
recorded in it representing a starting concentration of a solvent
whereby the chromatographic system may separate a preselected
component of a sample with the starting concentration of the
solvent. The memory has data recorded in it representing a
chromatographic curve with a starting concentration for purifying
the preselected component of a sample and an ending point.
[0053] The instrument array may include a plurality of multiple
fraction instruments, a general control system and at least some of
a plurality of multiple fraction instruments. The multiple fraction
instruments may include a corresponding one of a plurality of first
wireless communication devices, the general control system includes
a second wireless communication device and an input device for
programming the computer. The second wireless communication device
is positioned to communicate selectively or simultaneously with at
least one of the plurality of the first wireless communication
devices whereby the general control system may coordinate any of
the plurality of multiple fraction instruments.
[0054] Advantageously, at least some of said multiple fraction
instruments are liquid chromatographs and some are other types of
instruments. The liquid chromatographs include columns having
corresponding third wireless communication devices in communication
with them. The third wireless communication devices include a
nonvolatile memory having data indicating that the fractions
collected are to be applied to other analytical instruments and
instructions for the operations to be performed by the other
analytical instruments. The other analytical instruments may be
mass spectrometers for example.
[0055] Wireless communication devices connected to containers
receiving fractions from the liquid chromatographs may include a
nonvolatile memory having data indicating that the fractions
collected are to be applied to other analytical instruments and
instructions for the operations to be performed by the other
analytical instruments. The other analytical instrument may be a
mass spectrometer or any other instrument useful in further
purifying or analyzing the output from the liquid
chromatographs.
[0056] A chemical processor includes at least one reaction station
having a reaction time controller, a controllable pipette or pump,
a reactant vessel and a receptacle conveyor. The at least one
reaction station includes at least a first wireless communication
device and a plurality of receptacles. Each of the plurality of
receptacles is connected to communicate with and is attached to one
of a corresponding second wireless communication device. There is
at least one analytical instrument that is connected to and
communicates with a third wireless communication device and at
least one transfer console for transferring materials from a
receptacle to the at least one analytical instrument. At least some
of the first, second and third wireless communication devices have
a nonvolatile memory with data indicating at least one of the
history of materials in the receptacle and instructions for
processing the materials in the receptacle. The nonvolatile memory
includes data indicating both the history of the materials in the
receptacle and instructions for processing the materials in the
receptacle.
[0057] In operation, a receptacle containing a material to be
processed is moved to at least one reaction station where at least
one of the steps of adding a reagent to the receptacle, heating the
receptacle, delaying further action for a reaction time and
agitating the material in the receptacle is performed. The
materials and steps performed on the materials are recorded in a
wireless communication device attached to the receptacle and
processing instructions are recorded on the receptacle. The
material is transferred to a second receptacle and the processing
steps and materials are recorded on the second receptacle in a
wireless device The materials are moved to an analytical instrument
and a product of reaction may be separated into a third receptacle.
The history of the process and the materials may be recorded on the
third receptacle The steps and materials may be automatically
logged into an electronic notebook.
[0058] A chromatographic column includes an inlet end having an
inlet port, an outlet end having an outlet port, tubular side walls
between the inlet end and the outlet end, at least one wireless
communication device on at least one or more of the inlet end,
outlet end or tubular side walls. The at least one wireless
communication device may include a nonvolatile memory having data
recorded on it and the data may include a precision of the column
from run to run, data indicating a make and model of the column, a
date of manufacture and a lot number of the column.
[0059] Another embodiment of chromatographic column includes an
inlet end having an inlet port, an outlet end having an outlet
port, tubular side walls between the inlet end and the outlet end,
a sensor, at least one wireless communication device on at least
one of the inlet end, outlet end and tubular side walls. The sensor
communicates with one of a column and an environment near a column
part and contents of the column and communicates with the at least
one wireless communication device. The sensor and at least one
wireless communication device includes a plurality of sensors each
of which communicates with a corresponding one of a plurality of
wireless communication devices. One of the plurality of sensors
senses temperature and one of the plurality of sensors senses
pH.
[0060] A chromatographic system includes at least one
chromatographic column arrangement having a first column and a
second column. The outlet of the first column communicates with the
inlet port of the second column. There is at least one wireless
communication device on at least one of the first column inlet end,
first column outlet end and first column tubular side walls and at
least one wireless communication device on at least one of the
second column inlet end, second column outlet end and second column
tubular side walls. The at least one wireless communication device
on the first column includes a nonvolatile memory and the at least
one wireless communication device on the second column includes a
nonvolatile memory. With this arrangement, communication between
the wireless communications devices may indicate to the controller
an error in stacking the columns. Thus, an indication may be given
to the user indicating a connection between the first and second
columns is improper.
[0061] To control the inventory of component parts of a
chromatographic system, a part of the chromatographic system
includes a wireless communication device. Data is recorded on the
wireless communication device indicating the number of parts of the
chromatographic system that are available and data indicating the
date of manufacture of the part. The date of manufacture of the
part is periodically checked to reduce overall shelf time.
Moreover, the inventory may be controlled by manufacturing the
parts of the chromatographic system with a wireless communication
device on them and recording a calibration curve in the wireless
communication device so that the inventory may be broken down by
quality and use of the parts. Moreover, the nonvolatile memory has
data recorded on it and the data includes a precision of the column
from run to run, data indicating the make and model of the column
and a date of manufacture. This data may aid in controlling the
selection of columns to be removed from inventory and where they
should be shipped.
[0062] A chromatographic control system includes a plurality of
component parts of the liquid chromatographic control system with
at least one of the plurality of component parts having a selected
characteristic recorded on a tag associated with the one component
part. The tag is capable of transmitting information to a
microprocessor. The microprocessor includes a memory containing a
data base and the tag includes indicia that may be transmitted to
the microprocessor. The microprocessor includes a receiver means
for receiving the transmitted information and entering the
information into the data base indicating a number of component
parts having the selected characteristic. The data base may include
an inventory target number recorded into it and multiple
instruments.
[0063] One embodiment of an instrument management system includes a
plurality of multiple fraction instruments and a general control
system. At least some of the plurality of multiple fraction
instruments includes a corresponding one of a plurality of first
wireless communication devices. The general control system includes
a second wireless communication device and a memory containing a
data base. The data base includes data useful in managing a usage
of at least some types of component parts of the plurality of the
multiple fraction instruments. The data base includes data
indicating a number of at least some types of component parts in
the plurality of multiple fraction instruments, an average rate of
usage of the types of components parts and a manufacturer's
inventory of the type of component parts. The data base may include
a model number, a price, and a source of a type of part whereby
comparisons are made as to reliability of the type of part by
manufacturer and make of the part. The database may include a rate
of usage by individual customers whereby customers' needs can be
forecast and used for management purposes to determine an inventory
of the component parts needed and target inventory minimum and
maximum and an actual number of the component parts on hand. The
system provides an alert signal when either is exceeded.
[0064] In managing instrument systems, data may be transmitted from
each of a plurality of multiple fraction instruments useful in
managing usage of at least some types of component parts of the
plurality of multiple fraction instruments to a wireless
communication device connected to and in communication with a
general control system. The communication may be from a plurality
of wireless communication devices connected to and in communication
with a corresponding one of the plurality of multiple fraction
instruments. The data that is useful in managing the usage of at
least some types of component parts of the plurality of multiple
fraction instruments may be recorded in a data base within a memory
of the general control system and the useful data may be used in
managing the usage of at least some types of component parts of the
plurality of multiple fraction instruments. The data base may
include data indicating a number of at least some types of
component parts in the plurality of multiple fraction instruments
and an average rate of usage of the types of component parts and a
manufacturer's inventory of the type of component parts.
[0065] For management purposes, the data base may include: (1) a
model number, a price and a source of a type of part whereby
comparisons are made as to reliability of the type of part by
manufacturer; (2) the make and model number of the part; and (3)
the rate of usage of components by individual customers whereby
customer's needs can be forecast and used for management purposes.
The rate of usage of components may be used to determine an
inventory of the component parts needed. The data base may include
target inventory minimum and maximum and an actual number of the
component parts on hand. For example, the system provides an alert
signal when either is exceeded. The data base may include new
purchases by customers and increases and charges in materials,
parts and processes to predict increases and decreases in purchases
of the materials and parts using the information in the
database.
[0066] A fraction collection system includes at least one container
holder, a main frame and a microprocessor mounted to the main
frame. The main frame includes a liquid receiving means adapted to
be connected to communicate with a fluid outlet from a detector and
is shaped and sized to receive at least one container holder in a
container holder bed.
[0067] There is at least one distributor means in the fraction
collector for moving a distributor outlet from container to
container and communicating with the liquid receiving means,
whereby fractions may be deposited in containers. The
microprocessor communicates with a first wireless communication
device and at least one container holder communicates with a second
wireless communication device. The container holder bed includes a
third wireless communication device and the second and third
wireless communication devices transmit a signal to the third
wireless communication device when the at least one container
holder is positioned with respect to the at least one distributor
means to receive liquid. The second wireless communication device
includes a nonvolatile memory and the nonvolatile memory includes
data identifying characteristics of the at least one container
holder. The third wireless communication device includes a
nonvolatile memory containing data identifying characteristics of
the at least one container holder, wherein a signal may be sent to
the first wireless communication device when data stored in the
nonvolatile memories of the second and third wireless communication
device matches.
[0068] The second wireless communication device identifies an end
use to be made of the at least one container holder. A valve that
is automatically switchable to direct liquid to either the at least
one distributor means or to waste communicates with a fourth
wireless communication device wherein the first wireless
communication device transmits a signal to the fourth wireless
communication device to switch the liquid from flowing to the at
least one distributor means or flowing into waste when a peak is
over.
[0069] The fraction collection system may also include at least one
container holder, a main frame and a microprocessor mounted to the
main frame. The main frame includes a liquid receiving means
adapted to be connected to communicate with a fluid outlet from a
detector and is shaped and sized to receive the at least one
container holder in a container holder bed. There is at least one
distributor means for moving a distributor outlet from container to
container and communicating with the liquid receiving means,
whereby fractions may be deposited in containers. The
microprocessor communicates with a first wireless communication
device. There is at least one container in the container holder and
the at least one container holder communicates with a second
wireless communication device. The container holder bed includes a
third wireless communication device and the second and third
wireless communication devices transmits a signal to the third
wireless communication device when the at least one container
holder is positioned with respect to the at least one distributor
means to receive liquid.
[0070] To collect fractions, an identification of at least one
container holder is sent when the at least one container holder is
in position to receive liquid from a distributor of a fraction
collector to a controller. Liquid is inserted into containers in
the at least one container holder upon receiving the identification
of the at least one container holder in position to receive the
liquid and insertion is inhibited when the at least one container
holder is not in the proper position. The second wireless
communication device identifies characteristics of the at least one
container holder. The third wireless communication device supplies
data identifying characteristics of the at least one container
holder, wherein a signal may be sent to a first wireless
communication device when data stored in nonvolatile memories of
the second and third wireless communication device matches.
[0071] The third wireless communication device supplies data
identifying an end use of the at least one container holder. The at
least one container holder may be used in another instrument as
indicated by data recorded on the at least one container holder.
The wireless communication device associated with a rack, or micro
titer plate or other holder of containers for the fraction
collector may include a map of the containers such as for example X
and Y coordinates. This may be used to center a distributor arm
over the container or for a user or robot to locate a particular
container with a selected fraction.
[0072] The liquid sampler includes a pump for repeatedly drawing
liquid from a body of liquid, at least one container, at least one
container mounting fixture adapted for receiving at least one
container, at least one controller and a movable fixture for
providing at least one flow path. The pump has a first wireless
communication device and the at least one controller has a second
wireless communication device. The at least one controller
communicates with the pump through the first and second wireless
communication devices and includes a program for initiating pumping
and determining a container into which at least one sample is
deposited. The third wireless communication device is positioned to
communicate wirelessly with at least the first wireless
communication device and the second wireless communication device.
Container stations are connected to communicate with wireless
communication devices to identify the container station wherein the
at least one controller may direct fluid to that container
station.
[0073] To collect and analyze environmental samples, an instrument
includes at least one pumping system programmed to repeatedly draw
liquid from a body of liquid, a plurality of containers and at
least a corresponding one of a plurality of consoles for each
pumping system. Each of the plurality of consoles has a station for
at least a corresponding one of the plurality of containers. A
corresponding one of a plurality of container mounting fixtures is
provided to receive at last one column.
[0074] There is at least one corresponding controller for each of
the plurality of consoles and at least a corresponding one of a
plurality of movable fixtures for providing at least one flow path
in each of the plurality of consoles. The corresponding controller
communicates with at least one pump and includes a program for
initiating pumping and determining a container into which at least
one sample is deposited. Each of the pumps has a corresponding one
of a plurality of first wireless communication devices. The at
least one corresponding controller has a second wireless
communication device and a third wireless communication device. The
third wireless communication device is positioned to communicate
wirelessly with at least the first wireless communication device in
at least a corresponding one of a plurality of consoles and the
second wireless communication device.
[0075] In this liquid sampler, container stations are connected to
communicate with wireless communication devices to identify the
container station wherein the at least one corresponding controller
may direct fluid to that container station. An analyzing station
includes a wireless communication device wherein the analyzing
station may identify a source of each of the plurality of
containers.
[0076] To provide environmental sampling on site, liquid is pumped
from a body of liquid into at least one container within a
corresponding one of a plurality of container mounting fixtures
adapted to receive at least one container. A flow path is moved
over selected containers and pumping action is initiated. The flow
path is moved over the selected containers under the control of a
first wireless control device connected for communication with a
control system and a second wireless control device communicates
with the movable fixture. The controller has a second wireless
communication device and a third wireless communication device. The
third wireless communication device is positioned to communicate
wirelessly with at least the first wireless communication device
and the second wireless communication device. The container
stations are connected to communicate with wireless communication
devices to identify the container station wherein the controller
may direct fluid to that container station through the wireless
communication devices.
[0077] A portable instrument has a chromatographic column with
sensors spaced along its length. The sensors are connected to
communicate with wireless communication devices. The portable
instrument has an input and a readout device connected to a
wireless communication device wherein readings from said sensors
may be displayed. The portable instrument includes wireless
communication devices that may communicate remotely with other
instruments. The portable instrument may include a GPS to provide
location and the location may be recorded on the containers having
the sample in them. To environmentally test samples in the field, a
portable instrument containing wireless communication devices
measures samples and records the measurements on the wireless
communication devices. It may then transfer the measurements
wirelessly from the wireless communication device to other
instruments.
BRIEF DESCRIPTION OF THE DRAWINGS
[0078] The above noted and other features of the invention will be
better understood from the detailed description when considered in
connection with the following drawings, in which:
[0079] FIG. 1 is a block diagram of liquid chromatographic system
in accordance with an embodiment of the invention;
[0080] FIG. 2 is a block diagram of a preparatory liquid
chromatographic system in accordance with another embodiment of the
invention;
[0081] FIG. 3 is a schematic block diagram of a pump array in
accordance with an embodiment of the invention;
[0082] FIG. 4 is schematic diagram of a column and detector array
forming part of the embodiment of FIG. 3;
[0083] FIG. 5 is a block diagram of a chromatographic system in
accordance with an embodiment of the invention;
[0084] FIG. 6 is a simplified perspective view of a column having a
wireless communication device communicating with it;
[0085] FIG. 7 is a perspective view of a fraction collector in
accordance with an embodiment of the invention;
[0086] FIG. 8 is a perspective view of the fraction collector of
FIG. 7 shown from another angle;
[0087] FIG. 9 is a block diagram of a system for remotely
controlling and monitoring a plurality of liquid chromatographic
systems or other multiple fraction arrangements or processes in
accordance with an embodiment of the invention;
[0088] FIG. 10 is a block diagram of a chemical processing system
in accordance with an embodiment of the invention;
[0089] FIG. 11 is a chromatographic column having sensors for
factors such as temperature, pressure, pH and the like in
accordance with an embodiment of the invention;
[0090] FIG. 12 is a block diagram of a waste water sampling system
in accordance with an embodiment of the invention; and
[0091] FIG. 13 is a block diagram of an environment sampling system
in accordance with an embodiment of the invention.
DETAILED DESCRIPTION OF THE INVENTION
[0092] In FIG. 1, there is shown a block diagram of a liquid
chromatographic system 10 having a pumping system 12, a controller
18, at least one chromatographic column 14, a sample injector 20, a
detector 16, and a collection system 22. In the preferred
embodiment, an array of columns, detectors, sample collectors,
pumps and pump motors would be utilized as described more
completely in U.S. Pat. No. 6,427,526 granted Aug. 6, 2002, to
Davison, et al., but the invention is equally applicable to any
chromatographic system including the single column system shown in
FIG. 1 and any other multiple fraction instrument such as
environmental waste water collection systems. In this
specification, "multiple fraction instruments" shall mean
instruments used in scientific or investigative work such as in the
separation sciences or environmental studies that process multiple
fractions or samples or component parts in a manner that benefits
from identification or control of the individual fractions, samples
or component parts or the recall of information about individual
ones of the fractions or samples or component parts.
[0093] The pumping system 12 in the embodiment of FIG. 1 includes
first and second solvent reservoirs 24A and 24B, at least one pump
26 driven by at least one pump motor 32, liquid level sensors 28A
and 28B communicating with the solvent reservoirs 24A and 24B
respectively and purge systems 30A and 30B. The pumping system 12
supplies solvent to the column 14 and detector 16 or in the case of
a preparatory liquid chromatographic system utilizing an array of
columns and detectors, to the arrays of columns and detectors. The
supply of solvent is under the control of the controller 18. The
purge systems 30A and 30B communicates with the pump or pumps 26 to
purge the pumps and the lines between the pumps and the column
between chromatographic runs. The pump or pumps 26 supply solvent
to the column or columns or to the detector or detectors 16 under
the control of the controller 18.
[0094] The controller 18 receives signals from the detector or
detectors 16 indicating bands of solute and activates a fraction
collector 36 and readout display 34 in a manner known in the art.
One suitable fraction collection system is the FOXY.RTM.200
fraction collector available from Teledyne Isco, Inc., 4700
Superior Street, Lincoln, Nebr. 68504.
[0095] To supply solvent to the pump or plurality of pumps 26, the
pumping system 12 includes a plurality of solvent reservoirs such
as the reservoirs 24A and 24B. In the case in which a plurality of
pumps are utilized, the solvent reservoirs will communicate with
the pumps 26 through a manifold that channels solvent to each of
the pumps 26. Each of the pumps may also include a separate motor
or one motor may drive pistons from the plurality of pumps such as
the motor or plurality of motors 32. In some embodiments, there
will be a purge system such as the purge systems 30A and 30B for
purging the pump or pumps 26 and the connecting conduits. In the
preferred embodiment, the solvent reservoirs 24A and 24B
communicate with corresponding liquid level sensors 28A and 28B
that sense the amount of solvent in the reservoirs 24A and 24B so
that the reservoirs may continue to have solvent while the system
is operating.
[0096] The column or columns 14 and detector or detectors 16
receive the solvent from the pumping system 12 in a manner known in
the art. The sample injector 20 injects sample into the column 14
so that the solvent system may separate the components of the
sample and carry them through the detector 16 and to the analysis
and collection system 22.
[0097] The analysis and collection system 22 includes the fraction
collector 36, the detector 16 and the readout display 34. The
fraction collector 36 collects solute from the column or columns 14
and permits unselected material to flow through a waste system 38.
The detector 16 also receives the solute and applies signals to the
controller 18, which in turn controls the fraction collector 36 and
the readout display 34 to provide signals indicating the separate
species to be collected by the fraction collector 36 and to provide
a read out to the user.
[0098] At least some of the solvent reservoirs 24A and 24B, purge
systems 30A and 30B, liquid level sensors 28A and 28B, pumps 26,
pump motors 32, controllers 18, sample injectors 20, columns 14,
detectors 16, readout display or displays 34 and fraction
collectors 36 include one or more RFID devices. While in FIG. 1,
the liquid chromatographic system has these components hardwired
together, each of these components may communicate through a
separate one of RFID devices 40A-40Q.
[0099] In operating the chromatographic system 10 or similar
chromatographic systems using wireless transmitters as a substitute
for hardwiring between at least some of the components, a
controller 18 supplies packets of data to the RFID 40L and the RFID
40L transmits the data to other units or receives data and
transmits it to the controller 18. For example, in a gradient run,
the solvent reservoir 24A is connected to the RFID 40A and the
solvent reservoir 24B is connected to the RFID 40B. With this
arrangement, the RFID 40A identifies the solvent within the solvent
reservoir 24A and the RFID 40B identifies the solvent within the
solvent reservoir 24B.
[0100] During the chromatographic run, the controller 18 supplies
gradient information to the RFID 40L which transmits to the RFID
40D to operate the motor or motors 32. They in turn operate the
pumps 26 to pump solvent from the solvent reservoirs 24A and 24B.
The pumps RFID 40C may provide feedback information by delivering
packets of information concerning the pumping from their respective
reservoirs to the RFID's 40A and 40B, which in turn transmits the
information to the controller 18 to which it is connected. In this
way, the controller 18 through packets of data may control the
gradient as it is pumped through the column 14. At the beginning of
a gradient run, the controller 18 may transmit data to the RFID 40L
which in turn may transmit data to the RFID 40J to initiate the
injection of a sample from the sample injector 20 into the column
14. In the case of preparatory chromatography, the column 14 may
contain in the RFID device 401 that cooperates with it a
chromatogram to supply information to the controller 18 by
transmitting packets of information from the RFID 401 connected to
the column 14 to the RFID 40L connected to the controller 18. This
information may enable the controller 18 to transmit information
from its RFID 40L to the RFID 40D for the pump motors 32 and the
pump or pumps 26 through their respective RFID to pump the desired
solvent concentration for the preparatory purification. If the
solvent runs low in one of the solvent reservoirs 24A or 24B, the
liquid level sensors 28A and 28B supply this information to their
respective RFID devices 40E and 40F which may transmit information
to the appropriate one of solvent supplies 42A and 42B to replenish
the supply of the solvent in the solvent reservoirs 24A and
24B.
[0101] During the chromatographic run, the controller 18 receives
information from the detector 16. This information may be
transmitted by the RFID 40N connected to the detector 16 to the
RFID 40L connected to the controller 18. The controller 18 may in
turn transmit this information to the read out display 34 by
supplying the information to its RFID 40L which may transmit it
wirelessly to the RFID 40M which in turn may supply it to the read
out 34. Similarly, the detector 16 may transmit information from
its RFID 40N to the RFID 40K connected to the fraction collector 36
to activate the fraction collector 36 to collect peaks detected by
the detector 16. Moreover, the RFID 40N connected to the detector
16 may supply this information to the controller 18 through its
RFID 40L. The controller 18 may in turn supply information through
its RFID 40L to the RFID 40K on the fraction collector 36 to
control the positioning of collecting containers with respect to
the inlet to the fraction collector 36 so as to supply bands to
predetermined containers and follow a pattern that may be stored in
the controller 18 if desired. A RFID reader 56B may read RFIDs on
racks or other collector container holders and provide signals to
the controller indicating proper registration of the proper rack or
information about which location in a rack is to receive a
fraction.
[0102] In one embodiment, the RFID 401 connected to the column 14
may indicate the past history of the column. Prior to a
chromatographic run, this information may be obtained by the
controller 18 by transmitting a request for it from its RFID 40L.
The program and the controller 18 may compare this information with
the identification of the solvents obtained from the RFID 40A
associated with the solvent reservoir 24A and the RFID 40B
associated with the solvent reservoir 24B. If use of the column
indicates the new solvent conditions are not appropriate for use in
the column, the controller 18 may terminate the chromatographic run
and display a notice on the readout display 34 by transmitting
signals from the RFID 40L associated with the controller 18 to the
RFID 40D associated with the motor 32 and the RFID 40M associated
with the readout display 34. The fraction collector 36 may also
communicate through its RFID 40K with the controller 18. This
communication together with the communication from the column 14
and the detector 16 with the controller 18 may insure that racks or
individual containers are properly positioned prior to depositing
effluent from the column into the containers under the control of
the detector 16.
[0103] While in the preferred embodiment, the individual components
of the liquid chromatographic system 10 such as the detector 16,
pumps 26, solvent reservoirs 24A and 24B and the like communicate
directly with the controller 18 which may in return send signals to
other units such as the readout display 34, other communication
paths may be used. In the preferred embodiment, the center of
communication is the wireless communication device 40L that
communicates with the controller 18, which has substantial memory
in it. Therefore, it is possible, for example, for the detector 16
to communicate directly with the readout display 34 to display
peaks rather than transmitting the peaks to the controller 18
through the wireless communication device 40L and having the
wireless communication device 40L transmit the peaks to the readout
display 34 and fraction collector 36 through their respective
wireless communication devices 40M and 40K.
[0104] In FIG. 2, there is shown a block diagram of a preparatory
liquid chromatographic system 10A having a pumping system 12, a
column and detector array 14A, a collector system 16, a controller
18, a purge system 30A and a personal computer 130. The personal
computer 130 communicates with a wireless communication device 40Z.
The pumping system 12 applies solvent to the column and detector
array 14 under the control of the controller 18. The controller 18
supplies signals to a motor 32A which drives a pump array 26A by
wirelessly transmitting signals from the RFID 40U electrically
connected for communication with the controller 18 to the RFID 40T
electrically connected for communication with the motor 32A. The
movement of the pump array 26A provides a signal to the RFID 40S
connected to it which transmits the signals in return to the RFID
40U so that a jam or interruption is sensed and the controller 18
receives a feedback signal indicating proper movement of the pump
array 26A to pump liquid from solvent reservoir and manifolds 42C
and 42D to the column and detector array 14 from which a fluid
flows into the collector system 16 under the control of the
controller 18. Signals from the detectors in the column and
detector array 14 are transmitted by the RFID 40V to the RFID 40U
that communicates with the controller 18. The controller 18 in turn
sends signals reflecting the detection of bands to a readout
display 34A by transmitting them wirelessly to the wireless
communication device 40W that communicates with the readout display
34A. Signals transmitted by the wireless communication device 40U
from the controller 18 are also received by the wireless
communication device 40Y that communicates with a fraction
collector 36A to collect samples in a manner known in the art. A
suitable fraction collector system is the FOXY.RTM. 200 fraction
collector available from Teledyne Isco, Inc., 4700 Superior Street,
Lincoln, Nebr. 68504. The chromatographic system shown in FIG. 2
and described herein is also described without the wireless system
in U.S. Pat. No. 6,427,526 the disclosure of which is incorporated
herein by reference.
[0105] To supply solvent to the pump array 26A, the pumping system
12 includes a plurality of solvent reservoirs and manifolds, a
first and second of which are indicated at 42C and 42D
respectively, a pump array 26A and a motor 32A which is driven
under the control of the controller 18 to operate the array of
pumps 26A in a manner to be described hereinafter. The controller
18 also controls valves in the pump array 26A through the wireless
communication device 40S to control the flow of solvent and the
formation of gradients as the motor 32A actuates the pistons of the
reciprocating pumps in the pump array 26A simultaneously to pump
solvent from a plurality of pumps in the pump array 26A and to draw
solvent from the solvent reservoirs and manifolds such as 42C and
42D.
[0106] During this pumping process, a pump piston may become
jammed. If a pump in the pump array 26A should become jammed, there
is an automatic release mechanism for releasing the pressure from
at least that one pump to avoid damage. In the preferred
embodiment, the release mechanism is a fluid pressure release
mechanism for that pump set at a value above the rated pressure
such as at 170 psi so that the motor 32A may continuously move the
pistons up and down without damage. Moreover, valves in the pump
array 26A control the amount of liquid, if any, and the proportions
of liquids from different reservoirs in the case of gradient
operation that are drawn into the pump and pumped from it. The
manifolds communicate with the reservoirs so that a plurality of
each of the solvents such as the first and second solvents in the
solvent reservoir manifolds 42C and 42D respectively can be drawn
into the pump array 26A to permit a simultaneous operation of a
number of pumps.
[0107] While in the preferred embodiment, an array of reciprocating
piston pumps are used, any type of pump is suitable whether
reciprocating or not and whether piston or not. A large number of
different pumps and pumping principles are known in the art and to
persons of ordinary skill in the art and any such known pump or
pumping principle may be adaptable to the invention disclosed
herein with routine engineering, and in most cases, one motor
drives a plurality of pumps. While two solvents are disclosed in
the embodiment of FIG. 2, only one solvent may be used or more than
two solvents may be used. Because of the operation of a plurality
of pumps simultaneously driven by a single motor, efficiency and
cost reduction are obtained by this pumping mechanism.
[0108] process the effluent, the collector system 16 includes a
fraction collector 36A to collect solute, a manifold 42 and a waste
depository 44 to handle waste from the manifold 42. One or more
fraction collectors 36A communicate with the column and detector
array 14 to receive the solute from the columns either with a
manifold or not. A manifold may be used to combine solute from more
than one column and deposit them together in a single receptacle or
each column may deposit solute in its own receptacle or some of the
columns each may deposit solute in its own corresponding receptacle
and others may combine solute in the same receptacles. The manifold
42 communicates with the column and detector array 14 to channel
effluent from each column and deposit it into the waste depository
44. The fraction collector 36A may be any suitable fraction
collector such as that disclosed in U.S. Pat. No. 3,418,084 or the
above-identified FOXY.RTM. fraction collector.
[0109] The wireless communication device 40U in the preferred
embodiment transmits information to the wireless communication
device 40Z which records the information in an electronic notebook
stored in the memory of the personal computer 130 in a manner known
in the art. There are many electronic notebook systems and they
have formatting as part of the program. For example, Waters
Laboratory Informatics notebook will log all operations performed
and prepare customized reports.
[0110] In FIG. 3, there is shown a schematic block diagram of a
pump array 26A having a plurality of piston pump systems 60A-60J
(piston pump systems 60A-60E being shown for illustration in FIG.
3) although in the preferred embodiment there are ten such pumps
each arranged to communicate with corresponding ones of ten outlets
from the manifolds of the solvent reservoir and manifolds 42C and
42D (FIG. 2) to pump solvent from the reservoirs and manifolds 42C
and 42D into corresponding ones of the columns (not shown in FIG.
3). In FIG. 3, four of the pump systems 60A-60D are shown in block
form and a fifth pump system 60E is shown in greater detail with
the understanding that each of the ten pump systems are
substantially identical so that the explanation of the pump system
60E is an adequate explanation of all of the pump systems.
[0111] Each of the pump systems communicates with a corresponding
one of manifold outlets 58A-58J (58A-58E being shown in FIGS. 3)
and 59A-59J (59A-59E being shown in FIG. 3) to receive two
different solvents for the purpose of forming a gradient. They may
also communicate with a source of purge fluid as indicated by purge
conduits 66A-66J (66A-66E being shown in FIG. 3). With this
arrangement, each of the pumps draws solvent into it from the
solvent reservoirs in the solvent reservoirs and manifolds 42C and
42D (FIG. 2). The solvent flows from the pumps through a
corresponding one of outlets 68A-68J (68A-68E being shown in FIG.
3).
[0112] The pump system 66E includes an inlet conduit 58E from the
first solvent reservoir and manifold 40 (FIG. 2), the inlet conduit
59E from the second solvent reservoir and manifold 52, a three-way
solenoid valve 70E, a two-way solenoid valve 72E, and long flow
conduit 73E, a reciprocating piston pump 74E and a check valve 78E.
With this arrangement, the two different solvents from the conduits
58E and 59E are applied to the pump 74E through a common point
connecting the three-way solvent valve 70E and the two-way solvent
valve 72E. In the preferred embodiment, two cycles of solvent are
applied for each stroke of the piston pump 74E. The size of the
cylinder, the size of the flow conduit 73E, the speed of the refill
and delivery strokes of the piston are selected to ensure mixing
within the pump 74E and flow conduit 73E so as to pump a formed
gradient through a conduit 86E, through the check valve 78E and an
outlet conduit 68E to the column and collector array 14 (FIG. 2).
For this purpose, the pump cylinders are in the range of one inch
to eight inches long. In the preferred embodiment, the cylinders
are 3.5 inches long.
[0113] To provide two injections or charges of solvent during a
refill portion of a pump cycle, the two-way electronically
controlled solvent valve 72E opens once during each piston refill
stroke of the pump 74E under the control of a signal received from
wireless communication device 40S2 which receives a signal
wirelessly from the wireless communication device 40U (FIG. 2) that
communicates with the controller 18 (FIG. 2). Enclosures join the
delivery portion of the pump cycle. In the preferred embodiment,
the two-way valve 72E is a solenoid valve. To provide a gradient,
the three-way electronically-control proportioning valve 70E
switches between the two solvent reservoirs several times during
each refill stroke in response to a signal from the wireless
communication device 40S1 in communication with it. The wireless
communication device 40S1 receives a signal for this purpose from
the controller 18 by wireless transmission from the wireless
communication device 40U (FIG. 2) to open to the first solvent
reservoir and manifold 42C and then to the second solvent reservoir
and manifold 43D (FIG. 2) to provide both solvents in two stages
for better mixing. The proportion of the time the three-way valve
70E is open to the first solvent reservoir and manifold 42C and
then to the second solvent reservoir and manifold 42D determines
the composition of the mixture in the gradient. Both of the
solenoid operated valves 70E and 72E are under the control of the
controller 18 to which they electronically communicate through
wireless communication devices.
[0114] In FIG. 4, there is shown a schematic diagram of a column
and detector array 14 having a plurality of columns and detectors,
five of which are indicated as 100A-100E, a corresponding plurality
of outlet conductors 68A-68E, a corresponding plurality of solute
outlets 110-110E, a corresponding plurality of waste outlets
108A-108E from the manifold 42 (FIG. 2) and a fraction collector
36A. In the preferred embodiment, there are ten columns and
detectors. For illustration, the columns and detectors 100A-100D
are shown as a general block whereas the column and detector 100E
is shown in greater detail with the understanding that the columns
and detectors 100A-100D are substantially the same. Moreover, while
five columns and detectors are shown to correspond with the example
being used in this application, more or less could readily be used
and ten are used in the preferred embodiment.
[0115] The column and detector 100E includes an injector system
102E, a column stack 14A and 14B in the column and detector array
14, a detector 16E in the column and detector array 14, a waste
outlet 108E and the solute outlet 110E. With this arrangement,
solvent, whether a gradient or not, flows in the conduit 68E
through the injector 110E, through the column stack 14A and 14B
within the column and detector array 14, a flow cell 122E, where
solute may be detected and from there into the collection system 16
(FIG. 2) for the collection of solute and the disposal of waste.
The column stack (14A and 14B in FIG. 4) may instead be any type of
chromatographic column regardless of the mode of operation and it
is generally packed in accordance with the separation problem. In
the preferred embodiment, the column is REDISEP DISPOSABLE COLUMNS
sold by Teledyne Isco, Inc., 4700 Superior Street, Lincoln, Nebr.
68504. It is mounted to either receive a sample injection manually
from a syringe or automatically from the injector 101E as well as
receiving solvent on the outlet 68E. Its outlet flows through the
detector system in the column and detector array 14.
[0116] In FIG. 4, the stack of columns 14A and 14B are shown for
illustration. The outlet of the column 14A communicates with the
inlet of the column 14B in a manner known in the art so that the
inlet port of the column 14A receives solvent and sample from a
valve 103E and the outlet port of the column 14B is delivered to
the flow cell 122E. In this arrangement, the wireless communication
device 40U is connected to communicate with the column 14A and the
wireless communication device 40U3 is connected to communicate with
the column 14B. These wireless communication devices each contain
information about their characteristics so that a reader and
microprocessor may compare the information and determine if the
connection is correct or not and convey this information
appropriately to the user such as through a display or alarm or
inhibiting the operation of the pumps through the controller. For
example, there may be recorded on the wireless communication
devices associated with the columns: (1) the past history complete
enough to avoid incompatible solvent systems by having the
microprocessor with which it communicates indicate the incompatible
use; (2) a sample chromatographic curve for use by the
chromatographer; (3) a calibration curve; (4) the precision or an
indication of the precision of the column construction which may be
used to grade the column so that better grade columns may be sold
to higher price markets; (5) flow rates; (6) pressures; (7) solvent
mixtures; (8) pH; (9) conductivity; (10) dissolved oxygen and the
like. The efficiency of the column with certain chemistries or
processes can be determined and recorded.
[0117] At the start of the chromatographic run, the wireless
communication device 40J (FIG. 1) receives a signal from the
wireless communication device 40U (FIG. 2) that communicates with
the controller 18 and in turn switches the valve 103E so that
solvent flows into the injector 101E and from the injector through
the column (14A, 14B) and into the flow cell 122E for detection of
bands.
[0118] The detection system includes a light source 142E, the flow
cell 122E, a detector 16E and a valve 126E for channeling fluid
either to the waste outlet 108E through the conduit 44 or to the
collector outlet 110E. The light source 142E, hereinafter referred
to as the optical bench, applies light from a source common to each
of the column and detector assemblies 100A-100E and applies it
through each of the corresponding ones of the flow cells including
the flow cell 122E and from there to the corresponding detectors
including the detector 16E. The signal received indicates the
effluent to be channeled to the collector 36A and that to be
channeled to the waste for the particular column and detector
system.
[0119] The injector 102E includes a solid sample load cartridge in
the preferred embodiment and a four-way manual selective valve 103E
for controlling the selection of sample and injection into the
columns 14A and 14B. In the embodiment of FIG. 4, an individual
injector system (injector system 102E being shown in FIG. 4) is
provided for each of the columns although the outlet from one
injector could go to a manifold to supply the same sample to a
plurality of columns and/or the outlet from one injection cartridge
could go to a plurality of injection valves if desired. Similarly,
a single function collector 36 is shown but a plurality of such
collectors could be used with the individual valves connected to
more than one collector.
[0120] The injector system 102E includes the four-way valve 103E
for alternately injecting sample from the sample injector 110E,
which in the preferred embodiment is a cartridge, and selecting the
solvent gradient from the outlet 68E from the pumping system. Thus
a sample may be injected and then by turning the manual valve 103E,
the chromatographic run may be initiated. While a manual four-way
valve 103E is shown, automatic injector valves are also available
and may be utilized.
[0121] In FIG. 5, there is shown a block diagram of the
chromatographic system 10A having fraction collector diverter
valves 214, a flow cell and detector array 124, the controller 18,
a pressure transducer 218 and a valve array 212 for pumping
solvents. This block diagram illustrates the connections through
wireless communication devices between for example the controller
18, a pump drive motor 32A, the fraction collector diverter valves
214, the column and detector array 14 and the valve array 212. As
shown in FIG. 5, the controller 18 includes inter alia functional
components such as the pump controller 200 and the valve and
detector controller 201. The valve array 212 includes the pump
mixing valves 70, the inlet valves 72 and the purge valves 94.
[0122] As shown in FIG. 5, the pump controller 200 is connected to
the series pump drive 32A and a pressure transducer 218 in a
feed-back arrangement such as that described in U.S. Pat. No.
5,360,320, the disclosure of which is incorporated herein by
reference. Specifically, the feed-back circuit disclosed in
connection with FIGS. 8 and 9 in columns 11, 12, 13 and 14 of U.S.
Pat. No. 5,360,320 for controlling the pump disclosed in FIG. 4 of
that patent is utilized here. The pump controller 200 also
interacts with the valve and detector controller 201 to control the
flow and detector array 124 and the fraction collector diverter
valves 214 for the fraction collector 36A (FIG. 4). The valve and
detector controller 201 supplies signals to control mixing valves
70A-70J (shown collectively at 70), the inlet valves 72A-72J (shown
collectively at 72) and the purge valves 94 of the valve array 212.
With this arrangement, the detection of bands to be collected
controls the fraction collector valves to channel the collection
into the appropriate containers.
[0123] This system operates as described in U.S. Pat. No. 6,427,526
except instead of hard wiring between the units, wireless
communication devices transmit data or packets of data to control
the operations thereof.
[0124] In FIG. 6, there is shown a simplified perspective view of a
column 14 having a first wireless communication device 40U1 and a
second wireless communication device 40U2 positioned 180 degrees
from each other. In FIG. 1, they are shown mid-section of the
column but may be positioned anywhere in the column where they will
be in reasonably close communication with a wireless receiver. By
positioning them 180 degrees apart, the column becomes insensitive
to the rotational orientation since one or the other of the
wireless communication devices will have an unobstructed
communication path to a receiver mounted on the casing of the
chromatographic system.
[0125] In FIG. 7, there is shown a perspective view of a fraction
collector 36 including a main frame 46 and a plurality of racks
such as a first test tube rack 50 and a second test tube rack 52
exploded away and turned to show its bottom side. The main frame
includes a touch screen or LCD display 48, a distributor arm 60, an
RFID reader 56B, a wireless communication device 40K. Each of the
test tube racks has a wireless communication device 40K, which in
the preferred embodiment is an RFID device mounted to its bottom
side where it may come in proximity to a reader such as the RFID
reader 56B. The readers and wireless communication devices
determine if a rack is in position and may identify the rack such
as by the number of openings and cross section so as to provide
proper identification for the distributor arm 60 to move into
position and distribute fluid into the appropriate tubes such as
the test tube 54. In the embodiment of FIG. 7, a fraction collector
36 with two different racks 50 and 52 is shown, one of which is
exploded away but each of which may be moved automatically into
position where the registration and type may be checked. The
information may then be transmitted to the microprocessor
associated with the fraction collector 36 to distribute liquids
appropriately.
[0126] In FIG. 8, there is shown a perspective view of the fraction
collector 36 viewed from the bottom and back side showing the
distributor arm 60, the main frame 46, RFID readers 56B and 56C
connected to the RFID table 114, a conductor ribbon 112 for the LCD
display 48 (FIG. 7), and the main circuit board assembly 92. The
second and third test tube racks 50 and 64 are shown positioned
within the fraction collector 36. The fraction collector 36 is a 96
opening rack or any other appropriate size rack having the tube 84
within it and the test tube rack 50 is a 48 opening rack showing as
an example a test tube 64 within it.
[0127] In operation, the RFID devices such as 40K (FIG. 7) contain
an identification of the test tube rack by the arrangement of tubes
in the sizes within it so that when they register with the
appropriate RFID reader 56A (FIG. 7), 56B and 56C the reader can
indicate to the main circuit board 92 that the test tube rack is in
place so as to control the distributor arm 60 to distribute
effluent in the proper tubes or to waste. The RFID reader 56A, 56B
or 56C may also contain information about the size of the test
tubes 50 and 84 in the test tube racks so that the controller 18
(FIG. 1) may receive this information from the RFID reader 56A and
initiate a program that will move the distributor arm 60 to collect
the sample if necessary in successive tubes and avoid overflow. The
RFID devices such as the RFID wireless communication device 40K in
the second test tube rack 52 (FIG. 7) can identify the samples
collected in the test tubes, provide the test tube configuration
and identify the fractions or the like as well as including user
identification so that the test tube rack may continue to supply
user information to other processing units as needed and control
the distribution of the samples. Moreover, this information may be
utilized by transfer devices to transfer the samples for use with
other analytical equipment such as spectrometers or the like and
may be used with corresponding devices in the spectrometer for
further processing and transfer of information such as to
electronic notebooks.
[0128] The wireless communications system in the preferred
embodiment uses RFID TAGS such as THE Q5 programmable RFID tags
sold by Sokymat and operating at 125 KHz. The RFID reader modules
are ID-Innovations ID-12. They are encoded to identify the two
configurations, number of tubes and volume of the tubes.
[0129] In FIG. 9, there is shown a block diagram of a system 98 for
remotely controlling and monitoring a plurality of liquid
chromatographic systems or other multiple fraction instruments or
processes having a central controller 128 which may be a personal
computer or other computer, a multiple site service facility 116
which may be the facility of a manufacturer that manufacturers the
instrument and supplies parts and supplies for the instrument, an
internet service provider 118, a plurality of the instruments such
as the liquid chromatographs 10-10B, one or more storage or
maintenance facility such as those shown at 13-13B and other
instruments like the mass spectrometers or other separation
instruments such as those shown at 15-15B for example. The
component parts of the instruments 10-10B and 15-15B communicate
with each other and may communicate with storage or maintenance
facilities. For example, columns may be stored for use between runs
using the column and these columns may be stored with information
on them about the history of the column, including information
about projects to which the column is dedicated or information
about customers for whom the projects are being run or any other
such relevant information. The same may be true of collection
vessels or racks or the like. This information may also be
transmitted to the central controller 128 and from there to an
internet service provider 118 for transmission and gathering of
data at a multiple site service facility 116.
[0130] The multiple site service facility 116 may maintain
statistics on individual customers using a particular system so as
to anticipate supplies the customer may need. Moreover, repair
information may be transmitted such as for example if a
chromatographic system 10-10B fails in some respect the wireless
communication device on the instrument may detect the failure and
the information transmitted by way of the central controller 128 to
the multiple site service facility 116. For example, the multiple
site service facility may have statistics indicating a particular
customer is using a particular type of column at a fixed rate and
has an inventory of a predetermined number of columns. With this
information, the multiple site service facility 116 can predict
when the customer will need more columns and contact the customer
to arrange for sale of the columns. Similarly, the multiple site
service facility 116 may determine statistically when certain
components are likely to exceed their life. It may for example
determine that a certain type of fraction collector is useful for a
predetermined number of hours of operation from its statistical
data base and when a particular fraction collector approaches that
number, may notify the customer so as to be prepared for service or
repurchase. The efficiency of the columns for certain chemistries
and processes may be determined from statistics gathered from
multiple stations. Customer specific information may be obtained
and supplied to a customer or used in performing services for a
customer such as default conditions, good manufacturing practices,
billing information, IQ (installation qualifications), OQ
(operation qualifications) and PQ (performance qualifications)
including both test steps and results.
[0131] In FIG. 10, there is shown a block diagram of a chemical
processing system 132 having first and second chemical processing
stations 134 and 136 and an analytical or separation station 138.
The chemical processing stations 132 and 136 perform chemical
operations including combinatorial chemical processes in which a
range of known reagents or known quantities of reagents are
sequentially applied to some material under temperature and time
conditions to cause a reaction, or the time and temperatures are
sequentially changed to arrive at the parameters for a preferred
reaction. These stations include a mechanism for transferring the
product of the reaction to another container or instrument for
transferring to an analytical station for further analysis or
purification or separation of the reaction product.
[0132] Within the chemical processing station 134, there are a
plurality of reaction consoles such as 140 and 144 and similarly
within the reaction station 136, there are a similar plurality of
reaction consoles 146 and 148. Each of the reaction stations 134
and 136 also includes transfer consoles such as the transfer
console 150 in reaction station 134 and the transfer console 154 in
reaction station 136. The reaction stations apply reagents to
chemical materials and maintain them for the proper time and at the
proper temperature and pH for a desired reaction. They do this
automatically and continuously and each include an appropriate
wireless communication system such as 160A for the reaction
consoles 140 and 144, wireless communication system 160Q for the
reaction console 146 and wireless communication system 160R for the
reaction console 148. These wireless communication systems transfer
an identification of the substance being reacted upon and other
information such as the reactants, time, temperature, the user or
customer for whom the reaction is being performed and further
reactions that are necessary in accordance with FDA standards to
provide tamper-proof communication and reaction measures.
[0133] There are many different reaction consoles that may be used
and are on sale but a suitable reaction console is disclosed in
U.S. Pat. No. 4,168,955 issued to Robert W. Allington on Sep. 25,
1979, the disclosure of which is incorporated herein. Each of the
chemical processing stations 134 and 136 also includes the transfer
consoles 150 and 154 respectively and each of the transfer consoles
150 and 154 communicates with a corresponding one of the wireless
communication systems 160C and 160S. These devices apply
information relating to the reagent, the steps in using the reagent
to prepare the reaction product and the reaction product and future
operations such as the analysis or separation or purification
required. This information is applied to transfer containers such
as 156F and the information is applied to the transfer container
156F by a corresponding wireless communication system 160D.
[0134] These containers may be utilized by the analytical and or
separation station 138 by being applied to an analytical or
separation instrument 162 therein either manually or through
robotics for analysis or for separation. This instrument 162 for
example may be a liquid chromatograph capable of detecting and
recognizing by the time of the peaks particular materials or
capable of purification of separation of particular molecular
species. The separation and analysis reaction may be transferred by
a wireless communication system 160K communicating with the
analytical or separation instrument 162. The purified substance and
information concerning it may be transferred by the wireless
communication system 160K to containers for the purified or
separated material such as 160P and 1600 in communication with
their respective containers 158A and 158B. The containers 158A,
158B and 158C may be transferred by a transfer console 152 to a
transfer container 158D at the transfer console 152 and the
wireless communication system 160L may transfer information to the
wireless communication system 160M in communication with the
container such as 158D shown in FIG. 10. With this arrangement,
containers from the chemical processing station will have all of
the necessary information on it for further use or further
processing.
[0135] In FIG. 11, there is shown a column 14B having a plurality
of wireless communication devices 40U4-40U8, which in the preferred
embodiment are RFID devices, spaced along its length and
electrically connected for communication with sensors 164A-164E
inside the column 14B. The sensors 164A-164E may sense
characteristics within the column or may be spaced in the column to
sense a characteristic of a wall of the column or the outside
temperature as desired. In one embodiment, the sensors such as
164A-164E may be molded within the wall so that the sensors may be
in contact with the contents of the column 14B but the column 14B
remains sealed while the wireless communication devices 40U4-40U8
may transmit wirelessly outside the column 14B.
[0136] In some embodiments, instead of sensors and wireless
communication devices spaced along the wall of the column, a
transponder and wireless communication device may be located within
the column. For example, a temperature transponder and wireless
communication device may be encased in a protective casing and
located within the packing of the column to sense temperature and
transmit the temperatures outside of the column to provide feedback
for controlling the temperature in the column. An external heater
or cooling apparatus may be controlled by a temperature recorded in
a wireless communication device and the transmitted temperature to
heat or cool the column or the solvent being applied to the column
to maintain the temperature within a desired range. One such
communication device and suitable temperature sensor is
manufactured by KSW Microtek within the KSW-VarioSens product line.
These transponders are available from KSW Microtek;
Manfred-Von-Ardenne-Ring 12 D-01099 Dresden, Germany.
[0137] In FIG. 12, there is shown a block diagram of a waste water
sampler system 166 having a control system 168, one or more fill
station drive motors 170, a pump station 174, a pump drive section
176, a driver 172 for the pump drive station 176 and a distributor
178. The pump station 174 is adapted to communicate with a water
source 180 to sample water therefrom. To control the waste water
sampler system 166, the control system 168 includes the CPU 182
connected for communication with a wireless communication device
188A, the display 184 connected for communication with the wireless
communication device 188B and the keyboard 186 electrically
connected to a wireless communication device 188C for communication
therewith.
[0138] The control system 168 can be programmed to cause the pump
station 174 to pump samples of water from the water source 180 by
transmitting signals from the wireless communication device 188A to
wireless communication device 188G that is connected for
communication to the pump drive station 176. In response to signals
transmitted by wireless communication device 188A from the control
system 168, the pump station 174 pumps the samples into containers
within the distributor 178. To control the fill station drive motor
170, the control system signals from the wireless communication
device 188A to the wireless communication device 188E that is
connected to communicate with the distributor 178 and by
transmitting signals to the wireless control device 188D that is
connected for communication to the fill station drive motor 170.
The bottles are usually standard sized and shaped sample bottles
within the distributor 178 but include within them wireless
communication devices.
[0139] These wireless communication devices include a nonvolatile
memory that receives signals from the CPU 182 and records the time
and amount of water deposited into the containers for future
reference. The nonvolatile memory also records the temperature of
the water and a log of sample temperature from the time of sampling
until analysis. The temperature measurement can also be used to
provide feedback for non-contact closed loop control of sample
temperature by controlling a heating or cooling device. If the
container is in a container or rack, the weight of the container
will be an indication of the amount of sample and may be weighed by
a simple scale at the bottom of the container. The scale may be
connected to a wireless communication device and provide a
convenient readout of the amount of sample on a monitor to control
in a feedback manner the drawing of the sample.
[0140] The control system 168 controls the operation to
automatically fill a series of containers so that the distributor
178 includes sample containers that may be identified as to the
location where the water was drawn, the time the water was drawn,
the customer for which the water was drawn, the source of the
water, and the test steps to be performed on the water. The control
system 168 includes a central processor unit 182 with a typical
display and/or printing unit shown at 184 and typical input units
such as a keypad or electrical communication jack shown at 186. The
control system 168 is programmed and contains the necessary
interfaces to coordinate the operation of the pump station 174, the
distributor 178 and the fill station drive motor 170 in such a way
as to provide flexibility in drawing samples. It coordinates the
operation of the individual components to properly fill containers
while maintaining the integrity of volatile substances within the
liquids for later testing.
[0141] In FIG. 13, there is shown a block diagram of a sampling
arrangement including a central station 190 and a plurality of
remote sites with samplers illustrated at 192. The central station
190 includes an ice source 196, the bottle carrier source 198, a
container source 200, composite containers 204 and a plurality of
shipping cartons from a shipping carton source 202. The samplers,
periodic replacement ice, container carriers, containers and
shipping cartons for the samples are moved from the central station
190 to each of the remote sites with samplers 192 for use and
samples are removed from the remote sites and they are taken to the
laboratory which may be at the central station such as shown at
206. At the testing laboratory 206, an RFID wireless communication
device 208D is programmed with a test and the results and that
program are transferred to the individual containers. The
individual containers have on them, in addition to the source of
the testing laboratory 206 which is introduced by the RFID wireless
communication device 208E which is connected for communication with
the console at the testing laboratory 206. The shipping carton
source 202 is connected for communication with the wireless
communication device 208C to maintain an inventory as cartons are
removed and new empty cartons supplied. Similarly, the container
source 200 is connected for communication to the RFID wireless
communication device 208B which maintains an inventory of available
containers by receiving information programmed on it as new
containers are brought in and as old containers leave. The bottle
carrier source 198 similarly keeps an inventory.
[0142] With this arrangement, different configurations of
containers may be utilized with the same base at a plurality of
different sites and the samples may be conveniently brought from
the site to the appropriate location for the samples to be analyzed
or utilized. In operation, a sampler is brought to the site and
samples are drawn. A shipping carton container, carrier containers
and ice are brought to the site. The container carrier is removed
from the shipping carton, the ice is removed and the containers of
sample are removed from the sampler. The container carrier, ice and
containers are taken from the shipping carton and put into the
sampler. The old container carrier, carriers and ice are put into
the shipping carton and taken to the laboratory for analysis.
[0143] Each of the multiple fraction systems used above employ
wireless communication devices such as radio frequency
identification devices (RFID) to communicate between components,
stations and consoles so as to provide instructions for operations,
transfer information so as to maintain a record of operations that
have been performed and are to be performed and record data.
[0144] Although a preferred embodiment of the invention has been
described in substantial detail, many modifications and variations
of the invention are possible in light of the above description.
Accordingly, it is to be understood that, within the scope of the
appended claims, the invention may be practiced other than as
specifically described.
* * * * *