ÐÏà¡±á>þÿ :<þÿÿÿ9ÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿÿì¥Á%` ð¿×bjbj"x"x 8$@@×ÿÿÿÿÿÿ¤R R R R R R R f ****>f «¼^^^^^^^^*,,,,,,$ghÏ®PR ^^^^^PR R ^^e¾¾¾^¦R ^R ^*¾^*¾¾R R ¾^R ç“ýy;É*L¾*{0«¾}Pd}¾}R ¾l^^¾^^^^^PP´ ^^^«^^^^f f f Ä*f f f *f f f R R R R R R ÿÿÿÿICP Tutorial Notes (7/22/2008; amended 10/24) Phone numbers: Deb 4844 (MT) Marlene 6869 (ThF) (they alternate Wednesdays); ICP 6889 ICP ionizes the samples, breaking all bonds, therefore can only look at elemental concentrations. Starting up—unless you are an experienced user, Deb or Marlene will do this portion for you. Pump hoses are taken off tension when in not in use; need to set back with black on top and red beneath. WINLAB 32—select Manual Analysis Plasma: turn on. Spectra: Radial and Axial views. Calibrate plasma at the beginning of each day. Axial view is far more sensitive. Ruth’s samples generally have a lot of salt, so this view can get saturated, so choose Radial. Also, K and Na are easily ionized so always done radially. Analyze Blank: Probe is in H2O. Run 1M NH3Cl, then Std1, Std2, QC to calibrate. Wipe with fresh kimwipe between. Do not leave tube in the standards after sampled because it continues to draw from a limited supply. Normally put in H2O between; If K is problematic, may need to keep in blank between instead. Note: NH3Cl has other stuff in the background, Al, Ca, Na, Mg, a lot of K, which can make calibration difficult, but the presence of these in expected concentrations is useful for looking at these elements. Mg/L=ppm Calibration equation: want “triple 9s” Want RSDs below 2, need to rerun if >10. If mean corrected intensity <1000, then can have great variability in RSD. Read delay: time to allow sample to flush out of tube before analyzing new. **If you don’t tell system to save output, it won’t** **If fluid is not moving through the waste tube, STOP. It is backing up somewhere. It can move slowly, but must move*** Manual Analysis Control—this is where we pick up! Run only 10 samples, repeat QC, continue. To follow EPA protocols, should run blanks with each QC. Blank should come back 0. This is more important if study is for regulatory work. -If QC fails, pull the last run samples out, recalibrate (blank standard, then QC), and redo them. -Can use up/down arrows to find number that needs to be repeated. If >10, results won’t be reportable because variability in the background will mask. QC-want reported % to be within 10% of ppm on label. I.e., Al 50 ppm can be 45-55. Analyze Samples Each sample machine looks at wavelengths outlined in a protocol. Ruth always does the same, so they have a protocol saved. “Yanairesearch” looks at AL, Ca, K, Mg and Na. RSD-SD/mean*100 Continually check RSDs and intensity for reasonableness. Also look for agreement between elements at the two wavelengths (for the elements with more than one). Na 330-237 wavelength is “weak line” to begin with. Also if all numbers run very low, may be a clog. Call for Help! --if samples have visible particulate matter, do not stir. Best to refilter, but if can’t, allow to settle, then hold probe above sediment or it will suck up muck and get clogged. Each time you run a QC, enter ID as QC—it will not balk because there are other samples of the same name, nor will it overwrite the previous ones. If using the “autoanalyzer” you can set up to do this automatically, as well as rinse between samples. EPA detection limit test: What is and isn’t reportable based on 7 aliquots, SDx3. It one element is continually low, you may need to re-run separately, or look at the element axially while keeping the others radial. It will taker longer for each, but can do it all in one fell swoop. (This is not in Ruth’s standard protocol). (If all elements are low, think clog.) Shutting down Standards, QC stored in fridge when done. Our standards are “dirty” (high solids, high salts) so clean up includes a nitric acid rinse—do it while you export data (defaulty is *.csv) Plasma control: turn off Close software to ensure gas jets are off. Release tension on pump. Open standard compartment to look for leaks (leave open). Our questions Where should we keep extracts? Fridge. She’s concerned that freezing alters solubility, as well as losing spontaneity in processing (wouldn’t this require free access to the machine?) What kinds of things can go wrong? 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