Method Submissions-5th Set of Nutrients_6-30-14 - page 172

DeterminationofNa,Mg, P, K, Ca, Cr,Mn, Fe, Cu, Zn, Se, andMoby ICP-MS
h)
Generatea tune report (Go to fileand thenprint).
i)
Leaveprobe in tune solutionand selectHegasmodeandadjust parameters toobtain response shownD.2.b
j)
Generatea tune report (Go to fileand thenprint).
k)
Repeat steps (i) and (j)withH
2
gas. Typical responses in theH
2
gasmodeare shown inD.2.c
l)
In the tuning sensitivitywindow clickon
ALS
(automatic liquid sampler) and select
rinse
tomove the sampler
probe to theautosampler rinseport containing2%nitric acid for approximatelyoneminute. The
autosamper rinse solution shouldbe the solutionprepared inSectionE.1.
m)
Clickon
ALS>>GoTo>>position1
tomove theprobe intoa10%nitric acidcontainer previouslyplaced in
position1of autosampler.
n)
Toquantitate relativelyhigh concentrations greater than100ppb (analogmode) load thePA factor tuning
methodP_A.m. Pulsemode isused for concentrations less than100ppbanddoes not requirePA factor
tuning.
o)
Open the tunewindow
p)
Open thenogasmode tuning file, nogas.u
q)
Select
P/A Factor
from the
Tune
menu toopen theP/AFactor Tuningdialogbox
r)
Input themasses for theelements (seeelements inpulseanalog tune report -D.2.d) tobeused forP/A
coefficient adjustment.
s)
Set theP/A factor tune solutionon theautosampler.
t)
Move theautosamplerprobe to introduce the solution.
u)
Once the solution is introduced into the system, set theautosampler tuning solutionvial to0 (this causes
theautosampler to take the sample from the current vial position set previously).
v)
Click theRunbutton to initiate the tuningprocedure. When complete, P/A factor report isdisplayed.
w)
Close theP/A factor report. Elementsnot present orbelow100ppb in the tune solutionwill be indicatedby
a low sensitivitymessage.
x)
Click yes touseanewP/A factor.
y)
Lower the carrier gas flow rate if high sensitivity is reportedand repeat last three steps (v,w,x) andmerge
previous results.
z)
Place theprobe in theautosampler rinseport for 1minuteand then to the rinse solution inposition1 for at
least 15minutes.
aa)
Exit theTuning-Sensitivitywindow.
bb)
Load themethod.
cc)
Load the sequence. A typical sequence is shownbelow. Under the columnheaded “Type”:
CalBlk, is the calibrationblank (CB), seeE6.
CalStd, is the calibration standards, seeE7.
Blank, is theCBor undigestedpreparedblank (PB) prepared inE6. As aPB it isused to check carryover
problems. It isaQC item.
MTE-02
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