Method Submissions-5th Set of Nutrients_6-30-14 - page 168

DeterminationofNa,Mg, P, K, Ca, Cr,Mn, Fe, Cu, Zn, Se, andMoby ICP-MS
3.
Nitric acidmaintenance solution for rinsevial (approximately10%):
Mix100mLof concentratednitricacid
(C.3.g)with laboratorywater topreparea total volumeof 1000mL.Useperiod: Changequarterly (provide
actual dateon label indicatingwhen to change solution).
4.
P/A factor tune solution solution:
DiluteeachP/A factor stock tune solution100x (C.3.d)with laboratorywater,
thenmix the twodiluted solutions1:1 for useat the instrument. Expiration: 6months.
5.
1µg/LCe, Co, Li,Mg, Tl, andY tuning solution:
Pipet (digital) 1mLofHighPurityStandardmultielement
solution (C.3.c) and20mLnitric acid (C.3.f) intoa1000mL volumetric flask. Dilute to volumewith laboratory
water. Expiration: 6months.
6.
CalibrationBlank Solution:
Dispense (bottledispenser orpipet) 5mL of nitric acid (C.3.f) intoa50mL
volumetric flask. Pipet (digital) 0.5mLof the5mg/LNi/Ge/Temultielement internal standardand0.5mLof
methanol.Dilute tovolumewith laboratorywater. This solution is the calibrationblank (CalBlk) andpreparation
blank (PB). Use same lotsof reagent for samples. Expiration: 2days.
7.
Multielement standard solution set:
Prepare calibrationblank, calibrationStd1, calibrationStd2, calibration
Std3, and calibrationStd4 standard solutionsbypipetting (ClassA) 0, 1.00, 5.00, 20.00, and40.00mL
respectively, of the stockmultielement standard solution (C.3.a) into separate50mL volumetric flasksor sample
tubes. Add0.5mLof the5mg/LNi/Ge/Temultielement internal standard solution (ClassApipet or digital
pipet), 5mL (repipetteror Teflonbottledispenser) of J.T. BakerUltrex II ultrapure reagent nitricacid (C.3f), and
0.5mLof concentratedmethanol (99.99%, analytical reagent grade) toeach flask. Fill the flasks tovolumewith
laboratorywater. Expiration2days. Theanalyte concentrations in the calibration standard solutions and
internal standards (ISTD) areas follows:
Na
Mg
P
K
Ca
Cr
Mn
Fe
Cu
Zn
Se
Mo
mg/L
mg/L
mg/L
mg/L
mg/L
µg/L
mg/L
mg/L
mg/L
mg/L
µg/L
µg/L
Cal Blank
0
0
0
0
0
0
0
0
0
0
0
0
Cal Std1
0.5
0.2
0.5
1
1
0.8
0.005
0.05
0.005
0.02
0.4
0.8
Cal Std2
2.5
1.0
2.5
5
5
4
0.025
0.25
0.025
0.1
2
4
Cal Std3
10
4
10
20
20
16
0.1
1
0.1
0.4
8
16
Cal Std4
20
8
20
40
40
32
0.2
2
0.2
0.8
16
32
ISTD (50µg/L)
Ge
Ge
Ge
Ge
Ge
Ge
Ge
Ge
Ge
Ge
Te
Ge
MTE-02
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