Running ICAL - vivianlu9/EMAX_VOA_sandbox GitHub Wiki
For most ICALs, we spike standards into water at ten different concentrations (levels). The minimum amount of levels you need for an ICAL is five (six if you're using a quadratic curve), and you need at least one level before and after your midpoint. The level concentrations are the same for every instrument that runs the specific method. These concentrations are selected based on quarterly verification requirements as well as project-specific requirements at the time of running the calibration.
After we run the ICAL, we run an initial calibration verification (ICV) to confirm that the compound responses from the initial calibration are accurate. This is why it's important to test the standards before running the ICAL; this ensures that standards can be remade before calibration if needed.
If a compound fails the ICV, that compound is considered "not evaluated" and the ICAL cannot be used to report any samples that require that compound until the verification passes.
When you finish testing the tune and have all the settings saved, save the current method using the month/day you're running the ICAL.
Ex: Old method is
VO67G25and ICAL is being run on 09/15; new method would be saved asVO67I15.
Setting up APP IX is a bit different because APP IX is still analyzed under the current 8260 method, but it's processed using a different method.
In other words, when you run APP IX ICAL, you don't change the method name to the current month/day when you collect the data points, but you DO save the actual calibration method in Environmental Data Analysis using the conventional method.
Ex: You're running APP IX ICAL. The date is 10/12. Your 8260 ICAL was run under method
VO06J01. Your previous APP IX method was namedVO06H16. When setting up the ICAL sequence in MSTOP, the DataAcq method should be the same as your current 8260 ICAL (in this example it'sVO06J01). To set up the APP IX method in Data Analysis, load the previous APP IX method (VO06H16) and save THAT method as the current method (VO06J12).
Do NOT use
VO06J01to set up your APP IX method because that will copy the compound list from 8260, NOT APP IX.
[picture of correctly formatted APP IX ICAL sequence]
These methods are saved in the same way as normal methods, but there's one extra step. Because the SIM method is set to scan for very specific ions, using the regular SIM method would NOT visualize BFB because BFB is not the target ion being scanned for. You need to save a second method specifically set to Scan and use that only for evaluating BFB.
Ex: Your SIM method is saved as
VOF5J06. The Scan method you use to evaluate your tune check should be saved asVOF5J06A.
Note: Be careful when making changes to SIM ICALs. Normally, we save modifications to a method with A appended to the method name, but doing so for SIM would overwrite the Scan method for that ICAL. Never save SIM ICALs with an A at the end.
If we start ICAL early enough, sometimes it is possible to run multiple ICALs in one day. The naming convention for that depends on what you're running. Be careful not to overwrite the second ICAL if you need to save the first method under a new name.
We usually append an A to the method name if it's the second ICAL being run that day. This is especially common when running an APP IX ICAL in the same day as an 8260 ICAL. This applies for all methods that only require one method name.
Ex: The first ICAL is
VO01J25. If you run a second ICAL that day, the second method would be namedVO01J25A.
Since A is already being used by the Scan method for the SIM ICAL, we can't append an A at the end for the second ICAL. Instead, we use the next day's naming for the second ICAL.
Ex: First SIM ICAL is named
VOF5E23andVOF5E23Arespectively. The second ICAL would be namedVOF5E24(andVOF5E24Aif running SIM).
Generally, we'll grab the previous ICAL's run log and use that as a reference for the amount of standard to spike for each level. Be careful when referencing previous ICALs though, because:
a) the concentrations being used might differ, and
b) sometimes ICAL levels are spiked at different concentrations than expected.
The run log should have either one or two columns with numbers written down in each line. These numbers are the amount of standard spiked (in μL) for each level. A / B columns mean there were two different amounts spiked depending on the standard concentration. A / B should be defined somewhere on the run log.
*= midpoint level
For 8260 25mL:
Spike 1.0uL IS (250ppm) for all levels.
A (250ppm): GAS, CS2, 4-ADD (250/6250ppm), SS, FREON, FREON114, TAA-224 (250/1250ppm)
B: 8260 (50/1250ppm), KET-AA (250ppm)
| Level | 8260 (ppb) | KET-AA (ppb) | TBA/2-butanol (ppb) | A (uL) | B (uL) |
|---|---|---|---|---|---|
| 1 | 0.3 | 1.5 | 7.5 | 0.03 | 0.15 |
| 2 | 0.5 | 2.5 | 12.5 | 0.05 | 0.25 |
| 3 | 1.0 | 5.0 | 25 | 0.1 | 0.5 |
| 4 | 2.0 | 10 | 50 | 0.2 | 1.0 |
| 5 | 5.0 | 25 | 125 | 0.5 | 2.5 |
| 6* | 10 | 50 | 250 | 1.0 | 5.0 |
| 7 | 20 | 100 | 500 | 2.0 | 10 |
| 8 | 30 | 150 | 750 | 3.0 | 15 |
| 9 | 50 | 250 | 1250 | 5.0 | 25 |
| 10 | 100 | 500 | 2500 | 10 | 50 |
For APP IX 25mL:
Can spike 1.0uL IS (250ppm) or 5.0uL IS/SS (50ppm) for all levels.
Std: APP IX (250/2.5/5kppm), FREON (250ppm), 4-ADD (250/6250ppm)
| Level | APP IX/FREON (ppb) | 2-butanol (ppb) | Std (uL) |
|---|---|---|---|
| 1 | 0.5/5.0/10 | 12.5 | 0.05 |
| 2 | 1.0/10/20 | 25 | 0.1 |
| 3 | 2.0/20/40 | 50 | 0.2 |
| 4 | 4.0/40/80 | 100 | 0.4 |
| 5* | 10/100/200 | 250 | 1.0 |
| 6 | 30/300/600 | 750 | 3.0 |
| 7 | 50/500/1000 | 1250 | 5.0 |
| 8 | 100/1000/2000 | 2500 | 10 |
For 524.2:
Spike 1.0uL IS (524.2) (250ppm) for all levels.
A (250ppm): GAS, CS2, SS
B: 8260 (50/1250ppm), KET-AA (250ppm)
| Level | 524.2 (ppb) | KET (ppb) | TBA (ppb) | A (uL) | B (uL) |
|---|---|---|---|---|---|
| 1 | 0.3 | 1.5 | 7.5 | 0.03 | 0.15 |
| 2 | 0.5 | 2.5 | 12.5 | 0.05 | 0.25 |
| 3 | 1.0 | 5.0 | 25 | 0.1 | 0.5 |
| 4 | 2.0 | 10 | 50 | 0.2 | 1.0 |
| 5 | 5.0 | 25 | 125 | 0.5 | 2.5 |
| 6* | 10 | 50 | 250 | 1.0 | 5.0 |
| 7 | 20 | 100 | 500 | 2.0 | 10 |
| 8 | 30 | 150 | 750 | 3.0 | 15 |
| 9 | 50 | 250 | 1250 | 5.0 | 25 |
| 10 | 100 | 500 | 2500 | 10 | 50 |
For 8260 5.0g/5.0mL:
NaHSO4: Use preweighed 5.0g SoBi w/ stir bar for each level.
MeOH: Add additional methanol so that total amount of MeOH in each level = 100uL.
Spike 1.0uL IS (250ppm) for all levels.
A (250ppm): GAS, CS2, KET-4ADD (250/1250/2500ppm), SS, (FREON, FREON114)
B: 8260 (50/500ppm)
| Level | 8260 (ppb) | KET-AA (ppb) | TBA/2-butanol (ppb) | A (uL) | B (uL) | +MeOH (uL) |
|---|---|---|---|---|---|---|
| 1 | 1.0 | 5.0 | 10 | 0.02 | 0.10 | 100 |
| 2 | 2.0 | 10 | 20 | 0.04 | 0.20 | 100 |
| 3 | 5.0 | 25 | 50 | 0.1 | 0.5 | 100 |
| 4 | 10 | 50 | 100 | 0.2 | 1.0 | 100 |
| 5 | 20 | 100 | 200 | 0.4 | 2.0 | 100 |
| 6* | 50 | 250 | 500 | 1.0 | 5.0 | 100 |
| 7 | 100 | 500 | 1000 | 2.0 | 10 | 80 |
| 8 | 200 | 1000 | 2000 | 4.0 | 20 | 60 |
| 9 | 300 | 1500 | 3000 | 6.0 | 30 | 40 |
| 10 | 500 | 2500 | 5000 | 10 | 50 | 0 |
We usually prepare KET-AA & 4-ADD as a single mix when running soil ICAL because the concentrated mix allows for better recoveries for the 8260 compounds. TL;DR analyzing more than ~120uL of MeOH in a sample will cause compounds to saturate, especially the ones that elute later in the run.
For 624/624.1:
Spike 1.0uL 624 IS (150ppm) for all levels.
- A: GAS (250ppm)
- B: KET-AA (250ppm)
- C: 624 (50ppm)
- D: SS (150ppm)
| Level | 624 (ppb) | AA (ppb) | A (uL) | B (uL) | C (uL) | D (uL) |
|---|---|---|---|---|---|---|
| 1 | 1.0 | 2.0 | 0.02 | 0.04 | 0.1 | 0.05 |
| 2 | 2.0 | 4.0 | 0.04 | 0.08 | 0.2 | 0.1 |
| 3 | 5.0 | 10 | 0.1 | 0.2 | 0.5 | 0.25 |
| 4 | 10 | 20 | 0.2 | 0.4 | 1.0 | 0.5 |
| 5* | 20 | 40 | 0.4 | 0.8 | 2.0 | 1.0 |
| 6 | 50 | 100 | 1.0 | 2.0 | 5.0 | 2.5 |
| 7 | 100 | 200 | 2.0 | 4.0 | 10 | 5.0 |
| 8 | 200 | 400 | 4.0 | 8.0 | 20 | 10 |
For 8260SIM (25mL):
Spike 2.5uL SIM IS (5.0ppm) for all levels.
Std (5.0ppm): SIM, SS
| Level | Conc (ppt) | Std (uL) |
|---|---|---|
| 1 | 20 | 0.1 |
| 2 | 50 | 0.25 |
| 3 | 100 | 0.5 |
| 4 | 200 | 1.0 |
| 5* | 500 | 2.5 |
| 6 | 1000 | 5.0 |
| 7 | 2000 | 10 |
| 8 | 5000 | 25 |
For 8260SIM (5.0g):
Spike 1.0uL SIM IS (5.0ppm) for all levels.
Std (5.0ppm): SIM, SS
| Level | Conc (ppt) | Std (uL) |
|---|---|---|
| 1 | 50 | 0.05 |
| 2 | 100 | 0.1 |
| 3 | 200 | 0.2 |
| 4 | 500 | 0.5 |
| 5* | 1000 | 1.0 |
| 6 | 2000 | 2.0 |
| 7 | 5000 | 5.0 |
| 8 | 10000 | 10 |
For 1,4-dioxaneSIM (25mL):
Spike 5.0uL 1,4-DIOX IS (250ppm) for all levels.
Std: 1,4-DIOX (250ppm), SS (25ppm)
| Level | 1,4-diox (ppb) | SS (ppb) | Std (uL) |
|---|---|---|---|
| 1 | 1.0 | 0.1 | 0.1 |
| 2 | 2.0 | 0.2 | 0.2 |
| 3 | 5.0 | 0.5 | 0.5 |
| 4 | 20 | 2.0 | 2.0 |
| 5* | 50 | 5.0 | 5.0 |
| 6 | 100 | 10 | 10 |
| 7 | 500 | 50 | 50 |
For 1,4-dioxaneSIM (5.0g):
Spike 4.0uL 1,4-DIOX IS (250ppm) for all levels.
Use preweighed 5.0g SoBi w/ stir bar for each level.
Std: 1,4-DIOX (250ppm), SS (25ppm)
| Level | 1,4-diox (ppb) | SS (ppb) | Std (uL) |
|---|---|---|---|
| 1 | 5.0 | 0.5 | 0.1 |
| 2 | 10 | 1.0 | 0.2 |
| 3 | 50 | 5.0 | 1.0 |
| 4 | 100 | 10 | 2.0 |
| 5* | 200 | 20 | 4.0 |
| 6 | 500 | 50 | 10 |
| 7 | 1000 | 100 | 20 |
For TCPSIM (25mL):
Spike 1.0uL TCPSIM IS (2.5ppm) for all levels.
Std (2.5ppm): TCPSIM, SS
| Level | Conc (ppt) | Std (uL) |
|---|---|---|
| 1 | 5.0 | 0.05 |
| 2 | 10 | 0.1 |
| 3 | 20 | 0.2 |
| 4 | 50 | 0.5 |
| 5* | 100 | 1.0 |
| 6 | 500 | 5.0 |
| 7 | 2000 | 20 |
| 8 | 5000 | 50 |
For TCPSIM (5.0g):
Spike 1.0uL TCPSIM IS (2.5ppm) for all levels.
Std (2.5ppm): TCPSIM, SS
| Level | Conc (ppt) | Std (uL) |
|---|---|---|
| 1 | 50 | 0.1 |
| 2 | 100 | 0.2 |
| 3 | 200 | 0.4 |
| 4 | 500 | 1.0 |
| 5* | 1000 | 2.0 |
| 6 | 2000 | 4.0 |
| 7 | 5000 | 10 |
I usually prepare levels in sets of two. For example, I prepare levels 3 and 4 when the second level is purging. You can also do it one at a time, but I prefer doing them in sets to minimize the amount of times I need to get up. Don't prepare all of the levels at once unless you're running the ICAL overnight because some compounds (vinyl acetate, 2,2-dichloropropane) degrade over time.
For some methods (524.2, APP IX, and 8260 sodium bisulfate) however, this is not possible because certain compounds (styrene, methyl/vinyl acetate, pentachloroethane) will degrade if prepared too early. For those methods, it's better to prepare each level as late as possible so it can be purged and analyzed immediately after preparation.