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26 . System Description

For operation in the ultraviolet (UV) range, mirror M1 is raised to permit radiation from the

deuterium lamp to strike source mirror M2. Source change is automatic during

monochromator slewing.

Radiation from the respective source lamp is reflected from mirror M2 via mirror M3 through

an optical filter on the filter wheel assembly (FW) to mirror M4.

The filter wheel is driven by a stepping motor to be in synchronization with the

monochromators. Depending on the wavelength being produced, the appropriate optical

filter is located in the beam path to prefilter the radiation before it enters the

monochromator. Filter change is automatic during monochromator slewing.

From mirror M4 the radiation is reflected through the entrance slit of Monochromator I. All

slits are located on the slit assembly (SA). The radiation is collimated at mirror M5 and

reflected to the grating table G1. Depending on the current wavelength range, the collimated

radiation beam strikes either the UV/Vis grating or the NIR grating (NIR version only).

The radiation is dispersed at the grating to produce a spectrum. The rotational position of

the grating effectively selects a segment of the spectrum, reflecting this segment to mirror

M5 and then through the exit slit. The exit slit restricts the spectrum segment to a near-

monochromatic radiation beam. Grating change is automatic during monochromator slewing.

The exit slit of Monochromator I serves as the entrance slit of Monochromator II. The
radiation is reflected via mirror M6 to the appropriate grating on grating table G2 and then

back via mirror M6 through the exit slit to Mirror M7. The rotational position of grating table

G2 is synchronized to that of G1. The radiation emerging from the exit slit exhibits high

spectral purity with an extremely low stray radiation content.

In the UV/Vis and NIR range a choice is provided between a fixed slit width, a servo slit, and

a slit program. When the servo slit is selected, the slit widths change automatically during
scanning to maintain constant energy at the detector.

From mirror M7 the radiation beam is reflected via toroid mirror M8 to the chopper assembly

(C). As the chopper rotates, a mirror segment, a window segment and two dark segments

are brought alternately into the radiation beam.

When a window segment enters the beam, radiation passes through to mirror M9 and is then

reflected via mirror M10 to create the reference beam (R).

When a mirror segment enters the beam the radiation is reflected via mirror M10

to form

the sample beam (S).

When a dark segment is in the beam path, no radiation reaches the detector, permitting the

detector to create the dark signal.

The radiation passing alternately through the sample and reference beams is reflected by
mirrors M11, M12, M13, and M11

, M12

, M13

, respectively of the optics in the detector

assembly onto the appropriate detector. Mirror M14 is rotated to select the required detector.

A photomultiplier (PM) is used in the UV/Vis range while a lead sulfide (PbS) detector is used

in the NIR range. Detector change is automatic during monochromator slewing.

At the cell plane, each radiation beam is approximately 12 mm high. The width of the

radiation beams is dependent on the slit width. At a slit width of 5 nm each radiation beam is
approximately 4.5 mm wide.

Содержание Lambda 650

Страница 1: ...LAMBDA 650 850 950 Hardware Guide UV VIS SPECTROSCOPY ...

Страница 2: ...he implied warranties of merchantability and fitness for a particular purpose PerkinElmer shall not be liable for errors contained herein for incidental consequential damages in connection with furnishing performance or use of this material Copyright Information This document contains proprietary information that is protected by copyright All rights are reserved No part of this publication may be ...

Страница 3: ...34 Requirements 34 Unpacking 35 Connecting to the Line Power Supply 37 Connecting the System Components 38 Connecting to the PC 38 Setting up the Instrument in the Software 39 Calibrating the Instrument 42 Using the Instrument 45 Startup procedure 46 The Single Cell Holder 47 Description 47 Installing the Cell Holder 47 Aligning the Single cell Holder 48 Fine Alignment 49 Minimum Volume Applicatio...

Страница 4: ...4 Lambda 650 850 950 Hardware Guide Removing the Detector Unit 67 Accessory Connector Panel 69 Specific Accessory Installation Overviews 70 Pin Configuration 71 ...

Страница 5: ...Introduction ...

Страница 6: ...hapter 2 Safety Practices Important safety information is provided in this chapter It is the same information as given in the Lambda 650 850 950 Getting Started Guide that shipped with your instrument Chapter 4 System Description This chapter contains information on the components of the instrument how it works and instrument specifications Chapter 5 Lambda 650 Installation Information on installi...

Страница 7: ... refers to keys on the PC keyboard is used to show that you have to press two keys at the same time for example ALT F All eight digit numbers are PerkinElmer part numbers unless stated otherwise Notes Cautions and Warnings Three terms in the following standard formats are also used to highlight special circumstances and warnings NOTE A note indicates additional significant information that is prov...

Страница 8: ...uadros éste se proporciona información sobre este tipo de circunstancias F Caution Attention Nous utilisons le terme CAUTION ATTENTION pour signaler les situations susceptibles de provoquer de graves détériorations de l instrument ou d autre matériel Les détails sur ces circonstances figurent dans un encadré semblable à celui ci I Caution Attenzione Con il termine CAUTION ATTENZIONE vengono segnal...

Страница 9: ...s En los recuadros como éste se proporciona información sobre este tipo de circunstancias F Warning Danger Nous utilisons la formule WARNING DANGER pour avertir des situations pouvant occasionner des dommages corporels à l utilisateur ou à d autres personnes Les détails sur ces circonstances sont données dans un encadré semblable à celui ci I Warning Pericolo Con il termine WARNING PERICOLO vengon...

Страница 10: ...10 Introduction ...

Страница 11: ...Safety Practices ...

Страница 12: ...ation provided does not cover every safety procedure that should be practiced Ultimately maintenance of a safe laboratory environment is the responsibility of the analyst and the analyst s organization Please consult all manuals and CDs supplied with the Lambda 650 850 950 and accessories before you start working with the instrument Carefully read the safety information in this chapter and in the ...

Страница 13: ...strument with any covers or parts removed Servicing should be carried out only by a PerkinElmer service representative or similarly authorized and trained person Disconnect the instrument from all voltage sources before opening it for any adjustment replacement maintenance or repair If afterwards the opened instrument must be operated for further adjustment maintenance or repair this must only be ...

Страница 14: ...ipment Only use the Lambda 650 850 950 indoors and under the following conditions Temperature 15 o C to 35 o C Relative Humidity 80 maximum non condensing If possible avoid any adjustment maintenance and repair of the opened operating instrument If any adjustment maintenance and repair of the opened instrument is necessary this must be done by a skilled person who is aware of the hazard involved W...

Страница 15: ...ecommendations and local safety regulations WARNING Hazardous Chemicals Some chemicals used with this instrument may be hazardous or may become hazardous after completion of an analysis The responsible body for example Laboratory Manager must take the necessary precautions to ensure that the surrounding workplace and instrument operators are not exposed to hazardous levels of toxic substances chem...

Страница 16: ... reduced pressure When you dispose of lamps that are defective or otherwise unusable handle them correctly to minimize the implosion risk UV Radiation You should be aware of the health hazards presented by ultraviolet radiation When the deuterium UV lamp is illuminated do not open the spectrophotometer covers unless specifically instructed to do so in the manual Always wear UV absorbing eye protec...

Страница 17: ...ts Capacitors inside the instrument may still be charged even if the instrument has been disconnected from all voltage sources Electrical Protection Insulation Class I as defined in IEC 61010 1 Installation Category The instruments are able to withstand transient overvoltage according to Installation Category II as defined in IEC 61010 1 and IEC 664 Pollution Degree The equipment will operate safe...

Страница 18: ...0 4 3 IEC 61000 4 4 IEC 61000 4 5 IEC 61000 4 6 IEC 61000 4 11 This product complies with EN 55011 Group 1 Class A and with IEC 61000 3 2 and 61000 3 3 FCC rules and regulations This product is classified as a digital device used exclusively as industrial commercial or medical test equipment It is exempt from the technical standards specified in Part 15 of the FCC Rules and Regulations based on Se...

Страница 19: ...hen this label is attached to an instrument it means refer to the manual The following electrical warnings are shown on the rear of the instrument as identified in Figure 1 Figure 1 Lambda 650 850 950 Spectrometer Warning symbols shown on the spectrometer housing ...

Страница 20: ...20 Safety Practices The following warnings are shown on the inside of the lamp compartment as identified in Figure 2 Figure 2 Position of the lamp compartment Lamp compartment ...

Страница 21: ...h side of the fuse holder one at a time using a flat headed screwdriver 3 Gently pull out the fuse holder Figure 4 Removing the fuse holder 4 Replace the fuses with new ones of the same type and rating 3 15 A time delay NOTE The module has two fuses and you should always replace both at the same time even if only one blew as the other may have been weakened 5 Replace the fuse holder by aligning th...

Страница 22: ...ance especially if the instrument may be subject to vibrations or jolts contact your local PerkinElmer service representative for guidance or help If you are only moving the instrument within the laboratory or to a nearby laboratory then use four people and lift the instrument using the handholds as shown in Figure 5 Figure 5 Lifting the Instrument Placement of hands under instrument ...

Страница 23: ...System Description ...

Страница 24: ...the near infrared region The spectrometer features a double beam double monochromator ratio recording optical system These instruments are usable in a wide range of applications as indicated by their performance specifications Figure 6 Lambda 650 850 950 spectrometer features Lamp compartment Power switch Connector panel Sample compartment Detector compartment or accessory Purge inlets ...

Страница 25: ... 7 Schematic of Optical System Two radiation sources a deuterium lamp DL and a halogen lamp HL cover the working wavelength range of the spectrometer For operation in the near infrared NIR and visible Vis ranges source mirror M1 reflects the radiation from the halogen lamp onto mirror M2 At the same time it blocks the radiation from the deuterium lamp M6 SBA Dp Detector Compartment M11 M11 PM belo...

Страница 26: ...ing on grating table G2 and then back via mirror M6 through the exit slit to Mirror M7 The rotational position of grating table G2 is synchronized to that of G1 The radiation emerging from the exit slit exhibits high spectral purity with an extremely low stray radiation content In the UV Vis and NIR range a choice is provided between a fixed slit width a servo slit and a slit program When the serv...

Страница 27: ... while a filter source or detector change is in progress NOTE You can select the source or detector change wavelength within a defined wavelength range This facility is useful if a feature of special spectral interest is located at one of the default change wavelengths The spectrometer scans from higher toward lower wavelengths There is an optional depolarizing filter DP accessory which can be swu...

Страница 28: ...s mm UV Vis blazed at 240 nm Littrow mounting sample thickness compensated detector optics All reflecting optical system SiO2 coated with holographic grating monochromator with 1440 Lines mm UV Vis blazed at 240 nm Littrow mounting sample thickness compensated detector optics Beam Splitting System Chopper 46 Hz Cycle Dark Sample Dark Reference Chopper Segment Signal Correction CSSC Chopper 46 Hz C...

Страница 29: ...0001 T 0 0001 T N A N A N A Wavelength Accuracy 0 08 nm UV Vis 0 30 nm NIR 0 08 nm 0 15 nm Wavelength Reproducibility UV Vis Deuterium Lamp Lines NIR Deuterium Lamp Lines Standard deviation of 10 measurements UV Vis Standard deviation of 10 measurements NIR 0 020 nm 0 080 nm 0 005 nm 0 020 nm 0 020 nm N A 0 005 nm N A 0 06 nm N A Photometric Accuracy Double Aperture Method 1 A Double Aperture Meth...

Страница 30: ...A 8 A 6 A Photometric Display Unlimited Unlimited Unlimited Bandpass 0 05 nm 5 00 nm in 0 01 nm increments UV Vis range 0 20 nm 20 00 nm in 0 04 nm increments NIR range Fixed resolution constant energy or slit programming 0 05 nm 5 00 nm in 0 01 nm increments UV Vis range Fixed resolution constant energy or slit programming 0 17 nm 5 00 nm in 0 01 nm increments UV Vis range Fix resolution constant...

Страница 31: ... Optics Sample Compartment YES YES YES YES NO NO Instrument Dimensions W x D x H 1020 mm x 630 mm x 300 mm 1020 mm x 630 mm x 300 mm 1020 mm x 630 mm x 300 mm Instrument Weight 76 kg 76 kg 76 kg Digital I O RS 232 C RS 232 C RS 232 C Light Beam 90 mm above the base plate 120 mm beam separation 3 mm 12 mm beam height 90 mm above the base plate 120 mm beam separation 3 mm 12 mm beam height 90 mm abo...

Страница 32: ...32 System Description ...

Страница 33: ...Lambda 650 Installation ...

Страница 34: ...as shown in Figure 8 A constant temperature between 15 ºC and 35 ºC Constant humidity between 20 and 80 relative humidity An atmosphere free from dust and corrosive fumes Keep out of direct sunlight Illumination with diffuse lighting is ideal A suitable source of electrical power should be located in the vicinity of the instrument in this case a proper earth grounded 3 wire electrical outlet The s...

Страница 35: ... instrument 1 Unpack the components carefully using four people to lift the instrument itself Keep the packing materials for possible future storage or reshipment Figure 9 Lifting the Instrument 2 Check that you have the following items Part No Description UV WinLab Software Kit ES or Standard 09300004 Lambda 650 850 950 Getting Started Guide 09300005 Lambda 650 850 950 User Manuals CD B0505071 2 ...

Страница 36: ...nual attenuators are only supplied with a Lambda 650 3 Examine the components for any signs of damage in shipment Check the entire outer cabinet of the spectrometer for damage and make sure that terminals fuse holders etc are not damaged Open and close the sample compartment cover checking that it moves freely without binding Make sure that the compartment is free of dust or other foreign matter N...

Страница 37: ...rrect fuses are fitted in the holder at the rear of the spectrometer see Fuses on page 21 NOTE The module has two fuses 5 Make sure that the plug fitted to the line power cord provided with the spectrometer is suitable for your local electrical outlets If it is not remove it and fit a plug conforming to the local regulations 6 After all connections have been made between the various components of ...

Страница 38: ...gap between them Make sure that air can circulate freely over and under the system as well as behind it Do not place anything on or under any of the components that could hinder free air circulation Connecting to the PC The PC is connected using the connection marked COMPUTER on the right side of the instrument as shown in Figure 10 Figure 10 PC Connection NOTE We suggest that you place the ferrit...

Страница 39: ...nt is Service installed you should not need to do this 1 With the instrument switched on in the Main pane of the UV WinLab Explorer select Instruments The Instruments page is displayed 2 Double click Add New Instrument The New Instrument Wizard starts 3 Select the type of instrument from the drop down list The Description below the drop down list details the available instruments for the selected ...

Страница 40: ...is connected to 8 Click Next The software will automatically perform a check to see if the correct instrument is attached to the selected port and switched on and will display a Warning message if not You may then be asked to confirm the serial number of the instrument 9 Check the serial number on the right hand side of the instrument where the PC connects to the instrument correct it if necessary...

Страница 41: ...y installed NOTE Manual Attenuators are only available for the Lambda 650 the Lambda 850 and 950 have automatic attenuators The Common Beam Depolarizer requires a firmware command to be enabled 12 Click Next The Finished page displays all the selected settings 13 If all the settings are correct click Finish to close the wizard and add the instrument The Wizard closes a confirmation message that th...

Страница 42: ...these routines should be performed A check mark indicates the routine is selected and will be performed 17 Click Calibrate The calibrations are performed in the order listed in the table Messages below the table show the progress of the calibration When a calibration has passed a green check mark is displayed in the first column of the table If the test fails a red cross is displayed In such an ev...

Страница 43: ...forms an automatic search for the D2 peak at 656 1 nm The measured peak is then shifted to the exact wavelength Auto search 2 peaks enables you to change the offset and factor The software performs an automatic search for the D2 peak at 656 1 nm and the peak at 0 0 nm The measured peaks are then shifted to the exact wavelengths 0 T This calibrates the electronic offsets Select Auto to enable the s...

Страница 44: ...44 Lambda 650 Installation ...

Страница 45: ...Using the Instrument ...

Страница 46: ...ompartment and any accessories are properly installed NOTE If the sample compartment is obstructed during the startup procedure the spectrometer will not initialize correctly 3 Close the sample compartment 4 Switch on the power switch located at the top right hand corner of the instrument as shown in Figure 11 The switch will light up when there is power to the instrument Figure 11 Power Switch 5 ...

Страница 47: ...te in the sample compartment as shown in Figure 13 The plinth only fits one way round Figure 13 Fitting the plinth to the baseplate in the sample compartment 2 Screw the two thumbscrews by hand into the baseplate Install the single cell holder in the sample compartment as follows 3 Orientate the holder so that the word LAMBDA is toward the front of the sample compartment see Figure 14 below 4 Lowe...

Страница 48: ...ment of the single cell holder is carried out as follows 1 Open the sample compartment cover 2 Fill cells with a low absorbing solvent deionized water or ethanol 3 Insert one cell into the sample cell holder and one into the reference cell holder Make certain that the cell is pushed down fully NOTE The alignment procedure is for a given cell in a given holder After alignment the cell should always...

Страница 49: ...ndow for micro flowcells should be ideally approximately 15 mm above the base of the cell Figure 15 Correct alignment of the radiation beam in the cell sample area 10 If alignment is required turn the vertical adjustment screw on the lifter either clockwise to raise the cell or counterclockwise to lower the cell 11 Recheck the horizontal alignment of the radiation beam through the cell and correct...

Страница 50: ...tighten the milled posts and the locking screws on the cell holder 8 Reinstall the reference cell in the reference cell holder 9 The sample cell remains in its holder 10 Repeat steps 4 to 6 with the reference cell holder but this time obtain the lowest possible transmittance reading on the display This completes the fine alignment procedure NOTE When the cell holder has been aligned once you can t...

Страница 51: ... µL 0 01 cm 2 µL B0510076 2 5 µL 0 5 cm 5 µL B0510077 5 µL 0 1 cm 10 µL B0510078 5 µL 1 0 cm 10 µL B0505823 Cell window completely filled with liquid 30 µL 1 0 cm 50 µL B0190608 NOTE You should align microcells very carefully in the radiation beam by following the procedures in Aligning the Single cell Holder on page 48 When aligning microcells fill each cell with the minimum volume of liquid spec...

Страница 52: ...in Figure 16 The inlet nearest the rear of the instrument is for the sample compartment and the one nearest the front of the instrument is for the main optical compartment After purging these compartments the nitrogen escapes to atmosphere Figure 16 Connectors for the purge gas supply You should keep the sample compartment closed during routine operation to prevent the ingress of water vapor and o...

Страница 53: ...53 NOTE A Nitrogen Purge Accessory Kit comprising of a filter and a flow controller with flowmeter is offered as an option With this kit you can control the gas flow more accurately NOTE The Lambda 650 does not have this purge facility ...

Страница 54: ...54 Using the Instrument ...

Страница 55: ...Maintenance ...

Страница 56: ...tion and to ensure the highest possible level of performance It includes maintenance checks that should be done on a daily basis and maintenance procedures that should be done periodically depending on instrument use This chapter is divided into several sections each section covering maintenance procedures for a particular component of the system You should perform only the maintenance procedures ...

Страница 57: ...y If any type of sample handling system is installed and portions of it are left in the sample compartment such as a sipper and flowcell make certain that the system is cleaned at the end of the working day Generally such systems should be filled with deionized water when left overnight CAUTION Spills Take care not to spill liquids onto the spectrometer Expensive damage can result to the optics or...

Страница 58: ...pectrometer The windows seal the sample compartment and thus protect the instrument s optics from dust and fuming or aggressive samples Generally the windows should be installed at all times The windows are an optical component and require the same care and handling as cells The windows can be removed to clean them Each window has a magnetic frame and can be carefully removed by hand Windows are m...

Страница 59: ... or against other hard surfaces Avoid abrasive corrosive or stain producing cleaning agents and make certain that the exposed surfaces of cells are optically clean Always wipe the optical surfaces of cells dry and free of finger marks using a soft cloth or cleaning tissue just before placing them in the cell holder When measuring cold solutions always bear in mind that condensation can form on the...

Страница 60: ...eter and remove the plug from the electrical supply before starting with the replacement High Temperatures Risk of Burns Lamps soon become very hot make sure that the lamps and the lamp compartment have cooled to room temperature before you touch them UV Radiation The lamps emit intense UV radiation which can damage your eyes Do not open the lamp compartment when the lamps are on Do not gaze into ...

Страница 61: ...ogen Lamp 1 Switch off the spectrometer and disconnect the line power cord if necessary wait until the lamps and lamp compartment have cooled to room temperature 2 Remove the lamp compartment cover by lifting vertically from the handhold on the rear of the instrument Figure 20 Removing the lamp cover 3 Remove the lamp cover by undoing the two screws and lifting vertically 4 Carefully pull the halo...

Страница 62: ...e halogen lamp 9 Wipe the halogen lamp bulb with a soft cloth moistened with alcohol to remove dirt since this would otherwise be burned in when the lamp is hot 10 Replace the lamp compartment cover by lowering it into position This completes the halogen lamp replacement procedure NOTE Due to the pre aligned mounts the alignment of lamps after installation is generally so good that further alignme...

Страница 63: ...ulling the lamp mount vertically upward Save the thumbscrew for use with the new lamp assembly 6 Unpack the new lamp assembly taking care to hold it only by the metal mount to prevent finger marks on the lamp window 7 Slip the slot at the base of the lamp mount over the stud on the bracket in the lamp compartment and then secure with the thumbscrew 8 Plug the deuterium lamp connector into the sock...

Страница 64: ... supplies see essentials perkinelmer com Quantity Item Part Number 1 Pack of 10 fuses 3 15 A time delay B0155573 1 RS 232 printer cable B0166569 1 Deuterium Lamp pre aligned B0160917 1 Halogen Lamp pre aligned B0114620 1 Thumbscrew for lamp mount B0119371 1 Set of Sample Compartment Windows for Lambda 950 B0505982 1 Set of Sample Compartment Windows for Lambda 850 or 650 L6020417 1 Single Cell Hol...

Страница 65: ...hat may need to be made to the basic spectrometer before installing an accessory and an overview of the installation required for some of the specific accessories Full procedures for installing the accessories in the spectrometer are described in the directions provided with the respective accessories Removing the parts of the Sample Compartment Removing the Sample Compartment Cover 1 Open the sam...

Страница 66: ... sample compartment cover open or removed undo the four thumbscrews shown in Figure 24 Figure 24 Four thumbscrews on the sample compartment baseplate 2 Lift the baseplate up off the locating pins and remove it from the sample compartment Removing the Sample Compartment 1 After removing the sample compartment cover and baseplate as described above undo the four retaining screws shown in Figure 25 T...

Страница 67: ...d disconnect the instrument before removing or fitting a detector accessory unit 1 Switch off the spectrometer and disconnect the line power cord 2 Open the sample compartment cover 3 Undo the two retaining screws located under the blanking caps on the top of the detector Figure 26 and are accessible using the long posidrive screwdriver supplied with the instrument Figure 26 Undoing the retaining ...

Страница 68: ... the spectrometer The detector unit is installed by performing this procedure in reverse tightening the retaining screws and making sure the blanking caps are in place WARNING Make sure you screw down the detector unit as this creates the earth bonding for elctrical safety Details of the installation procedure for a sphere or Universal Reflectance Accessory URA are given in the relevant manual on ...

Страница 69: ...NOTE The insulation of externally connected accessories should meet the requirements of IEC 61010 1 or IEC 60950 Figure 29 Possible accessories for a Lambda 650 850 950 Sites for accessory PCBs 15 Pin Accessory Sockets marked ACCESSORY 1 on the left and ACCESSORY 2 on the right 15 way HD D type maximum voltage 12 to 24 V RS 232 Interface Socket marked COMPUTER 25 way D type maximum voltage 12 V Pe...

Страница 70: ...hanger manual Temperature Sensor Connector on Spectrometer Slot in accessory board Installation See temperature sensor description Cables Lead through the tube ports Sample Compartment Cover Unchanged NOTE When connecting the temperature sensor align the red mark on the plug with the red mark on the socket Pull back the collar on the plug to connect disconnect the plug Release the collar to secure...

Страница 71: ...The pin numbering is shown in Figure 31 and the configuration is given in the following table Figure 31 Pin configuration of 15 pin connector Pin Configuration Description Pin Configuration Description 1 GND D Ground Digital logic 9 Not used 2 5 V Logic power supply 10 Not used 3 Not used 11 12 V Analog power supply 4 GND P Ground Power 12 GND A Ground Analog 5 24 V Power Supply 13 12 V Analog pow...

Страница 72: ...72 Maintenance ...

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