Fluoride And Amine Ion Chromatography

Question 1

Chromeleon

Answer 1

• click control panels and double click ICS-1000
• click startup and let IC warm up for 20-25 minutes
• in titration and water lab, check eluent level before beginning; different for separate towers
• click relay 1 Open button to ensure sample
• eluent is same in titration and water lab; prepared by 10mLs of AS 22 concentrate to 1990 mLs of DI water in 2000mL volumetric flask (run time is 35 minutes
• after refilling eluent, change level indicator to reflect current level of eluent
• DONT EVER REFILL ELUENT DURING RUN
• water lab ic: click ICS-2000, double click panels, click startup

Question 2

Creating a sample sequence (Titration Lab IC)

Answer 2

• Press Ctrl, Tab to get to file sequence. From main menu, choose instrument 2 and under sequences lick current month and year and “Water Lab Anion” and double click it
• Verify fluoride standards are there
• click on lowest sample in list and click down arrow, this creates a new sample
• a 1.5 ppm fluoride std must be run w each weekend sample sequence in titration lab. It is analyzed once a week in Water Lab. It should run within 10% of the ARV (1.35-1.65)
• all other WWTP samples are diluted 1:1. This dilution gives factor of 2.0000, but 10mL of sample to 90 mL DI water would give 10.0000 dilution factor.
• BEST ORDER FOR WWTP SAMPLES IS: Final Clarifier(action level >1.4ppm) > 63 tank (same as clarifier) > 125 tank (same as 63) > Desalter
• always run DI water after dirty samples (I.e. 811 tank and 64 stripped sour water for amine)
• click save

Question 3

Prepare Fluoride sample

Answer 3

• 1.5 ppm std run straight

* dilute most samples 1:1, using 2.8mLs of sample to 2.8mLs of DI.

Question 4

Fluoride/Amine Sample Analysis

Answer 4

• DO NOT DUPLICATE VIAL POSITIONS IN SEQUENCE
• Verify plunger is jo and carousel spins freely, if not press carousel release. If you push this, you must refill DI water vials.
• DI water should be in vials 45-50 for rinsing

Question 5

Interpretation of Results

Answer 5

• All graphs should be examined for peaks integrating correctly
• a run can be watched in real time by going to control panel screen
• time counter to see how much time is left before run complete
• to enlarge peak, hold down on left mouse button and drag mouse as much as you want it expanded. You can right click to auto scale the peaks to the range you have zoomed in on. If large peak in area zoomed in on, autoscale will not help, because the largest peak will skew the scaling.
• to return to full size, right click and select full size
• the arrow is the peak tool used to integrate peaks, the delimiter tool may be used to move the end of a peak left or right.
• best way to integrate peaks is to right clean over peak and click delete lean. Determine correct baseline and hold down left button and drag to integrate entire series of peaks, going past acetate. Be sure ends of peak are where the baseline is flat. Next be sure the peak tool is positioned where you want the split to occur and right click and “split peak”
• if you double click a peak, a box will come up which allows you to name peak in case
• if no peak and you diluted sample, run non diluted sample
• nitrates come off in middle of the fluoride run so it is not necessary to analyze another sample of the units want nitrate analysis.
• when diluting samples, check to be sure number under amount column makes sense for sample. IC does not account for dilutions when calculating area
• to confirm sample fits within calibration range of parameter, given area can be compared to calibration standards, it must fit between highest and lowest standard areas, without dilution factor.
• never report area smaller or larger than smallest or largest area of calibration. Run weaker or stronger dilution of this happens. Report value as

Question 6

Amines

Answer 6

• only analyzed on water lab IC.
• set up the same except you use amine sequence instead of anion sequence
• most samples run straight, not diluted.
• WWTP samples should not need dilution unless dirty or excessive particulates
• if excessive area between peak and baseline may need to split peak

Question 7

Purpose

Answer 7

EPA limits have been lowered for fluoride in water and amines have been known to cause problems in WWTP plant. Can be toxic to the intriguer bugs in system. Necessary to identify compounds in WWTP streams and Refinery Sour Water streams