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iCAP Customer Familiarisation Manual

Page 66 of 72

This document is part numbered 849940090071

Version 1.02

10.4 Preventing blocking of

the nebuliser

The most common problem with the
nebuliser is the blockage of the tip by
the deposition of particulate matter. In
this section we provide a series of
suggestions to minimise blockage.

In most instances blockage in the
nebuliser is caused by either
particulate matter (from the sample)
or chemical deposits. It normally
occurs in the nozzle where the flow
passages are extremely small and
constriction is greatest in the annular
gas channel between the tip of the
capillary and the taper of the nozzle

.

o

Tip:

Filter the sample. The sample capillary is more tolerant of particulate

matter than the gas annulus. For high sample uptake nebulisers, the capillary
will frequently transport visibly turbid suspensions. We suggest that you filter or
centrifuge the sample if the solids are not of analytical importance. Particulates
and colloids of a polar nature such as silica, peptides, polyvalent metal
hydroxides and others tend to build up on the (polar) glass and impede the fluid
flow. In some instances you can prevent deposition by adjusting the pH of the
suspension away from its isoelectric point.

o

Tip:

Rinse the nebuliser. It is very important to rinse the nebuliser before

turning the gas off. It is advisable to rinse the nebuliser periodically throughout
the sequence (depending on the chemistry of your samples).

o

Solids may be deposited in the nozzle as sample solvent evaporates, further

constricting the flow passages and reducing the signal. Rinsing will minimise or
eliminate these deposits.

o

Gas flow through most nebuliser models creates a venturi suction at the capillary

tip which can be used to draw rinse liquid through the capillary.

o

After the testing of any salt solution, promptly rinse the system with a chemically

compatible rinse consisting only of volatiles (this is especially necessary in flow
injection analysis systems).

o

A low-pH (acidic) sample should be followed by a low-pH rinse, a high-pH
sample by a high-pH rinse and an organic sample by an appropriate solvent.
The final rinse should use deionised water and/or isopropyl alcohol

.

Note: Allow the nebuliser to dry before turning off the gas and make
sure that the liquid feed is disconnected or arranged so that siphoning into
the nebuliser while the gas is off cannot occur.

DO NOT use ultrasonic cleaning to remove particulate matter as

sympathetic vibrations may be set up in the capillary causing it to
bounce against the inside of the nozzle and chip, also do not use
any wire to clean capillary of the nebuliser. performance of the
nebuliser can decline as a result.

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Содержание iCAP 7000 Series

Страница 1: ...iCAP 7000 Series ICP OES Spectrometer Customer Familiarisation and Maintenance Manual March 2013 Thermo Fisher Scientific Inc www thermoscientific com http www thermofisher com ...

Страница 2: ... of the spray chamber drain 11 5 7 Position of the nebulizer in the spray chamber 12 5 8 Connection of spray chamber adaptor to torch assembly 13 5 9 Connection of pump tubing 14 5 10 Radial view window on a Duo instrument 16 5 11 iCAP Sprint Valve installation guide iCAP 7600 only 17 6 Autosampler Use 21 6 1 Introduction 21 6 2 Autosampler Installation 21 6 3 Autosampler Set up 21 7 Instrument Op...

Страница 3: ...tenance in the case of poor precision and detection limits 65 10 1 Introduction 65 10 2 Typical Maintenance Schedule 65 10 3 Replacing pump windings 65 10 4 Preventing blocking of the nebuliser 66 10 5 Removing solids from the nebuliser 67 10 6 Cleaning the glass mixing chamber 69 11 Sample Introduction Spares Consumables 70 ...

Страница 4: ...a spray chamber small droplets then pass through the center tube in the torch to the plasma Solvent is evaporated and the residual sample decomposes to atoms and ions that are excited by the electrical Radio Frequency RF generated Plasma to 9000K that will emit a unique set of wavelengths of light for each element as they decay to a lower energy state The intensity of this light is measured and th...

Страница 5: ...such that the light is dispersed at right angles to the direction of light dispersal by the grating This combined dispersal generates a two dimensional spectrum echellogram consisting of a wavelength and order separation The CID detector is cooled to 45ºC to increase sensitivity and dynamic range Warning Before operating your iCAP ensure you read and understand all the safety information in the iC...

Страница 6: ...with running your instrument including comprehensive software user guides can be found in The Quick Start Guide includes basic information required to get you started with operating your OES The User Manual details the operation and maintenance of your instrument hardware It also ut the safety hazards involved in working with the spectrometer and its accessories and the means by which such hazards...

Страница 7: ...analysing samples 4 2 Preparing the System for Use If the gas supplies have been switched off the optical components should be purged and for at least one hour before powering on the instrument This is to stop ice damage to the camera which is cooled to 45ºC It will take at least 4 8 hours of normal purge for the iCAP 7400 or iCAP 7600 instruments to measure aluminium at 167nm with the specified s...

Страница 8: ...e to a parked position after about thirty seconds After plasma has been turned off for at least 30 seconds turn off the chiller following the manufacturer s instructions turning off the chiller by removing the power can often cause breakages Allow five minutes after switching off the plasma before disconnecting the electrical power or other supplies to the instrument or accessories The tension on ...

Страница 9: ...ected and replaced if any wear or damage is visible Gloves must be warn when handling a torch as contamination from hands will make the torch harder to light and reduce its life The quartz body of the torch should be pushed into the metal torch mount Ensure the torch body is pushed fully into the metal torch mount The marked circle on the quartz torch should be aligned with the notch on the torch ...

Страница 10: ...lasma may go out 5 2 2 1 5mm RED band centre tube Best compromise for a radial instrument 5 2 3 2mm Blue band centre tube Best Compromise for a duo instrument 5 2 4 2mm Ceramic centre tube Used for specific sample types for example hydrofluoric acid digests 5 3 Centre tube holder Check the 4 o rings in the Center tube holder are not damaged Insure the centre tube is inserted fully into the plastic...

Страница 11: ...ill reduce the lifetime of the O ring seal When fitted the center tube should be 1 3mm lower than the intermediate tube as shown above 5 5 Torch holder insertion into the torch box Insert the torch holder into the torch box and turn the metal torch holder clockwise until the red orientation lock self locates in the torch box casting 5 6 Positioning of the spray chamber drain Insert the white plast...

Страница 12: ...nd replaced if any wear or damage is visible Using a twisting motion insert the nebulizer into the spray chamber so that the nozzle is level with the arc of the edge of the spray chamber Small movements in and out are required to optimize the measurement precision Modern designs of nebulizers have a collar to set the depth into the spray chamber By inserting the nebulizer into the spray chamber so...

Страница 13: ...older is fully rotated and locked into the torch Make sure the spray chamber adaptor is fully pushed into the torch body Make sure the spray chamber is tightly clamped to the spray chamber adaptor Problems in any of these areas may cause air leaks or disruption of the gas flows making the plasma difficult to ignite and may cause damage to the torch WARNING It is extremely important that the correc...

Страница 14: ...The drain pump tubing has white blue and white stops For all instrumentation the assembly procedure is similar Feed the sample capillary tubing from the rear of the nebulizer through the upper holder in the cover and towards the pump Ensure there are no twists or bends in the nebulizer and drain PTFE tubing that may prevent flow of the sample Pass the drain capillary tubing through the lower holde...

Страница 15: ...nd should be replaced if there are indications of wear Additional lengths of capillary tubing should be used to allow connection to the input of the sample pump tubing to the sample and the output of the drain pump tubing to a waste container For a freely aspirating nebulizer The pump tension can be adjusted with the plasma running and the pump stopped Lock the sample pump tubing and clamp into po...

Страница 16: ...w window on a Duo instrument For a Duo instrument check that the radial view bucket shaped window is in place and clean It is possible to rotate the window holder to gain access take the torch out before inspection When assembling the torch and radial view window insure the window is located against the torch as shown below ...

Страница 17: ...0 only 5 11 1 Connecting the tubing Fit the drain fitting to the spray chamber black ringed insert the fittings capillary tube into the yellow blue peristaltic pump tubing and attach it to the pump so that the waste runs counter clockwise across the pump Cut a length of the supplied drain tubing so it can reach between the pump tubing and the waste container ...

Страница 18: ...ve fitting and the carrier uptake tube bubbler into the white white peristaltic pump tubing Attach the pump tubing onto the peristaltic pump so that the bubbler runs counter clockwise across the pump Screw the green valve fitting into port 5 on the valve head Next take the white valve fitting tube and attach one end to port 3 on the valve head ...

Страница 19: ...vacuum valve connector on the iCAP Attach the vacuum pump waste tubing to the waste out connector on the iCAP and insert the other end into the waste container Screw the autosampler probe valve fitting into port 2 on the valve head Attach the sample loop into ports 1 and 4 on the valve head this is the same as the loop provided in the Field Service Test Kit ...

Страница 20: ...090071 Version 1 02 Screw the fitted nebulizer tube into port 6 Attach the other end on the nebulizer line and the nebulizer gas fitting onto the nebulizer 5 11 2 Manual sampling using the Sprint Valve Manual sampling uses the Inject position 5 with a standard or non aerating sample probe ...

Страница 21: ...d warranty requirements the iCAP 7000 accessories and associated equipment must be installed by a Thermo Fisher trained and certified engineer Refer to the Autosamplers Operators Manual for assembly and maintenance 6 3 Autosampler Set up For analysis with an autosampler the capillary tubing attached to the end of the autosampler probe should be attached to the end of the sample pump tubing on the ...

Страница 22: ...ng Height on a radial instrument 7 1 2 Radial instrument Plasma viewing height Used to select optimum height view height 7 1 3 Radial Axial View On a Duo instrument you have a choice of Axial and Radial views you will have to select the view you want to use manually General rule all low Wavelengths Axial View all High Wavelengths Radial view 7 1 4 RF Power 1150 works with most samples you may want...

Страница 23: ...n gauge near instrument Turn on the purge gas if separate Note for normal use gas should be left purging constantly Turn on the air supply for the Additional gas supply 7600 only if used Switch on power to iCAP Spectrometer Note for normal use power should be left on constantly Switch on Water Chiller Push Platen on to rollers of pump by way of the 4 3 pressure screws Make sure the drain tube is p...

Страница 24: ...will not light If the LED flickers even slightly the plasma will go out and this indicates there is a problem with the chiller Drain Flow sensor if this is red this indicates that the iCAP has not seen an air bubble in the drain sensor for two minutes it will turn the plasma off To reset the drain sensor turn the pump on to 45RPM Exhaust flow This interlock checks that the exhaust is of sufficient...

Страница 25: ...le introduction and Standards On installation the Torch Alignment and Autopeak must be completed first 4 Use Manual Sampling If an autosampler is configured this will enable the use of manual sampling Clicking OK will turn the plasma on and spectrometer optimization will be performed During these procedures the remaining warm up time is shown in the Dashboard page Note To allow the plasma to stabi...

Страница 26: ...LabBooks can be created from blank Templates existing Templates imported Templates of appropriate configuration or from existing LabBooks From Analytes use the Periodic Table to begin selecting your elements of choice by pausing cursor over the element symbol to see a preferred wavelength list as shown below ...

Страница 27: ...dic Table and a left click on the element of choice to auto pick from the top of the preferred wavelength list Where the first element wavelength is not desired a right click will bring up a window and allow optional selections This also will show interfering elements graphically assuming they are the same concentration as the analyte ...

Страница 28: ...ource parameters such as RF Power Nebulizer and Additional Gas flows if used and Exposure Time s may be adjusted The Acquisition Parameters window shows among other things default slit positions measure mode view used and left and right background settings Here Analysis Modes Speed Normal Sprint and sample pump RPM s can be set ...

Страница 29: ... and not in the standards list From the Standards window select New to add a standard where Elemental Standard should be selected The default concentration can be set prior to creating the standard by clicking the button to minimize typing Otherwise double click each Concentration field and type in values Repeat this for each standard and QC check required for the Method LabBook ...

Страница 30: ...anual Page 30 of 72 This document is part numbered 849940090071 Version 1 02 As above double click each Concentration field and type in appropriate values As above double click each Concentration field and type in appropriate values ...

Страница 31: ...menu When an autosampler is being used define Wash Time and Uptake Times by selecting the appropriate autosampler Rack type selection changes may also be made here NOTE For the iCAP 7600 Sprint Valve the Wash Time may be set to ZERO as this function is multi tasked with the Uptake Time which can also be reduced to about 20 seconds as using the Valve provides quicker sampling ...

Страница 32: ... the Sample list to build a sequence and define the samples to be analyzed Add lines individually for BLANK and each of the calibration standards and QC checks Use the label identifier and sample type drop down list as required If using an autosampler identify the rack and vial for each sample at the far right on this table Click the down arrow next to the Add lines button for multiple rows additi...

Страница 33: ...lick OK Under the Label column you can type individual identifiers or type one followed by a number such as sample 1 then highlight the column right click in the highlighted column and select Increment fill to fill down with numbering This same Increment fill technique can be used for sample type and rack and vial at the end of this table for sample tube locations ...

Страница 34: ...highlight the QC Check standard row click the Copy tool bar button click the location where you would a check performed then click the Insert tool bar button repeat for each location desired Every 10 samples is common for this example 5 was used For a final check at the end of the sample list the Append tool bar button can be clicked ...

Страница 35: ...ok click Save 7 6 Running the Analysis In the toolbar of your LabBook click Run to schedule the LabBook for execution will not be active unless properly saved The LabBook is added to the scheduler If the check box Automatic has been selected for Start Queue in the options settings of the scheduler the measurement is started immediately ...

Страница 36: ...iCAP Customer Familiarisation Manual Page 36 of 72 This document is part numbered 849940090071 Version 1 02 ...

Страница 37: ...he analyte wavelengths are correctly aligned in the centre of the sub array measurement window The iCAP 7000 Series Spectrometer will automatically check a reference line each time the plasma is ignited to maintain wavelength accuracy Auto Peak only needs to be run whenever a new wavelength is used for analysis The autopeak may also need to be run if the instrument has been switched off for an ext...

Страница 38: ...multiple standards may be used The result of the test is displayed in the bottom right side of the page If the test is unsuccessful or partially successfully there is a message in the log view tab stating the reason of the failure This is normally due to the solution not being aspirated for long enough before the test began or a problem with the solution 7 8 Setting the pump tension To ensure long...

Страница 39: ...orch body or centre tube has been replaced Click on Qtegra to open the program In the Dashboard Page click Torch Alignment to start the procedure Introduce a loaded Blank sample 2 ppm Zn solution And ensure you leave enough time for the sample to enter the plasma before clicking ok Aspirate until the process is finished The result of the test is displayed in the bottom right side of the page 7 10 ...

Страница 40: ...is part numbered 849940090071 Version 1 02 The report structure works by group with two types of groups Result Group and Method Parameter Group 7 10 1 Result Group The general structure of reports is shown here with Result groups divided into Headers Rows and Columns ...

Страница 41: ...071 Version 1 02 The general structure of reports is shown here with one group and several results samples Having selected the Result group option different groups can be created and selected for the report The order of the groups can be changed as well using the arrows next to Create report ...

Страница 42: ... This document is part numbered 849940090071 Version 1 02 A name for the Result Group can be added and ticking boxes selects groups to add to data reporting Press Create Report Selecting Show Calibration Graphs will display the graph before any results ...

Страница 43: ...ument is part numbered 849940090071 Version 1 02 The Header section allows selection of the information for each sample This is displayed before the results table The Rows section allows the selection of data appearing for each sample Concentration average RSD ...

Страница 44: ...dually or transfer Analytes to the right to select all Save Groups saves changes to the group settings Any groups saved can then be used or modified for other LabBooks The latest saved version is the live version Create Report applies settings to the current LabBook The report can be printed or saved Going back to the group settings allows changes which can be and applied by selecting Create Repor...

Страница 45: ...group As for the Result group name the group Select the source of the data to be included in the report create different groups to include different sources and within one source select the required fields to be included Table Options are used to set the formatting and the arrows next to Create Report are used to set the positioning ...

Страница 46: ... can be used to obtain help by e mail Problem reporting From the home page go to File Manager Right hand click a LabBook and select Export from the menu Select the location to save the data and press OK Other data such as instrument logs can also be exported as a csv file This is particularly useful when requesting Service Engineer help ...

Страница 47: ...ut down For the 7600 Sprint Valve open the Sprint Valve Configurator software from the desktop icon When the software starts most of the options will be grayed out click Connect to Sprint Valve Expand the screen using the arrow button on the right side of the window to open manual controls Verify both Sample and Rinse probes are in air verify or set to Load turn On the Vacuum Pump Control for seve...

Страница 48: ...iCAP Customer Familiarisation Manual Page 48 of 72 This document is part numbered 849940090071 Version 1 02 ...

Страница 49: ...should be followed Components contaminated with sample residues should be cleaned It is recommended that several spares for each part are available in case blockages sample contamination and breakages happen during analysis Suitable protective clothing glasses and gloves should be worn 8 1 2 Torch Cleaning The O rings in the metal torch mount 3 internal 2 external should be inspected and replaced ...

Страница 50: ...l then when dry re insert the POP window into the fore optic assembly Warning Do not open this access door when the plasma is running there is a potential UV radiation hazard All mirrors in the optical system are coated so be sure not to touch the mirror below the radial view POP window in the Duo configuration If further cleaning is necessary remove the quartz window from the POP window holder an...

Страница 51: ...ncludes checking sprint valve components for leaks or other damage Additional periodic maintenance tasks may be required including replacement of the following components peristaltic pump tubing rinse tubing and sample probe 8 2 4 1 Regular Inspection of Components XE inspection The procedure for cleaning the sprint valve inspection for leaks and replacing damaged components is detailed below It i...

Страница 52: ...E It is recommended to clean the 6 port valve every 20 000 cycles or approximately every 1 2 weeks However the frequency of cleaning interval will vary depending on application The valve head should be cleaned regularly as part of the routine maintenance of the sample introduction components spray chamber nebulizer etc To clean the valve complete the following steps To clean the valve head start b...

Страница 53: ...ion 1 02 Remove the Stator and the separator noting their orientation Carefully remove the rotor from the valve Using a clean cloth gently clean the channels ports and surfaces of the stator and rotor If necessary use low pressure canned air to blow the channels and ports free of any remaining debris ...

Страница 54: ...Familiarisation Manual Page 54 of 72 This document is part numbered 849940090071 Version 1 02 Carefully replace the rotor into the valve the rotor will only fit in the correct orientation forcing it will cause damage ...

Страница 55: ...e screws through the stator and separator and reattach it to the valve in the orientation noted during removal Using the hexagonal key tighten all three screws to firmly set the parts in place NOTE The screws should be finger tight with the separator unable to move independently over tightening can cause damage to the rotor ...

Страница 56: ... complete the following steps Remove and replace all tubing as necessary using care to remove replace tubing at barb fittings and at compression type fittings without damaging those fittings to which they connect For more information on how to install the rinse tubing refer to the installation section earlier 8 2 4 7 Replacing or Reorienting the 6 Port Valve XE valve replacement XE 6 port valve t ...

Страница 57: ...e retraining To replace or re orientate the 6 port valve Remove all of the tube connectors to the 6 port valve Using the provided hex key 9 64 loosen the hex screw on the locking collar which secures the base of the valve to the instrument Firmly but carefully remove the valve head Insert the new valve or reinsert the existing valve at the desired angle Rotate it so that the nebulizer port will be...

Страница 58: ...iCAP Customer Familiarisation Manual Page 58 of 72 This document is part numbered 849940090071 Version 1 02 ...

Страница 59: ... 02 Push in the valve to make sure that it is completely seated there should be no gap between the valve and the collar Use the hex key to tighten the locking collar Open the sprint valve Configurator software Expand the software using the arrow button on the right side of the window and click home valve ...

Страница 60: ...iCAP Customer Familiarisation Manual Page 60 of 72 This document is part numbered 849940090071 Version 1 02 Reconnect the tubing Check for any leaks using the manual cycle function ...

Страница 61: ...A 10 ppm solution of a few common elements such as Cu Mn Ba Cd Zn and Fe should be put together and a method made using the primary lines and default conditions After standardisation the standard should read back on the iCAP for example with a precision of typically 0 2 to 0 5 percent with a 10 second integration time If the precision obtained is substantially greater than this try Torch alignment...

Страница 62: ... fitting then with a magnifying glass look for any small obstruction Also check the capillary for obstructions iCAP Customer Familiarisation Manual This document is part numbered 849940090071 usually indicative of dripping In a glass or Teflon chamber the chamber operly that is there should be no water droplets building up on the walls of the spray This is usually caused by an oily film and can be...

Страница 63: ...scissor or pinch cut ends For best results razor cut at 45 for the drain Also check the sample peristaltic pump winding condition and platen pressure for proper adjustment Replace the winding if it is used or ump windings typically last only a couple of days Introduce an air bubble into the sample uptake tube and watch its migration through the tubing it should be smooth and consistent Worn roller...

Страница 64: ...this tes as the ability to read a 1 or 100 ppm standard after standardising on the 10 ppm Most of the time that problem is operator related As far as we are concerned at this point we have only one standard to test with If this simple standard will not repeat back for all elements check the pump winding first Replace it if it is used or collapsed Note Pump windings typically last only a couple of ...

Страница 65: ... acids and highly polar organic solvents e g methanol and ethanol Viton Solvents of low polarity e g alkanes aromatics and halogenated hydrocarbons such as gasoline kerosene Toluene xylene chloroform and carbon tetrachloride SOLVAFLEX Solvents of low polarity e g alkanes aromatics and halogenated hydrocarbons such as gasoline kerosene Toluene xylene chloroform and carbon tetrachloride A pump tubin...

Страница 66: ...ip Rinse the nebuliser It is very important to rinse the nebuliser before turning the gas off It is advisable to rinse the nebuliser periodically throughout the sequence depending on the chemistry of your samples o Solids may be deposited in the nozzle as sample solvent evaporates further constricting the flow passages and reducing the signal Rinsing will minimise or eliminate these deposits o Gas...

Страница 67: ...o the nozzle forcing the gas backwards through the annulus and the capillary back flushing Note Make sure the nebuliser is held securely during this operation Gently tap or flick the shell soundly with your fingernail a few times If this fails to dislodge the particle close off the liquid and gas input tubes with your fingertips When the pressure builds up move your fingertip quickly off the appro...

Страница 68: ... material is gone rinse the nebuliser with isopropyl alcohol and dry thoroughly Immerse the nozzle in a rinse solution Warm the solution for stubborn deposits Follow with a rinse of pure solvent then isopropyl alcohol and dry thoroughly If the deposit remains after prolonged soaking apply pressurised gas at the appropriate input s to help force the deposit away 10 5 4 Organic matter Immerse the no...

Страница 69: ...nsert the wire or any other object into the gas annulus 10 6 Cleaning the glass mixing chamber The glass mixing chambers need cleaning if an oily film is deposited on the chamber walls as these deposits can cause the sample to bead and form large droplets on the chamber walls When these large droplets finally drip to the drain a change in back pressure causes a spike to the sample injection and el...

Страница 70: ...1971 Torch body assembly torch holder including o rings 8423 155 50171 Centre tube holder assembly centre tube holder including o rings 8423 155 50181 Sampling O Ring Kit includes o rings for new and old torch assembly 8422 120 51401 Spray Chamber 8423 120 51411 Ball Joint Clip 8423 120 51421 Nebuliser 8423 120 51431 Spray Chamber Jacketed 8423 120 51441 Radial Spray Chamber HF 8423 120 51451 Duo ...

Страница 71: ...le Organics Kit Order pump tubing separately 842312052251 Mini Pump Tubing Aqueous mini pump sample tubing 7400 7600 842312052401 Aqueous mini drain tubing 7400 7600 842312052411 Organics mini pump sample tubing 7400 7600 842312052421 Organics mini pump drain tubing 7400 7600 842312052431 Sprint Valves Aqueous sprint valve kit 842312052631 Organic solvent sprint valve kit 842312052641 Sprint valve...

Страница 72: ...sembly for oil samples 1mm internal diameter 1 02ml volume 842347004054 Sample loop assembly for oil samples 1mm internal diameter 1 48ml volume 842347004055 Sample loop assembly for oil samples 1mm internal diameter 2ml volume 842347004056 Sample loop assembly for oil samples 1mm internal diameter 3ml volume 842347004057 ...

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