1593555 en ELS Detector C-650 Operation Manual
Table of content 1 About this manual 5 1.1 Abbreviations 5 2 Safety 6 2.1 User qualification 6 2.2 Proper use 6 2.3 Improper use 6 2.4 Safety warnings and safety signs 7 2.5 Product safety 9 2.5.1 General hazards 9 2.5.2 Warning labels on housing and assemblies 10 2.5.3 Personal protective equipment 10 2.6 General safety rules 10 2.6.1 Responsibility of the operator 10 2.6.2 Duty of maintenance and care 10 2.6.3 Spare parts to be used 10 2.6.
5.8 5.9 Control panel 26 5.8.1 Digital display 26 5.8.2 User interface 27 Initial test procedures 34 5.9.1 Preliminary activities 34 5.9.2 Electronic noise test 35 5.9.3 Background noise (stray light) test 35 5.9.4 Solvent noise test 36 5.9.5 Column noise test 37 6 Operation 38 6.1 Preparing the device for operation 38 6.2 Auto-zeroing the detector 38 6.2.1 Manual 38 6.2.2 External 39 6.3 Routine operation of the detector 39 6.
1 About this manual This manual describes the Low Temperature Evaporative Light Scattering Detector C-650 and provides all information required for its safe operation and to maintain it in good working order. It is addressed to laboratory personnel and operators in particular. Read this manual carefully before installing and running your system and note the safety precautions in chapter 2 in particular. Store the manual in the immediate vicinity of the device, so that it can be consulted at any time.
2 Safety This chapter points out the safety concept of the device and contains general rules of behavior and warnings from hazards concerning the use of the product. The safety of users and personnel can only be ensured if these safety instructions and the safety related warnings in the individual chapters are strictly observed and followed. Therefore, the manual must always be available to all persons performing the tasks described herein. 2.
2.4 Safety warnings and safety signs DANGER, WARNING, CAUTION and NOTICE are standardized signal words for identifying levels of hazard seriousness of risks related to personal injury and property damage. All signal words, which are related to personal injury are accompanied by the general safety sign.
Symbol Meaning Harmful to life-forms Pinch point. Mechanical hazard.
Additional user information Paragraphs starting with NOTE transport helpful information for working with the device/software or its supplementaries. NOTEs are not related to any kind of hazard or damage (see following example). NOTE Useful tips for the easy operation of the device/software. 2.5 Product safety The ELSD is designed and built in accordance with state-of-the-art technology. Nevertheless, risks to users, property, and the environment can arise when the device is used carelessly or improperly.
2.5.2 Warning labels on housing and assemblies The following warning sticker(s) can be found on the housing or assemblies of the C-650: Symbol 2.5.3 Meaning Location Hot item, hot surface Sticker / label, located at the heating block Personal protective equipment Always wear personal protective equipment such as protective eye goggles, protective clothing and gloves. The personal protective equipment must meet all requirements of the supplementary data sheets for the chemicals used.
3 Technical data This chapter introduces the device specifications. It contains the scope of delivery, technical data, requirements and performance data. 3.1 Scope of delivery Check the scope of delivery according to the order number. NOTE For detailed information on the listed products, see www.buchi.com or contact your local dealer. 3.1.1 Standard device Table 3.1: Standard device Product 3.1.
3.1.3 Optional accessories Table 3.3: Optional accessories Product Order number Flow splitter 3.2 11059007 Technical data overview Table 3:4: Technical data 12 3 Dimensions (L×H×D) 250×450×550 mm Connection voltage 115 VAC (±10 %)/60 Hz/1.8 A 230 VAC (±10 %)/50 Hz/1.7 A Weight 18.
4 Description of function This chapter explains the basic principle of the device, shows how it is structured and gives a functional description of the assemblies. 4.1 Overview over the device Fig 4.1: Overview over the device The C-650 is designed to detect compounds in the eluent from Preparative Chromatography. It is capable of monitoring eluent flow rates from 0.1 mL/min to 5 mL/min. Evaporative Light-Scattering Detection is a nearly universal technique which can detect any non-volatile analyte.
4.2 Functional principle There are three discrete steps in the operation of the detector; nebulization of the eluent, evaporation of the solvent and detection of the compound(s) of interest. Nebulization --> Evaporation --> Detection Nebulization involves the conversion of the eluent into a fine aerosol.
1 2 3 4 a Liquid inlet b Coloured seal c Ring d Gas inlet Fig 4.3: Design of the nebulizer Fig 4.
4.2.2 Evaporation of the solvent A heated tube is used to evaporate the solvent. The exit of the heated tube leads directly into the detection chamber. In liquid chromatography, water and organic solvents with low boiling points are typically employed (e.g. CH3OH, CHCl3, CH3CN). A typical mobile phase for a reverse phase separation using Evaporative Light-Scattering Detection might be CH3OH/H2O (60/40) while a typical mobile phase for normal phase separation might be C6H14/CHCl3 (60/40).
A plot of log I versus log m provides a linear response. The values of the constants (k and b) are dependent on a variety of parameters (e.g. the temperature and the nature of the mobile phase). An inlet to provide additional gas is located immediately before the detector chamber to provide a concentric shield for the carrier gas. This serves to eliminate diffusion of the carrier gas and eliminate contamination of the detection chamber. 4.
5 Putting into operation This chapter describes how the device is installed and gives instructions on initial startup. NOTE Inspect the device for damages during unpacking. If necessary, prepare a status report immediately to inform the postal company, railway company or transportation company. Keep the original packaging for future transportation. 5.1 Installation site Put the device on a stable, horizontal surface. Consider the maximum product dimensions and weight.
5.2 Electrical connections NOTE External connections and extension lines must be provided with a grounded conductor lead (3-pole couplings, cord or plug equipment). All used power cords must meet the input power requirements. It is recommended that all components of the Flash system are connected to a common ground. The detector should not be connected to an electrical line which also serves units with a large power drain or which may be subject to power surges.
The blue cables are contact closure “input” cables that are used to power the unit down (see section 6.5) via a signal from an external device to the detector.. Connecting the power cord: Place the ON/OFF switch to the OFF position and plug the power cord into the socket on the rear panel of the detector. Do not turn on the power at this time. The power cord of this detector contains three wires which must be connected to a grounded line.
After Parafilm is removed from the detector gas inlet, the tubing should be cut and firmly inserted into the fitting as shown below. 1 2 3 a Cutting the tube square c Pull the tube to check engagement of b Inserting the tube into the fitting until it bottoms the grab Fig 5.8: Inserting the gas inlet tube Two pieces of tubing are provided. If you are using the device with an external filter, connect the gas source to the filter and then connect the filter to the back of the unit.
5.4 Exhaust venting and drain requirements WARNING Risk of toxic fume inhalation. •• Always route the black exhaust tube from the detector into a ventilated fume hood or exhaust vent. The exhaust and drain should not be allowed to enter the laboratory atmosphere and any appropriate accessory (e.g. solvent filter) should be disposed of in a manner that meets the local regulatory authorities for health and safety requirements.
5.5 Installing the nebulizer/glass chamber assembly ParafilmTM is used to cover various openings inside the compartment, nebulizer and glassware to prevent dust particles from entering the detector during shipment. NOTE When installing the transparent black front cover, first fix its right side, and then push its left side. When removing the front cover, pull only its left side. The installed nebulizer/glass chamber assembly is shown in Fig 5.10.
Use the large black nut to position the nebulizer on the glass chamber. Fill the siphon overflow on the nebulizer/glass chamber assembly with the mobile phase that will be used for the separation. If you are using a very volatile solvent (e.g. hexane or CH2Cl2), then use water to fill the overflow. The liquid should fill the bent part of the siphon, but should not pool in the bottom of the evaporation tube. Make sure that no liquid leak could affect the detector performance or create laboratory pollution.
5.6 Installing the flow splitter 5.6.1 Connecting the flow splitter The flow splitter comes as complete kit (article number 11059007) and has to be mounted inside the detector as shown below: 1 2 3 4 8 5 6 7 Fig 5.12: Detection chamber/Flow splitter a Fastening screw e Inline filter b Flow adjustment knob f Flow from column outlet cU nion fitting to connect the splitter to the nebulizer g Flow to ELSD nebulizer h Restriction capillary ID 0.10 mm d Flow to fraction collector 1.
flask. This adjustment requires only a small rotation of the knob. Too big rotation could generate too high back pressure (about half clockwise rotation). NOTE The flow splitter is delivered equipped with a black restriction capillary having a 0.10 mm ID. This configuration is especially suited for normal phase separations using solvents with low viscosity. For reversed phase applications using solvents with viscosities higher than 0.
After the detector has completed the initialization procedures, the Status screen (Fig 5.14) will be presented. The signal should be close to zero. Signal Temp Press Gain 001 26°C 3.5b 1 Fig 5.14: Status screen The user interface is provided via a series of screens that are described in section 5.8.2. Some screens present information about the device status and cannot be edited by the user (e.g. the Status screen), while other screens (e.g. the Temperature/Gain screen, Fig 5.
gain can be set via the Temp/Gain screen (Fig 5.16) and the pressure units can be selected via the Noise Filter/Pressure Unit screen (Fig 5.18). Temperature value blinks if desired temperature is not reached and stable. The pressure value blinks if the gas pressure is lower than 2.0 bar. When the button is pressed; the Offset screen (Fig 5.15), which is used to select the desired offset is displayed. Offset screen Signal Offset (mV) 000 Fig 5.15: Offset To increase the offset value, click on the key.
When the detector is powered up or if you change the temperature, the temperature may first overshoot the setpoint slightly and then stabilize at the desired point. This initial overshoot is due to the regulation of the device and normal. NOTE To maintain appropriate temperature control, when the lowest temperature is required, it should be set at least 5°C above ambient. Temperature stabilization typical time is 30 minutes.
Noise Filter/Pressure unit screen Filter: 1 s Press Unit: bar Fig 5.18: Noise Filter/Pressure unit screen The Filter/Pressure Unit screen is used to indicate if digital filtering is desired for the signal data (improves signal-to-noise ratio) and the desired units for the pressure display. When the screen is presented, the cursor is on the Filter field. By pressing change the filtering strength within the following range: or keys, you “NO”: no filtering. 0.5 s: 0.5 second moving average filtering.
button followed by the button to turn it off. The # hours field indicates the number of hours that the LED has been in use. The lifetime of the LED is approximately 5000 h. When this period has been reached, a message indicating that the maximum usage of the lamp has been exceeded will be presented when the unit is powered up and the orange LED on the keyboard blinks. NOTE When you press the button, the Gas Valve screen (Fig 5.20) will be displayed.
The three options provided for external shutdown are summarized in the following table: Mode Photomultiplier Lamp Heating Gas flow General Off Off Off Off Standby Off Off On Off Cleaning Off Off On On To select the desired Power Down mode, use the then press to validate the selection. or key to access the desired mode and NOTE It will take a few minutes to attain operating status from General power down mode, as the temperature must stabilize.
Serial Number Screen Serial Number ######### Fig 5.23: Serial Number screen The Serial Number screen cannot be edited by the user. The last character indicates the detector hardware revision. When you press the button, the Firmware screen (Fig 5.24) will be displayed. Firmware Screen Firmware Version: V.v Firmware Date: MM/YY Fig 5.24: Firmware screen This information screen presents the firmware Version Bnd date, where MM is the month, and YY the year.
Factory Menu Code Screen Factory Menu Code ____ Authorized persons only Fig 5.25: Factory Menu Code screen The Factory Menu Code screen is used by the service engineer to access a variety of service features and is not designed to be employed by the user. 5.9 Initial test procedures 5.9.1 Preliminary activities This section presents a protocol that can be used to ensure that the detector is working in the proper way.
When the detector is powered up or if you change the temperature, the temperature may first overshoot the setpoint slightly and then stabilize at the desired point. This initial overshoot is due to the regulation of the device and should not be a concern. Provide gas to the detector and adjust the pressure to 2 bar (29 psi). If the pressure is less than 1,5 bar (21 psi), the pressure value blinks, indicating that the detector is not ready.
5.9.4 Solvent noise test To determine the solvent noise: nsure that the gas is flowing at 2 bar (29 psi), the temperature is set to 50 °C and stable and E the pump is switched off. witch on the light source and set the gain to 12 and monitor the signal. Do not autozero the S detector. The signal may be negative. ypass the column and connect the detector to the mobile phase delivery system and pump the B solvent that you expect to use for your analyses through it at a flow rate of 1 mL/min.
5.9.5 Column noise test NOTE When strongly retained compounds are slowly eluted from the column, excessive noise will be observed. To determine the column noise: Turn off the pump and connect the column. estart the pump and allow the mobile phase to flow through the system. It is suggested that R you flush the column with a strong solvent for a few minutes before attaching it to the detector. et the gain to 12 and monitor the baseline for a few minutes.
6 Operation This chapter describes the operations that should be performed on a routine basis when you want to collect chromatographic data using the C-650 and gives examples of typical device applications and instructions on how to operate the device properly and safely. 6.1 Preparing the device for operation CAUTION Risk of fire due to flammable liquids! • • Check all tubes for correct connection before starting the device. Make sure all tubes are in good condition (no cracks or cuts).
6.2.2 External To auto-zero the detector, a contact closure signal or a TTL signal is used to short circuit the contacts. The signal should be at least 1 second long, with a maximum current of 20 mA at 5 V. If a TTL signal is used please make sure to use the correct polarity identified on the cable. 6.3 Routine operation of the detector In general, operation of a Chromatography system with Evaporative Light-Scattering Detection is similar to operation of the system with other detectors.
NOTE If the mobile phase used is not easily volatile, such as DMSO or DMF, temperature should be increased to allow correct evaporation process. The temperature can be adjusted during the method optimization process. If you suspect that the compound of interest is thermally labile or semi-volatile, a lower temperature could be used to improve the sensitivity by reducing the thermal decomposition or evaporation.
Fig 6.27:Chromatogram with variing solvent quality The mobile phase should not contain non-volatile solvent modifiers. Volatile solvent modifiers (e.g. CHOOH, CH3COOH, CF3COOH, NH4 Formate, NH4. Acetate, (C2H5)3N)…) can be used, but they may increase the noise level at high gain settings. In addition, the solvent should not contain preservatives, (e.g. Tetrahydrofuran may contain BHT as a stabilizer). The wetted parts of the detector are made from PTFE, stainless steel, and glass.
6.4.5 Optimizing the noise filter The Digital Filter (Fig 5.18) allows maximizing Signal-to-Noise ratio by filtering the noise. The filter strength should be optimized according to the peak shape, and more specifically to the peak width.
7 Maintenance This chapter gives instructions on all maintenance work to be performed in order to keep the device in good working condition. WARNING Death or serious burns by electric current at cleaning. •• Switch off the device •• Disconnect the power cord and prevent unintentional restart •• Wait until the device is completely dry before reconneting to mains NOTICE Risk of housing and device damage by liquids and detergents.
The time required for each step depends on the application, solvents, type and concentration of the samples and should be determined accordingly. NOTE It is not necessary to access inside the device in routine operation. If the suggestions provided in this chapter do not remedy the problem, contact your local distributor. The LED used as the Light Source has a long but finite lifetime (~5000 hours) and should be replaced periodically by a skilled technician.
8 Troubleshooting 8.1 General troubleshooting information The ELSD C-650 Evaporative Light-Scattering Detector is designed to be incorporated into a Liquid Chromatography system. It is important to note that the detector response reflects the overall performance of the system, and a “problem” that is seen on the detector output may not necessarily be a “detector problem”. In almost all cases, there is one and only one cause for a problem.
8.3 Perform the noise test Repeat the tests described in section 5.9 and compare the observed data to the results that were obtained when the unit was initially installed. These tests can be very valuable to isolate the problem. As an example of this point, if the Electronic Noise test (section 5.9.2), Background Noise test (section 5.9.3) and Solvent Noise test (section 5.9.4) provide results that are similar to that obtained when the unit was initially installed, but the Column Noise test (section 5.9.
8.5 Nebulizer cleaning and replacement procedures If the mist of the nebulizer is not homogeneous, the nebulizer, the needle or the PTFE tube may be obstructed. To remove the obstruction, pump a solvent (recommendation: ethanol) that can dissolve the foreign material. As an alternative, the nebulizer can be placed in an ultrasonic bath to dissolve the foreign material. Handle the nebulizer carefully and do not disassemble the rear part of the nebulizer, which is protected by the colored thermal seal.
•• emove the gas inlet quick fitting and the black plastic nut to avoid damaging the seals with R the cleaning solvent. Fig 8.28: Removing parts from the nebulizer To clean the nebulizer: •• •• ill an ultrasonic bath with water. Fill a beaker (50 or 100 mL) with approximately 2 cm of an F appropriate solvent. The solvent is dependent on the nature of the material that is present in the nebulizer. In most cases, ethanol is a satisfactory solvent.
NOTE If the nebulizer cleaning procedure does not solve the problem, contact your local distributor for a nebulizer replacement. In case the black gas tubing has been removed, make sure you are using the correct orientation, where the white one-way valve is at the lower end (near the gas arrival). Avoid leaks at all connections and check for possible leakage when you turn the pump on again.
8.7.2 Device decontamination •• Set the evaporation temperature to 100 °C and the gas pressure to 2 bar (29 psi). Pump the appropriate solvent through the system at the rate of 1 mL/min. The solvent will be determined by the nature of the samples that were previously analyzed by the detector. If you do not know the nature of the sample, ethanol is a good choice. Do not use solvents that can potentially corrode the device. Maintain the flow and temperature during 3 hours at least. •• 8.
9 Shutdown, storage, transport and disposal This chapter instructs how to shut down the device, how to pack it for storage or transport, and specifies the storage and shipping conditions. 9.1 Preparing the device for storage and transport To prepare the device for storage and transport, unplug the power cord and remove all glass parts from the device. 9.2 Storage and transport Store the device at a dry place. Store and transport the device in its original packaging.
10 Spare parts This chapter lists spare parts, accessories, and options including their ordering information. Order the spare parts from BUCHI. Always state the product designation and the part number when ordering spare parts. Use only genuine BUCHI consumables and genuine spare parts for maintenance and repair to assure good system performance and reliability. Any modifications to the spare parts used are only allowed with the prior written permission of the manufacturer.
11 Declarations and requirements 11.1 FCC requirements (for USA and Canada) English: This equipment has been tested and found to comply with the limits for a Class A digital device, pursuant to both Part 15 of the FCC Rules and the radio interference regulations of the Canadian Department of Communications. These limits are designed to provide reasonable protection against harmful interference when the equipment is operated in a commercial environment.
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ELSD C-650 Operation Manual Quality in your hands BÜCHI Labortechnik AG CH – 9230 Flawil 1 T +41 71 394 63 63 F +41 71 394 65 65 buchi@buchi.com www.buchi.com BUCHI UK Ltd. GB – Oldham OL9 9QL T +44 161 633 1000 F +44 161 633 1007 uk@buchi.com www.buchi.co.uk BUCHI Hong Kong Ltd. HK – Central T +852 2389 2772 F +852 2389 2774 china@buchi.com www.buchi.com.cn Nihon BUCHI K.K. JP – Tokyo 110-0008 T +81 3 3821 4777 F +81 3 3821 4555 nihon@buchi.com www.nihon-buchi.
