公开(公告)号：US3985019A

公开(公告)日：1976-10-12

申请号：US630101

申请日：1975-11-10

Applicant: Detlef R. Boehme ,  Kenneth C. Judah ,  Miner N. Munk

Inventor： Detlef R. Boehme ,  Kenneth C. Judah ,  Miner N. Munk

IPC: F04B13/02 ,  F04B49/20 ,  G01N30/32 ,  G01N30/34 ,  G01N30/36 ,  G01N31/08

CPC classification number: G01N30/36 ,  F04B49/20 ,  G01N30/34 ,  G01N2030/322 ,  G01N2030/326

Abstract: A liquid chromatography system including a liquid chromatography column, first and second reservoirs for solvents to be utilized as the mobile phase, reciprocating pumping means for flowing the solvents through the column, and motor means for driving the pump through successive pumping cycles including pump and fill subcycles. First and second solenoid-actuated proportioning valves are positioned at the low pressure side of the pump, i.e. between the first and second reservoirs and the pump inlet. Gradient setting means are provided for setting a preselected solvent proportion to be used over a time period. Means responsive to the gradient setting opens one of the said proportioning valves during a predetermined portion of the fill subcycle. The valves are actuated in complementary fashion with respect to opening and closing; hence the fill subcycle is divided between flow proceeding from the first and second valves in accordance with the gradient setting.

Abstract translation: 一种液相色谱系统，包括液相色谱柱，用作流动相的溶剂的第一和第二储存器，用于使溶剂流过色谱柱的往复泵送装置和用于通过连续泵送循环驱动泵的马达装置，包括泵和填充物 亚循环 第一和第二电磁致动比例阀位于泵的低压侧，即在第一和第二储存器与泵入口之间。 提供梯度设定装置，用于设定在一段时间内使用的预选溶剂比例。 响应于梯度设定的装置在填充子循环的预定部分期间打开所述比例阀中的一个。 阀门相对于打开和关闭以互补的方式启动; 因此，根据梯度设置，从第一和第二阀进行的流动之间划分填充子循环。

公开(公告)号：US3934456A

公开(公告)日：1976-01-27

申请号：US490549

申请日：1974-07-22

Applicant: Miner N. Munk

Inventor： Miner N. Munk

IPC: G01N30/32 ,  G01N30/34 ,  G01N31/08

CPC classification number: G01N30/34 ,  G01N2030/322 ,  G01N2030/347

Abstract: Solvent gradient generating apparatus in a liquid column chromatography system. A multi-compartment vessel having an input/output port pair for each compartment is coupled between a high pressure pump and the column cell for providing both gradient generation and pulse damping. A piston, which is slidably contained within the vessel, sealably provides the compartments. Means external to the vessel are provided for controlling the rate of movement of the piston within the vessel. The volume of each compartment is controlled by the position of the piston, and the rate of movement of the piston controls mixing of the solvent components delivered to the column cell. Each compartment has input and output ports. In one embodiment, both input ports are coupled to the high pressure pump while only one output port is coupled to the column cell. In another embodiment, only one input port is coupled to the pump and the other input port and one output port are sealed.

Abstract translation: 液柱色谱系统中的溶剂梯度发生装置。 具有用于每个隔室的输入/输出端口对的多隔室容器被耦合在高压泵和柱单元之间，用于提供梯度产生和脉冲阻尼。 可滑动地容纳在容器内的活塞可密封地提供隔室。 设置在容器外部的装置用于控制活塞在容器内的运动速度。 每个隔室的体积由活塞的位置控制，并且活塞的运动速率控制输送到柱室的溶剂组分的混合。 每个隔间都有输入和输出端口。 在一个实施例中，两个输入端口耦合到高压泵，而只有一个输出端口耦合到列电池。 在另一个实施例中，仅一个输入端口耦合到泵，另一个输入端口和一个输出端口被密封。

公开(公告)号：US06281975B1

公开(公告)日：2001-08-28

申请号：US09521071

申请日：2000-03-07

Applicant: Miner N. Munk

Inventor： Miner N. Munk

IPC: G01N2100

CPC classification number: G01N30/74 ,  G01N21/0303 ,  G01N21/05 ,  G01N2021/0346 ,  G01N2030/746 ,  G01N2201/0639

Abstract: A bent capillary flow cell with protruding end bulbs coaxial with centerline of an elongated center cylindrical section of capillary tubing. The bulbs provide a high light throughput entrance window for the cell. Light is piped along the elongated center section by total internal reflection at the outside surface of the cell wall. An external light absorbing band is placed in optical contact with outer surface of the cell wall over a transition cone region between the bulb and center cylindrical section of the cell. Each of the external light absorbing bands extend a short prescribed distance over the cylindrical wall to absorb light rays that would otherwise be light piped within the cell wall and have little exposure to the liquid in the cell.

Abstract translation: 弯曲的毛细管流动池，突出的端部灯泡与细长的毛细管中心圆柱形部分的中心线同轴。 灯泡为电池提供高光通量入口窗口。 光通过在细胞壁的外表面处的全内反射沿着细长中心部分管道。 外部光吸收带放置成在电池的灯泡和中心圆柱形部分之间的过渡锥形区域上与电池壁的外表面光学接触。 每个外部光吸收带在圆柱形壁上延伸一个短的规定距离，以吸收否则将在细胞壁内轻微管道并且几乎不暴露于细胞中的液体的光线。

公开(公告)号：US4475813A

公开(公告)日：1984-10-09

申请号：US413220

申请日：1982-08-30

Applicant: Miner N. Munk

Inventor： Miner N. Munk

IPC: G01N21/01 ,  G01N21/25 ,  G01N21/27 ,  G01N21/64 ,  G01N30/74 ,  G01N30/94 ,  G01N21/59

CPC classification number: G01N21/255 ,  G01N21/64 ,  G01N30/94

Abstract: Improved optical systems for liquid chromatographic apparatus comprise flow cells with light transparent portions through which one or more beams of light may be passed through an effluent stream flowing in the cell, one or more light sources on one side of the flow cell to project light through the cell and its contained effluent stream, one or more light limiting apertures positioned on the opposite side of the cell in the paths of the light beams, one or more positive light focusing elements positioned in the path of the light beams from the cell to the apertures to image the center of the cell at the apertures and a light sensor positioned in the path of the light beam on the side of each aperture opposite to its respective light focusing element.Improved methods of chromatographic analysis using the new optical systems are also disclosed.

Abstract translation: 用于液相色谱装置的改进的光学系统包括具有光透明部分的流动池，一个或多个光束可以通过该细胞通过流过细胞的流出物流，流动池的一侧上的一个或多个光源将光通过 电池及其包含的流出物流，位于光束路径中的电池相对侧上的一个或多个限光孔，一个或多个正光聚焦元件，其定位在从电池到光源的光束的路径中 用于在孔处成像细胞的中心的孔，以及位于每个孔的与其各自的聚光元件相对的侧面上的光束路径中的光传感器。 还公开了使用新的光学系统的改进的色谱分析方法。

公开(公告)号：US4457846A

公开(公告)日：1984-07-03

申请号：US396389

申请日：1982-07-08

Applicant: Miner N. Munk

Inventor： Miner N. Munk

IPC: G01N30/00 ,  G01N30/12 ,  G01N30/16 ,  B01D15/08

CPC classification number: G01N30/16 ,  G01N30/00 ,  G01N2030/121

Abstract: In the analysis of substances by liquid chromatography, samples to be analyzed are introduced into the chromatography column by being loaded into a fluid permeable section in a cartridge, placing the sample loaded section over the inlet end of the column and flowing solvent through such section into the column. The cartridge may be a plate with an opening through it with the ends of the opening covered by permeable membranes or the opening may be packed with porous material. The cartridge may have a plurality of such openings and these may be in the form of a line on a rectangular plate or a circle on a circular plate. The new methods and devices of the invention are particularly useful in micro-scale liquid chromatographic procedures.

Abstract translation: 在通过液相色谱分析物质时，将待分析的样品通过装载到筒中的流体可渗透部分中而引入色谱柱，将样品加载部分放置在柱的入口端并将溶剂流过该部分进入 列。 盒可以是具有开口的板，其开口的端部被可渗透膜覆盖，或者开口可以填充有多孔材料。 盒可以具有多个这样的开口，并且它们可以是矩形板上的线或圆形板上的圆形。 本发明的新方法和装置在微量级液相色谱方法中特别有用。

公开(公告)号：US4032445A

公开(公告)日：1977-06-28

申请号：US630400

申请日：1975-11-10

Applicant: Miner N. Munk

Inventor： Miner N. Munk

IPC: F16L55/04 ,  F04B43/067 ,  G01N30/32 ,  G01N30/36 ,  B01D15/08

CPC classification number: G01N30/32 ,  G01N30/36

Abstract: In a liquid chromatography system including a chromatographic column, a reservoir for a slightly compressible liquid mobile phase, piston means cooperating with the reservoir for pumping the liquid phase through the chromatographic column, and means for displacing the piston at a pre-selected velocity, an improvement is disclosed enabling maintenance of a constant flow in the presence of flow resistance changes at the chromatographic column. Such flow resistance changes may arise, for example, in consequence of viscosity changes occurring in the liquid phase during the course of gradient elution operation. According to the improvement, pressure control means are provided in the flow path between the reservoir and column, the pressure control means being adapted for maintaining a substantially constant pressure at the reservoir. In consequence, flow rate changes arising from expansion or contraction of the liquid phase in consequence of compressibility are precluded.

公开(公告)号：US3999439A

公开(公告)日：1976-12-28

申请号：US490547

申请日：1974-07-22

Applicant: Miner N. Munk

Inventor： Miner N. Munk

IPC: G01N1/00 ,  G01N30/22 ,  G01N30/36 ,  G01N1/10

CPC classification number: G01N30/36 ,  G01N30/22

Abstract: An injection apparatus and method for use in high pressure liquid chromatography. A cylindrical sample holding means containing several sample cells is maintained in a chamber whose pressure is approximately equal to that of the head of the chromatograph separation column. The sample cells are bores through the cylinder, parallel to its axis and spaced along a cylinder of revolution concentric to the axis. The cells are preloaded with samples to be analyzed. Stationary carrier fluid inlet and outlet conduits extend into the chamber above and below corresponding points on the cylinder defined by the sample cell placement. The inlet conduit is connected to a high pressure source of carrier fluid. As the sample holder is rotated, successive sample cells are aligned with the inlet and outlet conduits such that the sample is forced through the outlet conduit into the column. This structure eliminates the need for movable high pressure seals between the outlet conduit and the sample cells, due to the maintenance of all the cells at an elevated pressure.

Abstract translation: 一种用于高压液相色谱的注射装置和方法。 将含有几个样品池的圆柱形样品保持装置保持在其压力近似等于色谱仪分离柱头部的室中。 样品池通过圆柱体，平行于其轴线并沿着与轴线同心的旋转圆柱体间隔开。 细胞预先加载待分析的样品。 固定的载体流体入口和出口导管延伸到由样品池放置定义的圆柱体上的对应点上方和下方的腔室中。 入口管道连接到高压载体流体源。 当样品保持器旋转时，连续的样品池与入口和出口导管对准，使得样品被迫通过出口导管进入柱。 这种结构消除了在出口管道和样品池之间的可移动高压密封的需要，这是由于所有电池在升高的压力下的维持。

公开(公告)号：US3950104A

公开(公告)日：1976-04-13

申请号：US490593

申请日：1974-07-22

Applicant: Miner N. Munk

Inventor： Miner N. Munk

IPC: G01N21/41 ,  G01N30/74 ,  G01N21/46 ,  G01F1/68 ,  G01N1/10

CPC classification number: G01N21/41 ,  G01N30/74

Abstract: Apparatus and method for detecting the refractive index and rate of fluid flowing through an elongated flow cell, having applications in liquid chromatography. The cell may be of circular cross section and has an input window in one end, an exit window in the other, and a longitudinal side wall. A light source directs divergent light through the entrance window, longitudinally through the cell, to pass through the exit window and be sensed by a photoelectric detector outside the exit window. In a first embodiment, heat transmission apparatus connected to the cell establishes a constant temperature gradient in the cell. This temperature gradient, preferably, has a component perpendicular to the longitudinal dimension of the cell and extending toward the center of the cell. This causes the density of the fluid in the cell to vary as an increasing function of its distance from the walls. The index of refraction of the fluid thus, in this embodiment, increases with distance from the cell walls. This causes the divergent light to be bent away from the cell walls, and toward the center of the cell. The degree of this bending, and hence the fraction of light entering the entrance window which passes through the exit window, increases with the refractive index of the fluid. By appropriate selection of the cell dimensions, of the value of the temperature gradient and of a substantially constant flow rate of the fluid, the bending of the light passing through the cell may be governed such that the fraction of entering light which exits from the cell is a highly dependent function of variations in the refractive index of the fluid in the flow cell. In another embodiment, a fluid having a known refractive index value has its flow rate determined by measuring the absorbance of a beam of light passed therethrough after establishing a temperature gradient in the fluid such that the degree of light bending is influenced by the flow rate.

公开(公告)号：US5608517A

公开(公告)日：1997-03-04

申请号：US395784

申请日：1995-02-28

Applicant: Miner N. Munk

Inventor： Miner N. Munk

IPC: G01N21/03 ,  G01N21/05 ,  G01N30/02 ,  G01N30/74

CPC classification number: G01N21/0303 ,  G01N21/05 ,  G01N30/74 ,  G01N2021/0346 ,  G01N2030/027 ,  G01N2030/746

Abstract: A coated flow cell and a method for making the coated flow cell are provided. The flow cell comprises a flow passage internally coated with a polymer having an index of refraction lower than that of water. In this manner, light directed into the flow cell is internally reflected or "piped" down the length of the flow passage. As a result, flow cells having path lengths significantly longer and accepting incident angles of light much greater than possible with prior art flow cells. A method for internally coating the flow cell is also provided.

Abstract translation: 提供涂布流动池和制造涂覆流动池的方法。 流动池包括内部涂覆有折射率低于水的聚合物的流动通道。 以这种方式，引导到流动池中的光在流动通道的长度内部反射或“管道化”。 结果，具有明显更长的路径长度并且接受光的入射角比现有技术的流动池更大的流动池。 还提供了用于内部涂覆流动池的方法。

公开(公告)号：US4942018A

公开(公告)日：1990-07-17

申请号：US328750

申请日：1989-03-23

Applicant: Miner N. Munk

Inventor： Miner N. Munk

IPC: G01N30/32 ,  G01N30/34 ,  G01N30/36 ,  G01N30/60

CPC classification number: G01N30/36 ,  G01N30/34 ,  G01N2030/322 ,  G01N2030/347 ,  G01N30/6065

Abstract: Solvent composition gradients in high performance liquid chromatography (HPLC) are generated with a packed bed gradient generator. Natural dispersion occurs in flow through a bed of particles due to eddy and molecular diffusion. This dispersion changes a sharply defined front between two solvents into a desirable error function type gradient profile at the interface between the solvents. The packed-bed gradient generator is a cylindrical tube filled with chemically inert glass beads. Other axial column contours such as a double taper column or bell-shaped entrance and exit regions can be used to tailor the gradient profile. The static packed-bed gradient generator can be placed either on the low pressure inlet side of the high pressure pump, or the high pressure outlet side of the pump. While low pressure operation may provide added convenience, high pressure operation provides additional pulse dampening ability. The high pressure placement of the packed-bed generator would be the only option for use with syringe pumps common in microbore HPLC.

Abstract translation: 使用填充床梯度发生器产生高效液相色谱（HPLC）中的溶剂组成梯度。 由于涡流和分子扩散，自然分散发生在通过颗粒床的流中。 该分散体将溶剂之间的界面处的两个溶剂之间的明确界定改变成期望的误差函数型梯度曲线。 填充床梯度发生器是填充有化学惰性玻璃珠的圆柱形管。 可以使用其他轴向柱轮廓，例如双锥形柱或钟形入口和出口区域来定制梯度轮廓。 静态填充床梯度发生器可以放置在高压泵的低压入口侧或泵的高压出口侧。 虽然低压操作可以提供更多的便利性，但是高压操作提供额外的脉冲阻尼能力。 填充床发生器的高压放置将是与微孔HPLC中常见的注射泵一起使用的唯一选择。