摘要:
Sample is applied to a chromatographic column containing shape stabilized packing and the liquid phase is pumped through the shape stabilized packing at a rate of flow greater than the standard rate of flow to obtain at least one of a target resolution and target time of run. Because of the improved resolution provided by the shape stabilized packing at higher rates of flow of solvent, the chromatographer can either obtain better resolution with a standard gradient or shorten the time of the run and reduce the amount of solvent needed by increasing the slope of the gradient.
摘要:
An isocratic gradient profile is inserted into a gradient profile during a flash chromatographic run when TLC indicates that it will be difficult to separate the component being purified from its closest impurity by a gradient. TLC is utilized to determine at least two retention factors with two significantly different solvent strengths for the same solvent system. The two or more retention factors are used to determine a solvent strength in which the retention factor of a target component and the retention factor of a closest impurity are within 0.8 of each other. The isocratic gradient profile is started when this solvent strength is reached during the gradient chromatographic run. It is ended when the earlier of four events occurs, which are: (1) the end of a second peak if a first peak is detected at an isocratic-gradient profile starting-solvent strength or within a predetermined starting tolerance of the isocratic-gradient profile starting-solvent strength detection; (2) the end of the first peak after the starting tolerance; (3) the detection of a peak during the isocratic gradient profile or isocratic segment run after the regular isocratic time period; or (4) an operator initiated termination of the isocratic gradient profile or isocratic segment run. The gradient profile then resumes and continues to the end of the run.
摘要:
To make an inexpensive chromatographic column and perform chromatography with it, column walls and a column end with a port are molded integrally from plastic. A closure is integrally molded with a port as well. One type of closure includes part of a snap-on fastener integrally molded to it to cooperate with corresponding parts molded integrally with the column walls and another type of closure is welded to the tubular walls. In the preferred embodiment the welding is spin welding. The end and closure have channels molded into them radiating from a port and opening toward packing material such as silica beads or porous polymeric plugs. Filters and secondary seals may be located at the ends to prevent leakage of packing material.
摘要:
To make an inexpensive chromatographic column and perform chromatography with it, column walls and a column end with an inlet port are molded integrally from plastic and a snap-on end is molded integrally with an outlet port from plastic. A filter is placed in one end of the column and the column is filled with packing material up to the second end. A filter is placed on top of the packing and a snap-on end with a molded outlet port is snapped onto the body with linear motion until an interference fit is formed. As the body and snap-on end are moved together cantilever members formed integrally with the snap on end are bent outwardly by detent members until the detent members are captured by an opening in the cantilever members.
摘要:
To economically perform preparatory chromatography, a plurality of pumps each having a corresponding one of a plurality of pistons and a corresponding one of a plurality of cylinders are driven by one motor to draw and pump solvent simultaneously into corresponding columns. To form a gradient, the pumps are connected to two-way valves that are connected alternately to a first solvent and a second solvent, whereby the time said valve is in a first position controls the amount of solvent drawn from the first reservoir into said pumps and the amount of time in said second position controls the amount of said second solvent drawn from the second reservoir into said pumps and the solvent is mixed in the pumping systems. The detectors are photodiodes mounted to light guides in the flow cells that generate signals related to light absorbance and communicate with a controller, whereby the controller receives signals indicating solute between the light guides and causes collection of solute. An over-pressure system compensates for pressure over a predetermined level.
摘要:
To provide or maintain pump prime in a liquid chromatographic system when changing solvents or solvent reservoirs or starting up a chromatographic run, first and second solvents are supplied to a mixer through corresponding first and second lines and from the mixer to a chromatographic column. Air in one of the lines is removed by a pump and the line is filled with solvent.
摘要:
A sample injection apparatus includes a sample container and a tube that communicates with the inlet of a liquid chromatographic column. The sample container receives at least a preparatory-sized sample. A syringe pump pulls sample from the sample container and applies it to the inlet of the liquid chromatographic column.
摘要:
To make an inexpensive chromatographic column and perform chromatography with it, column walls and a column end with a port are molded integrally from plastic. A closure is integrally molded with a port as well. One type of closure includes part of a snap-on fastener integrally molded to it to cooperate with corresponding parts molded integrally with the column walls. In another type of closure for higher pressures, the closure is spin welded to the tubular walls. In still another type of closure for still higher pressures, a retaining plate is pressed into the column to hold the packing in place. The closures have channels molded into them radiating from a port and opening toward packing material such as silica beads or porous polymeric plugs. Filters and secondary seals may be located at the ends to prevent leakage of the packing material. The packing is balanced spherical or spheroid-like derivitized silica packing.
摘要:
To make an inexpensive chromatographic column and perform chromatography with it, column walls and a column end with an inlet port are molded integrally from plastic and a snap-on end is molded integrally with an outlet port from plastic. A filter is placed in one end of the column and the column is filled with packing material up to the second end. A filter is placed on top of the packing and a snap-on end with a molded outlet port is a snapped onto the body with linear motion until an interference fit is formed. As the body and snap-on end are moved together cantilever members formed integrally with the snap on end are bent outwardly by detent members until the detent members are captured by an opening in the cantilever members.
摘要:
In a piston pump for pumping liquid carbon dioxide at a temperature below 30 degrees Fahrenheit and pressures at least as high as 7500 psi, the volume leaving the pump is determined by measuring only pressure or other parameter related to flow and movement of the plunger. The position of the piston is measured and the resulting displacement is integrated to determine volume of fluid pumped.