Procedure for ICP analysis
University of Vermont
The new Perkin Elmer Dual view ICP at the UVM Plant and Soil Science Department,
P. Bierman and Erik Clapp
29 September, 1997
Call Jennifer Larsen for appointment (656-0489 ), Plant and Soil Science room 224 is in the Hills Building
Keys to ICP room and Hills Building are hanging by door in cosmo lab
Machine is usually accessible after 4 p.m.; after training machine is available on weekends
A run of one batch (in duplicate) will take about 3 to 3.5 hours including 30 minutes to check standards before running so bring lots to read!
Standard values (micrograms solute/gram solution)
# Be Al
S-1 0.999 3.002
S-2 2.003 59.172
S-3 0.438 1.405
S-4 0.900 30.001
BACK AT THE RANCH
1. Get rack of samples to analyze and get standard rack. Refill all four standard tubes. Empty and refill blank tube with 40 ml of 1.2 N HCl. Fill other standard tubes to 40 ml level with new standard solution. Check bottle ID carefully.
2. Print ICP LOAD ORDER. It is one subpage of the batch sheet for the batch you are running; bring box of gloves. Put all of this in the large plastic box to carry over to Hills.
3. TAKE A DOS DISK AND GOGGLES as well as paper clips or a stapler. All of this should be kept in the white box.
AT PLANT AND SOIL
3. Sit before machine. Call up "btemplat" sample information file. The sample info file tells the machine where the samples are located in the autosampler and in which order the samples need to be run. Under "FILE" hit open and sample info file. Curse down until you find btemplat. Click to open. Immediately resave (USE THE SAVE AS COMMAND) this file as B## (where ## is the batch number). DO NOT OVERWRITE THE TEMPLATE FILE. Change batch ID to the appropriate number in the parameters box and change batch number in file description box.
Type, in the open spaces, your sample names in direct order from the ICP LOAD SHEET. This of course will be the same order in which you load the samples on the autosampler. MAKE SURE that high level samples have an H before them and that low level samples have a L before them. DO NOT TYPE OVER BLANK AND STANDARD DESIGNATIONS as these are critical to data reduction and samples and standards must be run in an exact order. If L and H are forgotten, bad things will happen to your data as the machine will overwrite samples of the same name. Print the sample info file.
Use the ICP LOADSHEET to fill in the blanks consecutively in btemplat. Make sure to enter L and H where indicated. SAVE THE FILE as a sample info file. WRITE THE NAME OF THE FILE DOWN on the ICP LOAD SHEET.
Use the sample info file and the ICP load sheet to load blank and standards in autosampler, keeping caps in order. Place the samples in batch order starting at autosampler hole number 9. Place the caps on the top of the machine in order so that you can recap samples. Place the high level (5 ml) samples in the first 8 spots (first row of small tube spaces). Place the low level samples in the next 8 spots (the second row of small tube spaces).
Blank position 1
S-1 position 2
S-2 position 3
S-3 position 4
S-4 position 5
position 9 to 16 are 5 ml dilutions in batch order
positions 17 to 24 are 2.5 ml dilutions in batch
5. Check to make sure machine is in axial mode. To do this click under system and make sure last line says, "change to radial viewing." If the machine asks...do not save torch type in hardware init file...
6. Load method, "bman Be Al axial". Goto FILE...OPEN...METHOD...scroll down and click
7. Go to 'auto" screen and get into set up. Check for proper method and that method selected matches that in upper right corner of main screen. Check that correct sample information file is referenced. Check that data are saved to file entitled B##RESA. RES is for results, A is for the first replicate.
8. Go to Analyze screen. CHECK THAT THE PROPER METHOD IS DISPLAYED. Hit analyze all. The machine will click and whir. First it will gather intensities for the blank and all four standards. This will take 15 minutes.
After calibration you will get a printout with linearity and intensity information. BRING THE PRINTOUT BACK AND FILE WITH THE BATCH. The machine will run the blank and the four standards. Check that the blank for the 300 nm lines is < 0.1; the 200 nm lines may be higher. Check that the standards are within 4% of nominal values and that neither 300 nm line is way out, more than 4% different from its stated value. If the standards run successfully allow the run to continue.
Find a good book, space out, get a drink but keep an eye on the standards that are interspersed with the unknowns as these are your only assurance of ongoing quality. Check also that the blank is within 0.1 of zero. Check that standards are within 4 to 5% of reality. Check to make sure that all three spectral lines for each element are in general agreement (a couple percent difference is not unexpected particularly for the 200 nm lines). Only if things get really wacky should you stop the analysis. If one of the three lines is way out, note this on the batch sheet for later reprocessing.
13. To download the data to disk do the following.
Go to reformat under UTILITIES in the FILE menu.
Under results data set enter the filename containing the data you just collected or use browse to find the file.
Under reformatted file, click the button next to the empty space. type your file name followed by a T for transfer file. Change the extension to txt. Set the directory
Check to see that the file is delimited by commas
Click on sample, and check the box for sequence number
Click on mean, and check the box for concentration in calibration units
Go to top and hit Save results. Data will fly across screen if all is well
These commands have exported the raw ICP data to a file that excel can read although in a funky order.
Close reformat widow. Hit OK twice.
Hit the start button on lower left. Go to programs. Start excel.
Now...open Excel. Go to FILE and OPEN your data file from the ICP. It is hiding in the directory C:\vers12\icpusers\user1\report\.
Make sure that the "files of type" is set to text files
To parse the file pick "delimited", then hit next
pick comma, then hit next
then finish.
Once you have an excel file, click on DATA and then on Pivot Table Report
hit next twice.
drag run seq to row
drag analyte to column
drag mean-st to data
hit finish
Save the file to your floppy AS a file type MICROSOFT EXCEL 5.0/95 WORKBOOK (*.xls) and bring the file home. WRITE THE FILE NAME ON THE ICP LOAD SHEET.
Now that the first run is finished, leave the samples in place and make a duplicate run. Do this by clicking on AUTO and SET UP.
IMPORTANT CHANGE THE FILE name to which data are saved, the results file, by changing the suffix A to a suffix B....This is of critical importance. If the suffix doesn't change all will be for naught as the original file will be overwritten. GO TO ANALYZE and hit analyze all. The machine will do its thing. Down load the data in a similar fashion to the first run. WRITE ALL FILE NAMES ON THE ICP LOAD SHEET.
14. Follow shut down instructions on wall. MAKE SURE TO LOCK UP!
BRING HOME.....
1. Your samples in their rack.
2. The 50 ml tubes with blank and standard and their rack.
3. A printout of the sample info file
4. A print out of the run results for both replicates
5. A disk with the excel file for the run
WHEN YOU GET BACK TO THE LAB
1. Write down the date and number of hours you actually ran samples on the clip board in the lab
2. Put the print outs in the batch notebook under the right batch
3. Return the plastic box to the lab store room
4. Put your samples back under the hood
Only when data have been checked should your samples be drained to acid waste and the tubes discarded as Be waste.