WUUUUUUUEEUELULUULULUUULUUUUUUL UU LULU UUUUULUULU ES 11.7 Flame Analysis Experiment Introduction This section is designed for first-time users and sets out a typical flame analysis using copper standards. Hardware setting and software parameters are entered using GBC Avanta Ver 2.0 software. ‘The following should only be taken as a guide. The method will need slight modification depending on whether the Avanta ¥, Avanta or 932 is used, ‘Lamp Selection To perform flame analyses the instrument must be configured for flame analysis. To do this perform the following: LL. 12. 13. 14, 15. Left Click on the Instrument icon. A picture of the AAS appears. Right Click anywhere on the front of the instrument panel. A pop-up menu is displayed. Left Click on the Properties selection. An Instrument properties window appears. In the Configuration page ensure that the Flame radio button is selected. This analysis will be performed in manual mode without an auto-sampler. Therefore ensure that the radio button for 'No sampler is selected in the Accessories section found on the same page. } Left Click onthe OK button o escape, Only the AAS with lame should be displayed on the screen. Insert a copper hollow cathode lamp anywhere in the lamp turret. The lamp position must now be entered in the software 3.1. 32: 33. Right Click on the AAS lid Left Click on the Properties selection. Enter 'Cu' in the ‘Element Lamp Table’ in the position corresponding to the number where you actually installed it. Motorised turret. To physically rotate the lamp turret Left Click on “Insert Lamp’. Then Left Click on any number (1 to 4(or 8)) corresponding to the lamp turret position. The lamp turret will then rotate to that position giving access to the chosen lamp position. In this way all 4 (or 8) lamps 95can be inserted. The elements can then be entered in the ‘Element Lamp Table”. 34, Manual Turret/Single Lamp holder. Insert the lamp and then follow appropriate Window Prompt directions. * ‘The actual position where the Cu lamp is entered will depend on which position it was actually installed. Similarly for the Stabilisation delay times enter 0.00. 3.5. When finished Left Click on the 'OK' button to go back to the instrument window. Lamp Aligiment Double Left Click on the AAS lamp turret lid. The "HC and D2 Alignment Status" Window is displayed. The Hollow Cathode Lamp and the Dz lamp must be aligned. Adjust the two knobs found to the left of the Hollow Cathode Lamp until a maximum 'Reference HC' emission value is observed via the meter. Similarly adjust the two knobs located to the left of the D2 lamp until a maximum signal is observed via the ‘Reference D2' meter. (Avanta E. The HCl lamp will be automatically aligned and hence this cannot be manually adjusted). To peak the EHT Left Click on the 'Peak EHT” will be lowered to enable the HCI signal to be approximately 100, Left Click on the to close the window. Method Development Method development is achieved by Left Clicking on the Method Icon. A Notebook appears and by Clicking on the 'Page Markers’ all of the components of the Method Window can be assessed. On the ‘Description’ page select the element Cu by either typing Cu in the element field or by Left Clicking on the arrow next to the element field and selecting the clement from the periodic table. In the 'Matrix' Field any text may be entered which is related to the application (for e.g. ‘River Water). In the 'Notes' field more detailed text can be entered if desired (for e.g. any associated methodology, sampling details, extraction procedures, operator details or details of the sample to be analysed). 96 CORALTTELOLTEREROELEEA eee reer eeeeennneenenrt1e10. il 12. 14, 15 The ‘Instrument’ page sows the default parameters for Cu (3.0 mA lamp current, 324.7 nm wavelength, 0.5 nm slit width and normal slit height). Left Click on the Background correction field to turn the background correction on. On the ‘Measurement’ page select ‘Integration’ for the Measurement Mode, 5 second read time, 0.0 s Time Constant and 3 Replicates. As the analysis is to be in manual mode and a sampler has not been selected in the Instrument properties, the Delay time, Rinse time, Probe height and Micro Sampling mode will not be accessible and will be greyed out. On the Calibration page select Concentration as the Calibration mode. Type any text for the Cone Units such as "ppm" or "ag/mL" Enter 2 in the Decimal places field to enable the results to be reported to 2 decimal places. Select Stop for the Cal. Failure Action field ‘The number of standards to be used and the corresponding concentration are centered in the Calibration Table found on the Standards page. Every time you Left Click on the Add button an extra standard is added to the point where the standard is highlighted (To highlight a standard Left Click anywhere in the Std row). Every time you Left Click on the Remove button a standard is removed from the point where the standard is highlighted. Up to 10 standards can be entered. For this experiment we perform a calibration using 3 standards so Left Click on the Add or Remove button until there are only 3 standards shown in the Calibration table. Prepare 1, 3 and 5 ppm copper standards in 1% HNO3, To enter the concentration values in the software, Left Click on the Cone value in the std 1 row and type 1 and press ENTER. Next Left Click on the Cone value in the Std 2 row (or move focus by using the cursor keys) and type 3 and press ENTER. Similarly enter 5 as the third standard. ‘As readings are taken the absorbances will be added to the Value column. Ifyou Left Click on the View graph button it will show the current calibration graph based on the Cone and Value numbers. The QC parameters are entered on the Quality page. For the purpose of this experiment this will be disregarded. The gas flow rates are controlled from the Flame Control page. Numerical values can be entered but it is better if the system is optimised for the particular element to be analysed, (If fitted Burner Rotation and Burner Vertical/Horizontal are also controlled from this page). To do this Left Click on the Optimise button. Ensure that all gases are ON. Ifa programmable Gasbox is fitted Left Click on the Ignite Flame button and the flame will light. For manual gas box use the front controls. 9716. 17. 18. 19. 20. Aspirate a 5 ppm copper solution and in turn adjust the workhead centre, angle zero, fuel flow, uptake rate and workhead height until a maximum signal (0.700 abs) is obtained as shown by the Inst. Absorbance meter on the page. Once the instrument is optimised Left Click on the 1 button on the top Right hand side of the page to close the window. The method for Copper has been developed. To save this method Left on File (or ALT F). The Left Click on Save As (or A). ‘Type GBCCOPPER in the File name prompt and press ENTER. Note that Method (GBCCOPPER) is displayed on top of the Method window indicating that "GBCCOPPER' is the method currently used. Creating a Samples file 1. Left click on the Samples Module, the samples window will be displayed. 2. Double left click on the first sample listed in the measurement list and a pop- up box will be displayed with the sample types. Select calibration and left click on the tick for OK. 3. Calibration will now be your first sample in the analysis, 4, To add samples to your measurement list, select the button ‘add measurement” and new samples will be added to the end of your list. Performing an An: Left Click on the Result icon. The results page will be displayed. Left Click on the Green START icon to start an analysis. Present the blank, the 1, 3 and 5 ppm standards and samples (the standards can be run as samples) as prompted. When you want to stop the analysis, Left mouse Click on the Red stop button. 98 LELECEPEPCOLUL CPOE OOOO Oe eee eeee cc cceeeeeret-41.8 Flame Optimisation This tutorial demonstrates optimisation of flame and instrument conditions and also shows that flame optimisation is an easy task to perform. Either Air- acetylene or Nitrous oxide-acetylene flame types can be used however using the latter gas combination demonstrates the ease of switching between oxidants. The main features to use in this tutorial are the workhead adjuster and Gas Flows Optimisation software controls. ‘Total time to complete the exercise should be 30 to 60 minutes. Instrument optimization is best performed systematically to achieve greatest productivity and sensitivity. Selecting the initial conditions: Use the same approach to method set up as for the earlier tutorial Flame ‘Analysis Experiment. This assumes some background knowledge for your chosen element for a manual AAS where the gas flows are not computer controlled. The Avanta does not require any prior knowledge specific to the chemical element on the operator's part, except understanding the generic steps involved to optimize conditions for any element Enter the Flame page of the Method module and select the preliminary values for gas flows and bumer angle. Set the flame type to Nitrous oxide - acetylene. ‘Yo optimize: i Leff click the optimise button. NB: Use only the controls in the Gas Flows Optimisation window. That includes Gasbox ignition and shutdown. Using the most concentrated standard optimize flame conditions and burner position using the procedure outlined below. The parameters to be optimized are: burner position (light beam position in the flame) ‘burner angle sample up take rates flame stoichiometry 99Optimization of flame atomization system: 1 Aspirate the top working standard, observing the absorbance signal While adjusting the horizontal burner position. The optimum Position is, found when the absorbance signal is a maximum, btimize the preliminary vertical bumer height in the same way. This Position i the frst set point. When the gas flow rates are changed the Adjust the gas flow rates for the signal is achieved, Reset vertical burner position to give maximum signal, Adjust nebulizer setting to give maximum signal, Repeat steps 3 through to 5 until the maximum possible absorbance reading has been achieved, support and fuel until a maximum 100 PEHHOOHHHHHONNDaaaca.11.9 Graphite Furnace Analysis Introduction This section is designed for first-time users and sets out a typical furnace analy ing lead standards. Hardware setting and software parameters are entered using GBC Avanta Version 2.0 software. The following should be taken only as a guide. ‘The method will need slight modification depending on what type of GBC AAS instrument is used. To perform furnace analyses the instrument must be configured for furnace analysis. To do this perform the following: i. 2, 3, -Left Click on the ‘Instrument ' icon. A picture of the AAS appears. -On the AAS icon Right Click anywhere on the front of the instrument panel -Left Click on the Properties selection. An instrument properties window appears. In the Configuration page ensure that the Furnace button is selected. -This analysis will be performed in auto-sampler mode using the PAL auto-sampler, Therefore ensure that the PAL3000 field in the ‘Accessories field found on the same page is checked by Left Clicking on it. -Left Click on the OK button to escape. Only the AAS with a system 3000 with PAL auto-sampler should be displayed on the screen. Lamp Selection L Physically insert a lead hollow cathode lamp anywhere in the lamp turret. The lamp position must now be entered in the software, Right Click on the AAS lid Left Click on the Properties selection. Enter 'Pb' in the ‘Element Lamp Table’ in the position corresponding to the number where you actually installed it ‘Motorised Turret: To physically rotate the lamp turret Left Click on ‘Insert Lamp' Then Left Click on any number (1 to 4(or 8) corresponding to the lamp turret position, ‘The lamp turret will then rotate to that position gibing access to the chosen lamp position, In this way all 4 (or 8) lamps can be inserted. Left Click on the OK button. The elements can then be entered in the ‘Element Lamp Table’ Manual Turret/Single Lamp holder: Insert the lamp and then follow appropriate Window Prompt directions. ; The actual position where the Pb lamp is entered will depend on which position it was actually installed. Similarly for the Stabilisation delay times enter 0.00. 1017. When finished Left Click on the 'OK' button to go back to the instrument window. Lamp Alignment : 1. Double Left Click on the AAS lamp turret lid. The “HC and D2 Alignment Status Window is displayed. 2 The Hollow Cathode Lamp and the D2 lamp must be aligned. 3. Adjust the two knobs found to the left of the Hollow Cathode Lamp until a maximum ‘Reference HC’ emission value is observed via the meter. 4. Similarly adjust the two knobs located to the left of the D2 lamp until a ‘maximum signal is observed via the ‘Reference D2' meter. rence =porlotesto NOTE: “For the Avanta Sigma the hellow cathode lamp will be {puro automatically aligned and hence this cannot be manually adjusted. ost B Beak the EHT Left Click on the 'Peak EHT' button, The FHT will Goas(euent€ MOBS lowered to enable the HCL signal to be approximately 100. ac ello. _ Left Click on the x to close the window. Workhead Installation 1, Remove the bumer/spray chamber assembly. Position the GF3000 workhead centrally on the rear of the burner/workhead adjuster, and secure using the two anchoring screws. Switch ON the AAS and Computer. Align the furnace workhead as set out below. 2. Optimising the Furnace Workhead Position ‘When the furnace workhead is in place: 4. Right click on the furnace workhead and select optimize workhead adjuster. ” 5. Adjust the workhead center and workhead height (via the software for the Avanta Sigma and manually for the Avanta and 952) while holding white card to visually ensure the light beam passes through the furnace tube. 6. Either via the software or manually, continue using the vertical and horizontal adjustment controls until maximum light (minimum absorbance) throughput is achieved as measured on the Status Panel by the Instrument Absorbance’ meter. Method Development Method development is achieved by the Left Clicking on the Method Icon, A Notebook appears and by Clicking on the ‘Page Markers' all of the components of the Method Module can be accessed. 1. -On the ‘Description’ page select the element Pb by either typing Pb in the Element field or by Left Clicking on the arrow next to the Element field and selecting the element from the periodic table. 2. -In the 'Matrix' Field any text may be entered which is related to the application (for e.g. 'River Water). In the 'Notes' field more detailed 102PSPSPS OOOOCUUUEUUEEUUUUUULESCUUCULE EULER DEED abt default = oltfecto dunivec) = oluseaclo text can be entered if desired (for e.g. any associated methodology, sampling details, extraction procedures, operator details or details of the sample to be analysed). 3. ~The Instrument page shows the default parameters for Pb (3.0 mA lamp current, 217.0 nm wavelength, 1.0 nm slit width and reduced slit height). Left Click on the Background correction field to turn the background correction on. 4. On the Measurement page select 'Peak Area' for the Measurement Mode, 0.0s Time Constant and 3 Replicates. 5. -On the Calibration page select Concentration as the Calibration mode. Type any text for the Conc Units such as "ppb" or "ug/L". 6. -Enter 2 in the Decimal places field to enable the results to be reported to 2 decimal places. 7. -Select Stop for the Cal, Failure Action field. © The number of standards to be used and the corresponding concentration are entered in the Calibration Table found on the Standards page. © Every time you Left Click on the Add button an extra standard is added to the point where the standard is highlighted.(To highlight a standard Left Click anywhere in the Std fow)) lq, © Every time you Left Click on the remove button a st is removed from the point where the standard is highlighted. © Upto 10 standards can be entered. For this experiment we perform a calibration using 3 standards so Left Click on the Add ‘or Remove button until there are only 3 standards shown in the Calibration table. -Prepare a 20 ppb lead standard in 1% HINO3. Using this one standard, the PAL auto-sampler will prepare a calibration using 6, 10 and 20 ppb. To enter the concentration values in the software, Left Click on the Cone value in the Std row and type 6 and press ENTER. Next Left Click on the Cone value in the Std 2 row (or move focus by using the cursor keys) and type 10 and press, ENTER, Similarly enter 20 as the third standard. ‘If you have ‘auto save method after Cal’ selected in the calibration page, as readings are taken the absorbances will be added to the Abs column. if you Left click on the View graph button it will show the current calibration graph based on the Conc and Value numbers. The QC parameters are entered on the Quality page. For the purpose of this experiment this will be disregarded. = ceisg OmiFe Cle /AG Nates CCC ae The furnace program myst now Beénered in the ‘GF Program page To highlight a particular furnace step (for example oni step 4) Left Click in any of the 4 white columns in step 4. Every time you Left Click on the Remove Button, the highlighted furnace will be deleted. 103© Use the below example as a guide as to what your program may look like: Final [Remp] Hold | Ges 90100 150 Inet 120 18.0 | 10.0 | Inert 800 100 50 Inert 800 0.0 1.9 |None, 2100 07 1.3 None 210010 20 In elBelwzelie-[ Note: Steps 1 and 2 cannot be deleted. A syringe : Indicates the injection step. Only one of these per furnace program. Anopen book: Indicates the read step, Only one read step per furnace progam. A graph: Indicates that the signal graphics to be shown for this step. User can select which steps (none to all) where signal graphics are to be displayed. Step 1 will be the inject step. For Example, to enter the parameters in step 2: In the step 2 row; -Left Click in the Final Temp column and type 90° Left Click in the Ramp time column and type 10.0 -Lefi Click in the Hold time column and type 15.0 Double Left Click in the Gas type column and Left Click on the Inert option Step 6 is the read step and signal graphics (Enable Read) should be displayed for this step. To select this right click on step 6 and select ‘set read step", Left Click on the OK button when finished. * Right Click anywhere in the Method Module and select Properties. In the ‘Samples’ choose the Auto-Cale option under ‘Sample Preparation, * Go to the Sample Preparation page to set up the PAL auto- sampler parameters. Select an injection speed of 9uL/s. Enter 10 for the Sample Volume (uL) * Enter 0 for the Modifier volume (uL) Enter 0 for the Aux. Mod volume (uL) Enter 10 for the Total Volume (uL} 104* In the Bulk standards tab enter the concentration of your bulk standard and the position of it on the auto sampler. The method for Lead has been developed. To save this method Left Click on File (or ALT F). The Left Click on Save As (or A). Type GBCLEAD inn the File name prompt and press ENTER. Note that “Method GBCLEAD is displayed on top of the Method window indicating that GBCLEAD mth is the method currently used, Performing an analysis. Left Click on the Result icon. The results page will be displayed. Load the 20ug/L Pb standard in the AUTOMIX position on the PAL auto- sampler. Ensure that there is distilled water in the 'Blank’ position and any samples to be analysed in positions 1 to 10. Left Click on the Green START Icon to start an analysis. Present the blank, the 1,3 and 5 ppm standards and samples (the standards can be run as samples) as prompted. When you want to stop the analysis, left mouse Click on the Red stop button. | | 40- | 4. 105