PerkinElmer Aanalyst100

Transcription

1 Using of AAS Model PerkinElmer Aanalyst100 Mr.Pisipong Meunprasertdee Scientist Instrument Center Faculty of Science and Technology 1 Using of AAS Model PerkinElmer Aanalyst100 2 AAS Training Jan 5-6,

2 Turn on Flame-AAS 3 Turn on AAS 1. Switch on electric system 4 AAS Training Jan 5-6,

3 2. Switch on hood and air conditioner 5 3. Turn on UPS, wait to alarm stop and electric current be still - Turn on computer and AAS 6 AAS Training Jan 5-6,

4 4. Turn on AAS 5. Turn on computer 7 6. Switch on Air pump and Close Drain daily valve 8 AAS Training Jan 5-6,

5 7. Open gas valve (Acetylene), the pressure should not be less than 70 psi 9 8. Insert HCL lamp will use 10 AAS Training Jan 5-6,

6 9. Click AAwinlab Analyst icon to open program >> wait to check green at Aanalyst 100 >> click Exit Choose Flame Technique >> click Menus and Toolbar 12 AAS Training Jan 5-6,

7 Sensitivity check and set up flow rate 13 Check Sensitivity - Use 4 ppm Cu, choose Cu lamp by click Lamp icon on Tool bar 14 AAS Training Jan 5-6,

8 - Click Set up botton of Cu element and wait to set finish, close window 15 - Click Method to choose Cu 16 AAS Training Jan 5-6,

9 - Scroll down to choose Cu method, click OK 17 - Adjust Burner position, in-out, left-right, check to middle point of burner 18 AAS Training Jan 5-6,

10 - Choose Wavelength scan in Tools menu 19 -Click Scan On/Off to scan the approximately wavelength (Scan every time before use lamp) 20 AAS Training Jan 5-6,

11 - Click Flame icon and ignite flame by click On Flame control page (Safety Interlocks show green check) - Click Adjust icon to check the ratio of Oxidant : Fuel (4 : 2) 21 - Choose Continuous graphics in Tool bar dip nebulizer tube in blank 22 AAS Training Jan 5-6,

12 Click Autozero before inject 4 ppm Cu and adjust to approximately flow rate by turn around Flow adjustment AAS Training Jan 5-6,

13 - click Analyses >> Characteristic cond. - Type concentration in gab of Sample concentration (mg/l) such as 4 - Type Abs in gab of Instrument Reading (A) such as Calculation result will show in Measures Characteristic Concentration such as Standard value will show in Comparison Characteristic Concentration such as Abs must near standard value in ±20% ±20% 25 Method set up 26 AAS Training Jan 5-6,

14 Method set up - Click Lamp icon again, choose lamp that will use and click Method to choose method file of used element 27 - Check Sensitivity of lamp before - Click MethodEd Tool bar 28 AAS Training Jan 5-6,

15 - [Inst.] type Read time in Timing (2-5), choose type of Signal and choose type of flame, click [Calib] 29 - [Calib] Choose Equation type, Max.Decimal places and Max.significant fig, Unit and Replicates, click [Standard Concs.] 30 AAS Training Jan 5-6,

16 - [Standard Concs.] type the concentrations of standard from first to last values and type middle concentration in Reslope 31 Standard curve plotting 32 AAS Training Jan 5-6,

17 - Click 4 Tool bars: Results, calib., Peaks and Manual 33 - Click Tile in Window bar to arrange 4 pages 34 AAS Training Jan 5-6,

18 - Analyze blank before 35 - Inject Blank solution before inject standard solution 36 AAS Training Jan 5-6,

19 - Insert standard and click Analyze Standard from first to last concentration respectively 37 - Analyze to complete 5 concentrations 38 AAS Training Jan 5-6,

20 - The Abs that out off range of standard curve, we can reject or accept by click Analyses >> Edit Calibration - Choices as Include, Ignore or Re-analyze 39 IDL determination 40 AAS Training Jan 5-6,

21 - Limits of Detection = Signal to noise ratio - Definition (IUPAC) = The concentration which will give an absorbance signal three the magnitude of the baseline noise - = 3 x standard deviation of blank (10 rep.) - IDL = Instrument Detection Limit 3 x SD SD X SD 41 - Change Replications in MethodEd from 3 to 10 Rep. and analyze blank by click Analyze sample and calculate IDL = SD x 3 42 AAS Training Jan 5-6,

22 43 Sample Analytical 44 AAS Training Jan 5-6,

23 - Dip Nebulizer tube in sample before click analyze Sample 45 Emission Analytical 46 AAS Training Jan 5-6,

24 - Change used Lamp Current to 0 (zero) 47 - Choose Method such as K 48 AAS Training Jan 5-6,

25 - Before plot standard curve, it will analyze highest standard before analyze blank and first standard next AAS Training Jan 5-6,

26 Turn off Flame-AAS 51 Turn off Flame-AAS - Turn off all of Window that finish used - Clean nebulizer and burner: 1. Aqueous solution flood by 1% Nitric acid 5 min - flood by DI water 5 min 2. Organic solvent flood step by step - flood dby organic icsolvent 5 min - flood by Acetone 5 min - flood by 1% Nitric acid 5 min 52 - flood by DI water 5 min AAS Training Jan 5-6,

27 - Shutdown Flame - Turn off gas valve 53 - Bleed the remain gas in system 54 AAS Training Jan 5-6,

28 - Shut down Software - Shut down computer - Turn off AAS - Turn off UPS 55 - Handle Waste in Drain - Turn off Hood - Turn off Air Compressor and release air out 56 AAS Training Jan 5-6,

29 - Turn off air condition - Switch off electric system - Record data in Logbook Happy Ending ^^ 57 Maintenance AAS 58 AAS Training Jan 5-6,

30 Gas supplies Check valves and connections to tightly and right The acetylene gas pressure must higher than 70 psi (6 bar, 600 kpa) because acetone will contaminate t to burn Handle waste in Drain when full 59 Light source Do not repair HCL by yourself If window lamp has dirty mark, should clean by soft and ddry cloth th(d (don t use water or reagent 60 AAS Training Jan 5-6,

31 Burner head Clean burner by soft brush with soft surfactant both inner and outer of burner Clean by DI water Dry by clean air pump 61 Burner chamber Clean burner by soft brush with soft surfactant both inner and outer of burner Clean by DI water Dry by clean air pump 62 AAS Training Jan 5-6,

32 Nebulizer After use, Flow by 1% HNO3 and DI water If it clog by particals, use stainless wire stab through from upper to last If it has some sticky matter in capillary tube, Flow by diluted surfactant such as 0.1% Triton X Thank for your attention. Reference: PerkinElmer. 1998Aanalyst 100/300 Atomic Absorption Spectrometer Hardware Guide. The Perkin-Elmer Corporation, USA. 64 AAS Training Jan 5-6,