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J
ournal of
AOAC I
nternational
V
ol.
98, N
o.
6, 2015
acid (ultrapure reagent grade) with 20 mL Tergitol solution (
a
)
and laboratory water to prepare a total volume of 1000 mL.
Expiration: 3 months; store at room temperature.
(c)
P/A factor tuning working solution.—
Dilute and/or
combine P/A factor tuning stock solutions (or equivalent) to
manufacturer’s recommended dilution level with laboratory
water for use with the instrument. Expiration: 6 months; store
at room temperature.
(d)
Calibration blank (Cal Blk) and preparation blank (PB)
solution.—
Add approximately 15 mL laboratory water to a
50 mL volumetric flask. Dispense (using bottle dispenser or
pipet) 5 mL nitric acid (ultrapure reagent grade) into the same
volumetric flask. Pipette (using digital pipet) 0.500 mL ISTD
stock and 0.500 mL methanol into the flask. Dilute to volume
with laboratory water. This solution serves as both the Cal Blk
and PB. The Cal Blk is used as the initial calibration point, while
the PB is used as a QCS (
see
below). Use the same lots of reagent
for samples. Expiration: 2 days; store at room temperature.
(e)
Calibration standard solution set.—
Prepare Cal Blk, Cal
Std 1, Cal Std 2, Cal Std 3, and Cal Std 4 standard solutions
by pipetting (with Class A glass pipet) 0.00, 1.00, 5.00, 20.00,
and 40.00 mL, respectively, of the multielement standard stock
solution into separate 50 mL volumetric flasks or sample tubes.
Add 0.500 mL ISTD stock (using Class A pipet or digital pipet),
5 mL (using repipetter or Teflon bottle dispenser) nitric acid
(ultrapure reagent grade), and 0.500 mL methanol to each flask.
Fill the flasks to volume with laboratory water. Expiration:
2 days; store at room temperature. The analyte and ISTD
concentrations in the calibration standard solutions are shown
in Table
2015.06A
.
E. Sample Preparation
(a)
Prepare samples in duplicate. In sample vessels, weigh
test portions to the nearest 0.0001 g. For liquid products, the test
portion size is 1.0 g. For powdered products, the test portion size
is net 0.20 g of a powder sample, which should be taken from
a 10% (w/w) reconstitution in warm (60°C) water (i.e., 2.0 g
of the 10% reconstitution). Add 0.500 mL ISTD stock using
a calibrated digital pipet, 5 mL nitric acid (ultrapure reagent
grade), and 2 mL 10% hydrogen peroxide. (
Note
: the PB/Cal Blk
solution prepared with the standards is the correct sample blank
for this method. Specifically, do not microwave digest the sample
blank, which can subject the blank to contamination. Also note
that the digital pipet used for the addition of ISTD solution must
be calibrated at point of use to ensure that it delivers a nominal
volume of 0.500 mL within a tolerance of ±0.8% and precision
better than 0.2% RSD).
(b)
Seal the vessels, and place into microwave oven. Execute
a heating program equivalent to that shown in Table
2015.06B
,
suitable for total digestion of the sample.
(c)
After digestion, place vessels in a fume hood. Unscrew
the cap/venting nut slowly to gradually release the pressure.
Then, completely remove the cap.
(d)
Add approximately 20 mL laboratory water to the
contents of the vessel, swirl to mix, and transfer contents to a
50 mL sample vial. Add 0.5 mL methanol to the sample vial
and dilute to approximately 50 mL with laboratory water.
Shake briefly. The transfer or the final volume does not need to
be quantitative because ISTDs were added prior to digestion;
therefore, the analyte/ISTD ratios will be constant.
F. Determination
(a)
Using the appropriate tuning solutions, tune the
instrument for optimal sensitivity in the KED mode and/or
reaction mode according to the instrument design. Also, tune
the instrument to find the P/Acalibration factors that are needed
for those calibration curves that will extend above roughly
100 µg/L (depends on instrument type). Table
2015.06C
summarizes typical instrument parameters for analysis.
(b)
Analyze test solutions using an ICP/MS instrument
standardized with the indicated standard solutions
(Table
2015.06A
). Ge is used as the ISTD for the 11 elements
not including Se. Those 11 elements are determined in the He
collision mode, using KED. Te must be used as the ISTD for
Se determinations, and we recommend that Se be determined
in H
2
mode, i.e., reaction mode. Analyze Cal Std 3, or other
suitable QC solution, every 10 test portions to monitor for
instrument drift and linearity (result must be within 4% of
Table 2015.06B. Microwave operating parameters:
Stages 1 and 2 are operated sequentially, without removing
vessels from the oven
Stage 1 sample digestion
1
Power
100% (1600 W)
2
Ramp to temp., min
20
3
Hold time
20
4
Temp., °C
180
5
Cool down, min
20
Stage 2 sample digestion
1
Power
100% (1600 W)
2
Ramp to temp., min
20
3
Hold time, min
20
4
Temp., °C
200
5
Cool down, min
20
Total, h
2
Table 2015.06C. Typical ICP/MS parameters for Agilent
7700x
RF power, W
a
1600
RF matching, V
1.8
Sampling depth, mm
9
Extract 1 lens, V
0
Carrier gas, L/min
0.9
Make-up gas, L/min
0.2
Nebulizer (glass concentric)
MicroMist
Spray chamber temp., °C
2
Interface cones
Ni
He cell gas flow rate, mL/min
4.5
H
2
cell gas flow rate, mL/min
4.2
Nebulizer pump rate, rps
0.1 (0.5 mL/min)
Peristaltic pump tubing
White/white, 1.02 mm id
Drain tubing
Blue/yellow, 1.52 mm id
a
RF = Radio frequency.
Candidates for 2016 Method of the Year
78