Agilent 1100 Series Capillary LC System System Manual s1
Notices © Agilent Technologies, Inc. 2002 Warranty No part of this manual may be reproduced in any form or by any means (including electronic storage and retrieval or translation into a foreign language) without prior agreement and written consent from Agilent Technologies, Inc. as governed by United States and international copyright laws. The material contained in this document is provided “as is,” and is subject to being changed, without notice, in future editions.
In This Manual… This manual contains information for using your Capillary LC System. 1 Installing your Capillary LC System This chapter describes how to install and configure the Capillary LC System. 2 Optimizing Performance This chapter discusses how to optimize your capillary LC system to achieve best chromatographic results. 3 Capillaries and Fittings Overview of the capillaries and according fittings used in the capillary LC System.
iv 1100 Series Capillary LC System Manual
Contents 1 Installing your Capillary LC System Site Requirements 2 Physical Specifications 4 System Installation Process 6 Installing a Capillary LC System with a Non-Thermostatted Sampler Install the Diode Array Detector (DAD) (G1315B) 8 Install the Thermostatted Column Compartment (TCC) (G1316A) Install the Micro Well-plate Sampler (G1377A) 10 Install the Capillary Pump (G1376A) 11 Install the Micro Vacuum Degasser (G1379A) 12 Install the Solvent Cabinet 13 7 9 Installing a Capillary LC System wi
contents 2 Optimizing Performance Hints for Successful Use of the Capillary Pump Pump issues 30 Fused Silica Capillary issues 31 Sampler issues 32 Column thermostat issues 32 DAD issues 32 Solvent Information 30 33 Prevent Blocking of Solvent Inlet Filters 34 Checking the solvent inlet filters 34 Cleaning the Solvent Filters 35 Hints for the Micro Vacuum Degasser When to use Alternative Seals 37 How to Choose the Primary Flow Static Mixer and Filter 40 The standard static mixer The standard filter 40
contents 4 Basic System Troubleshooting System Pressure Abnormally Low 56 System Pressure Abnormally High 57 EMPV failed to initialize (micro mode only) 58 Unstable column flow and/or system pressure Poor peak shape 59 61 Failure to produce peaks, or abnormally small peaks, after injection Wandering Detector Baseline 63 User interface displays error messages for specific modules 5 62 64 Parts and Materials Micro Vacuum Degasser 66 Micro Vacuum Degasser Cover Parts 68 Capillary Pump 69 Solven
contents Vial Trays 94 Thermostatted Column Compartment 95 Micro Column Switching Valve 97 Thermostatted Column Compartment Sheet Metal Kit 98 Thermostatted Column Compartment Cover Parts 99 Thermostatted Column Compartment Leak Parts 100 Diode Array Detector 101 DAD - Optical Unit Assembly 103 500 nl Flow Cell 105 Fan Assembly Parts 107 Holmium Oxide Filter 108 Diode Array Detector Cover Parts 109 Common Parts 110 Control Module (G1323B) 110 Rear panel 111 Power and Status Light Pipes 112 Leak Parts 113
contents CAN Cable 132 External Contact Cable RS-232 Cable Kit 134 LAN Cables 134 6 133 Options Extended Flow Range Kit (G1376-69707) 136 Installing the Extended Flow Range Kit 138 0.1 - 2.5 ml/min Flow Capillary Kit (5065-4495) 139 Installing the 0.1 - 2.
contents A Safety Information General 176 Operation 176 Safety Symbols 177 Lithium Batteries Information 178 Danish Information: 178 Radio Interference 179 Sound Emission 179 Solvent Information 179 Agilent Technologies on Internet 180 Index x 181 1100 Series Capillary LC System Manual
Agilent 1100 Series Capillary LC System System Manual 1 Installing your Capillary LC System Site Requirements 2 Physical Specifications 4 System Installation Process 6 Installing a Capillary LC System with a Non-Thermostatted Sampler 7 Installing a Capillary LC System with a Thermostatted Micro Sampler 14 Get the System Ready for the First Injection 22 Inject the Check-out Sample 26 Agilent Technologies 1
1 Installing your Capillary LC System Site Requirements A suitable environment is important to ensure optimum performance of the Capillary LC system. Power Consideration The modules power supply has wide ranging capability (see Table 1 on page 4). It accepts any line voltage in the range described in the above mentioned table. Consequently there is no voltage selector in the rear of the modules.
Installing your Capillary LC System 1 Bench Space The modules dimensions and weight (see Table 2 on page 5) allow to place the Capillary LC system on almost any laboratory bench. It needs an additional 2.5 cm (1.0 inches) of space on either side and approximately 8 cm (3.1 inches) in the rear for the circulation of air and electric connections. If a Thermostatted Well Plate Sampler is installed, an additional 25 cm (10 inches) of space on either side for the circulation of air, and approximately 8 cm (3.
1 Installing your Capillary LC System Physical Specifications Table 1 Common Physical Specifications Type Specification Comments Line voltage 100 – 120 or 220 – 240 VAC, ± 10 % Wide-ranging capability Line frequency 50 or 60 Hz, ± 5 % Ambient operating temperature 4 – 55 °C (41 – 131 °F) Ambient non-operating temperature -40 – 70 °C (-4 – 158 °F) Humidity < 95 %, at 25 – 40 °C (77 – 104 °F) Operating Altitude Up to 2000 m (6500 ft) Non-operating altitude Up to 4600 m (14950 ft) Safety
Installing your Capillary LC System 1100 Table 2 1 Module Specific Specifications Agilent 1100 Module Part Number Weight Dimension (h × w × d) Power consumption Capillary Pump G1376A 17 kg 39 lb 345x435x180 (mm) 13.5x17x7 (inches) 220 VA max Micro Vacuum Degasser G1379A 7.5 kg 16.5 lb 345x435x80 (mm) 13.5x17x3.1 (inches) 30 VA max Thermostatted Micro Autosampler (Micro-ALS) G1387A 14.2 kg 31.3 lb 345x435X200 (mm) 13.
1 Installing your Capillary LC System System Installation Process Damaged Packaging If the delivery packaging shows signs of external damage, please call your sales and service office immediately. Inform your service representative that something may have been damaged during shipment. CAU TI O N 6 If there are signs of damage, please do not attempt to install the damaged module.
Installing your Capillary LC System 1 Installing a Capillary LC System with a Non-Thermostatted Sampler These instructions will produce a single stack of modules, with the Diode Array Detector (DAD) on the bottom. Required cables, tubes and capillaries for each module are included with the system shipment, or found in the module accessory kits.
1 Installing your Capillary LC System Install the Diode Array Detector (DAD) (G1315B) Ensure the line power switch at the front of the DAD is off. WA RN ING Connect the power cable to power only after you have finished the hardware installation of all modules in the stack. 1 Ensure the line power switch at the front of the Diode Array Detector (DAD) is off. 2 If the system is to be connected to the user interface by LAN, install the JetDirect card into the DAD.
Installing your Capillary LC System 1 Install the Thermostatted Column Compartment (TCC) (G1316A) WA RN ING Connect the power cable to power only after you have finished the hardware installation of all modules in the stack. 1 Ensure the line power switch at the front of the Thermostatted Column Compartment (TCC) is off 2 Place the TCC on top of the DAD. Make sure that the two modules are interlocked correctly. 3 Connect the Can-bus cable (5181-1516) to one of the CAN connectors at the rear of the TCC.
1 Installing your Capillary LC System Install the Micro Well-plate Sampler (G1377A) WA RN ING Connect the power cable to power only after you have finished the hardware installation of all modules in the stack. 1 Ensure the line power switch at the front of the micro well-plate sampler (micro WPS) is off. 2 Place the micro WPS on top of the TCC. Make sure that the two modules are interlocked correctly. 3 Remove the sampler shipping protection foam.
Installing your Capillary LC System 1 Install the Capillary Pump (G1376A) WA RN ING Connect the power cable to power only after you have finished the hardware installation of all modules in the stack. 1 Ensure the line power switch at the front of the capillary pump is off. 2 Place the capillary pump on top of the micro WPS. Make sure that the two modules are interlocked correctly. 3 Connect the power cable to the power socket at the rear of the capillary pump.
1 Installing your Capillary LC System Install the Micro Vacuum Degasser (G1379A) WA RN ING Connect the power cable to power only after you have finished the hardware installation of all modules in the stack. 1 Ensure the line power switch at the front of the micro vacuum degasser is off. 2 Place the degasser on top of the pump. Make sure that the two modules are interlocked correctly. 3 Connect one end of the remote cable (5061-3378) to the rear of the degasser.
Installing your Capillary LC System 1 Install the Solvent Cabinet 1 Place the solvent cabinet on top of the degasser. Make sure that the two modules are interlocked correctly. 2 The solvent cabinet accessory kit has 4 bottle head assemblies (G1376-60003). 3 Connect a bottle head assembly to each of the degasser INLET ports. Use the labels provided with each bottle head assembly to appropriately label each bottle head assembly.
1 Installing your Capillary LC System Installing a Capillary LC System with a Thermostatted Micro Sampler These instructions will produce two stacks of modules. The left-hand stack will consist of the capillary pump, degasser and solvent cabinet. The right-hand stack will consist of the thermostatted micro sampler (bottom), thermostatted column compartment (TCC), and diode array detector (DAD) on top.
Installing your Capillary LC System 1 Install the Thermostat for 1100 Samplers (G1330B) CAU TI O N Connect the power cable to the thermostat module power socket only after you have connected the thermostat-to-sampler cable (G1330-81600) between the thermostat module and the micro sampler. Failure to follow this warning will result in damage to the electronics of the thermostat module and the sampler. 1 Place the thermostat for 1100 samplers (thermostat module) on the bench.
1 Installing your Capillary LC System Install the Micro Sampler (G1387A Micro Autosampler (ALS), or G1378A Micro Well-plate Sampler) CAU TI O N Connect the power cable to the thermostat module power socket only after you have connected the thermostat-to-sampler cable (G1330-81600) between the thermostat module and the sampler. Failure to follow this warning will result in damage to the electronics of the thermostat module and the sampler.
Installing your Capillary LC System 1 Install the Thermostatted Column Compartment (TCC) (G1316A) WA RN ING Connect the power cable to power only after you have finished the hardware installation of all modules in the stack. 1 Ensure that the line power switch at the front of the thermostatted column compartment (TCC) is off. 2 Place the TCC on top of the micro sampler. Make sure that the two modules are interlocked correctly.
1 Installing your Capillary LC System Install the Diode Array Detector (DAD) (G1315B) WA RN ING Connect the power cable to power only after you have finished the hardware installation of all modules in the stack. 1 Ensure the line power switch at the front of the diode array detector DAD is off. 2 If the system is to be connected to the user interface by LAN, install the JetDirect card into the DAD. See Replacing the Interface Board in the DAD Reference Manual. 3 Place the DAD on top of the TCC.
Installing your Capillary LC System 1 Install the Capillary Pump (G1376A) WA RN ING Connect the power cable to power only after you have finished the hardware installation of all modules in the stack. 1 Ensure the line power switch at the front of the capillary pump is off. 2 Place the capillary pump on the bench, positioned to the left of the micro sampler thermostat module. 3 Connect the power cable to the power socket at the rear of the capillary pump.
1 Installing your Capillary LC System Install the Micro Vacuum Degasser (G1379A) WA RN ING Connect the power cable to power only after you have finished the hardware installation of all modules in the stack. 1 Ensure the line power switch at the front of the micro vacuum degasser (degasser) is off. 2 Place the degasser on top of the pump. Make sure that the two modules are interlocked correctly. 3 Connect one end of the remote cable (5061-3378) to the rear of the degasser.
Installing your Capillary LC System 1 Install the Solvent Cabinet 1 Place the solvent cabinet on top of the degasser. Make sure that the two modules are interlocked correctly. 2 The solvent cabinet accessory kit has 4 bottle head assemblies (G1376-60003). 3 Connect a bottle head assembly to each of the degasser INLET ports. Use the labels provided with each bottle head assembly to appropriately label each bottle head assembly.
1 Installing your Capillary LC System Get the System Ready for the First Injection When you are using the system for the first time after installation, best results are obtained by performing the following 3-step system preparation, in the order given below: 1 Manually priming the solvent channels. 2 Purging the pump. 3 Conditioning the system under method conditions. WA RN ING 22 When opening capillary or tube fittings, solvents may leak.
Installing your Capillary LC System 1 Manually Priming the Solvent Channels. NO TE This procedure should be done before the modules are turned on. 1 The degasser accessory kit contains a 20ml plastic syringe and a solvent tube adapter for this syringe. Push the adapter onto the syringe. 2 Pour the intended analytical solvents into the solvent bottles, and install the bottles on the desired solvent channels. Install Isopropanol on channels which will not be used right away.
1 Installing your Capillary LC System Purging the Pump 1 Make sure that the 1/8 inch plastic waste tube is tightly connected to the barbed waste fitting of the pump EMPV, and routed to an appropriate waste container. 2 Turn on the LC System. All system parameters should be set to default. The degasser should also be turned on at this time. 3 Initialize the system. Then, access the pump controls and make sure the pump mode is set to Normal. 4 Access the pump Purge control.
Installing your Capillary LC System 1 Conditioning the System Under Method Conditions If you wish to condition the analytical column at this time, leave the column installed in the TCC. If you do not wish to condition the analytical column at this time, then remove the column. In the TCC, connect the sampler-to-column capillary (G1375-87304) directly to the DAD flow cell inlet capillary (G1315-68703).
1 Installing your Capillary LC System Inject the Check-out Sample The purpose of the instrument check is to demonstrate that all modules of the instrument are correctly installed and connected. It is not a test of the instrument performance. A single injection of the Agilent Technologies isocratic test sample (Agilent part number 01080-68704) is made under the method conditions given below: Table 4 Method conditions for injecting a test sample Flow: 15.0 µl/minute Stoptime: ~7.
Installing your Capillary LC System 1 Procedure 1 Make a single injection of the isocratic test standard under the conditions given Table 4 on page 26. 2 Compare the resulting chromatogram with the typical chromatogram shown in Figure 1. Typical Chromatogram A typical chromatogram for this analysis is shown in Figure 1. The exact profile of the chromatogram will depend on the chromatographic conditions.
1 28 Installing your Capillary LC System 1100 Series Capillary LC System Manual
Agilent 1100 Series Capillary LC System System Manual 2 Optimizing Performance Hints for Successful Use of the Capillary Pump 30 Solvent Information 33 Prevent Blocking of Solvent Inlet Filters 34 Hints for the Micro Vacuum Degasser 36 When to use Alternative Seals 37 How to Choose the Primary Flow 38 Static Mixer and Filter 40 How to Optimize the Compressibility Compensation Setting 41 This chapter shows how to optimize your capillary LC system to achieve best chromatographic results: Agilent Technologi
2 Optimizing Performance Hints for Successful Use of the Capillary Pump Pump issues • Flush the pump extensively. First with in the purge mode, second with a pressure applied to remove all the gas bubbles. It is recommended to do this first with 100% A and than 100%B. • The system pressure must be higher than 20 Bar at the pump outlet. • In micro mode abnormally high column flow variations are an indication of dirt within the system, blocked filters or loose pump valves.
Optimizing Performance 2 • To achieve the best flow stability, especially in the micro mode, %Ripple must be within acceptable values, typically no worse than 2%. Fused Silica Capillary issues • When you connect a capillary (especially at the column) press it smoothly into the fitting to avoid air gaps. Incorrect setting will result in dispersion causing tailing or footing peaks. NO TE Do not overtighten the fused silica capillaries.
2 Optimizing Performance Sampler issues • For fast gradient use valve to bypass function after the sample is transferred to the column. This function results in smaller delay times and sharper gradient curves. • When doing automated gradient runs, use the fast composition change/reconditioning function to equilibrate the system between runs. Column thermostat issues • Use the column brackets to put the column in contact with the heat exchanger.
Optimizing Performance 2 Solvent Information Always filter solvents through 0.4 µm filters, small particles can permanently block the capillaries and valves. Avoid the use of the following steel-corrosive solvents: • Solutions of alkali halides and their respective acids (for example, lithium iodide, potassium chloride, and so on).
2 Optimizing Performance Prevent Blocking of Solvent Inlet Filters Contaminated solvents or algae growth in the solvent bottle will reduce the lifetime of the solvent filter and will influence the performance of the capillary pump. This is especially true for aqueous solvents or phosphate buffers (pH 4 to 7). The following suggestions will prolong lifetime of the solvent filter and will maintain the performance of the capillary pump.
Optimizing Performance 2 Cleaning the Solvent Filters • Remove the blocked solvent filter from the bottle-head assembly and place it in a beaker with concentrated nitric acid (65%) for one hour. • Thoroughly flush the filter with bidistilled water (remove all nitric acid, some columns can be damaged by nitric acid). • Replace the filter. CAU TI O N Never use the system without solvent filters.
2 Optimizing Performance Hints for the Micro Vacuum Degasser If you are using the vacuum degasser for the first time, if the vacuum degasser was switched off for any length of time (for example, overnight), or if the vacuum degasser lines are empty, you should prime the vacuum degasser before running an analysis. The vacuum degasser can be primed by pumping solvent with the capillary pump at high flow rate (2.5 ml/min).
Optimizing Performance 2 When to use Alternative Seals The standard seals for the capillary pump can be used for most applications. However that use normal phase solvents (for example hexane) are not suitable for the standard seals and require a different seal when used for a longer time in the capillary pump. In this case we recommend the use of polypropylene seals, part number 0905-1420 (pack of 2). These seals have less abrasion compared to the standard seals.
2 Optimizing Performance How to Choose the Primary Flow Primary Flow is a parameter which exists only when the capillary pump is used in the Micro mode. Primary flow is defined as the flow volume and composition available at the inlet to the EMPV. Using this available primary flow, the EMPV and flow sensor work together to deliver and control the requested column flow.
Optimizing Performance 2 Fast Gradients range (800-1300 µl/min) In this range, the pump gradient delay time is as short as possible. This range is specifically recommended for fast-gradient analyses (<3 min.). Solvent consumption is highest in this range. Table 5 gives approximate primary flow values (in µl/min) as a function of selected primary flow range vs.
2 Optimizing Performance Static Mixer and Filter The capillary pump is equipped with a static mixer and an inline filter in front of the EMPV. The standard static mixer The standard static mixer has a volume of typically 420 µl. To reduce the delay volume of the capillary pump you can remove the mixer. Conditions to remove the static mixer: • The delay volume of the capillary pump should be reduced to a minimum for fastest gradient response. • The detector is used at medium or low sensitivity.
Optimizing Performance 2 How to Optimize the Compressibility Compensation Setting The compressibility compensation default settings are 50 × 10-6 /bar (best for most aqueous solutions) for pump head A and 115 × 10-6 /bar (to suit organic solvents) for pump head B. The settings represent average values for aqueous solvents (A side) and organic solvents (B side). Therefore it is always recommended to use the aqueous solvent on the A side of the pump and the organic solvent on the B side.
2 Optimizing Performance 5 Starting with a compressibility setting of 10 × 10-6 /bar increase the value in steps of 10. Re-zero the integrator as required. The compressibility compensation setting that generates the smallest pressure ripple is the optimum value for your solvent composition. 6 Repeat step 1 through step 5 for the B channel of your capillary pump. Optimize your compressibility settings by using the values for various solvents listed in the following table: .
Optimizing Performance 2 The Fast Composition Change/Reconditioning Function Purpose The capillary pump and the micro well-plate sampler are recommended for capillary LC applications. Capillary LC methods have very low column flow rates, typically in the range of 1-20 µl/min. At such low flow rates, re-equilibrating the system to the initial mobile phase composition between automated gradient runs may require a long time.
2 Optimizing Performance 2 When the Fast System Flush time has elapsed, the micro well-plate sampler needle is returned to the needle-seat. The pump returns to the normal operating mode, reconditioning the column at the flow and initial composition defined in the current method. The column is reconditioned for the Column Reconditioning time defined in the user interface. If multiple injections are in progress, the next injection will begin when Fast Composition Change/Reconditioning is completed.
Agilent 1100 Series Capillary LC System System Manual 3 Capillaries and Fittings Capillary Flow Diagram 46 Connecting capillaries for the capillary LC system 47 Fittings and Ferrules 52 Instructions to connect a capillary.
3 Capillaries and Fittings Capillary Flow Diagram The flow diagram in Figure 2 gives an overview of the capillaries and according fittings used in the capillary LC System.
Capillaries and Fittings 3 Connecting capillaries for the capillary LC system Table 7 Generic capillaries for use with a capillary LC system Diameter (µm) Length (mm) Material Volume (µl) Pressure drop (Bar) Part number Item Fitting type* 1 A/A SST† G1311-67304 2 A/A SST G1312-67300 3 A/A SST G1312-67302 4 A/A SST G1312-67304 5 A/A 250 130 SST 6.4 0 01090-87308 6 A/A 250 130 SST 6.4 0 01090-87308 7 A/A 170 280 SST 6.
3 Capillaries and Fittings Table 8 Specific capillaries for use with a 20 µl flow sensor Item Fitting type Diameter (µm) Length (mm) Material Volume (µl) Pressure drop (Bar) Part number 8 B/B 50 220 PFS* 1 2 G1375-87301 9 B/C 50 550 PFS 1 6 G1375-87310 10 C/D 50 500 PFS 1 5 G1375-87304 11 D/E 50 400 PFS 1 4 G1315-68703 13 (micro ALS) C/B 50 200 PFS 1 2 G1375-87302 13 (micro WPS) C/B 100 200 PFS <1 G1375-87312 * PFS: Peek coated fused silica The pre
Capillaries and Fittings Table 10 3 Specific capillaries for use with a flow higher than 200 µl/min Item descriptions see list below) Fitting type* Diameter (µm) Length (mm) Material Volume (µl) Pressure drop (Bar) Part number see description 1 below A/A 170 280 SST† 6.4 2 G1375-87400 see description 2 B/C 125 550 PFS** 6.8 15 G1375-87318 13 B/C 100 200 PFS 1.
3 Capillaries and Fittings Table 11 Specific capillaries for use with a micro CSV and a 20 µl flow sensor From To Fitting Type* Diameter Length (µm) (mm) Volume (µl) Pressure drop (Bar) Part number Inj. valve (Port 6) Micro CSV (Port 4) C/D 50 280 1 3 G1375-87309 Inj.
Capillaries and Fittings 3 From injection valve Column 1 Column 2 3 2 4 5 6 1 To detector Figure 3 Table 13 Micro column switching valve connections Additional capillaries Description Fitting type Diameter (µm) Length (mm) Material Volume (µl) Pressure Part number drop (Bar) OQ/PV capillary C/D 50 400 PFS * 0.8 4.4 G1375-87314 MS capillary C/2xD 50 1100 PFS * 2.2 12 5065-9906 MS capillary E/2xD 50 700 PFS * 1.4 7.
3 Capillaries and Fittings Fittings and Ferrules Table 14 Fittings and ferrules Fitting Name Type Description A Swagelock 1/16” SST fitting, front and back ferrule 10/pk 5062-2418 B Lite Touch M4/16” SST fitting 10/pk 5063-6593 B Lite Touch 1/32” SST ferrule and lock ring 10/pk 5065-4423 C Rheodyne PEEK fitting 6 fitt/2 plug 5065-4410 D Finger Tight Double winged nuts and 1/32” ferrules 10/pk E Lite touch Detector M4/16” SST fitting 10/pk 5063-6593 E Lite touch Detector SST
Capillaries and Fittings 3 Instructions to connect a capillary. With Swagelock fitting (type A) • Slide the nut, the compression ring and the ferrule onto the tubing. • Insert into the receiving port and finger tighten the fitting into the port. • Using a 1/4 inch wrench tighten the fitting 3/4 wrench turn. With Rheodyne fitting (type C). • Slide the fitting on the capillary. • Insert into the receiving port, and finger tighten the fitting into the port.
3 Capillaries and Fittings Hints for Successful use of Capillaries and Fittings • Never overtighten a fitting. • Never cut a capillary • Take care when you bend a capillary (diameter never below 40 mm). • Avoid the use of alkaline solutions (pH > 8.5) which can attack the fused silica from the capillaries. • When connecting, press the capillary smoothly into the fitting to avoid air gaps. • If a capillary leaks, never retighten it under flow.
Agilent 1100 Series Capillary LC System System Manual 4 Basic System Troubleshooting System Pressure Abnormally Low 56 System Pressure Abnormally High 57 EMPV failed to initialize (micro mode only) 58 Unstable column flow and/or system pressure 59 Poor peak shape 61 Failure to produce peaks, or abnormally small peaks, after injection 62 Wandering Detector Baseline 63 User interface displays error messages for specific modules 64 In this troubleshooting guide, you will find a Possible Causes/Suggested Acti
4 Basic System Troubleshooting System Pressure Abnormally Low Symptoms: The current system pressure is significantly below the typical system pressure produced by this method with this column. System Pressure Abnormally Low: Possible causes and actions Possible Causes Suggested Actions Notes Leaks somewhere in the system • Use a flashlight and absorbent tissue to search for leaks throughout the system.
Basic System Troubleshooting 4 System Pressure Abnormally High Symptoms: The current system pressure is significantly above the typical system pressure produced by this method with this column. System Pressure Abnormally High: Possible causes and actions Possible Causes Suggested Actions The analytical column has become plugged • Replace the column. Otherwise, backflush the column or replace the column inlet frit.
4 Basic System Troubleshooting EMPV failed to initialize (micro mode only) Symptoms: An attempt to pump in the micro mode has resulted in either an EMPV Initialization Failed error message, or a permanent EMPV Initialization not ready message. EMPV failed to initialize: Possible Causes and Suggested Actions Possible Causes Suggested Actions Notes The no-flow pressure of the system is higher than 10 bar.
Basic System Troubleshooting 4 Unstable column flow and/or system pressure Symptoms: In the micro mode, the pump flow control system is active. The flow control system continuously measures the actual value of column flow, and maintains the requested column flow despite changes in system restriction. If the flow control becomes defective, actual column flow, hence system pressure, will fluctuate.
4 Basic System Troubleshooting Unstable column flow and/or system pressure: Possible Causes and Suggested Actions (continued) Possible Causes Suggested Actions Notes Dirty solvent inlet filters. Solvent intake is being restricted. %Ripple might also be too high. • Temporarily remove solvent inlet filters to see if they are the cause of the problem. If so, clean or replace the solvent inlet filters.
Basic System Troubleshooting 4 Poor peak shape Symptoms: The peak shape has taken on a fronting or tailing characteristic.
4 Basic System Troubleshooting Failure to produce peaks, or abnormally small peaks, after injection Symptoms: There are no peaks, or the peak size is significantly below the typical peak size for this method with this column. Failure to produce peaks, or abnormally small peaks, after injection: Possible Causes and Suggested Actions Possible Causes Suggested Actions Notes A leak in a sample carrying area of the system.
Basic System Troubleshooting 4 Wandering Detector Baseline Critical Decision Determine if the problem is in the DAD, or coming from the LC system: Remove the flow cell from the DAD. Close the cell cover, and see if the baseline performance improves. 1 If baseline performance has not improved: a Replace the lamp(s). b Evaluate the environment for excessive drafts, temperature changes, etc. 2 If baseline performance has improved, focus attention on the possible causes and suggested actions below.
4 Basic System Troubleshooting Wandering Detector Baseline Possible Causes and Suggested Actions (continued) Possible Causes Suggested Actions Notes Unstable flow and/or system pressure. • Refer to the problem Unstable flow and/or system pressure above. If your system suffers from this problem, go through the possible causes and suggested actions described there. Failure to maintain stable column flow or system pressure can also cause unwanted baseline activity.
Agilent 1100 Series Capillary LC System System Manual 5 Parts and Materials Micro Vacuum Degasser 66, Capillary Pump 69, Micro Well-plate Sampler 77, Thermostatted Micro Autosampler 86 Thermostatted Column Compartment 95, Diode Array Detector 101, Common Parts 110 Cables 121 This chapter shows detailed illustrations and lists for the parts identification for the complete system. It is divided into module specific parts sections and a common parts section.
5 Parts and Materials Micro Vacuum Degasser Table 16 gives an overview over the main assemblies: Table 16 66 Micro vacuum degasser main assemblies Item Description Part Number 1 Vacuum degasser control assembly G1322-66500 2 Board clip G1322-43100 3 Solenoid valve G1322-60003 4 Vacuum tube set G1379-67300 5 Fixing plate no PN 6 Vacuum pump G1322-60000 7 Leak tray G1379-27300 8 Leak pan, degasser G1379-47300 9 Vacuum chamber G1379-60001 10 Sensor assembly (included in the
Parts and Materials 5 11 1 2 3 4 5 9 6 9 7 8 Figure 4 Micro vacuum degasser main assemblies 1100 Series Capillary LC System Manual 67
5 Parts and Materials Micro Vacuum Degasser Cover Parts Table 17 Micro vacuum degasser cover parts Item Description Part Number 1 Cabinet kit, includes base, side panels, top and front cover 5062-8579 2 Tube clip 5041-8387 3 Logo plate, Agilent 1100 5042-1381 4 Front cover 5062-8580 1 2 3 4 Figure 5 68 Micro vacuum degasser cover parts 1100 Series Capillary LC System Manual
Parts and Materials 5 Capillary Pump Table 18 gives an overview over the main assemblies of the capillary pump.
5 Parts and Materials 1 14 13 2 12 11 10 9 3 8 4 7 5 6 Figure 6 70 Capillary pump main assembly 1100 Series Capillary LC System Manual
Parts and Materials 5 Solvent Cabinet and Bottle Head Assembly Table 19 Item Solvent cabinet and bottle-head assembly Description Part Number Solvent cabinet, complete assembly 5062-8581 1 Solvent tubing 5 m 5062-2483 2 Tube screw (pack of 10) 5063-6599 3 Ferrules with lock ring (pack of 10) 5063-6598 4 Bottle amber Bottle transparent 9301-1450 9301-1420 5 Solvent inlet filter (SST) 01018-60025 6 Leak pan, solvent cabinet 5042-1307 7 Front panel, solvent cabinet 5062-8580 8 Nam
5 Parts and Materials Capillary Pump Hydraulic Path Table 20 72 Capillary pump hydraulic path Item Description Part Number 1 Mixer G1312-87330 2 Damper to mixer capillary 01090-87308 3 EMPV to FS cap (220 mm, 50 µm) for 20 µl flow sensor EMPV to FS cap (220 mm, 100 µm) for 100 µl flow sensor G1375-87301 G1375-87305 4 Outlet ball valve to piston 2 capillary G1312-67300 5 FS to inj valve cap (550 mm, 50 µm) for 20 µl flow sensor FS to inj valve cap (550 mm, 100 µm) for 100 µl flow sensor
Parts and Materials 5 1 11 2 3 4 5 6 7 10 9 8 Figure 8 Capillary pump hydraulic path 1100 Series Capillary LC System Manual 73
5 Parts and Materials Pump-Head Assembly Table 21 Item 74 Pump-head assembly Description Part Number Pump head assembly, includes items marked with (*) G1311-60004 1* Outlet ball valve G1312-60012 2* Screw lock 5042-1303 3* Screw M5, 60 mm 0515-2118 4* Apdater G1312-23201 5 Pump chamber housing G1311-25200 6* Active inlet valve (complete with cartridge) Replacement cartridge for active inlet valve G1312-60010 5062-8562 7 Seal (pack of 2) or Seal (pack of 2), for normal phase appl
Parts and Materials 5 1 2 3 11 4 10 5 9 6 7 8 Figure 9 Pump head assembly 1100 Series Capillary LC System Manual 75
5 Parts and Materials Capillary pump cover parts Table 22 gives an overview over the cover parts of the capillary pump.
Parts and Materials 5 Micro Well-plate Sampler 13 1 12 2 3 4 11 14 5 10 9 6 7 8 Figure 11 Micro well-plate sampler main assemblies 1100 Series Capillary LC System Manual 77
5 Parts and Materials Table 23 78 Micro well-plate sampler main assemblies Item Description Part Number 1 Ribbon Cable (from SU to MTP) G1313-81602 2 Sample Transport assembly for G1377A G1377-60009 3 Sampling Unit assembly for G1377/78A (The assembly comes without injection valve and analytical head) G1377-60008 4 SLS board (not shown) G1367-66505 5 Analytical Head assembly (40 µl) for G1377/78A G1377-60013 6 Micro Injection valve assembly for G1377/78A 0101-1050 7 Needle Seat as
Parts and Materials 5 Sampling Unit for the Micro Well-plate Sampler 1 16 2 3 15 4 14 5 6 7 8 13 9 10 12 11 Figure 12 Sampling unit for the micro well-plate sampler 1100 Series Capillary LC System Manual 79
5 Parts and Materials Table 24 Item Sampling unit for the micro well-plate sampler Description Part Number Sampling Unit assembly for G1377/78A (The assembly comes without injection valve and analytical head) G1377-60008 1 Sampling unit connector board (SUD) G1313-66503 2 Belt gear for metering unit and needle arm 1500-0697 3 Stepper motor for metering unit and needle arm 5062-8590 4 Loop capillary, 40 µl for G1377/78A Loop capillary, 8 µl for G1377/78A G1377-87300 G1375-87315 5 Loop ca
Parts and Materials 5 Micro Analytical Head Assembly Table 25 Item Micro analytical head assembly Description Part Number Micro Analytical head assembly 40 µl, includes items 1 – 6 G1377-60013 1 Screws 0515-0850 2 Micro Plunger assembly 5064-8293 3 Adapter 01078-23202 4 Micro seal support assembly G1377-60002 5 Metering seal (pack of 1) 5022-2175 6 Head body G1377-27700 Screw M5, 60 mm lg, for mounting of assembly 0515-2118 1 2 3 4 5 6 Figure 13 Micro analytical head assembly
5 Parts and Materials Micro Injection Valve Assembly Table 26 Item Note: NO TE Micro injection valve assembly Description Part Number Micro Inj.-valve assembly, incl. items 1 – 2 – 3 – 5 – 6 0101-1050 2 Isolation seal 0100-1852 3 Micro rotor seal (Vespel) 0100-2088 5 Micro Stator head 0100-2089 6 Stator screws 1535-4857 The micro injection valve assembly has no ceramic stator face.
Parts and Materials 5 Micro Well-plate Sampler - Vial Trays Table 27 Micro well-plate sampler vial trays and tray base Item Description Part Number 1 Tray for 2 plates + 10 × 2-ml vials G1367-60001 2 Tray for 100 × 2-ml vials, thermostattable G1329-60001 3 Tray for 100 × 2-ml vials G1313-44500 4 Screws for springs 0515-0866 5 Spring G1313-09101 6 Spring stud 0570-1574 7 Tray base (includes items 4,5,6) G1329-60000 8 Adapter air channel G1329-43200 Plug channel (not shown) G13
5 Parts and Materials Table 28 Recommended plates and closing mat Description Rows Columns Plate height 384 Agilent 16 24 14.4 384 Corning 16 24 384 Nunc 16 96 Agilent Part Number Package 80 5042-1388 30 14.4 80 No Agilent PN 24 14.4 80 No Agilent PN 8 12 14.3 400 5042-1386 5042-1385 10 120 96 CappedAgilent 8 12 47.1 300 5065-4402 1 96 Corning 8 12 14.3 300 No Agilent PN 96 CorningV 8 12 14.3 300 No Agilent PN 96 DeepAgilent31mm 8 12 31.
Parts and Materials 5 Micro Well-Plate Sampler Cover Parts Table 29 Item Micro well-plate sampler cover parts Description Cabinet kit, includes base, side panels, top and front cover Part Number 5065-4446 Name plate for Agilent 1100 Series 5042-1381 Light protection kit, includes dark front cover and side window 5064-8272 Figure 16 Micro well-plate sampler cover parts 1100 Series Capillary LC System Manual 85
5 Parts and Materials Thermostatted Micro Autosampler Table 30 offers an overview over the main assemblies of the Thermostatted Micro Autosampler. The item numbers refer to Figure 17 on page 87.
Parts and Materials 5 12 1 11 2 10 3 4 9 8 5 7 6 Figure 17 Thermostatted micro autosampler main assemblies 1100 Series Capillary LC System Manual 87
5 Parts and Materials Thermostat for 1100 Samplers Table 31 Description Part Number Thermostat for 1100 samplers, exchange assembly G1330-69020 Figure 18 88 Thermostat for micro autosampler and micro well-plate sampler Thermostat 1100 Series Capillary LC System Manual
Parts and Materials 5 Sampling Unit for the Micro Autosampler Figure 19 offers an overview over the main assemblies of the Thermostatted Micro Autosampler. For descriptions of the item numbers refer to Table 32.
5 Parts and Materials Table 32 Item 90 Sampling unit for the micro autosampler Description Part Number Micro sampling unit assembly (The assembly comes without injection valve and analytical head) G1329-60018 1 Sampling unit connector board (SUD) G1313-66503 2 Belt gear for metering unit and needle arm 1500-0697 3 Stepper motor for metering unit and needle arm 5062-8590 4 Loop capillary (8 µl) Loop capillary (40 µl) G1375-87303 G1329-87302 5 Analytical head assembly (40 µl) G1377-6001
Parts and Materials 5 Micro Analytical Head Assembly Table 33 Item Micro analytical head assembly Description Part Number Micro Analytical head assembly 40 µl, includes items 1 – 6 G1377-60013 1 Screws 0515-0850 2 Micro Plunger assembly 5064-8293 3 Adapter 01078-23202 4 Micro seal support assembly G1377-60002 5 Metering seal (pack of 1) 5022-2175 6 Head body G1377-27700 Screw M5, 60 mm lg, for mounting of assembly 0515-2118 1 2 3 4 5 6 Figure 20 Micro analytical head assembly
5 Parts and Materials Micro Injection Valve Assembly Table 34 Item NO TE Micro injection valve assembly Description Part Number Micro Inj.-valve assembly, incl.
Parts and Materials 5 Thermostatted Micro Autosampler Cover Parts Table 35 Thermostatted micro autosampler cover parts Item Description Part Number 1 Autosampler Cover kit (include base, side panels and top cover) G1329-68703 2 Name plate for Agilent 1100 Series 5042-1381 3 Transparent front cover G1313-68704 4 Door repair kit (includes transparent side and front door) G1329-68707 5 Light protection kit (includes opaque side and front door, opaque front cover) G1329-68708 Cabinet upgra
5 Parts and Materials Vial Trays Table 36 Thermostatted autosampler vial trays and tray base Item Description Part Number 1 Tray for 100 × 2-ml vials, thermostattable G1329-60001 2 Adapter, air channel G1329-43200 3 Tray base (includes items 4, 5, 6).
Parts and Materials 5 Thermostatted Column Compartment Table 37 gives an overview over the main assemblies of the Thermostatted column compartment.
5 Parts and Materials 9 1 1 2 8 3 4 5 7 Figure 24 96 6 Thermostatted column compartment main assemblies 1100 Series Capillary LC System Manual
Parts and Materials 5 Micro Column Switching Valve Table 38 Item Micro column switching valve Description Part Number Column switching valve (complete assembly) 0101-1051 1 Rotor seal 3 grooves (Vespel) 0100-2087 2 Stator ring No PN 3 Stator Head 0100-2089 4 Stator screw 1535-4857 1 2 3 4 Figure 25 Micro column switching valve 1100 Series Capillary LC System Manual 97
5 Parts and Materials Thermostatted Column Compartment Sheet Metal Kit Table 39 Item Thermostatted column compartment sheet metal kit Description Part Number Sheet metal kit includes items 1, 2 and 3 G1316-68701 4 RFI shield G1316-00600 5 RFI spring side G1316-09100 6 RFI spring bottom G1316-09102 1 2 3 5 4 6 Figure 26 98 Thermostatted column compartment sheet metal kit 1100 Series Capillary LC System Manual
Parts and Materials 5 Thermostatted Column Compartment Cover Parts Table 40 Thermostatted column compartment cover parts Item Description Part Number 1 Plastic kit, includes base, sides and top G1316-68703 2 Front cover G1316-68704 3 Name plate Agilent 1100 Series 5042-1381 1 3 2 Figure 27 Thermostatted column compartment cover parts 1100 Series Capillary LC System Manual 99
5 Parts and Materials Thermostatted Column Compartment Leak Parts Table 41 Thermostatted column compartment leak parts Item Description Part Number 1 Leak funnel 5041-8388 2 Leak funnel holder G1316-42300 3 Leak sensor 5061-3356 4 Waste assembly, includes complete Y-tubing assembly with leak funnel G1316-60002 5,7 Leak Kit, includes leak top and leak base G1316-68700 6 O-ring for ambient temperature sensor 0400-0002 Corrugated waste tube, 120 cm (re-order 5 m) 5062-2463 7 6 1 5 2
Parts and Materials 5 Diode Array Detector Table 42 gives an overview over the main assemblies of the diode array detector:.
5 Parts and Materials 9 1 8 2 7 3 6 4 5 Figure 29 102 Diode array detector main assemblies 1100 Series Capillary LC System Manual
Parts and Materials 5 DAD - Optical Unit Assembly Table 43 gives an overview over optical unit parts:.
5 Parts and Materials 12 8 11 6 13 1 14 15 4 3 7 2 7 5 10 9 16 Figure 30 104 Optical Unit Parts 1100 Series Capillary LC System Manual
Parts and Materials 5 500 nl Flow Cell 1 12 11 2 3, 4 3, 4 13 10 5 7 9 16 14 Figure 31 Table 44 Item 15 17 8 500 nl Flow Cell 500 nl Flow Cell - parts Description 500 nl Flow Cell Kit Part Number G1315-68714 Flow cell assembly, 10 mm, 500 nl, 5 MPa completely assembled includes items 1, 2, 3, 4, 11, 12, 13, 14, 15, and 16 1 Capillary column to detector (400 mm, 50 µm) G1315-68703 2 Capillary column to detector (700 mm, 75 µm) G1315-68708 3 Fitting Screw - for 4 mm wrench, QTT=2 (r
5 Parts and Materials Table 44 500 nl Flow Cell (continued)- parts Item Description Part Number 12 Cell Seal Assembly 10 mm see kit below 13 Quartz Cell Body 10 mm G1315-80001 14 Handle for clamp unit G1315-84901 15 Clamp unit G1315-84902 16 Screw M 2.
Parts and Materials 5 Fan Assembly Parts Table 45 Fan assembly parts Item Description Part Number 1 Heater assembly G1315-60000 2 Fan 3160-1016 3 Temperature sensor assembly G1315-60003 1 2 3 Figure 32 Fan assembly parts 1100 Series Capillary LC System Manual 107
5 Parts and Materials Holmium Oxide Filter Table 46 NO TE Holmium oxide filter assembly parts Item Description Part Number 1 Holmium oxide filter 79880-22711 2 Holmium oxide filter lever G1315-45001 3 Spring 1460-1510 4 Holmium oxide filter motor assembly, includes items 2 and 4 G1315-68700 When the filter motor has been removed, the filter lever should not be reused. Use always a new filter lever to assure correct fit on the filter motor shaft.
Parts and Materials 5 Diode Array Detector Cover Parts Table 47 Diode array detector cover parts Item Description Part Number 1 Name plate Serial Number (w/o serial number) 5042-1314 2 Plastics, includes base, sides and top 5062-8565 3 Name plate Agilent 1100 Series 5042-1381 4 Front cover 5062-8582 1 2 3 4 Figure 34 Diode array detector cover parts 1100 Series Capillary LC System Manual 109
5 Parts and Materials Common Parts This chapter shows the parts identification of the common parts like rear panel, power and status light pipes, leak parts, foam parts, sheet metal kit and the different accessory kits. For cables see page 121.
Parts and Materials 5 Rear panel Table 49 Rear panel Item Description Part Number 1 Standoff — remote connector 1251-7788 2 Nut M14 — analog output 2940-0256 3 Screw, M4, 7 mm lg — power supply 0515-0910 4 Standoff — GPIB connector 0380-0643 1 4 2 3 Figure 36 Rear panel 1100 Series Capillary LC System Manual 111
5 Parts and Materials Power and Status Light Pipes Table 50 Power and status light pipes Item Description Part Number 1 Light pipe — power switch 5041-8382 2 Power switch coupler 5041-8383 3 Light pipe — status lamp 5041-8384 4 Power switch button 5041-8381 1 2 4 3 Figure 37 112 Power and Status Light Pipes 1100 Series Capillary LC System Manual
Parts and Materials 5 Leak Parts Table 51 Leak parts Item Description Part Number 1 Holder, leak funnel 5041-8389 2 Leak funnel 5041-8388 3 Tube clip 5041-8387 4 Leak plane, pump Leak plane, degasser Leak plane, ALS, WPS Leak plane, TCC, for details see page 100 Leak plane, DAD 5041-8390 G1379-47300 G1313-44501 G1316-68700 G1315-45501 5 Leak sensor 5061-3356 6 Corrugated waste tube (reorder pack), 5m 5062-2463 5 1 2 3 4 6 Figure 38 Leak parts 1100 Series Capillary LC System Man
5 Parts and Materials Foam parts Table 52 Foam parts Description Part number Foam kit for the capillary pump G1376A Foam kit for the micro autosampler G1389A Foam kit for the micro well-plate sampler G1377A Foam kit for the thermostatted column compartment G1316A Foam kit for the diode array detector G1315B (the foam kit includes the base and the top) G1312-68702 G1313-68702 5064-8248 G1316-68702 G1315-68722 Interface board guides (board guides for the G1376A/ G1389A/ G1377A/ G1315B) 5041-8395 Bus
Parts and Materials 5 Micro Degasser Accessory Kit Table 54 G1329A - Micro degasser accessory kit contents G1322-68705 Description Part Number Fitting tool 0100-1710 Solvent tubing kit (4 tubes degasser to pump) G1322-67300 Syringe * 5062-8534 Syringe adapter 9301-1337 Waste tube † 5062-2463 * Reorder number (pack of 10) † Reorder number (5m) Capillary Pump Preventive Maintenance Kit G1376-68710 Table 55 Capillary pump preventive maintenance kit G1376-68710 Description Part Number Gold
5 Parts and Materials Capillary Pump Accessory Kit Table 56 116 Capillary pump accessory kit G1376-68705 Description Part Number Insert tool 01018-23702 SST Solvent inlet filter (x4) 01018-60025 Waste tube 0890-1760 SST replacement frit (0.5 µm) 5022-2185 Wrench open end 7/16 - 1/2 inch (x 2) 8710-0806 Wrench open end 1/4 - 5/16 inch (x1) 8710-0510 Wrench open end 14 mm (x 1) 8710-1924 Wrench open end 4 mm, (x 1) 8710-1534 Hex key 2.
Parts and Materials 5 Micro Well-plate Sampler Accessory Kit G1377-68705 Table 57 Micro well-plate sampler accessory kit G1377-68705 Description Quantity Part Number 96 well-plate 0.
5 Parts and Materials Thermostatted Micro Autosampler Accessory Kit Table 58 118 Thermostatted micro autosampler accessory kit G1329-68715 Description Part Number Tubing assembly no PN CAN cable, 1 m long 5181-1519 Screw cap vials, clear 100/pk 5182-0714 Blue screw caps 100/pk 5182-0717 Label halftray no PN Fitting 5061-3303 Hex Key 8710-0060 Wrench 4 mm both ends 8710-1534 Wrenches 1/4 - 5/16 inch 8710-0510 Rheotool socket wrench 1/4 inch 8710-2391 Hex key 4 mm, 15 cm long, T-han
Parts and Materials 5 Column Compartment with Micro Column Selection Valve Accessory Kit Table 59 Column compartment with micro column selection valve (CSV) accessory kit G1316-68725 Description Part Number Column holder (x2) 5001-3702 Fingertight fitting (x2) reorder number (10 /pack) 5065-4422 Column identification tag (x1) reorder number (3 / pack) 5062-8588 Corrugated waste tube reorder number (5 m) 5062-2463 CAN cable 5181-1516 Wrenches 1/4 - 5/16 inch 8710-0510 ESD wrist strap no PN
5 Parts and Materials DAD Accessory Kit Table 60 120 DAD accessory kit G1315-68705 Description Part Number Accessory kit G1315-68705 Tubing assembly waste 1.2 m lg no PN Tubing flexible (to waste) 2 m lg 0890-1713 Fitting male PEEK, Qty=1 0100-1516 Capillary column – detector 380 mm lg, 0.17 i.d.
Parts and Materials 5 Cables WA RN ING Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations.
5 Parts and Materials Table 61 122 Cables overview (continued) Type Description Part Number BCD cables 3392/3 integrators 18594-60510 3396 integrator 03396-60560 General purpose (spade Lugs) 18594-60520 Auxiliary Agilent 1100 Series vacuum degasser G1322-61600 CAN cables Agilent 1100 module to module, 0.
Parts and Materials 5 Analog Cables One end of these cables provides a BNC connector to be connected to Agilent 1100 Series modules. The other end depends on the instrument to which connection is being made.
5 Parts and Materials Table 64 Agilent 1100 to BNC connector Connector 8120-1840 Table 65 Pin BNC Pin Agilent 1100 Signal Name Shield Shield Analog - Center Center Analog + Agilent 1100 to general purpose Connector 01046-60105 Pin 3394/6 Pin Agilent 1100 1 Signal Name Not connected 2 Black Analog - 3 Red Analog + Remote Cables One end of these cables provides a Agilent Technologies APG (Analytical Products Group) remote connector to be connected to Agilent 1100 Series modules.
Parts and Materials Table 66 Agilent 1100 to 3390 integrators Connector 01046-60203 Table 67 5 Pin 3390 Pin Agilent 1100 Signal Name Active (TTL) 2 1 - White Digital ground NC 2 - Brown Prepare run Low 7 3 - Gray Start Low NC 4 - Blue Shut down Low NC 5 - Pink Not connected NC 6 - Yellow Power on High NC 7 - Red Ready High NC 8 - Green Stop Low NC 9 - Black Start request Low Pin 3392/3 Pin Agilent 1100 Signal Name Active (TTL) 3 1 - White Digital ground NC
5 Parts and Materials Table 68 Agilent 1100 to 3394 integrators Connector 01046-60210 Pin 3394 Pin Agilent 1100 Signal Name 9 1 - White Digital ground NC 2 - Brown Prepare run Low 3 3 - Gray Start Low NC 4 - Blue Shut down Low NC 5 - Pink Not connected NC 6 - Yellow Power on High 5,14 7 - Red Ready High 6 8 - Green Stop Low 1 9 - Black Start request Low 13, 15 NO TE 126 Active (TTL) Not connected START and STOP are connected via diodes to pin 3 of the 3394 conn
Parts and Materials Table 69 5 Agilent 1100 to 3396A integrators Connector 03394-60600 Pin 3394 Pin Agilent 1100 Signal Name 9 1 - White Digital ground NC 2 - Brown Prepare run Low 3 3 - Gray Start Low NC 4 - Blue Shut down Low NC 5 - Pink Not connected NC 6 - Yellow Power on High 5,14 7 - Red Ready High 1 8 - Green Stop Low NC 9 - Black Start request Low 13, 15 Active (TTL) Not connected Agilent 1100 to 3396 Series II / 3395A Integrators Use the cable 03394-6060
5 Parts and Materials Table 70 Agilent 1100 to 3396 Series III / 3395B integrators Connector 03396-61010 Pin 33XX Pin Agilent 1100 Signal Name 9 1 - White Digital ground NC 2 - Brown Prepare run Low 3 3 - Gray Start Low NC 4 - Blue Shut down Low NC 5 - Pink Not connected NC 6 - Yellow Power on High 14 7 - Red Ready High 4 8 - Green Stop Low NC 9 - Black Start request Low 13, 15 Table 71 Connector 5061-3378 128 Active (TTL) Not connected Agilent 1100 to HP 1050,
Parts and Materials Table 72 Agilent 1100 to HP 1090 LC, HP 1040 DAD or signal distribution module Connector 01046-60202 5 - Key Table 73 5 Pin HP 1090 Pin Agilent 1100 Signal Name Active (TTL) 1 1 - White Digital ground NC 2 - Brown Prepare run Low 4 3 - Gray Start Low 7 4 - Blue Shut down Low 8 5 - Pink Not connected NC 6 - Yellow Power on High 3 7 - Red Ready High 6 8 - Green Stop Low NC 9 - Black Start request Low Pin Agilent 1100 Signal Name Active (TTL)
5 Parts and Materials BCD Cables One end of these cables provides a 15-pin BCD connector to be connected to the Agilent 1100 Series modules. The other end depends on the instrument to be connected to.
Parts and Materials Table 75 Agilent 1100 to 3396 integrators Connector 03396-60560 Table 76 5 Pin 3392/3 Pin Agilent 1100 Signal Name BCD Digit 1 1 BCD 5 20 2 2 BCD 7 80 3 3 BCD 6 40 4 4 BCD 4 10 5 5 BCD0 1 6 6 BCD 3 8 7 7 BCD 2 4 8 8 BCD 1 2 9 9 Digital ground NC 15 +5V Low Wire Color Pin Agilent 1100 Signal Name BCD Digit Green 1 BCD 5 20 Violet 2 BCD 7 80 Blue 3 BCD 6 40 Yellow 4 BCD 4 10 Black 5 BCD0 1 Orange 6 BCD 3 8 Red 7
5 Parts and Materials Auxiliary Cable One end of this cable provides a modular plug to be connected to the Agilent 1100 Series vacuum degasser. The other end is for general purpose.
Parts and Materials 5 External Contact Cable 5 10 15 1 6 11 One end of this cable provides a 15-pin plug to be connected to Agilent 1100 Series module’s interface board. The other end is for general purpose.
5 Parts and Materials RS-232 Cable Kit This kit contains a 9-pin female to 9-pin female Null Modem (printer) cable and one adapter. Use the cable and adapter to connect Agilent Technologies instruments with 9-pin male RS-232 connectors to most PCs or printers.
Agilent 1100 Series Capillary LC System System Manual 6 Options Extended Flow Range Kit (G1376-69707) 136 0.1 - 2.5 ml/min Flow Capillary Kit (5065-4495) 139 Micro Column Switching Valve G1388A#055 143 500 nl Flow Cell Kit G1315-68714 153 This chapter describes the different options available for the capillary LC System.
6 Options Extended Flow Range Kit (G1376-69707) The extended flow range kit described in Table 80 lets you adapt your capillary pump to enable it to work with flows up to 100 µl/min. In order to decrease the system pressure when you increase the flow until 100 µl/min some capillaries must be changed. These capillaries, (8, 9, 10, 11, 13) are shaded in Figure 39 on page 137.
Options 6 SSV EMPV Filter Pump head B Pump head A 1 1 2 6 2 7 8 Mixer 3 3 Flow sensor Damper 5 9 4 14 11 Column 10 Flow cell 13 Analytical head Injection valve Needle 15 16 12 Waste Figure 39 Waste Capillary pump flow diagram 1100 Series Capillary LC System Manual 137
6 Options Installing the Extended Flow Range Kit Frequency When the flow rate is higher than 20 µl/min Tools required 4 mm open wrench (8710-1534) Torque adapter G1315-45003 1/4 - 5/16 inch open wrench (8710-0510) 2.5 mm hex key (8710-2412) Parts required Extended flow range kit (G1376-69707) 1 Using the 4 mm / 1/4 - 5/16 inch open wrenches disconnect the capillaries 8, 9, 10, 11 and 13. Refer to Figure 39 on page 137 to identify their location.
Options 6 0.1 - 2.5 ml/min Flow Capillary Kit (5065-4495) It is possible to use the capillary pump with a flow rate higher than 100 µl/min. For this the pump must be used in the normal mode and some hardware modifications are necessary. From 100 to 200 µl/min, bypassing the electronic flow control is needed. No other hardware modifications are necessary.
6 Options Installing the 0.1 - 2.
Options 6 12 Replace the loop capillary with the capillary G1329-87302 if you have a micro autosampler (G1389A) or with the capillary G1377-87300 if you have a micro well-plate sampler (G1377/78A). NO TE Don‘t forget to change the loop or syringe size to 40 µl in the injector configuration windows of the user interface. Needle seat assembly must be G1329-87101 with the 100 µm capillary (G1389A). Needle seat assembly must be G1375-87317 with the 100 µm capillary ((G1377/78A).
6 Options . Table 82 % of organic phase Pressure (bar) for Methanol Pressure (bar) for Acetonitrile 0 165 162 20 170 169 40 158 154 60 132 128 80 100 95 100 75 72 . Table 83 142 Pressure drop at 2.5 ml/min for different concentrations (no column) Pressure drop for different columns and different flow rates, with a gradient from 0 to 100% Acetonitrile in 10 minutes. Column (id and length) Flow rate (ml/min) Pressure (bar) 100 x 2.1 mm 0.4 92 (max.) 100 x 2.1 mm 0.
Options 6 Micro Column Switching Valve G1388A#055 The micro column switching valve allows to work with 2 columns and to select either the one or the other. The offline column is sealed by connecting head to rail. Switching should be done when the flow is off and the pressure is zero. Figure 40 shows the flow diagram when column 1 is active. Figure 41 shows the flow diagram when column 2 is active.
6 Options The micro column switching valve allows also to work with a column back-flushing. The sample is injected into series-connected precolumn and analytical column. After the valve has switched, the analytical column flow continues in normal direction. Only the precolumn is back-flushed, eluting highly retained peaks directly to the detector.
Options 6 Parts Identification for Micro Column Switching Valve Table 84 Item Micro column switching valve Description Part Number Column switching valve (complete assembly) 0101-1051 Fused silica capillaries, 50 µm, 280 mm) G1375-87309 Micro Valve Fitting Kit, (includes 6 fittings, 2 plugs) 5065-4410 1 Stator screw 1535-4857 2 Stator Head 0100-2089 3 Stator ring No PN 4 Rotor seal 3 grooves (Vespel) 0100-2087 4 3 2 1 Figure 43 Micro column switching valve 1100 Series Capillary LC
6 Options Replacing Rotor Seal of Micro Column Switching Valve Frequency If valve leaks Tools required 5.5 mm wrench 9/64 inch hex key Parts required Refer to “500 nl Flow Cell Kit G1315-68714" on page 153. 1 Remove capillaries from ports 1, 5, and 6. 2 Loosen each fixing stator screws two turns at a time. Remove bolts from head. 15 Remove the stator head and the rotor seal. 16 Install the new rotor seal, re-install the stator head. 17 Insert the stator screws in the stator head.
Options 6 Removing the Micro Column Switching Valve When required If valve failed or bottom foam part has to be removed for other replacements Tools required Screwdriver Pozidriv 1 PT3 Wrench 5.5 mm for capillary connections Preparations for this procedure: • • • • • Turn off the column compartment. Disconnect the power cable. Disconnect capillaries. Remove column compartment from stack and place it on the working bench. Remove the front cover, top cover and top foam section. 2 Unscrew the Z-panel.
6 Options 4 Lift the Z-panel together with the top plastic panel half-way out of the guide. 5 Locate the ambient temperature sensor in the top plastic part and push it towards the rear. 6 Carefully remove the ambient temperature sensor plugged into the rear of the top plastic panel. 7 Pull the top plastic panel together with the Z-panel completely out of the guide.
Options 8 Remove the Valve from its location. 1100 Series Capillary LC System Manual 6 For the installation refer to “Installing the Micro Column Switching Valve" on page 150.
6 Options Installing the Micro Column Switching Valve When required For first time installation or after it was removed Tools required Screwdriver Pozidriv 1 PT3 Wrench 5.5 mm for capillary connections Preparations for this procedure are: • The column compartment is open as described in “Removing the Micro Column Switching Valve" on page 147 2 Replace the valve into its location. 1 If no column switching valve was installed, remove the RFI-shield and the plastic cover (no longer used).
Options 3 Carefully insert the top plastic panel together with the Z-panel into the guide and press it half-way down. 6 4 Carefully plug the ambient temperature sensor into the rear of the top plastic panel. Not e Ensure that the ambient temperature sensor is completely plugged into the rear of the top plastic panel. Ensure that during the next steps the flexible cables close to the heat exchanger assemblies are not damaged. 5 Press the Z-panel together with the Top Plastic Panel completely down.
6 Options 7 Fix the Z-panel with the two screws. 8 Reconnect the grounding connection of the valve at the Z-panel. 9 Replace the foam section, the top cover and front cover. 10 Replace the column compartment into stack. 11 Reconnect capillaries. 12 Reconnect the power cable. 13 Turn on the column compartment.
Options 6 500 nl Flow Cell Kit G1315-68714 This section describes the 500 nl flow cell for Agilent 1100 Series diode array detector and multiple wavelength detector. Features • small dispersion through: • 500 nl, 10 mm pathlength flow cell • novel PEEK jacked quartz capillaries (inlet 50 µm i.d., outlet 75 µm i.d.
6 Options Special Information for Maintenance The supplied parts with the flow cell allow different fittings and capillaries, see Figure 44. Before fitting it to the flow cell, think about which type you want to use. Depending on this you may have to use special parts mentioned in the procedure.
Options Figure 45 6 Removing Ferrule The cell fittings are factory installed and tested for leakage. These connections should not be used as an instrument interface. It should be opened only for maintenance and/or special adaptions. CAU TI O N Do not overtighten the cell fittings. This may break the cell quartz body. With the instrument accessory kit comes a 4-mm wrench and with the Sealing Kit a special adapter.
6 Options Installation of the Flow Cell The flow cell is supplied with blank capillaries at the instrument side to allow the use of different fittings, see Figure 44 on page 154. If you are using small i.d capillary columns from e.g. LC Packings, see also “Connecting Small I.D. Capillaries” on page 160. The steps below describe the connection to the internal hydraulic connector and might not be used in case the capillaries are routed directly to the column and/or waste .
Options Step 3 and 4 have to be done for each of the two flow cell capillaries, if this connection type is desired. There is no stop within the union “Top Seal” for plane capillaries. Therefore one prefixed ferrule is required at least. 6 3 Slide the screw, back ferrule and front ferrule onto the PEEK capillary (see detail for correct direction). This is for cell side only! back ferrule front ferrule screw 4 Carefully press the capillary into the adjustment union.
6 Options 6 The figure below shows the sealing principle within Depending on the fitting type you select, the figure in the union “top seal”, hand tightened before torque is step 7 may look different. applied. The figures in step 7 and 8 show alternatively the supplied PEEK fittings and the two supplied (top sealing) unions from the kit (the original union(s) must be replaced). The figure in step 9 shows the connection with the supplied SST fittings.
Options 9 Insert the PEEK capillaries from the flow cell body together with the SST fitting, ferrule and cone into the union and tighten it. 6 Remove the flow cell and perform a leak test. If no leak is observed, install the flow cell and you are ready to work. Make sure that the flow cell assembly is inserted correctly and fits perfectly in the optical unit (especially when PEEK capillaries are used).
6 Options Connecting Small I.D. Capillaries Columns from e.g. LC Packings have capillary connections which are of very small i.d. with FEP sleeves. To use it with the 500 nl flow cell use the information below. NO TE A PEEK sleeve with the appropriate internal and outer diameter is required to fit the SST fitting and the ferrules on the quartz capillary. insert quartz capillary column Figure 47 160 quartz capillary FEP sleeve SST fitting PEEK sleeve front and back ferrule Connecting small i.d.
Options 6 Replacing or Cleaning Parts CAU TI O N The quartz block can be cleaned with alcohol. DO NOT touch the inlet and outlet windows at the quartz block. 1 Disconnect the capillaries from the capillary holder and remove the flow cell. 2 Unscrew the cell body from the holder. 3 Unscrew the capillaries from the flow cell. DO NOT use the adapter at this time! 4 Using a toothpick, press on the plastic part and slide the quartz body out of the cell housing.
6 Options 5 The quartz body and the cell seal assembly can be separated for cleaning purpose. 6 This figure shows the correct holding of the quartz body and the cell seal assembly. 7 Replace the cell seal assembly onto the quartz body. It is recommended to use a new assembly. 8 Slide the quartz body completely into the cell body to the front stop (use for example a toothpick).
Options 6 9 Insert the flow cell capillaries and tighten them 10 Reassemble the flow cell body to the holder. fingertight.Use of the wrench and torque adapter as described page 155 and tighten the fittings alternate 11 Re-install the flow cell and connect the capillaries to the union holder. Remove the flow cell and perform a leak test. If no leak is observed, install the flow cell and you are ready to work.
6 164 Options 1100 Series Capillary LC System Manual
Agilent 1100 Series Capillary LC System System Manual 7 Performance Specifications Performance Specifications Agilent 1100 Series Capillary Pump 166 Performance Specifications Agilent 1100 Series Micro Vacuum Degasser 168 Performance Specifications Agilent 1100 Series Thermostatted Micro Autosampler 169 Performance specification Agilent 1100 Series Micro Well-plate Sampler 170 Performance Specifications Agilent 1100 Thermostatted Column Compartment.
7 Performance Specifications Performance Specifications Agilent 1100 Series Capillary Pump Table 86 Type Specification System delay volume Typically 5 µl from EFC to column head, for flow rates up to 20 µl/min (default setup). Typically 14 µl from EFC to column head, for flow rates up to 100 µl/min (default setup).
Performance Specifications Table 87 7 Performance Specification Agilent 1100 Series Capillary Pump (continued) Type Specification Delay volume Typically 3 µl from the electronic flow control to the pump outlet for flow rates up to 20 µl/min. Typically 12 µl from the electronic flow control to the pump outlet for flow rates up to 100 µl.
7 Performance Specifications Performance Specifications Agilent 1100 Series Micro Vacuum Degasser Table 88 168 Performance Specifications Agilent 1100 Micro Vacuum Degasser Type Specification Flow rate 0 – 5 ml/min per channel (5 – 10 ml/min at reduced degassing performance) Number of channels 4 Internal volume per channel Typically 1 ml per channel Materials in contact with solvent PTFE – FEP – PEEK pH range 1 – 14 Analog output (AUX) For pressure monitoring, range 0 – 3 V Evaporation o
Performance Specifications 7 Performance Specifications Agilent 1100 Series Thermostatted Micro Autosampler Table 89 Performance Specifications Agilent 1100 Series Thermostatted Micro Autosampler Type Specification Sample capacity 100 x 2 ml vials in 1 tray. Microvials (100 or 300 µl) with sleeves (reduced cooling performance with microvials) Settable injection volume 0.01 to 8 µl with small loop capillary 0.01 to 40 µl with extended loop capillary Precision Typically < 0.
7 Performance Specifications Performance specification Agilent 1100 Series Micro Well-plate Sampler Table 90 170 Performance specifications Agilent 1100 series micro well-plate sampler Type Specification GLP features Early maintenance feedback (EMF), electronic records of maintenance and errors Communications Controller-area network (CAN).
Performance Specifications 7 Performance Specifications Agilent 1100 Thermostatted Column Compartment. All specifications in Table 91 are valid for distilled water at ambient temperature (25 °C), set point at 40 °C and a flow range from 0.2–5 ml/min.
7 Performance Specifications Performance Specifications Agilent 1100 Series DAD Reference conditions for data of Table 92: • cell path length 10 mm, response time 2 s, • flow 1 ml/min LC-grade Methanol, • slit width 4 nm. Linearity measured with caffeine at 265 nm.
Performance Specifications Table 92 7 Performance Specifications Agilent 1100 Series Diode Array Detector Type Specification Maximum pressure 50 bar Control and data evaluation Agilent ChemStation for LC Analog outputs Recorder/integrator: 100 mV or 1 V, output range 0.
7 174 Performance Specifications 1100 Series Capillary LC System Manual
Agilent 1100 Series Capillary LC System System Manual A Safety Information The following general safety precautions must be observed during all phases of operation, service, and repair of this instrument. Failure to comply with these precautions or with specific warnings elsewhere in this manual violates safety standards of design, manufacture, and intended use of the instrument. Agilent Technologies assumes no liability for the customer’s failure to comply with these requirements.
A Safety Information General This is a Safety Class I instrument (provided with terminal for protective earthing) and has been manufactured and tested according to international safety standards. Operation Before applying power, comply with the installation section. Additionally the following must be observed. Do not remove instrument covers when operating.
Safety Information A Capacitors inside the instrument may still be charged, even though the instrument has been disconnected from its source of supply. Dangerous voltages, capable of causing serious personal injury, are present in this instrument. Use extreme caution when handling, testing and adjusting. Safety Symbols Table 93 shows safety symbols used on the instrument and in the manuals.
A Safety Information Lithium Batteries Information WA RN ING Danger of explosion if battery is incorrectly replaced. Replace only with the same or equivalent type recommended by the equipment manufacturer. Lithium batteries may not be disposed-off into the domestic waste. Transportation of discharged Lithium batteries through carriers regulated by IATA/ICAO, ADR, RID, IMDG is not allowed.
Safety Information A Radio Interference Never use cables other than the ones supplied by Agilent Technologies to ensure proper functionality and compliance with safety or EMC regulations. Test and Measurement If test and measurement equipment is operated with equipment unscreened cables and/or used for measurements on open set-ups, the user has to assure that under operating conditions the radio interference limits are still met within the premises.
A Safety Information • High concentrations of inorganic acids like nitric acid, sulfuric acid especially at higher temperatures (replace, if your chromatography method allows, by phosphoric acid or phosphate buffer which are less corrosive against stainless steel).
Index Numerics 500 nl flow cell, 153 A accuracy of temperature column compartment, 171 accuracy of wavelength, 172 Agilent on internet, 180 ambient non-operating temperature, 4 ambient operating temperature, 4 analog output micro degasser, 168 ASTM environmental conditions, 3 reference, 173 ASTM drift tests, 3 B battery safety information, 178 bench space, 3 buffer application, 30 bunching of wavelength, 172 C cables, 2 capillaries additional, 51 generic, 47 high flow, 49 low flow, 48 use with micro CSV,
Index M maximum flow rate, 168 metering seal, 81, 91 micro column switching valve (optional) description, 143 installing, 150 removing, 147 two column selection, 143 micro vacuum degasser parts, 66 micro-well-plate sampler installing, 10 N non-operating altitude, 4 non-operating temperature, 4 number of channels micro degasser, 168 O operating altitude, 4 operating temperature, 4 operation, safe, 176 P parts identification ALS analytical head, 91 ALS cover parts, 93 ALS injection valve, 82, 92 ALS therm
Index system pressure high, 57 low, 56 unstable, 59 system troubleshooting, 55 T TCC installing, 9 temperature range, 171 stability, 171 temperature, ambient, 3 thermostatted capillary LC system installing, 14 troubleshooting, 55 U unpacking the pump, 4 V voltage range, 4 W warm-up time, 171 wavelength accuracy and bunching, 172 range, DAD, 172 1100 Series Capillary LC System Manual 183
Index 184 1100 Series Capillary LC System Manual
s1 In This Book This manual contains technical reference information about the Agilent 1100 Series capillary LC system. The manual describes the following: • installation, • optimizing performance, • diagnostics • parts and materials, • available options • specifications.
