6850/6890 分流动画 Split/Splitless 进样口 – 部件 衬管 O-圈 进样垫 衬管 Split Splitless Inlet Component Identification: The drawing on the left will be used to demonstrate Split operation of the Agilent 6850 and 6890 Split/Splitless Capillary Inlet. The internal components in the injection port are as follows: 1) Septum 2) Inlet Liner 3) Liner O-Ring seal 4) Gold Inlet seal 5) Capillary Column 镀金密封垫 毛细管柱 5/4/00

6850/90 Split/Splitless 进样口 – 部件 Septum SEPTUM PURGE VENT Inlet Split Port Split Splitless Inlet Component Identification: The components external to the inlet injection port will also be identified as follows: 1) Carrier gas supply connection 2) EPC Proportional Valve 1 3) Flow Sensor 4) Septum 5) Inlet Split vent 6) Split vent trap 7) Pressure sensor 8) Purge on/off valve 9) EPC Proportional Valve 2 10) Septum Purge Regulator 11) Septum Purge Vent 12) Split Vent

6850/90 分流动画 – 缺省条件 TOTAL FLOW CONTROL LOOP SEPTUM PURGE PRESSURE SENSOR SEPTUM PURGE REGULATOR PSI ML/MIN 80 PSI FLOW SENSOR INPUT PRESSURE SPLIT VENT PROPORTIONAL VALVE 1 SPLIT VENT TRAP PURGE VALVE OPEN GOLD SEAL The Capillary Inlet is shown in Split Mode with no flow or pressure setpoints entered. PROPORTIONAL VALVE 2

6850/90 分流动画 – 总流量设定 TOTAL FLOW CONTROL LOOP SEPTUM PURGE PRESSURE SENSOR SEPTUM PURGE REGULATOR PSI 205 ML/MIN 80 PSI FLOW SENSOR INPUT PRESSURE SPLIT VENT 205 ML/MIN PROPORTIONAL VALVE 1 SPLIT VENT TRAP PURGE VALVE OPEN GOLD SEAL The Inlet Total Flow is set to 205 ml/minute. Proportional valve 1 opens to introduce flow, and then controls at the setpoint. The flow path is through the inlet liner, around the outside of the liner and out the split vent through the filter, Purge Valve and Proportional Valve 2. Proportional valve 2 is completely open until a pressure setpoint is entered. PROPORTIONAL VALVE 2 PRIMARY FLOW PATH REDUCED FLOW PATH

BACK PRESSURE CONTROL LOOP 6850/90 分流动画 – 进样口压力设定 TOTAL FLOW CONTROL LOOP SEPTUM PURGE REGULATOR FIXED @ 3ML/MIN PRESSURE SENSOR 10 PSI 205 ML/MIN 80 PSI FLOW SENSOR INPUT PRESSURE BACK PRESSURE CONTROL LOOP SPLIT VENT 200 ML/MIN PROPORTIONAL VALVE 1 SPLIT VENT TRAP PURGE VALVE OPEN GOLD SEAL An Inlet pressure of 10 PSI is entered. 10 PSI is the pressure required to establish 2 ml/minute of flow on this particular column at the oven starting temperature. Proportional valve 2 starts to close off, increasing Inlet back pressure, then controlling at 10 PSI. Once the inlet pressurizes, the septum purge and column flows are established. The Total flow is equal to the sum of Column + Split Vent + Septum Purge flows. PROPORTIONAL VALVE 2 PRIMARY FLOW PATH REDUCED FLOW PATH COLUMN FLOW 2 ML/MIN PRESSURIZED GAS

BACK PRESSURE CONTROL LOOP 6850/90分流动画 准备进样 TOTAL FLOW CONTROL LOOP SEPTUM PURGE REGULATOR FIXED @ 3ML/MIN PRESSURE SENSOR 10 PSI 205 ML/MIN 80 PSI FLOW SENSOR INPUT PRESSURE BACK PRESSURE CONTROL LOOP SPLIT VENT 200 ML/MIN PROPORTIONAL VALVE 1 SPLIT VENT TRAP PURGE VALVE OPEN Mode: Split Temp 250 250 Pressure 10.0 10.0 Split Ratio 100 Split Flow 200 Tot Flow 205.0 205.0 Gas Saver OFF The Capillary Inlet is Ready for Injection. The split ratio is equal to the split vent flow rate divided by the column flow rate - in this example 100:1. PROPORTIONAL VALVE 2 Split Ratio - 100:1 COLUMN FLOW 2 ML/MIN

BACK PRESSURE CONTROL LOOP 6850/90分流动画 插针 TOTAL FLOW CONTROL LOOP SEPTUM PURGE REGULATOR FIXED @ 3ML/MIN PRESSURE SENSOR 10 PSI 205 ML/MIN 80 PSI FLOW SENSOR INPUT PRESSURE BACK PRESSURE CONTROL LOOP SPLIT VENT 200 ML/MIN PROPORTIONAL VALVE 1 SPLIT VENT TRAP PURGE VALVE OPEN GOLD SEAL The sample syringe is inserted into the injection port. PROPORTIONAL VALVE 2 Split Ratio - 100:1 COLUMN FLOW 2 ML/MIN

BACK PRESSURE CONTROL LOOP 6850/90 分流动画 进样 TOTAL FLOW CONTROL LOOP SEPTUM PURGE REGULATOR FIXED @ 3ML/MIN PRESSURE SENSOR 10 PSI 205 ML/MIN 80 PSI FLOW SENSOR INPUT PRESSURE BACK PRESSURE CONTROL LOOP SPLIT VENT 200 ML/MIN PROPORTIONAL VALVE 1 SPLIT VENT TRAP PURGE VALVE OPEN GOLD SEAL The plunger is depressed, injecting liquid sample into the inlet. PROPORTIONAL VALVE 2 Split Ratio - 100:1 COLUMN FLOW 2 ML/MIN

BACK PRESSURE CONTROL LOOP 6850/90 分流动画 样品蒸发 TOTAL FLOW CONTROL LOOP SEPTUM PURGE REGULATOR FIXED @ 3ML/MIN PRESSURE SENSOR 10 PSI 205 ML/MIN 80 PSI FLOW SENSOR INPUT PRESSURE BACK PRESSURE CONTROL LOOP SPLIT VENT 200 ML/MIN PROPORTIONAL VALVE 1 SPLIT VENT TRAP PURGE VALVE OPEN Glass Wool GOLD SEAL The sample is vaporized. It is important to be sure that the inlet liner has sufficient internal volume to contain the solvent vapor. The amount of vapor will depend on the solvent used, the injection volume, and the inlet temperature and pressure. Because of the very short sample residence time in the inlet it is beneficial to use an inlet liner that has some glass wool inserted to provide adequate surface area for complete sample vaporization and mixing. This will help minimize boiling point discrimination during the split process. PROPORTIONAL VALVE 2 Split Ratio - 100:1 COLUMN FLOW 2 ML/MIN

BACK PRESSURE CONTROL LOOP 6850/90 分流动画 样品分流 - 良好的衬管设计? TOTAL FLOW CONTROL LOOP SEPTUM PURGE REGULATOR FIXED @ 3ML/MIN PRESSURE SENSOR 10 PSI 205 ML/MIN 80 PSI FLOW SENSOR INPUT PRESSURE BACK PRESSURE CONTROL LOOP SPLIT VENT 200 ML/MIN Glass Wool PROPORTIONAL VALVE 1 SPLIT VENT TRAP PURGE VALVE OPEN The recommended split liner is shown above. This liner incorporate the following design features: 1) Glass wool held in position by glass indents to provide mixing and to wipe the syringe needle after the injection. 2) The O.D. is slightly smaller than splitless liners to provide an unrestricted path for the split flow. 3) A taper at the bottom of the inlet to direct sample to the column. 4) A glass positioning bead to provide clearance between the bottom of the liner and the gold seal. This further reduces split flow restriction, improving split precision. 5) The liner is also deactivated. Agilent Split Liner - 5183-4647 Smaller O.D. Liner Open Split Flow Path PROPORTIONAL VALVE 2 Tapered Liner Glass Positioning Bead Split Ratio - 100:1 COLUMN FLOW 2 ML/MIN

BACK PRESSURE CONTROL LOOP 6850/90 分流动画 分流继续 TOTAL FLOW CONTROL LOOP SEPTUM PURGE REGULATOR FIXED @ 3ML/MIN PRESSURE SENSOR 10 PSI 205 ML/MIN 80 PSI FLOW SENSOR INPUT PRESSURE BACK PRESSURE CONTROL LOOP SPLIT VENT 200 ML/MIN PROPORTIONAL VALVE 1 SPLIT VENT TRAP PURGE VALVE OPEN The entire split process in the inlet occurs in a fraction of a second. In this example if the liner has an internal volume of 1 ml, then the split occurs in 1/200 of a minute. PROPORTIONAL VALVE 2 Split Ratio - 100:1 COLUMN FLOW 2 ML/MIN

BACK PRESSURE CONTROL LOOP 6850/90 分流动画 分流完成 TOTAL FLOW CONTROL LOOP SEPTUM PURGE REGULATOR FIXED @ 3ML/MIN PRESSURE SENSOR 10 PSI 205 ML/MIN 80 PSI FLOW SENSOR INPUT PRESSURE BACK PRESSURE CONTROL LOOP SPLIT VENT 200 ML/MIN PROPORTIONAL VALVE 1 SPLIT VENT TRAP PURGE VALVE OPEN In this example if 1 micro liter of sample was injected, .01 ul went onto the GC column. PROPORTIONAL VALVE 2 Split Ratio - 100:1 COLUMN FLOW 2 ML/MIN

BACK PRESSURE CONTROL LOOP 6850/90 分流动画 样品分离并检测 TOTAL FLOW CONTROL LOOP SEPTUM PURGE REGULATOR FIXED @ 3ML/MIN PRESSURE SENSOR 10 PSI 205 ML/MIN 80 PSI FLOW SENSOR INPUT PRESSURE BACK PRESSURE CONTROL LOOP SPLIT VENT 200 ML/MIN PROPORTIONAL VALVE 1 SPLIT VENT TRAP PURGE VALVE OPEN Once the split is complete the sample is separated on the GC column, detected and the chromatogram is completed. PROPORTIONAL VALVE 2 Split Ratio - 100:1 COLUMN FLOW 2 ML/MIN

6850/90 分流 省气模式 – 设定 55 ml/min 动画 在进样完成后 TOTAL FLOW CONTROL LOOP SEPTUM PURGE REGULATOR FIXED @ 3ML/MIN PRESSURE SENSOR 10 PSI 55 ML/MIN 80 PSI FLOW SENSOR INPUT PRESSURE BACK PRESSURE CONTROL LOOP SPLIT VENT 50 ML/MIN PROPORTIONAL VALVE 1 SPLIT VENT TRAP Mode: Split Temp 250 250 Pressure 10.0 10.0 Split Ratio 100 Split Flow 200 Tot Flow 205.0 205.0 Gas Saver ON Saver Flow 50.0 Saver Time 0.5 PURGE VALVE OPEN A useful and cost saving feature of the 6850 and 6890 GC’s is gas saver. The gas saver can be turned on during the GC run any time after the injection split is completed. The gas saver total flow is lower than the total flow during injection. The total flow stays low during the rest of the run and between runs, thus saving large amounts of carrier gas and money. PROPORTIONAL VALVE 2 Split Ratio - 100:1 COLUMN FLOW 2 ML/MIN