Laboratory Procedure Manual: Urine Multi-Elements in Urine by ICP-UCT-MS 3018.7

Laboratory Procedure Manual
Analytes: Antimony, Barium, Beryllium, Cadmium,

Cesium, Cobalt, Lead, Manganese,
Molybdenum, Platinum, Strontium,
Thallium, Tin, Tungsten, and Uranium
Matrix: Urine
Method: Multi-elements in urine by ICP-UCT-MS
Method No: 3018.7

Revised: May 7, 2019
As performed by: Inorganic and Radiation Analytical Toxicology

Division of Laboratory Sciences
National Center for Environmental Health
Contact: Mr. Jeffery M. Jarrett

Phone: 770-488-7906
Fax: 770-488-4097
Email: [email protected]
James L. Pirkle, M.D., Ph.D.

Director, Division of Laboratory Sciences
Important Information for Users

The Centers for Disease Control and Prevention (CDC) periodically refines these laboratory
methods. It is the responsibility of the user to contact the person listed on the title page of each
write-up before using the analytical method to find out whether any changes have been made
and what revisions, if any, have been incorporated.
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Public Release Data Set Information
This document details the Lab Protocol for testing the items listed in the following table:
This method file describes measurements of UM_K.
Variable
File Name SAS Label
Name
URXUBA Barium, urine (μg/L)
URXUCD Cadmium, urine (μg/L)
URXUCO Cobalt, urine (μg/L)
URXUCS Cesium, urine (μg/L)
URXUMN Manganese, urine (μg/L)
URXUMO Molybdenum, urine (μg/L)
UM_K URXUPB Lead, urine (μg/L)
URXUSN Tin, urine (μg/L)
URXUSR Strontium, urine (μg/L)
URXUSB Antimony, urine (μg/L)
URXUTL Thallium, urine (μg/L)
URXUTU Tungsten, urine (μg/L)
URXUUR Uranium, urine (μg/L)
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1. Summary of test principle and clinical relevance

A. Clinical relevance:
These methods are used to achieve rapid and accurate quantification of elements of
toxicological and nutritional interest including antimony (Sb), barium (Ba), beryllium (Be),
cadmium (Cd), cesium (Cs), cobalt (Co), lead (Pb), manganese (Mn), molybdenum (Mo),
platinum (Pt), strontium (Sr), thallium (TI), tin (Sn), tungsten (W), and uranium (U). Use
these methods to screen urine when people are suspected to be acutely exposed to these
elements or to evaluate chronic environmental or other non-occupational exposure. [1-4].
B. Test principle:
Inductively coupled plasma mass spectrometry (ICP-MS) is a multi-element analytical
technique capable of trace level elemental analysis [1-4]. This method is used to measure
the 15 elements described here (antimony, barium, beryllium, cadmium, cesium, cobalt,
lead, manganese, molybdenum, platinum, strontium, thallium, tin, tungsten, and
uranium) or any subgroup of these.
Urine samples are diluted 1+9 with 2% (v/v) concentrated nitric acid. Nitric acid is used in
the diluent to solubilize and stabilize metals in solution. The diluent for the 15 element
panel contains iridium (Ir) and rhodium (Rh) for multi-internal standardization. Internal
standards are a constant concentration in all blanks, calibrators and samples. Monitoring
the instrument signal ratio of a metal to its internal standard allows correction for the
sample-to-sample matrix differences, instrument noise, and signal drift.
Liquid samples are introduced into the mass spectrometer through the inductively
coupled plasma ionization source. Using argon gas, the liquid sample is forced through a
nebulizer, aerosolizing the sample into small droplets, and then carried through the spray
chamber into the ICP. A plasma is created by coupling radio-frequency (RF) power with a
flowing argon stream. The plasma is characterized by a temperature of 4500-6500 K and
predominant species of positive argon ions and electrons. The aerosolized sample
droplets pass through a region of the plasma where the thermal energy vaporizes the
liquid droplets; atomizes the molecules of sample; and then ionizes the atoms. The ions,
along with the argon, enter the mass spectrometer through an interface that separates
the ICP (at atmospheric pressure, ~760 torr) from the mass spectrometer (operating at a
pressure of 10-5 torr). The ions pass through a focusing region, the collision/reaction cell
(Universal Cell Technology or UCT), the quadrupole mass filter, and finally are counted in
rapid sequence at the detector allowing individual isotopes of an element to be
determined.
In principle, the UCT is an enclosed, pressurizable cell that can operate in one of three
different modes. In “standard” mode (also called “vented” mode) the cell is not
pressurized, and ions pass through the cell to the quadrupole mass filter unaffected. In
“Dynamic Reaction Cell” (DRC) mode the cell is pressurized with a gas which will collide or
react with the incoming ions to either eliminate an interfering ion (e.g., neutralize or
change into a new mass) or change the ion of interest to a new mass which is free from
interference. During DRC mode, the RPq and RPa settings of the software control the
range (the bandpass) of ions that will have a stable trajectory through the UCT. Bandpass
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control is used to prevent undesirable reactants into or product ions out of the UCT during
DRC mode. Normally, the ions traveling through the UCT cell would slow down due to
multiple collisions leading to a loss of momentum. In DRC mode, the voltage applied by
the axial field technology (AFT) and the additional push from spectator ions, that are
stable in the DRC bandpass, keep the ions moving axially through the pressurized UCT
chamber. In “Kinetic Energy Discrimination” (KED), mode the UCT is pressurized with a
non-reactive gas which collides with the incoming ions. Collisions occur more frequently
with larger (polyatomic) ions than smaller, (single atom) analyte ions, thus lowering the
kinetic energy of the polyatomic ions relative to the atomic ions. In KED mode, the UCT is
maintained at a cell rod offset (CRO) voltage more negative than the quadrupole rod
offset (QRO) of the quadrupole mass filter, creating an energy barrier between the two
quadrupoles. The faster moving atomic analyte ions can overcome the energy barrier
while the larger, slower polyatomic ions cannot separating the analyte ions from the
interference ions. This energy barrier is called the kinetic energy discriminator (KED).
In this method, the instrument is operated in DRC mode when analyzing for cadmium and
manganese; in KED mode when analyzing for cobalt; and in standard mode when
analyzing for all other analytes. When analyzing for cadmium, the UCT is pressurized with
oxygen and operated in DRC mode. The 95Mo16O+ ions which would normally interefere
with the detection of 111Cd react with oxygen in the cell to eliminate the interference on
low-level 111Cd analysis. When low level Cd analysis is not the principle purpose of the
analysis (e.g. emergency response situations concerned with identifying acute Cd
exposures), Cd analysis can be performed in vented (standard) mode and still yield
quantitative results suitable for the identification of elevated exposures with the caveat
described in Section 2.ii. The UCT is also pressurized with oxygen gas and operated in DRC
mode when analyzing for 55Mn. The 39K16O+ ions which would normally interfere with the
detection of 55Mn at m/z 55 react with the oxygen in the cell and no longer represent
interference to 55Mn analysis. The UCT is pressurized with helium gas and operated in KED
mode when analyzing for cobat (59Co). The quadrupole rod offset (QRO) is maintained 2 to
3V more positive than the cell rod offset (CRO) which prevents the larger polyatomic
interference ion (43Ca16O+) from leaving the UCT, eliminating the interference on 59Co. The
QRO and CRO settings are typically optimized by manufacturer service representatives at
installation and preventive maintenance visits.
Electrical signals resulting from the detection of ions are processed into digital
information that is used to indicate first the intensity of the ions and then the
concentration of the element. This method was originally based on the method by
Mulligan et al. [7]. The vented mode portion of this method, prior to using KED / helium
mode for analysis of cobalt, was published by Caldwell et al. [5]. The DRC portions of this
method are based on work initially published by Tanner et al. [2, 3] and Jarrett et al. [6].
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2. Limitations of method; interfering substances and conditions

A. Interferences addressed by this method:
The UCT is used in KED / helium mode in this method to eliminate interference from
calcium oxide (43Ca16O) at m/z 59. If not eliminated, the 43Ca16O interference can increase
observed urine cobalt results by approximately 0.3 µg/L at urine calcium levels of 500
µg/mL (assuming 1.5L excretion per day, ninety percent of health females and males have
urinary total calcium levels <170 µg/mL and <200 µg/mL [7], respectively).
The UCT is used in DRC mode (filled with oxygen) in this method to eliminate interference
from molybdenum oxide (95Mo16O) onto cadmium at m/z 111 [6]. If not eliminated, the
molybdenum oxide interference has been reported to increase observed urine cadmium
results by approximately 0.2 µg/L at urine molybdenum concentations equivalent to the
95th percentile (137 µg/L) of the U.S. population [8]. Vented mode analysis can provide
suitable urine cadmium quantitation when the primary concern is to identify acute
exposures to cadmium (e.g., emergency response), but results should be interpreted with
the caveat that the 95Mo16O+ interference on 111Cd is not eliminated.
The UCT is used in DRC mode (filled with oxygen) in this method to reduce the potassium
oxide (39K16O) interference on manganese at m/z 55. If not eliminated, the 39K16O
interference can increase observed urine manganese results by approximately 0.4 µg/L at
urine potassium concentrations equivalent to 400 mg/L urine potassium. Urine potassium
can vary between 650 mg/L – 3250 mg/L[9].
The UCT is used at a high RPq setting in DRC mode (filled with oxygen) to eliminate a
bromine oxide (79Br16O 2 ) interference from being formed in the UCT that would interfere
with cadmium at m/z 111. This interference is observed to be significant only in DRC
mode where 79Br16O entering the UCT combines with oxygen. If not eliminated, the
Br O 2 interference can increase observed urine cadmium results by approximately 0.7
79 16
µg/L at urine bromine concentrations of 40 mg/L (typical levels in urine are approximately
4 mg/L [10]).
B. Limitations of the method:
Accuracy and precision of this method can be critically impacted by elemental

contamination. See Section 3.A regarding contamination control in the pre-analytical
processes. Use high purity water and chemicals (See Section 5.E) and pre-rinsed or pre-
screened containers in reagent and sample preparation (See Section 6). Occasionally, we
observe contamination in sample preparations due to the Hamilton dilutor components
(e.g. valve and syringes) particularly if components are new or infrequently used.
Manganese, especially, can be problematic in the valve of the Hamilton. Monitor
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instrument and diluter cleanliness before and during analysis (See Section 8.B.iv) and rinse
or replace components identified as causing elevated background levels in the reagent
and blank checks. A rinse of the diluter pipette tip with concentrated nitric acid can be
used to eliminate urine residue on the outside of the plastic tip.
Specificity tests indicated that at there is no observable impact on observed cadmium

results from this method at urine zirconium levels up to 10 µg/L. Levels of zirconium in
human urine reported in the literature as <0.1 µg/L [11]. However, specificity tests
indicate that polyatomic interferences related to zirconium (e.g., 96Zr15N, 96Zr14N1H,
Zr O H, 92Zr18O1H, or 92Zr19F) can increase observed urine cadmium results by
94 16 1
approximately 0.4 µg/L (in DRC mode) when a urine sample has elevated levels of
zirconium, 1000 µg/L. In standard (vented) mode the bias from the interferent is expected
to be even higher, 0.7 µg/L per 1000 µg/L.
3. Procedures for collecting, storing, and handling specimens; criteria for

specimen rejection; specimen accountability and tracking
A. Procedures for collecting, storing, and handling specimens:
Specimen handling conditions, special requirements, and procedures for collection and
transport are discussed in the Division of Laboratory Science’s (DLS) Policies and
Procedures Manual [9]. In general
Transport urine specimens frozen (packed in dry ice during shipment is preferred when
possible).
Once received, store long term at ≤ -20 °C until time for analysis. Short-term storage at 2-
8 °C is acceptable. Refreeze at ≤ -20 °C portions of the sample that remain after analytical
aliquots are withdrawn. Thawing and refreezing samples has not been found to
compromise sample results.
Acceptable containers for analytical aliquots include lot screened polypropylene (PP)
cryovials or tubes (i.e. 2 to 5 mL cryogenic vial or 15mL centrifuge tube). Avoid colored
plastics and containers containing o-rings when possible due to increased risk of trace
element contamination from coloring agents or o-ring materials. Externally threaded
containers are preferred because they are less prone to contamination of the specimen
and to leaks (internally threaded containers can develop leaks when biological material
dries within the threads, compromising resealing).
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B. Criteria for specimen rejection:

Specimen characteristics that compromise test results are indicated above. Other reasons
for rejecting a sample for analysis are listed below. In all cases, request a second urine
specimen.
Optimal amount of urine is ≥ 1.8 mL. The volume of urine used for one analysis is 0.5 mL.
Less volume is consumed when only subsets of the 15 elements are analyzed.
Improper collection procedures or collection devices can contaminate the urine by

contact with dust, dirt, etc.
C. Transfer or referral of specimens; procedures for specimen accountability and
tracking
Location, status, and final disposition of the specimens will be tracked and records are
maintained according to the Division’s Policies and Procedures Manual [12] Use only
numerical identifiers for samples within the laboratory (e.g., case ID numbers) in order to
safeguard confidentiality. Only the medical supervisor (MS) or project coordinator (PC) i.e.
non CDC personnel will have access to the personal identifiers.
4. Safety precautions
A. General Safety:
If concentrated acids come in contact with any part of the body, quickly wash the
affected area with copious quantities of water for at least 15 minutes.
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B. Radiation safety:
Calibration standards used in this method contain µg/L natural uranium. Staff performing
this method in the CDC laboratory must maintain the status of Radiation Worker through
the Radiation Safety Office and practice appropriate radiation safety when handling these
solutions in accordance to the CDC’s license with the Nuclear Regulatory Commission
(NRC).
C. Waste disposal:
1) Waste discarded down sink: Do not discard solutions at the sink having a pH lower than
5.0 or higher than 11.5 (limits defined by Dekalb County, GA). Inactivate biological
compounds and cellular constituents in mixed chemical and biological waste, such as the
waste carboy of the ICP-MS, by adding an approved disinfectant (e.g. household bleach at
a 1:100 dilution or equivalent) prior to drain disposal. Flush the sink with copious
amounts of water.
2) Waste to be picked up by the CDC radiation safety office: Solutions used in the CDC
laboratory having uranium concentrations equal to or greater than 500 µg/L (e.g. single
element stock standard, multi-element stock standard, and intermediate stock standard).
3) Waste to be picked up by CDC hazardous waste program: Submit request for
hazardous waste removal of all other liquid waste generated in the CDC laboratory for
this method.
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5. Instrument and material sources

A. Sources for ICP-MS instrumentation:
B. Sources for ICP-MS parts & consumables

NOTE: The minimum number of spares recommended before reordering (if owning one
instrument) are listed as “# Spares =” in the descriptions below.
1) Female nut for 1.6mm O.D. (1/16”) tubing. Like part P-420 (Upchurch Scientific, Oak
Harbor, WA, www.upchurch.com).
2) PEEK ferrule. Like part P-260x (10pk SuperFlangeless ferrule, Upchurch Scientific, Oak
Harbor, WA, www.upchurch.com).
3) Conical Adapter Body. Like part P-692 (Upchurch Scientific, Oak Harbor, WA,
www.upchurch.com).
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1. Screws (for hyper skimmer cone): PerkinElmer part # 09919737 (PerkinElmer,

Shelton, CT, www.perkinelmer.com) or equivalent. # Spares = 4 screws per
instrument.
1) Valve: CTFE High-flow valve head for SC-FAST (uses ¼-28 fittings). Like part # SC-0599-
1010 (Elemental Scientific Inc., Omaha, NE., www.elementalscientific.com).
2) Stator: CTFE Stator for 6 port SC-FAST high flow valve (¼-28 fittings). Like part # SC-
0599-1010-01 (Elemental Scientific Inc., Omaha, NE., www.elementalscientific.com).
3) Rotor: Composite rotor for 6 port SC-FAST high flow valve (¼-28 fittings). Like part # SC-
0599-1010-05 (Elemental Scientific Inc., Omaha, NE., www.elementalscientific.com).
4) Sample loop: 3 mL Teflon loop with white connector-nuts for high flow valve head, like
part # SC-0315-30 (Elemental Scientific Inc., Omaha, NE., www.elementalscientific.com).
Subsets of elements can be analyzed using different loop sizes to minimize sample
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consumption (e.g. 0.5 mL loop for a single element, 1.0 mL loop for 3 element subset,
2.0mL loop for 8 element subset, etc…).
5) Probe, autosampler: Teflon, carbon fiber support, 0.8mm i.d., blue marker, 1/4-28
fittings. Like part number SC-5037-3751 (Elemental Scientific Inc., Omaha, NE.,
www.elementalscientific.com). # Spares = 2.
6) Probe, carrier solution: Teflon, carbon fiber support, 0.5mm i.d., orange marker, 1/4-28
fittings. Like part number SC-5037-3501 (Elemental Scientific Inc., Omaha, NE.,
7) Tubing, carrier solution: 0.5mm i.d. Teflon tubing (orange marker) with red ¼-28 male
nut. Connects to high flow FAST valve head, port #2. Like part # SC-0316-0500 (Elemental
Scientific Inc., Omaha, NE., www.elementalscientific.com).
8) Tubing, nebulizer: See “Nebulizer, PolyPro-ST micro flow”
9) Tubing, rinse station: Teflon tubing and adapters (to attach to back of SC autosampler
for filling rinse stations and to attach to rinse containers). Like part # SC-0302-0500,
Elemental Scientific Inc., Omaha, NE., www.elementalscientific.com).
10) Tubing, vacuum: Vacuum line for SC-FAST high flow valve, connects to port #6, black
nut for connection to valve head, natural brown color nut on other end for connection to
SC autosampler vacuum port. Like part # SC-0321 (Elemental Scientific Inc., Omaha, NE.,
www.elementalscientific.com).
1) Gas connection:
(a) Teflon tubing: 4mm o.d., 2.4mm i.d. Teflon tubing (like part # ES-2502, Elemental
Scientific Inc., Omaha, NE., www.elementalscientific.com). # Spares = 1.
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(b) Adapter kit: Plastic adapters to connect Teflon tubing (2.4mm i.d.) to ¼” male
Swagelok (compression) port on ICP-MS. Parts can be obtained as components in a
“gas fittings kit for microflow nebulizer”, kit part # ES-2501-1000, Elemental Scientific
Inc., Omaha, NE., www.elementalscientific.com). # Spares = 1.
(c) Nebulizer Gas line (NexION 2000): Like #N8152385 (PerkinElmer Shelton, CT,
www.perkinelmer.com).
(d) Matrix Gas line (NexION 2000): Like #N8152374 (PerkinElmer Shetlon, CT,
www.perkinelmer.com)
2) Liquid connection: Connects nebulizer to port #3 of high flow FAST valve head with
green, 1/4- 28 fitting. Like part # SC-0317-0250 (Elemental Scientific Inc., Omaha, NE.,
1) Welch Directorr Gold: For non-synthetic oil roughing pumps. Available direct from
manufacturer as part # 8995G-15 (1 gallon, Welch Rietschle Thomas, Skokie, IL,
www.welchvacuum.com), or equivalent. # Spares = 4.
2) Fomblin Y14/5 fluid: For synthetic fluid roughing pumps. PerkinElmer part # N8122265
(1 kg bottle, PerkinElmer, Shelton, CT, www.perkinelmer.com) or equivalent. # Spares =1
per instrument.
1) Internal o-rings: ID = ¼”, OD = 3/8”, thickness = 1/16”. Need 2 o-rings per injector
support setup. PerkinElmer part # N8122008 (PerkinElmer, Shelton, CT,
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www.perkinelmer.com) or equivalent (such as part # V75-010, O-rings West, Seattle, WA,

www.oringswest.com). # Spares = 20.
2) External o-rings: ID = 3/8”, OD = 1/2”, thickness = 1/16”. Need 2 o-rings for each
injector support setup. PerkinElmer part # N8122009 (PerkinElmer, Shelton, CT,
www.perkinelmer.com) or equivalent (such as part # V75-012, O-rings West, Seattle, WA,
www.oringswest.com). # Spares = 20.
1) NexION 300D/350D: PerkinElmer part # N8145013 (PerkinElmer, Shelton, CT,

www.perkinelmer.com) or equivalent. # Spares = 2.
2) NexION 2000: Quartz cyclonic with matrix port C3 high sensitivity, PerkinElmer part #
N8152383 (PerkinElmer Shelton, CT, www.perkinelmer.com). Or equivalent. # Spares = 2.
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1) Standard PVC, 2-stop (black / black) peristaltic pump tubing, i.d. = 0.03”. PerkinElmer
part # 09908587 (PerkinElmer, Shelton, CT, www.perkinelmer.com) or equivalent. #
Spares = 6 packs of 12 tubes.
2) Standard PVC, 3-stop (black/ black/black) peristaltic pump tubing, i.d. 0.76 mm.
Spectron part # SC0056 (Spectron, Ventura, CA, www.spectronus.com) or equivalent.
#Spares = 6 packs of 12 tubes. Use this type of tubing with ESI DXi micro-peristaltic pump.
1) Standard PVC, 2-stop (black / white) peristaltic pump tubing, i.d. = 0.125” or
equivalent. PerkinElmer part # N812-2012 (PerkinElmer, Shelton, CT,
www.perkinelmer.com) or equivalent. # Spares = 6 packs of 12 tubes.
2) Standard Santoprene, 3-stop (grey/ grey/ grey) peristaltic pump tubing, i.d. 1.30 mm.
Spectron part # SC0311 (Spectron, Ventura, CA, www.spectronus.com) or equivalent.
#Spares = 6 packs of 12 tubes. Use this type of tubing with ESI DXi micro-peristaltic pump.
C. Sources for ICP-MS maintenance equipment and supplies:
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D. Sources for general laboratory consumable supplies:
1) 100mL volumetric flasks (like catalog # 40000100, Thermo Scientific, Fisher Scientific,
Pittsburgh, PA., www.fishersci.com). Plastic or glass is acceptable.
2) 200mL volumetric flask (like catalog # 40000200, Thermo Scientific, Fisher Scientific,
3) 500mL volumetric flask (like catalog # 40000500, Thermo Scientific, Fisher Scientific,
4) 1L volumetric flask (like catalog # 40001000, Thermo Scientific, Fisher Scientific,
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E. Sources of chemicals, gases, and regulators:
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1) Regulator for argon (at dewar): Stainless steel, single stage, specially cleaned regulator
with 3000 psig max inlet, 0-200 outlet pressure range, CGA 580 cylinder connector, and
needle valve shutoff on delivery side terminating in a ¼” Swagelok connector. Part
number “KPRCGRF415A2/AG10-AR1” (Georgia Valve and Fitting, Atlanta, GA,
www.swagelok.com), or equivalent. # Spares = 1.
2) Regulator for argon (between bulk tank and PerkinElmer filter regulator): Single Stage
316SS Regulator, with 0-300 psi Inlet Gauge, 0-200 psi Outlet Gauge, Outlet Spring Range,
0-250 psi, ¼” Swagelok Inlet Connection, ¼ turn Shut off Valve on Outlet with ¼”
Swagelok Connection and Teflon Seals. Part number KPR1GRF412A20000-AR1 (Georgia
Valve and Fitting, Atlanta, GA, www.swagelok.com), or equivalent. # Spares = 1.
3) Regulator for argon (filter regulator on back of ICP-MS): Argon regulator filter kit.
Catalog number N8125006 (PerkinElmer, Shelton, CT, www.perkinelmer.com).
1) Regulator for helium: Stainless steel, two stage, specially cleaned regulator with 3000
psig max inlet, 0-25 outlet pressure range, CGA 350 cylinder connector, and needle valve
shutoff on delivery side terminating in a ¼” Swagelok connector. Like part #
KCYADPF412A2AD10 (Georgia Valve and Fitting, Altanta, GA, wwww.swagelok.com) or
equivalent. # Spares = 1.
2) He Filter, advanced filter system: Part # N9303963 (PerkinElmer, Shelton, CT,
www.perkinelmer.com) or equivalent; Replacement cartridge part # N9303964
(PerkinElmer, Shelton, CT, www.perkinelmer.com) or equivalent. # Spares = 2.
1) Regulator for oxygen: Stainless steel, two stage regulator for use with high purity
oxygen (cleaned to be free of all oils). Maximum inlet pressure 3600-5000 psi. Inlet gauge
pressure 0-5000 psi (no oil in gauge). Maximum delivery pressure 50–100 psi with a 0-30
psi outlet gauge (no oil in gauge). CGA 540 cylinder connector on inlet side and an angle
pattern (90 degree) stainless steel needle valve on the delivery side terminating in a 1/8”
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stainless steel Swagelok connector. Like part # GEORG/KCYCFR/ORS2/540 (Georgia Valve

and Fitting, Atlanta, GA, www.swagelok.com), or equivalent.
6. Preparation of reagent and materials

A. Intermediate internal standard mixture:
1) If not previously dedicated to this purpose, acid wash a 200 mL volumetric flask (PP,
PMP, or Teflon™). For example, with 2% (v/v) HNO3 and >18 Mohm∙cm water (at least 3
times each) and verify cleanliness through analysis of rinsate.
2) Partially fill the 200 mL volumetric flask with >18 Mohm∙cm water (approximately 100-
150 mL).
3) Carefully add 4 mL of concentrated nitric acid. Mix into solution.
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4) Add 8,000 µg of rhodium (e.g. 8 mL of 1,000 µg/mL Rh stock standard).

5) Add 8,000 µg of iridium (e.g. 8 mL of 1,000 µg/mL Ir stock standard).
6) Fill to mark (200mL) and mix thoroughly.
7) Store at ambient temperature and label appropriately. Expiration is 1 year from date of
preparation.
B. Intermediate Triton X-100™ solution:
1) If not previously dedicated to this purpose, acid wash a 2 L bottle (PP, PMP, or
Teflon™). For example, with 2% (v/v) HNO3 and >18 Mohm∙cm water (at least 3 times
each) and verify cleanliness through analysis of rinsate.
2) Partially fill the bottle with >18 Mohm∙cm water (approximately 1-1.5 L).
3) Add 40 mL of Triton X-100™ and stir until completely dissolved. Use a Teflon™ stir bar
and stir plate if necessary (acid wash stir bar before use).
4) Carefully add 100 mL of concentrated nitric acid.
5) Fill to 2 L and stir thoroughly.
preparation.
C. Diluent and carrier:
1) If not previously dedicated to this purpose, acid wash a 2 L container (PP, PMP, or
Teflon™). For example, with 2% (v/v) HNO3 and >18 Mohm∙cm water (at least 3 times
2) Partially fill the 2 L container with >18 Mohm∙cm water (~2/3 full).
3) Carefully add 40 mL concentrated nitric acid and mix.
4) Add spike of internal standard solution (to use other concentrations or volumes, adjust
the volumes proportionally).
5) Add 500 µL of the 40 µg/mL Rh and Ir internal standard solution.
6) Make up to volume (2 L) with >18 Mohm∙cm water.
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preparation.
D. ICP-MS rinse solution:
1) If not previously dedicated to this purpose, acid wash a 4 L container (PP, PMP, or
Teflon™). For example, with 5% (v/v) HNO3 and ≥18 Mohm∙cm water (at least 3 times
2) Partially fill the bottle with >18 Mohm∙cm water (approximately 2-3 L).
3) Add 4 mL of the 2% Triton X-100™ / 5% (v/v) nitric-acid intermediate stock solution and
mix well.
4) Carefully add 200 mL of concentrated nitric acid and mix well.
5) Fill to 4 L using >18 Mohm∙cm water.
preparation.
E. Multi-element stock calibration standard
1) Solution A: 5% HNO3 solution containing Ba, Be, Cd, Cs, Co, Pb, Mn, Sr, Tl, and U.
Concentrations are listed in Table 3 of Appendix C.
2) Solution B: 5% HNO3, 1% HF, 0.5% HCl solution containing Sb, Mo, Pt, Sn, and W.
Concentrations are listed in Table 3 of Appendix C.
3) Storage: Store at ambient temperature and label appropriately. Expiration is
determined by manufacturer or is 1 year after the container is opened (whichever comes
first).
F. Intermediate multi-element stock calibration standard
1) If not previously dedicated to this purpose, acid wash a 100 mL PP, PMP, or Teflon™
volumetric flask. For example, with a 2% (v/v) HNO3 / 1% (v/v) HCl solution and ≥18
Mohm∙cm water (at least 3 times each) followed by verifying cleanliness through analysis
of rinsate. Dedicate to purpose.
2) Partially fill the 100 mL volumetric flask with the 2% (v/v) nitric acid and 1% (v/v)
hydrochloric acid prepared in Section 6.e.iii (50-75% full).
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3) Using the volume listed in Table 4 of Appendix C, pipette the appropriate volume of the
multi-element stock calibration standard solutions (both A and B) into the volumetric
flask. Dilute to the volumetric mark with the 2% (v/v) nitric acid and 1% (v/v) hydrochloric
acid using a pipette for the final drops. Mix each solution thoroughly. Final concentrations
are listed in Table 4 of Appendix C.
4) Once mixed, transfer to an acid-cleaned, labeled, 50 mL container (PP, PMP, or
Teflon™) for storage.
5) Label appropriately and store at ambient temperature. Expiration is 1 year from the
date of preparation.
G. Multi-element intermediate working calibration standards
1) Cleaning flasks: If not previously dedicated to this purpose, acid wash PP, PMP, or
Teflon™ volumetric flasks. For example, with a 2% (v/v) HNO3 / 1% (v/v) HCl solution and
≥18 Mohm∙cm water (at least 3 times each) followed by verifying cleanliness through
analysis of rinsate. Dedicate to purpose.
2) 2% (v/v) HNO3 & 1% (v/v) HCl diluent (S0) preparation: In a cleaned 2L volumetric flask,
add 1-1.5L >18 Mohm∙cm water, 40 mL high purity concentrated HNO3, and 20 mL high
purity concentrated HCl. Fill to the mark and mix thoroughly. Use this diluent to fill the
remaining volumetric flasks during preparation of the intermediate working calibration
standards.
3) Dilutions & storage:
(a) Fill two acid-cleaned 50-mL containers (PP, PMP, or Teflon™) with the HNO3 and
HCl diluent. Label appropriately (including “S0”) and store at ambient temperature.
Expiration is 1 year from the date of preparation.
(b) Partially fill the volumetric flasks with the HNO3 & HCl diluent (50-75% full).
(c) Using the volumes listed in Table 5 of Appendix C, pipette the appropriate volume
of the multi-element stock calibration standard or the multi-element intermediate
stock calibrator solutions (both A and B) into each of the volumetric flasks. Dilute each
to the volumetric mark with the HNO3 & HCl diluent using a pipette for the final drops.
Mix each solution thoroughly. Final concentrations are listed in Table 5 of Appendix C.
(d) Once mixed, transfer to acid-cleaned, labeled, 50-mL containers (PP, PMP, or
Teflon™) for storage.
(e) Store at ambient temperature and label appropriately. Expiration is 1 year from
date of preparation.
H. Working multi-element calibrators
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I. Base urine
1) Collect urine anonymously by placing screened containers and collection cups in the
restrooms with a sign stating the reason the specimens are being collected, the name of
the investigator to contact for additional information, and requesting that people provide
a urine specimen (see supervisor regarding potential Institutional Review Board, IRB,
requirements).
2) Once collected, analyze to ensure that concentrations of the analytes in this method
are relatively low, so as to not interfere with the proper measurement of calibrators (see
Table 2 in Appendix C for suggested maximum base urine concentrations).
3) Once screened, mix the urine collections together in a larger container (polypropylene
(PP), polymethylpentene (PMP), or Teflon™) which has been acid washed. For example,
with 2% (v/v) HNO3 and ≥18 Mohm∙cm water (at least 3 times each) and verify cleanliness
through analysis of rinsate. Add large Teflon™ stir bar and stir for 30+ minutes.
4) Label appropriately and store long-term in smaller volume tubes (e.g. 50-mL acid-
washed or lot screened polypropylene tubes) at ≤ -20 °C. Expiration date is 3 years from
the date of preparation.
J. Internal quality control materials (“Bench” QC)
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1) Collection of urine: Collect urine anonymously by placing screened containers and / or

collection cups in the restrooms with a sign stating the reason the specimens are being
collected, the name of the investigator to contact for additional information, and
requesting that people provide a urine specimen. Volume of urine to collect is dependent
on the desired pool size. This write-up will assume a 10-L pool size for both the low and
high bench QC.
2) Screening urine: Screen collected samples for metal content before mixing together to
make separate pools that will be spiked to low, high, and elevated levels. Samples can be
screened individually or after combining several together (reduces number of analyses).
3) Keep urine refrigerated whenever possible to minimize microbial growth.
4) Because this is only a quick screen of the metal content, the number of replicates in
the urine method can be reduced to one in order to reduce analysis time.
5) Spike analyte concentrations for the low bench QC pool in the low-normal population
range. Spike analyte concentrations for the high bench QC pool less than some
preselected target concentration values in the high normal population range. See the
National Report on Human Exposure to Environmental Chemicals for estimations of the
normal population ranges for metals (http://www.cdc.gov/exposurereport/).
6) Combining collected urine: Be attentive not to combine only diluted matrix urine
samples into the low pool and only concentrated matrix urine samples into the pool for
high and elevated QC. The goal is for combining samples is to approach an ‘average’
matrix for each pool.
7) Graduate four acid-washed 10-L carboys (PP or PMP) in 0.5 L increments (two will be
used for decanting into).
8) Combine collected urine samples into separate acid-washed 10-L carboys (PP or PMP),
according to their concentrations, for the low high, and elevated bench QC pools.
9) Mix each urine pool using large acid washed, Teflon™ coated stir bars and large stir
plates. Keep urine refrigerated whenever possible.
(a) Acidify each urine pool to 1% (v/v) HNO3 by adding the appropriate volume of
concentrated HNO3. Stir for 30+ min on large stir plates.
(b) Settling out of solids:
(i) Refrigerate the urine (no stirring) for 1-3 days to allow for settling out of solids.
(ii) For each urine pool, decant the urine into another of the acid-washed 10-L
carboys to remove the urine from the solids settled out on the bottom of the carboy.
(iii) Repeat steps (i) and (ii) until minimal solids are left at the bottom of the carboy
after sitting overnight.
(c) Spiking of urine
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(i) Analyze a sample of each urine pool. Record these results for future recovery
calculations.
(ii) Use these results to determine target analyte concentrations possible for the
pools
(iii) Calculate the volume of single element standards needed to spike each pool to
the desired concentrations.
(iv) While stirring the pools on large stir plates, spike each pool with calculated
volumes of single element standards (all spiking standards used must be traceable to
NIST).
(v) Continue to stir pools for 30+ minutes after spiking, then reanalyze.
(vi) Repeat steps 4 and 5 until all analytes reach target concentrations keeping track
of the total volume of spiking solution added to each urine pool.
(d) Dispensing and storage of urine
(i) Container types: Dispense urine into smaller, lot screened containers (e.g. 2 mL
cryovials). This allows for one vial of QC to be used in only a small number of
analyses, reducing chances of contamination due to long-term use of the same
container.
(ii) Labels: Place labels on vials after dispensing and capping if the vials are originally
bagged separately from the caps. This minimizes the chance for contamination
during the process. Include at least the name of QC pool (text and bar code), date of
preparation, and a vial number on the labels.
(iii) Dispensing: Dispensing can be accomplished most easily using a benchtop
automatic pipette in continuous cycling dispense mode. Complete this process in a
clean environment (i.e., a class 100 cleanroom area or hood). Allow urine pool to
reach ambient temperature before dispensing (to prevent temperature gradients
possibly causing concentration gradients across the large number of vials being
dispensed and to prevent condensation problems during labeling of vials). Replace
the tubing attached to the dispensing syringe (left when looking at front of benchtop
automatic pipette) with a length of clean Teflon™ tubing long enough to reach into
the bottom of the 10L carboy while it is sitting on the stir plate. Check cleanliness of
benchtop automatic pipette before use by analyzing 1-2% (v/v) HNO3 which has been
flushed through the benchtop automatic pipette with a portion of the same solution
which has not been through the benchtop automatic pipette. Approximately one
hour before dispensing begins, with the large stir plate close to the left side of the
benchtop automatic pipette, begin stirring the urine pool to be dispensed. Also
during this time, flush the benchtop automatic pipette with urine from the pool to be
dispensed. Place the ends of the tubing attached to both the sample and dispensing
syringes into the carboy of urine so that urine won’t be used up during this process.
Be sure to secure both ends of tubing in the carboy with Parafilm so they will not
come out during the flushing process. After dispensing the urine into the vials, cap
the vials and label them. Placing labels on vials after capping minimizes the chance
for contamination during the process.
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(iv) Homogeneity testing: After dispensing, check homogeneity of analyte

concentrations in pool aliquots by analysis of vials selected from across those
dispensed. Seek guidance from a statistician regarding the number of vials needed
for homogeneity analysis.
(e) Storage: Store long-term according the same storing and handling criteria
described in Section 3.
K. UCT Optimization solutions:
1) Base urine in diluent (1 + 9): In a 50 mL lot screened or acid-washed polypropylene

tube, prepare a 50 mL portion of working calibrator 0 as described in Table 8 in Appendix
C (multiply volumes by 5).
2) Base urine in diluent (1 + 9) + 0.24 µg/L Cd: In a 50 mL lot screened or acid-washed
polypropylene tube, prepare a 50 mL portion of working calibrator 2 as described in Table
8 in Appendix C (multiply volumes by 5).
3) Base urine in diluent (1 + 9) + 300 µg/L Mo: In a 50 mL lot screened or acid-washed
8 in Appendix C (multiply volumes by 5). Add 0.015 mL of 1000 mg/L Mo.
4) Base urine in diluent (1 + 9) + 0.24 µg/L Cd + 300 µg/L Mo: In a 50 mL lot screened or
acid-washed polypropylene tube, prepare a 50 mL portion of working calibrator 2 as
described in Table 8 in Appendix C (multiply volumes by 5). Add 0.015 mL of 1000 mg/L
Mo.
5) Store at ambient temperature and prepare as needed. Label appropriately, i.e. “Store
at ambient temperature”, preparation date, expiration date one year from preparation
date, and preparer’s initials.

2) Base urine in diluent (1 + 9) + 0.3 µg/L Mn: In a 50 mL lot screened or acid-washed
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3) Base urine in diluent (1 + 9) + 400 µg/L K: In a 50 mL lot screened or acid-washed

8 in Appendix C (multiply volumes by 5). Add 0.02 mL of 1000 mg/L K
4) Base urine in diluent (1 + 9) + 0.3 µg/L Mn + 400 µg/L K: In a 50 mL lot screened or
described in Table 8 in Appendix C (multiply volumes by 5). Add 0.02 mL of 1000 mg/L K.
5) Store at ambient temperature and prepare as needed. Label appropriately, i.e. “Store
at ambient temperature”, preparation date, expiration date one year from preparation
date, and preparer’s initials.

2) Base urine in diluent (1 + 9) + 0.225 µg/L Co: In a 50 mL lot screened or acid-washed
3) Base urine in diluent (1 + 9) + 50 µg/mL Ca: In a 50 mL lot screened or acid-washed
polypropylene tube, prepare a 50 mL portion of working calibrator 0 as descreibed in
Table 8a ( multiply volumes by 5). Add 0.25 mL of 10,000 mg/L Ca.
4) Base urine in diluent (1 + 9) + 0.225 µg/L Co+ 50 µg/mL Ca: In a 50 mL lot screened or
described in Table 8a ( multiply volumes by 5). Add 0.25 mL of 10,000 mg/L Ca.
L. Axial field voltage optimization for DRC mode of UCT:
M. For dual detector calibration:
1) Partially fill a 50 mL lot screened or acid-washed polypropylene tube with 2% (v/v)

HNO3
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2) Add a 0.1 mL of 100 ug/mL special mix standard.

3) Add 0.01 mL of any additional 1,000 ug/mL single element stock standard desired to be
added.
4) Dilute to the 50 mL mark with 2% (v/v) HNO3.
5) Label appropriately and store at ambient temperature. Expiration date is one year
from preparation date.
7. Analytical instrumentation setup
(See Section 5 for details on hardware used, including sources)
A. Instrumentation and equipment setup:
1) Liquid handling
(a) FAST valve setup: See Appendix B, Figure 1 for diagram and Section 5.b “FAST / ESI
SC4-DX autosampler accessories” for source information.
(i) Port 1: sample loop (white nut).
(ii) Port 2: 0.5 mm ID probe (red nut) for carrier solution.
(iii) Port 3: nebulizer line (green nut) for transfer of liquid to nebulizer.
(iv) Port 4: sample loop (white nut).
(v) Port 5: 0.8 mm ID probe (blue nut) for diluted samples.
(vi) Port 6: vacuum line (black nut).
(b) Carrier solution uptake: Use peristaltic pump to control uptake flow rate of carrier
solution to the SC-FAST valve. Use of a ‘peristaltic to Teflon tubing adapter’ for
prevents damage to small i.d. tubing when making connections (see consumables
descriptions in Section 5.b).
(c) Spray chamber waste removal: Use of a ‘peristaltic to Teflon tubing adapter’
prevents damage to small i.d. tubing when making connections (see consumables
descriptions in Section 5.b).
(i) Between spray chamber and peristaltic tubing:
1. Spray chambers with threaded connection: Use vendor-supplied threaded
connector on base of chamber, connecting tubing directly to peristaltic pump
tubing through a PEEK adapter or directly.
2. Spray chambers without threaded connection: Use of a specialized push-on
connectors available from various vendors (like UFT-075 from Glass Expansion,
Pocasset, MA) are preferred for safety reasons to direct connection of PVC tubing
(e.g. 1/8” i.d. x ¼” o.d.).
(ii) Between peristaltic pump tubing and waste container: Connect 1/8” i.d. x ¼” o.d.
PVC tubing to the white / black peristaltic pump tubing using a tubing connector
(PerkinElmer item # B3140715). Place the free end of the PVC tubing through the lid
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of the waste jug (be sure it is secure). Place the waste container in a deep secondary
containment tray in case of overflow.
(d) Rinse solution for autosampler:
(i) Rinse solution jug: Leave one of the caps on the top of the rinse jug loose to allow
air venting into the jug as liquid is removed. Otherwise the jug will collapse on itself
as the liquid is removed and a vacuum is created inside. Use secondary containment
tray.
(ii) Rinse solution uptake to autosampler rinse station: Use tubing of different lengths
and inner diameters between the rinse solution container and the autosampler rinse
station to control uptake rate of rinse solution. These can be obtained from the
autosampler manufacturer, their distributors, or custom built in the lab. Optimize
these factors along with fill time in the software so that waste of rinse solution is
minimized and rinse station does not go empty.
(iii) Autosampler rinse station waste removal: Gravity drain of waste to the waste
container is sufficient. Use minimum drain tubing to make this connection. If this
tube is too long, the rinse station will not drain properly.
(e) Coolant for ICP-MS: Use a chiller or heat exchanger with collant approved by
PerkinElmer. If using refrigerated chiller, set the temperature control on the chiller to
approximately 18 °C.
2) Gas delivery and regulation
(a) Argon gas: Used for various ICP-MS functions including plasma and nebulizer.
(b) Regulator for argon source (if a dewar): Set delivery pressure of this regulator at
least 10 psi higher than the delivery pressure of the step-down regulator to allow for
pressure drop across tubing that stretches to the instrument.
(c) Step down regulator (if source of argon is a bulk tank): Place this single stage
regulator in the lab so that incoming argon pressure can be monitored and adjusted.
Set delivery pressure to 10 psig above the delivery pressure of the filter regulator on
the ICP-MS.
(d) Filter Regulator at ICP-MS: Single stage “argon regulator filter kit” supplied with
the ICP-MS. Set the delivery pressure depending on the instrument setup:
(i) NexION with a 0-150psi gauge on the filter regulator: 90-100 psi when plasma is
running.
(e) Helium gas: Used for kinetic enery discrimination interference removal from cobalt
isotopes.
(i) Connect gas cylinder to helium filter system, then connect the filter system to the
UCT gas inlet channel and set delivery pressure per Table 1 in Appendix C. See Section
Section 5.E for part numbers and details.
(ii) Ensure NexION control software settings match the UCT gas channel setup.
(f) Oxygen (99.999+%) gas: Used for dynamic reaction cell interference removal from
cadmium and manganese isotopes.
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(i) Connect the gas cylinder to the UCT gas inlet channel and set delivery pressure per
Table 1 in Appendix C. See Section Section 5.E for part numbers and details.
(ii) Ensure NexION control software settings match the UCT gas channel setup.
(g) BioUCell: Upgrade the universal cell technology (UCT) to a BioUCell from
PerkinElmer (No catalog number. Ask for product information from the PerkinElmer
service representatives who do repair calls and preventive maintenance visits).
1) Hardware setup: Setup syringes (10.0 mL of left, 1.0 mL on right), a 12 gauge Concorde
CT probe dispense tip, the Microlab cable management system, a foot pedal, and PEEK
valves.
2) Flushing: It is necessary to flush the diluter prior to use so that the diluter does not
contaminate the processed samples with the elements tested by this method. Method
validation experience identified the syringes and valves are the primary components of
concern for contamination. The elements most frequently impacted by this
contamination include manganese and lead.
(a) Initial setup: Initial rinsing (e.g., a new diluter or new diluter components) typically
involves flushing with 2%-5% (v/v) nitric acid for ~10 L with constant checking. This
process may take a couple of days. One technique that could help is to fill the syringes
to full with the 2%-5% (v/v) nitric acid and leave them for a few hours.
(b) Daily preparation:
(i) Flushing: At the beginning of each day of use, the rinsing typically required is
between 6-10 priming cycles with the sample diluent that will be used for the day.
(ii) Tip rinse: Best cleanliness is observed when the tip is rinsed with concentrated
nitric acid prior to use for dilution preparations. Dip the delivery tip deep into a tube
(e.g., 15mL polypropylene) of concentrated nitric acid and take up the concentrated
nitric acid into the delivery tip as if preparing a patient urine sample dilution (see
Table 8 in Appendix C for volume settings). Dispense the acid into the waste
container while rinsing the exterior of the delivery tip with water from a squirt bottle
and flush tip with 1-2 dispense cycles. This step can be repeated periodically
throughout the sample preparation to prevent urine matrix from adhering to the
exterior surface of the delivery tip.
(iii) Background check: Due to the critical importance of avoiding contamination,
before each use of the diluter test background levels of method elements in water
(same used in blank preparations), diluent before it is pumped through the diluter
and diluent after it is pumped through the diluter. Background levels will very based
on water source and sensitivity of instrument used, so it is best to compare against
historical performance and the difference between blank levels and low calibrator
levels.
(c) Troubleshooting: Over time, contamination can get worse with some diluters,
especially for manganese. When rinsing takes so long that it prevents timely starting of
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the analysis we observed changing one (especially the left one) or both valves on the
diluter typically resolves the issue. The syringes can also be replaced, when necessary.
B. Parameters for Instrument and Method:
See Tables and Figures in Appendix C for a complete listing of the instrument and method
parameters and software screen shots.
8. The run: quality, execution, evaluation, and reporting
A. Bench QC, reference materials and calibration verification:
B. Perform, evaluate and report a run:
1) Power on the computer, printer, and autosampler, and instrument computer

controller.
2) Peristaltic pump: Set proper tension on peristaltic pump tubing.
3) Software: Start software for the ICP-MS and autosampler control.
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4) Daily pre-ignition maintenance checks: Perform and document daily maintenance

checks (e.g., Ar supply pressure, interface components cleanliness and positioning,
interface pump oil condition, vacuum pressure, etc.).
5) Place probe in adequate volume of carrier or rinse solution: If using an ESI FAST,
manually place carrier probe into carrier solution. If not, send the autosampler probe to a
rinse solution (e.g. autosampler rinse station).
6) Start the plasma
7) Start the peristaltic pump: Start the pump running slowly, making sure that the
rotational direction is correct for the way the tubing is set up.
8) Warm-up time: Allow warm-up time suggested by the manufacturer for the ICP-MS
(e.g. RF generator) after igniting the plasma. There will be another warm-up time (or
“stability time”) for the UCT later in this procedure.
9) Daily performance check: Perform and document a daily performance check and any
optimizations necessary. Save new parameters to the “default.tun” and “default.dac”
files.
10) UCT Stability time: Best analyte-to-internal standard ratio stability is typically
observed after 1-1.5 hours of analysis of urine samples using the DRC/KED mode method
(~12 measurements of the 15 element panel). Prepare 50mL+ of a calibrator (e.g.
standard 2) to be analyzed repeatedly before the beginning of the run to achieve a stable
analyte-to-internal standard ratio. Time to reach stability is instrument-specific and
learned from performance of runs. See Table 7 in Appendix C for example of setup in the
Samples / Batch window and Table 8 in Appendix C for details of making a working
standard.
11) Readying the instrument for quick-start analysis: Leave the plasma running to
eliminate the need for an initial instrument warm-up period and / or a UCT stabilization
period as long as appropriate planning is made for sufficient solution supply and waste
collection. Analysis of conditioning samples (diluted urine matrix) can also be scheduled
to occur at roughly a predetermined time. Accomplish this by setting up multiple sample
analyses with extended rinse times (e.g. one 15 element analysis with a 1400s rinse time
will take approximately 30 minutes to complete). Initial samples would be non-matrix,
while final samples would be diluted matrix for conditioning. If running a UCT-only
method during these scheduled analyses, the ICP-MS will remain in DRC or KED mode for
approximately 45 minutes without depressurizing the cell.
12) Software setup for Analysis: Verify & set up the correct files and data directories for
your analysis (See Table 1 in Appendix C for defaults). Update the software to reflect the
current sample set. Use a bar code scanner to input data whenever possible. See Table 1
in Appendix C for times and speeds. There are two method files for this one method (see
Table 1 in Appendix C). It is necessary to use both to accomplish each run because the
current PerkinElmer software will not allow for more than one blank per method file. The
ONLY DIFFERENCE between these two files is on the Sampling tab where one lists the
autosampler positions of the urine blank and urine calibrators (the “urblk” method file)
and the other lists the autosampler position of the aqueous blank (the “aqblk” method
file). The ONLY TIME when it matters which of these files is used is when the
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measurement action includes “Run blank” or “Run standards”. When the measurement
action is only ‘run sample’, it does not matter whether the “urblk” or “aqblk” method file
is used. Analysts typically follow the pattern below, however, for the sake of consistency
and as a reminder of which blank must be used for which type of sample. See Table 7 in
Appendix C. Use to analyze the initial urine blank (blank for the calibration curve), the
urine calibrators, and the urine blank checks at the very beginning of the run. The urine
blank method defines the autosampler location of the urine blank and the urine
calibrators. The “aqblk” method file must be used to analyze all QC materials and patient
samples. The aqueous blank method defines the aqueous blank in autosampler location.
1) Thaw urine samples; allow them to reach ambient temperature.

2) Flush the Hamilton dual syringe diluter (See Section 7.ii.2) for details).
3) Prepare the following solutions into pre-labeled containers benchtop automatic
pipette or other volumetric sample transfer device. See Table 8 in Appendix C for a
summary. Prepare samples in the cleanest environment available to prevent trace
element contamination and an environment which provides personnel protection (e.g.
Class II, Type A/B3 biological safety cabinet).
(a) Aqueous Blank: Prepare at least two aqueous blanks. One will be the actual reagent
blank for patient and QC samples and the other will be a backup (“Aqueous Blank
Check”) in case the original aqueous blank is unusable.
(b) Calibrators: Prepare the working calibrators (S0-S5). Prepare S0 in triplicate. One of
these S0 preparations will be the zero standard (urine blank) for the calibrators; the
other two will be analyzed twice after the last calibrator to collect run blank data that
can be used to verify and document washout after the calibrators.
(c) Patient & QC Samples: Before taking an aliquot for analysis, homogenize the
sample (e.g. vortex for 3-5 seconds, or invert 5-10 times). After preparation, mix and
cover diluted samples. Place prepared dilutions on the autosampler of the ICP-MS in
the order corresponding to the sequence setup in the ICP-MS software. Ambient
temperature storage of original samples for the work day is acceptable.
1) Verify proper operation of the instrument (proper loop filling, sample reaching
nebulizer in correct timing, autosampler arm moving properly, etc . . .)
2) Verify that background signal from instrument and reagents are low. Helpful checks
when diagnosing high background problems include:
(a) Water (≥ 18 Mohm∙cm) to be used in Aq Blank Checks and dilutions.
(b) Diluent before and after being flushed through the benchtop automatic pipette. If
contamination is observed from the pipette, repeat the flushing steps described in
Section 7.ii.2).
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(c) Comparison with other instruments.

3) Verify analyte / internal standard ratio stability: The net intensity (analyte / internal
standard ratio) of the measurements made while stabilizing the UCT can be evaluated to
determine the readiness of the system to begin analysis. Continual trending in this ratio
indicates that unwanted instrument drift will occur within the run.
4) Evaluate the Axial Field Voltage (AFV) optimized value. Monitor the change between S0
and S5 for measured intensities (cps) of the internal standard iridium in DRC mode. If the
percent difference between the iridium intensities is greater than 5% (especially if greater
in S5), then run the axial field voltage optimization. See Section 6.f.ii for preparation of
optimization solutions.
5) Verify calibration curves meet R2 requirements (minimum of 0.98, typically 0.99 to
1.000).
6) Verify bench QC results are within the acceptable limits. If an analyte result for the
beginning QC material(s) falls outside of the ± 3SD limits, then the steps below are
recommended. If these steps do not result in correction of the out-of-control values for
QC materials, consult the supervisor for other appropriate corrective actions.
(a) Evaluate the blank results.
(b) Evaluate the reproducibility of the 3 replicates within the measurements.
(c) Evaluate the consistency of the internal standard across the measurements (esp.
the calibrators).
(d) Evaluate calibration curves. If a particular calibrator is obviously in error, it can be
re-analyzed as a sample (old or new dilution) and incorporated into the curve through
data reprocessing as a calibrator. As a last resort, a single calibration point per analyte
between and including S2 and S4 can be removed from the curve. Follow up on
repeated problems with calibrators with appropriate corrective actions (e.g. re-
preparation of intermediate working standards or troubleshooting instrument
parameters).
(e) Prepare a fresh dilution of the failing QC material (same vial) and reanalyze it to see
if the QC dilution was not properly made.
(f) Prepare a fresh dilution of the failing QC material (unused vial) and analyze it to see
if the QC vial had become compromised.
(g) Prepare and analyze new working calibrators.
(h) Test a different preparation of intermediate working calibration standards.
7) Verify good precision among replicates of each measurement.
8) Verify consistent measured intensities of the internal standards. Some sample-to-
sample variations are to be expected, however, intensities drifting continuously in one
direction resulting in failing results for ending QC indicate the instrument needs
additional pre-conditioning before the run or environmental conditions are changing too
much around the instrument.
9) Verify elevated patient results. Refer to Figure 19 in Appendix C for flowchart.
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(a) Confirming an elevated concentration: Repeat for confirmation any sample having
a concentration greater than the 1UB threshold. See Table 10 in Appendix C.
(b) Dilution of a sample to within the calibration range: Repeat in duplicate with extra
dilution any sample having a concentration greater than the highest calibrator to bring
the observed result within the concentration range of the calibrators. See Table 9 of
Appendix C for high calibrator concentrations and validated extra dilutions.
(c) Confirming proper washout after an elevated sample: When monitoring the
analysis in real-time, if an observed sample concentration is greater than the highest
concentration tested for washout (see Table 10 in Appendix C), do the following to
verify that the run is still in control for low concentration samples before proceeding
with analysis.
(i) Stop run following elevated sample
(ii) Verify that the run is still in control for lower concentration samples before
proceeding with analysis. Analyze 2 urine blank checks followed by a low bench QC
washout check. If the low bench QC wash check is not in control (within ± 3SD limits),
repeat these 3 check samples until washout is verified before proceeding with
analysis.
Example:
3018 UrBlkChk Wash1
3018 UrBlkChk Wash2
LUXXXXX Wash
(iii) If the run is not verified in-contol for low concentration samples before the next
samples are analyzed, see Section 8.b.vii.2. for directions.
(d) Overnight operation or using auto stop: Ensure sufficient solution supply and waste
collection during unattended operation. Turn on the AutoStop feature of the ICP-MS
software. Delay the shutdown at least 10 minutes (use peristaltic pump speed
approximately that of the method wash) to rinse the sample introduction system of
urine matrix before turning off the plasma. It will be necessary to replace the sample
peristaltic pump tubing the next day since it will have been clamped shut overnight.
Enable AutoStop in on the Run List window. Select “Batch Completed” for Stop
Criteria.
1) Electronic records: Transfer data electronically to the laboratory information system.

When keyboard entry must be used, proofread transcribed data after entry.
(a) Export data from the ICP-MS software using “original conditions” or files and
folders used during the analysis. Use descriptive report filenames (e.g. 2005-
0714a_group55.txt). In the Syngistix software under “Report Format” (see Figure 9 in
Appendix C) choose the “Use Separator” option, and under the “File Write” Section
choose “Append.”
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(b) Move the generated .TXT data file to the appropriate subdirectory on the network
drive where exported data are stored prior to import to the laboratory information
management system.
(c) Import the instrument file into the laboratory information system with appropriate
documentation (e.g. instrument ID, analyst, calibration standards lot number, and run
or sample specific comments).
(i) Paper records: Run sheets must be documented with
a. Analyst initials
b. Instrument ID
c. Date of analysis and run # for the day
1) Rules for bench quality control evaluation: The following are the CDC DLS QC rules for
two QC pools per run with two or more QC results per pool.
(a) If both QC run means are within 2Sm limits and individual results are within 2Si
limits, then accept the run.
(b) If one of the two QC run means is outside a 2Sm limit - reject run if:
(i) Extreme Outlier – Run mean is beyond the characterization mean ± 4Sm
(ii) 3S Rule - Run mean is outside a 3Sm limit
(iii) 2S Rule – Two or more of the run means are outside the same 2Sm limit
(iv) 10 X-bar Rule – Current and previous 9 run means are on same side of the
characterization mean
1. If one of the 4 QC individual results is outside a 2Si limit - reject run in the cases
stated below. Note: Since runs have multiple results per pool for 2 pools, the R 4S
rule is applied within runs only. Si = Standard deviation of individual results. Sm =
Standard deviation of the run means. Sw = Within-run standard deviation.
2. Extreme Outlier – One individual result is beyond the characterization mean ± 4Si
3. R 4S Rule – Within-run ranges for all pools in the same run exceed 4Sw (i.e., 95%
range limit)
(c) Implications of QC failures: If the DLS SAS program declares the run “out of control”
for any analyte, use the following to determine the implications on usability of the
data from the run.
(i) 13 – 15 elements in the run
1. 1, 2 or 3 analytes “out of control”: ONLY the analytes which were “out of
control” are invalid for reporting from the run.
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2. 4 or more analytes “out of control”: All results, regardless of analyte, are invalid
for reporting from the run.
(ii) 4 – 12 elements in the run
1. 1 or 2 analytes “out of control”: ONLY the analytes which were “out of control”
are invalid for reporting from the run.
(iii) 3 elements in the run
1. 1 analyte “out of control”: ONLY the analyte which was “out of control” is invalid
(iv) 1 – 2 elements in the run: ONLY the analyte which was “out of control” is invalid
1) Elevated concentrations: Refer to Figure 19 in Appendix C for flowchart.

(a) Results greater than the first upper boundary (1UB): Confirm by repeat analysis of
a new sample preparation concentrations observed greater than the “first upper
boundary” (defined in the laboratory database as the “1UB”). Report the first
analytically valid result, as long as the confirmation is within 10%. Continue repeat
analysis until a concentration can be confirmed.
(b) Results greater than the second upper boundary (2UB): Report any patient results
confirmed to be greater than the second upper boundary (2UB) as an “elevated
result”.
(c) Results greater than highest calibrator: Samples that exceed the high calibrator
must be prepared with minimum extra dilution in duplicate to bring the observed
result within the calibration range (≤ S5). Report the first analytically valid result (i.e.
the first one within the calibration range), as long as the confirmation is within 10%.
Continue repeat analysis until a concentration can be confirmed.
(d) Concentrations requiring verification of washout: Following a result greater than
the highest concentrations tested for washout (see Table 10 of Appendix C) do the
following:
(i) If the run was determined to be in-control for low concentration samples before
the next samples were analyzed, no further action is required.
(ii) If the run was not determined to be in-control for low concentration samples
before the next samples were analyzed confirm by re-analysis the results for the 2
samples immediately following the elevated sample. Report the results if they
confirm the initial results within ±10% or ±3SD of the low bench QC, whichever is
greater.
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2) Unacceptable reproducibility: If the range of the three replicate readings (maximum

replicate concentration value - minimum replicate concentration value) for a single
sample analysis is greater than the range maximum criteria listed in Table 10 in Appendix
C and the range of the three replicate readings is greater than 10% of the observed
concentration, do not use the measurement for reporting. Repeat the analysis of the
sample.
9. Routine equipment maintenance and data backups

A. Equipment maintenance:
Analysts are expected to regularly evaluate the need for, and when necessary perform,
cleaning, replacement, or re-positioning of components in ICP-MS the sample
introduction system, interface, ion optics region, and equipment required resources (e.g.
autosampler, exhaust, compressed gases, and coolant). Frequency of equipment
maintenance will be dependent on instrument throughput. Maintenance activities will be
documented in the instrument logbook.
B. UCT optimizations:
UCT conditions (cell gas flow rate and RPq value) can be verified by analyzing the UCT
optimization solutions (see Section 6.K) as needed to ensure proper reduction of potential
ICP-MS interferences.
C. Data backup:
Data on the instrument computer will be backed up via two backup routines. Files used
and produced by the ICP-MS in analyzing samples will be backed up and kept a minimum
of three years after analysis.
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10. Reporting thresholds

A. Reportable range of test results:
Urine element concentrations are reportable in the range between the method LOD and
the high calibrator times the maximum permitted extra dilution (see Table 9 of Appendix
C). Above the high calibrator, extra dilutions are made of the urine sample to bring the
observed concentration within the calibration range.
B. Reference Range (normal range):
In this method the 95% reference ranges (see Table 11 in Appendix C) for these elements
in urine fall within the range of the calibrators.
C. Action Levels:
Due to the uncertainty of the health implications of elevated concentrations of many of
the elements determined with this method, there is no routine notification for elevated
levels of every analyte determined with this method. The present NRC standard for
workplace removal is 15 µg/L of U in urine [13]. Other action levels for reporting to
supervising physicians are determined on a study-by-study basis.
11. Method calculations

A. Method limit of detection (LOD):
The method detection limits for elements in urine specimens are defined as 3 times S 0,
where S 0 is the estimate of the standard deviation at zero analyte concentration. S 0 is
taken as the y-intercept of a linear or 2nd order polynomial regression of standard
deviation versus concentration (4 concentration levels of the analytes in urine each
measured 60 times across at least a 2-month timeframe). Method LODs are re-evaluated
periodically.
B. Method limit of quantitation (LOQ):
The Division of Laboratory Sciences does not currently utilize limits of quantitation in
regards to reporting limits [12].
C. QC limits:
Before QC materials can be used in the QC process, they quality control limits are
calculated based on concentration results obtained in at least 20 separate runs. It is
preferable to perform separate analyses on separate days and using multiple calibrator lot
numbers, instruments, and analysts to best mimic real-life variability. The statistical
calculations are performed using the SAS program developed for the Division of
Laboratory Sciences.
12. Alternate methods for performing test and storing specimens if test system
fails:
If the analytical system fails, setup analysis on other ICP-MS instrument, if available. If no
other instrument is available, store the specimens at ≤ -20 °C until the analytical system
can be restored to functionality.
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13. Method Performance Documentation

Method performance documentation for this method including accuracy, precision,
sensitivity, specificity and stability is provided in Appendix A of this method
documentation. The signatures of the branch chief and director of the Division of
Laboratory Sciences on the first page of this procedure denote that the method
performance is fit for the intended use of the method.
14. Summary Statistics and QC Graph

Please see following pages.
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2019-2020 Summary Statistics and QC Chart

URXUSB (Antimony, urine (ug/L))
Start End Standard Coefficient of

Lot N Date Date Mean Deviation Variation
5200 87 30JUL19 21AUG20 4.4083 0.1097 2.5
5199 87 30JUL19 21AUG20 0.1642 0.0093 5.7
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URXUBA (Barium, urine (ug/L))

5200 88 30JUL19 21AUG20 13.3332 0.2419 1.8
5199 88 30JUL19 21AUG20 1.4909 0.0363 2.4
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URXUCD (Cadmium, urine (ug/L))

5200 90 30JUL19 21AUG20 6.0246 0.1764 2.9
5199 90 30JUL19 21AUG20 0.2221 0.0207 9.3
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URXUCS (Cesium, urine (ug/L))

5200 92 30JUL19 25AUG20 13.4666 0.2356 1.7
5199 92 30JUL19 25AUG20 3.9417 0.0675 1.7
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URXUCO (Cobalt, urine (ug/L))

5200 91 30JUL19 21AUG20 4.2033 0.0951 2.3
5199 91 30JUL19 21AUG20 0.2926 0.0130 4.5
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URXUPB (Lead, urine (ug/L))

5200 85 30JUL19 21AUG20 6.6813 0.0945 1.4
5199 85 30JUL19 21AUG20 0.4366 0.0134 3.1
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URXUMN (Manganese, urine (ug/L))

5200 88 30JUL19 21AUG20 6.9036 0.1712 2.5
5199 88 30JUL19 21AUG20 4.8772 0.1308 2.7
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URXUMO (Molybdenum, urine (ug/L))

5200 94 30JUL19 25AUG20 114.585 1.055 0.9
5199 94 30JUL19 25AUG20 42.891 0.441 1.0
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URXUTL (Thallium, urine (ug/L))

5200 87 30JUL19 21AUG20 2.4653 0.0377 1.5
5199 87 30JUL19 21AUG20 0.1736 0.0043 2.5
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URXUSN (Tin, urine (ug/L))

5200 92 30JUL19 24AUG20 19.804 1.050 5.3
5199 92 30JUL19 24AUG20 1.590 0.090 5.7
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URXUSR (Strontium, urine (ug/L))

5200 88 30JUL19 24AUG20 449.424 12.785 2.8
5199 88 30JUL19 24AUG20 82.246 1.705 2.1
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URXUTU (Tungsten, urine (ug/L))

5200 86 30JUL19 21AUG20 3.9264 0.0532 1.4
5199 86 30JUL19 21AUG20 0.2227 0.0056 2.5
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URXUUR (Uranium, urine (ug/L))

5200 89 30JUL19 21AUG20 0.40075 0.01573 3.9
5199 89 30JUL19 21AUG20 0.01694 0.00085 5.0
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15. References
1. Thomas, R., Practical guide to ICP-MS: a tutorial for beginners. Third ed. 2013,
New York, New York: Marcel Dekker. 336.
2. Tanner, S.D., Baranov, Vladimir I, Theory, Design, and Operation of a Dynamic
Reaction Cell for ICP-MS. Atomic Spectroscopy, 1999. 20(2): p. 45-52.
3. Tanner, S.D., V.I. Baranov, and D.R. Bandura, Reaction cells and collision cells
for ICP-MS: a tutorial review. Spectrochimica Acta Part B-Atomic Spectroscopy,
2002. 57(9): p. 1361-1452.
4. PerkinElmer SCIEX Instruments, ELAN DRC II Hardware Guide. 2001, Canada.
5. Caldwell, K.L., et al., Inductively coupled plasma mass spectrometry to measure
multiple toxic elements in urine in NHANES 1999-2000. Atomic Spectroscopy,
2005. 26(1): p. 1-7.
6. Jarrett, J.M., et al., Eliminating molybdenum oxide interference in urine cadmium
biomonitoring using ICP-DRC-MS. Journal of Analytical Atomic Spectrometry,
2008. 23(7): p. 962-967.
7. Seiler Hans G, Sigel Astrid, and Sigel Helmut, eds. Handbook on metals in
clinical and analytical chemistry. 1994, Marcel Dekker, Inc.: New York, New York.
8. Centers for Disease Control and Prevention, Fourth National Report on Human
Exposure to Environmental Chemicals, Updated Tables, January 2019, Volume
1. 2019, CDC: Atlanta, GA.
9. Tietz Fundamentals of Climical Chemistry and Molecular Diagnostics, C.A.
Burtis, D.E. Bruns, and B.G. Sawyer, Editors. 2015, W.B. Saunders Company:
Philidelphia, PA.
10. GE, A. Iodine supplementation markedly increases urinary excretion of fluoride
and bromide. 2003 [cited 2018 2/12/2018]; Available from:
http://www.naturallifeenergy.com/files/Iodine-removes-fluoride.pdf.
11. Rodushkin, I. and F.I. Ödman, Application of inductively coupled plasma sector
field mass spectrometry for elemental analysis of urine. Journal of trace elements
in medicine and biology, 2001. 14(4): p. 241-247.
12. Division of Laboratory Sciences, Division of Laboratory Sciences Policies and
Procedures Manual. 2017, version 6.0, Centers for Disease Control and
Prevention: Atlanta, GA.
13. U.S. Nuclear Regulatory Commission, Regulatory guide 8.22 (revision 1).
Bioassay at uranium mills. 1988: Atlanta, GA.
16. Appendix A. Method Performance Documentation

A. Accuracy
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Accuracy compared to Reference Material

Mean concentration should be within ±15% of the nominal value except at 3*LOD, where it should be within ± 20%
Method name: Urine Multi-Element ICP-UCT-MS

Method #: 3018
Matrix: Urine
Units: µg/L
Reference material: SRM 2668 L1, SRM 2668 L2 10x dilution, SRM 2668 L2 4x dilution
Analyte: antimony
Measured concentration
Reference Nominal Difference from
Replicate Day 1 Day 2 Day 3 Day 4 Day 5 Mean SD CV (%)
material value nominal value (%)
Level 1 1 0.225 0.233 0.248 0.233 0.235
0.242 0.23 0.01 3.77 -4.7
2 0.221 0.225 0.229 0.219 0.238
Level 2 1 2.16 2.11 2.11 2.13 2.18
2.24 2.15 0.03 1.35 -3.8
2 2.17 2.15 2.17 2.17 2.19
Level 3 1 5.56 5.16 5.65 5.43 5.49
5.6 5.47 0.18 3.21 -2.2
2 5.53 5.17 5.64 5.50 5.60

Method #: 3018
Matrix: Urine
Units: µg/L
Reference material: SRM 2668 L1 2x dilution, SRM 2668 L1, SRM 2668 L2 20x dilution
Analyte: barium
Level 1 1 0.920 0.950 1.03 0.900 0.976
0.98 0.96 0.05 4.84 -2.3
2 0.910 0.960 1.03 0.924 0.975
Level 2 1 1.86 1.97 2.56 1.90 1.95
1.96 2.0 0.21 10.83 0.4
2 1.85 1.88 1.96 1.86 1.88
Level 3 1 12.5 12.4 12.4 12.1 12.8
13 12.5 0.25 2.05 -4.2
2 12.5 12.3 12.5 12.2 12.9
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Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: beryllium
Level 1 1 0.536 0.514 0.520 0.525 0.563
0.54 0.53 0.02 4.42 -1.9
2 0.522 0.508 0.500 0.538 0.574
Level 2 1 1.10 1.08 1.06 1.09 1.09
1.07 1.09 0.02 1.59 1.4
2 1.11 1.05 1.08 1.10 1.09
Level 3 1 5.54 5.22 5.06 5.38 5.66
5.5 5.42 0.21 3.87 -1.4
2 5.51 5.31 5.26 5.57 5.72


Method #: 3018
Matrix: Urine
Units: µg/L
Reference material: SRM 2668 L1 2x dilution, SRM 2668 L1, NYDOH Wadsworth TEU PT sample UE17-07
Analyte: cadmium
Level 1 1 0.536 0.550 0.539 0.569 0.511
0.53 0.53 0.02 3.89 0.7
2 0.555 0.527 0.510 0.533 0.506
Level 2 1 1.03 1.07 1.05 1.13 1.05
1.06 1.06 0.03 3.22 0.1
2 1.08 1.09 1.05 1.04 1.01
Level 3 1 3.75 3.88 3.89 4.01 3.78
3.8 3.81 0.10 2.61 0.3
2 3.76 3.75 3.81 3.65 3.85
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Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: cesium
Level 1 1 2.51 2.50 2.48 2.51 2.58
2.45 2.51 0.04 1.48 2.6
2 2.47 2.48 2.50 2.54 2.57
Level 2 1 4.99 4.97 5.01 5.01 4.99
4.9 4.98 0.05 1.09 1.7
2 4.98 4.89 5.10 4.98 4.94
Level 3 1 11.5 10.8 11.4 10.8 11.4
11.05 11.16 0.33 2.95 1.0
2 11.4 10.8 11.4 10.8 11.4


Method #: 3018
Matrix: Urine
Units: µg/L
Reference material: Seronorm Trace Elements in Urine L_ lot 1403080 2x dilution, SRM 2668 L2 40x dilution, SRM 2668 L2
10x dilution
Analyte: cobalt
Level 1 1 0.395 0.416 0.398 0.396 0.424
0.4 0.41 0.01 2.60 2.0
2 0.396 0.415 0.413 0.416 0.411
Level 2 1 1.28 1.22 1.27 1.34 1.34
1.3 1.30 0.05 3.76 -0.2
2 1.26 1.26 1.29 1.35 1.37
Level 3 1 5.25 5.15 5.00 4.97 5.46
5.2 5.18 0.16 3.16 -0.3
2 5.20 5.14 5.14 5.08 5.45
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Method #: 3018
Matrix: Urine
Units: µg/L
Reference material: SRM 2668 L1 2x dilution, SRM 2668 L1, NYDOH Wadsworth TEU PT sample UE17-07
Analyte: lead
Level 1 1 0.611 0.600 0.810 0.593 0.617
0.617 0.64 0.08 13.15 4.5
2 0.611 0.600 0.799 0.594 0.610
Level 2 1 1.24 1.20 1.60 1.24 1.28
1.234 1.27 0.12 9.31 2.8
2 1.23 1.19 1.23 1.23 1.25
Level 3 1 6.07 6.13 6.32 6.30 6.19
6 6.18 0.12 1.93 3.0
2 5.93 6.14 6.25 6.28 6.18


Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: manganese
Level 1 1 0.537 0.570 0.746 0.457 0.556
0.54 0.58 0.10 17.27 7.3
2 0.540 0.590 0.760 0.479 0.557
Level 2 1 1.18 1.11 1.59 1.20 1.24
1.08 1.23 0.13 10.83 13.9
2 1.17 1.16 1.17 1.24 1.24
Level 3 1 4.91 4.94 4.79 4.62 4.83
4.76 4.82 0.11 2.35 1.2
2 4.85 4.85 4.90 4.62 4.87
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Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: molybdenum
Level 1 1 24.6 25.3 25.8 24.1 24.7
25.8 24.90 0.60 2.40 -3.5
2 24.4 25.0 25.9 24.4 24.8
Level 2 1 50.2 49.7 52.7 49.9 50.3
51.6 50.19 1.07 2.13 -2.7
2 49.4 49.4 51.0 48.9 50.4
Level 3 1 168 165 163 162 169
168.7 165.91 2.29 1.38 -1.7
2 165 166 166 165 169


Method #: 3018
Matrix: Urine
Units: µg/L
Reference material: NYDOH Wadsworth TEU PT sample UE17-07, SRM 2668 L1 2x dilution, SRM 2668 L1
Analyte: platinum
Level 1 1 0.293 0.295 0.304 0.368 0.300
0.29 0.31 0.03 8.84 6.7
2 0.273 0.305 0.310 0.345 0.300
Level 2 1 0.527 0.624 0.639 0.344 0.384
0.52 0.50 0.13 25.00 -3.7
2 0.518 0.622 0.622 0.346 0.382
Level 3 1 0.917 1.217 1.250 0.812 1.190
1.04 1.07 0.19 17.81 3.3
2 0.904 1.217 1.260 0.798 1.180
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Method #: 3018
Matrix: Urine
Units: µg/L
Reference material: Seronorm Trace Elements in Urine L1 2x dilution, NYDOH Wadsworth TEU PT samples UE17-08 and
UE17-07
Analyte: strontium
Level 1 1 53.7 53.2 53.4 53.3 53.2
59.5 53.43 0.48 0.89 -10.2
2 54.5 53.8 53.1 52.9 53.1
Level 2 1 176 180 211 205 175
196 191.07 16.00 8.37 -2.5
2 183 182 213 208 178
Level 3 1 473 491 485 521 501
470 493.32 18.22 3.69 5.0
2 461 493 491 517 501


Method #: 3018
Matrix: Urine
Units: µg/L
Reference material: NYDOH Wadsworth TEU PT sample UE17-07, SRM 2668 L1, SRM 2668 L2 10x dilution
Analyte: tin
Level 1 1 0.908 0.940 0.888 1.01 1.01
0.85 0.94 0.05 5.76 11.1
2 0.901 0.930 0.867 1.01 0.983
Level 2 1 2.19 1.76 1.77 2.40 2.27
1.69 1.94 0.25 12.77 14.6
2 1.79 1.80 1.81 1.75 1.83
Level 3 1 15.5 15.4 15.5 15.8 16.1
17.1 15.79 0.35 2.25 -7.7
2 15.3 15.8 15.9 16.5 15.9
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Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: thallium
Level 1 1 0.350 0.355 0.362 0.352 0.359
0.3595 0.35 0.01 2.02 -2.3
2 0.338 0.352 0.351 0.342 0.350
Level 2 1 0.723 0.687 0.730 0.729 0.742
0.719 0.72 0.02 2.56 0.1
2 0.716 0.695 0.738 0.706 0.731
Level 3 1 2.75 2.63 2.83 2.97 2.69
2.88 2.79 0.14 4.85 -3.2
2 2.77 2.69 2.89 3.02 2.63


Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: tungsten
Level 1 1 0.586 0.593 0.608 0.583 0.594
0.626 0.59 0.01 1.47 -5.8
2 0.581 0.582 0.591 0.598 0.583
Level 2 1 1.22 1.19 1.23 1.23 1.22
1.252 1.21 0.02 1.65 -3.1
2 1.19 1.19 1.23 1.24 1.20
Level 3 1 3.08 2.90 3.10 3.01 3.13
3.125 3.05 0.08 2.74 -2.5
2 3.03 2.96 3.14 2.98 3.13
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Method #: 3018
Matrix: Urine
Units: µg/L
Reference material: SRM 2668 L1, NYDOH Wadsworth TEU PT sample UE17-08, SRM 2668 L2 40x dilution
Analyte: uranium
Level 1 1 0.0320 0.0355 0.0320 0.0349 0.0302
0.034 0.033 0.002 6.68 -4.1
2 0.0314 0.0360 0.0326 0.0318 0.0296
Level 2 1 0.154 0.174 0.155 0.152 0.133
0.15 0.153 0.013 8.73 2.0
2 0.156 0.170 0.154 0.152 0.131
Level 3 1 0.319 0.317 0.311 0.299 0.276
0.33 0.302 0.016 5.39 -9.6
2 0.299 0.321 0.308 0.296 0.276
61 of 138
Metals - Urine
NHANES 2019-2020
B. Precision
Precision
Total relative standard deviation should be ≤ 15% (CV ≤ 15%)

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: antimony
Quality material 1
Run Result 1 Result 2 Mean SS 1 SS 2 2*mean^2
1 0.172 0.164 0.168 1.521E-05 1.521E-05 0.05658248
2 0.165 0.187 0.176 0.00012321 0.00012321 0.061952
3 0.153 0.161 0.157 1.89225E-05 1.89225E-05 0.049329405
4 0.171 0.164 0.168 1.26025E-05 1.26025E-05 0.056213045
5 0.214 0.210 0.212 3.24E-06 3.24E-06 0.08997282
6 0.175 0.173 0.174 1.21E-06 1.21E-06 0.06048242
7 0.166 0.160 0.163 1.156E-05 1.156E-05 0.053138
8 0.180 0.189 0.184 1.936E-05 1.936E-05 0.06785928
9 0.160 0.158 0.159 9.025E-07 9.025E-07 0.050593805
10 0.150 0.184 0.167 0.000289 0.000289 0.055778
Grand sum 3.4563 Grand mean 0.172815
Rel Std Dev

Sum squares Mean Sq Error Std Dev (%)
Within Run 0.000990435 9.90435E-05 0.00995206 5.76
Between Run 0.00460077 0.000511197 0.014355369 8.31
Total 0.005591205 0.017467688 10.11
Quality material 2
1 4.65 4.61 4.63 0.00037636 0.00037636 42.95161928
2 4.41 4.35 4.38 0.000921123 0.000921123 38.34164881
3 4.48 4.56 4.52 0.001521 0.001521 40.90963058
4 4.46 4.51 4.49 0.000689063 0.000689062 40.27800505
5 4.32 4.33 4.33 2.401E-05 2.401E-05 37.41644018
6 4.39 4.37 4.38 4.9E-05 4.9E-05 38.3688
7 4.38 4.16 4.27 0.011739722 0.011739722 36.47690285
8 4.69 4.71 4.70 0.000172923 0.000172922 44.19974221
9 4.58 4.48 4.53 0.00216225 0.00216225 41.01824738
10 4.47 4.65 4.56 0.008037122 0.008037122 41.54981641
Sum squares Mean Sq Error Std Dev Rel Std Dev

Within Run 0.051385145 0.005138514 0.071683433 1.60
Between Run 0.342049081 0.038005453 0.128193094 2.86
Total 0.393434226 0.146874041 3.28
62 of 138
Metals - Urine
NHANES 2019-2020
Precision

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: barium
Quality material 1
1 1.50 1.51 1.50 2.401E-05 2.401E-05 4.50660242
2 1.53 1.51 1.52 6.80625E-05 6.80625E-05 4.616241125
3 1.50 1.51 1.50 4.624E-05 4.624E-05 4.51320968
4 1.54 1.53 1.54 2.25625E-05 2.25625E-05 4.731810845
5 1.51 1.50 1.50 1.19025E-05 1.19025E-05 4.509304805
6 1.50 1.63 1.56 0.00423801 0.00423801 4.87469088
7 1.52 1.43 1.48 0.002129822 0.002129823 4.363353405
8 1.46 1.53 1.49 0.001306822 0.001306823 4.468555125
9 1.47 1.44 1.46 0.00016384 0.00016384 4.23928962
10 1.46 1.50 1.48 0.000366723 0.000366723 4.385833445
Rel Std Dev

Within Run 0.01675599 0.001675599 0.040934081 2.72
Between Run 0.01668655 0.001854061 0.009446219 0.63
Total 0.03344254 0.04200988 2.79
Quality material 2
1 13.2 13.3 13.27 0.001751422 0.001751423 352.321167
2 13.2 13.5 13.33 0.018496 0.018496 355.2231888
3 13.7 14.0 13.86 0.012825563 0.012825562 384.3073156
4 13.5 13.6 13.57 0.003404722 0.003404723 368.1188378
5 13.4 13.4 13.37 1.681E-05 1.681E-05 357.3961537
6 13.5 13.6 13.52 0.001685103 0.001685103 365.4915734
7 13.2 12.9 13.09 0.026520123 0.026520122 342.437067
8 13.5 13.8 13.62 0.021272222 0.021272223 370.8317611
9 13.4 13.1 13.26 0.02461761 0.02461761 351.915144
10 13.2 13.3 13.27 0.00373321 0.00373321 352.2813505

Within Run 0.22864557 0.022864557 0.151210307 1.13
Between Run 0.912711108 0.101412345 0.198176422 1.48
Total 1.141356678 0.249275854 1.86
63 of 138
Metals - Urine
NHANES 2019-2020
Precision

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: beryllium
Quality material 1
1 0.405 0.419 0.412 5.329E-05 5.329E-05 0.33932322
2 0.410 0.432 0.421 0.000119902 0.000119903 0.353724605
3 0.434 0.425 0.429 2.025E-05 0.00002025 0.36842528
4 0.436 0.422 0.429 5.041E-05 5.041E-05 0.36791042
5 0.428 0.426 0.427 8.1E-07 8.1E-07 0.36414578
6 0.428 0.430 0.429 9.025E-07 9.025E-07 0.368511125
7 0.418 0.406 0.412 3.721E-05 3.721E-05 0.33915848
8 0.439 0.446 0.442 1.156E-05 1.156E-05 0.39090482
9 0.418 0.400 0.409 8.01025E-05 8.01025E-05 0.334807445
10 0.413 0.432 0.423 9.31225E-05 9.31225E-05 0.357097005
Rel Std Dev

Within Run 0.00093512 9.3512E-05 0.00967016 2.28
Between Run 0.001874098 0.000208233 0.007573675 1.79
Total 0.002809218 0.012283019 2.90
Quality material 2
1 7.11 7.05 7.08 0.00081796 0.00081796 100.196168
2 7.11 7.30 7.20 0.00877969 0.00877969 103.7404888
3 7.26 7.47 7.37 0.01104601 0.01104601 108.5571655
4 7.16 7.20 7.18 0.000438902 0.000438903 103.0631602
5 7.35 7.39 7.37 0.00032041 0.00032041 108.6750759
6 7.37 7.46 7.41 0.002002563 0.002002562 109.8354668
7 7.08 7.12 7.10 0.000378302 0.000378302 100.7845031
8 7.30 7.69 7.50 0.03810304 0.03810304 112.3860289
9 7.15 7.20 7.18 0.000522123 0.000522123 103.0200934
10 7.05 7.39 7.22 0.030397922 0.030397923 104.2697964

Within Run 0.185613845 0.018561385 0.136240172 1.88
Between Run 0.359975064 0.039997229 0.103527399 1.43
Total 0.545588909 0.171111972 2.36
64 of 138
Metals - Urine
NHANES 2019-2020
Precision

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: cadmium
Quality material 1
1 0.243 0.215 0.229 0.00021 0.00021 0.10479
2 0.207 0.211 0.209 0.00000 0.00000 0.08740
3 0.208 0.209 0.21 0.00000 0.00000 0.08686
4 0.234 0.200 0.22 0.00030 0.00030 0.09422
5 0.251 0.230 0.24 0.00010 0.00010 0.11568
6 0.210 0.240 0.23 0.00023 0.00023 0.10161
7 0.220 0.188 0.204 0.00025 0.00025 0.08303
8 0.266 0.248 0.257 0.00008 0.00008 0.13205
9 0.240 0.237 0.239 0.00000 0.00000 0.11405
10 0.212 0.243 0.227 0.00025 0.00025 0.10342
Rel Std Dev

Within Run 0.00284592 0.000284592 0.016869855 7.48
Between Run 0.005027012 0.000558557 0.01170395 5.19
Total 0.007872932 0.020532278 9.10
Quality material 2
1 5.91 6.02 5.97 0.00304704 0.00304704 71.20779122
2 5.99 6.01 6.00 6.48025E-05 6.48025E-05 71.98440085
3 6.05 6.06 6.05 5.929E-05 5.929E-05 73.30425362
4 5.90 6.22 6.06 0.025520062 0.025520063 73.49447561
5 5.65 5.68 5.67 0.000220523 0.000220523 64.28759441
6 6.10 6.15 6.12 0.000490622 0.000490622 74.99083045
7 6.03 5.95 5.99 0.00139876 0.00139876 71.72905538
8 6.17 6.19 6.18 7.744E-05 7.744E-05 76.41693938
9 5.55 5.68 5.61 0.003950123 0.003950123 62.99245525
10 5.83 5.91 5.87 0.001604002 0.001604003 68.91027805

Within Run 0.07286533 0.007286533 0.085361191 1.43
Between Run 0.620566222 0.068951802 0.17559224 2.95
Total 0.693431552 0.195241306 3.28
65 of 138
Metals - Urine
NHANES 2019-2020
Precision

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: cesium
Quality material 1
1 3.92 3.96 3.94 0.000347823 0.000347823 31.06217381
2 3.95 4.06 4.01 0.003136 0.003136 32.12171552
3 4.06 4.05 4.06 4.356E-05 4.356E-05 32.91525248
4 4.11 4.09 4.10 2.97025E-05 2.97025E-05 33.62574025
5 3.97 4.00 3.99 0.00019881 0.00019881 31.82264642
6 4.01 4.05 4.03 0.00039204 0.00039204 32.45923592
7 3.96 3.79 3.87 0.007370223 0.007370222 30.01962613
8 4.04 4.24 4.14 0.01030225 0.01030225 34.30901448
9 3.90 3.89 3.90 5.476E-05 5.476E-05 30.34672418
10 3.93 3.96 3.94 0.00019044 0.00019044 31.12289408
Rel Std Dev

Within Run 0.044131215 0.004413121 0.066431329 1.66
Between Run 0.13533797 0.015037552 0.072884946 1.82
Total 0.179469185 0.098617123 2.47
Quality material 2
1 13.3 13.4 13.4 0.000945563 0.000945562 356.7521161
2 13.6 13.8 13.7 0.01447209 0.01447209 375.4238413
3 13.9 14.0 13.9 0.004064063 0.004064063 388.5942298
4 13.9 14.0 13.9 0.00295936 0.00295936 387.5216641
5 13.6 13.6 13.6 0.00024336 0.00024336 368.9197171
6 13.8 13.8 13.8 5.041E-05 5.041E-05 381.6973981
7 13.2 12.8 13.0 0.04016016 0.04016016 340.0414733
8 14.0 14.3 14.2 0.035344 0.035344 400.671432
9 13.5 13.3 13.4 0.00579121 0.00579121 358.3753464
10 13.3 13.6 13.5 0.022967403 0.022967403 362.0444496

Within Run 0.253995235 0.025399524 0.15937228 1.17
Between Run 2.019866835 0.224429648 0.31546008 2.31
Total 2.27386207 0.353432576 2.59
66 of 138
Metals - Urine
NHANES 2019-2020
Precision

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: cobalt
Quality material 1
1 0.306 0.303 0.304 2.7225E-06 2.7225E-06 0.185257845
2 0.279 0.282 0.281 1.8225E-06 1.8225E-06 0.157641125
3 0.301 0.318 0.31 7.14025E-05 7.14025E-05 0.191394845
4 0.271 0.301 0.29 0.000217563 0.000217563 0.163306125
5 0.287 0.272 0.28 5.329E-05 5.329E-05 0.1562405
6 0.295 0.286 0.29 2.16225E-05 2.16225E-05 0.168838605
7 0.288 0.298 0.29 2.601E-05 2.601E-05 0.17181522
8 0.299 0.316 0.31 6.80625E-05 6.80625E-05 0.189174005
9 0.305 0.323 0.31 7.65625E-05 7.65625E-05 0.196878125
10 0.298 0.288 0.29 2.704E-05 2.704E-05 0.17146368
Rel Std Dev

Within Run 0.001132195 0.00011322 0.010640465 3.60
Between Run 0.002707975 0.000300886 0.009686758 3.28
Total 0.00384017 0.014389329 4.87
Quality material 2
1 4.20 4.27 4.23 0.001369 0.001369 35.86875602
2 4.30 4.35 4.32 0.000663063 0.000663062 37.33948945
3 4.26 4.24 4.25 7.14025E-05 7.14025E-05 36.10035421
4 4.31 4.34 4.32 0.00026244 0.00026244 37.34553888
5 4.24 4.27 4.26 0.00015376 0.00015376 36.22366728
6 4.16 4.23 4.19 0.00125316 0.00125316 35.15746658
7 4.12 4.04 4.08 0.00123201 0.00123201 33.2928
8 4.20 4.33 4.26 0.004375823 0.004375822 36.36595045
9 4.13 4.20 4.17 0.001207562 0.001207562 34.74028013
10 4.22 4.27 4.24 0.00061504 0.00061504 35.9976125

Within Run 0.02240652 0.002240652 0.047335526 1.12
Between Run 0.093226168 0.010358463 0.063709541 1.51
Total 0.115632688 0.079369752 1.88
67 of 138
Metals - Urine
NHANES 2019-2020
Precision

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: lead
Quality material 1
1 0.413 0.437 0.425 0.000144 0.000144 0.36108002
2 0.487 0.434 0.460 0.000715563 0.000715563 0.423660125
3 0.408 0.417 0.413 1.89225E-05 1.89225E-05 0.340560045
4 0.434 0.434 0.434 1.225E-07 1.225E-07 0.376625205
5 0.445 0.437 0.441 1.64025E-05 1.64025E-05 0.388873805
6 0.432 0.471 0.452 0.00038416 0.00038416 0.40788512
7 0.434 0.434 0.434 1E-08 1E-08 0.37688562
8 0.427 0.426 0.427 1.6E-07 1.6E-07 0.3638045
9 0.457 0.427 0.442 0.000226502 0.000226503 0.391347045
10 0.426 0.430 0.428 3.4225E-06 3.4225E-06 0.366796125
Rel Std Dev

Within Run 0.00301853 0.000301853 0.017373917 3.99
Between Run 0.00344156 0.000382396 0.006345965 1.46
Total 0.00646009 0.018496602 4.25
Quality material 2
1 6.54 6.61 6.57 0.00121801 0.00121801 86.33505608
2 6.52 6.61 6.56 0.00232324 0.00232324 86.16956642
3 6.65 6.69 6.67 0.00025921 0.00025921 88.98313608
4 6.61 6.66 6.64 0.000657922 0.000657923 88.06635613
5 6.47 6.42 6.45 0.000540563 0.000540563 83.12632861
6 6.61 6.74 6.67 0.00405769 0.00405769 89.057858
7 6.66 6.80 6.73 0.005249002 0.005249002 90.60868345
8 6.77 6.78 6.78 3.78225E-05 3.78225E-05 91.81344541
9 6.62 6.66 6.64 0.000362903 0.000362903 88.16724841
10 6.57 6.75 6.66 0.00755161 0.00755161 88.68722562

Within Run 0.044515945 0.004451595 0.066720271 1.01
Between Run 0.153586484 0.017065165 0.079415271 1.20
Total 0.198102429 0.10372261 1.56
68 of 138
Metals - Urine
NHANES 2019-2020
Precision

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: manganese
Quality material 1
1 4.64 4.65 4.65 1.64025E-05 1.64025E-05 43.17156121
2 4.78 4.86 4.82 0.001685103 0.001685102 46.50626125
3 4.82 4.91 4.86 0.002194923 0.002194923 47.29073005
4 4.74 5.00 4.87 0.01640961 0.01640961 47.45133362
5 4.26 4.39 4.33 0.00389376 0.00389376 37.45105058
6 4.76 4.90 4.83 0.005234523 0.005234523 46.68581821
7 4.91 5.14 5.02 0.01343281 0.01343281 50.47512338
8 4.96 5.53 5.24 0.082685003 0.082685003 54.97285513
9 4.76 5.03 4.89 0.018920003 0.018920003 47.91323941
10 4.97 5.16 5.07 0.00833569 0.00833569 51.32668562
Rel Std Dev

Within Run 0.30561565 0.030561565 0.174818663 3.60
Between Run 1.097570678 0.121952298 0.213764745 4.40
Total 1.403186328 0.276146576 5.68
Quality material 2
1 6.73 6.80 6.76 0.001447803 0.001447803 91.50474481
2 6.81 6.88 6.84 0.00138384 0.00138384 93.65056082
3 6.90 6.95 6.93 0.000504003 0.000504003 95.91263501
4 6.80 7.14 6.97 0.029395103 0.029395103 97.08514513
5 6.17 6.38 6.28 0.01087849 0.01087849 78.75376002
6 6.84 7.04 6.94 0.00954529 0.00954529 96.39105858
7 6.98 7.42 7.20 0.04700224 0.04700224 103.6368045
8 7.11 7.77 7.44 0.10699441 0.10699441 110.7429149
9 6.75 7.96 7.36 0.36216324 0.36216324 108.2273569
10 7.11 7.36 7.23 0.015989603 0.015989603 104.616666

Within Run 1.17060804 0.117060804 0.342141497 4.89
Between Run 2.06104162 0.229004624 0.236583833 3.38
Total 3.23164966 0.415972011 5.95
69 of 138
Metals - Urine
NHANES 2019-2020
Precision

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: molybdenum
Quality material 1
1 44.1 44.1 44.1 1.5625E-06 1.5625E-06 3886.789295
2 42.6 42.3 42.4 0.019044 0.019044 3603.088138
3 43.1 43.8 43.4 0.096379203 0.096379202 3775.205414
4 43.2 43.0 43.1 0.015625 0.015625 3711.031861
5 42.8 42.7 42.8 0.00804609 0.00804609 3655.98005
6 43.3 43.7 43.5 0.041148122 0.041148123 3785.013317
7 43.2 41.5 42.4 0.698645223 0.698645223 3593.069698
8 42.8 43.9 43.4 0.267030562 0.267030563 3758.83516
9 43.4 43.4 43.4 6.4E-07 6.4E-07 3760.369986
10 43.5 43.6 43.5 0.0025 0.0025 3786.379433
Rel Std Dev

Within Run 2.296840805 0.229684081 0.47925367 1.11
Between Run 5.052863064 0.561429229 0.407274569 0.94
Total 7.349703869 0.628932949 1.46
Quality material 2
1 115 115 115 0.090150062 0.090150063 26382.58401
2 113 113 113 0.03952144 0.03952144 25500.67845
3 117 118 117 0.47045881 0.47045881 27481.99457
4 115 115 115 0.046246502 0.046246503 26566.16226
5 114 113 114 0.199943123 0.199943122 25955.00877
6 115 117 116 0.48650625 0.48650625 26940.68284
7 113 111 112 0.965404502 0.965404503 25228.89165
8 115 116 116 0.02439844 0.02439844 26720.61667
9 116 116 116 0.00044944 0.00044944 26994.74831
10 116 117 116 0.413899223 0.413899222 27018.89554

Within Run 5.473955585 0.547395558 0.739861851 0.64
Between Run 44.17485412 4.908317124 1.476638339 1.28
Total 49.64880971 1.651622336 1.44
70 of 138
Metals - Urine
NHANES 2019-2020
Precision

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: platinum
Quality material 1
1 0.157 0.163 0.160 9E-06 9E-06 0.05094432
2 0.160 0.157 0.159 1.96E-06 1.96E-06 0.05030792
3 0.153 0.159 0.156 7.84E-06 7.84E-06 0.04873442
4 0.157 0.157 0.157 1E-08 1E-08 0.04936082
5 0.152 0.154 0.153 8.1E-07 8.1E-07 0.04675682
6 0.156 0.154 0.155 8.1E-07 8.1E-07 0.04798802
7 0.156 0.151 0.154 7.84E-06 7.84E-06 0.0471245
8 0.160 0.161 0.161 3.6E-07 3.6E-07 0.05158472
9 0.158 0.150 0.154 1.681E-05 1.681E-05 0.04749362
10 0.162 0.153 0.157 2.16225E-05 2.16225E-05 0.049455125
Rel Std Dev

Within Run 0.000134125 1.34125E-05 0.003662308 2.34
Between Run 0.000124361 1.38178E-05 0.000450185 0.29
Total 0.000258486 0.003689874 2.36
Quality material 2
1 1.36 1.35 1.35 6.80625E-05 6.80625E-05 3.670695125
2 1.31 1.34 1.32 0.000235622 0.000235622 3.494574845
3 1.39 1.41 1.40 4.9E-05 4.9E-05 3.908808
4 1.31 1.29 1.30 4.55625E-05 4.55625E-05 3.382340405
5 1.33 1.34 1.33 6.084E-05 6.084E-05 3.55751138
6 1.31 1.32 1.31 6.76E-06 6.76E-06 3.45108992
7 1.32 1.31 1.31 2.209E-05 2.209E-05 3.44478752
8 1.37 1.37 1.37 3.025E-07 3.025E-07 3.746953125
9 1.31 1.30 1.30 2.304E-05 2.304E-05 3.38104008
10 1.31 1.33 1.32 0.000103022 0.000103023 3.488761125

Within Run 0.001228605 0.00012286 0.011084246 0.83
Between Run 0.018367964 0.002040885 0.030967922 2.32
Total 0.019596569 0.032891834 2.47
71 of 138
Metals - Urine
NHANES 2019-2020
Precision

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: strontium
Quality material 1
1 82.4 82.9 82.7 0.05827396 0.05827396 13667.73191
2 79.4 80.0 79.7 0.091839302 0.091839302 12705.12048
3 82.4 82.3 82.3 0.004809423 0.004809423 13554.46549
4 81.0 81.2 81.1 0.018157563 0.018157562 13150.77075
5 81.3 81.1 81.2 0.016991122 0.016991123 13188.8776
6 81.5 82.0 81.7 0.076701302 0.076701302 13362.80616
7 82.1 81.2 81.7 0.19598329 0.19598329 13334.00023
8 77.6 81.0 79.3 2.773057563 2.773057563 12576.13943
9 82.6 83.2 82.9 0.103265822 0.103265823 13749.97686
10 80.6 80.8 80.7 0.01249924 0.01249924 13024.33441
Rel Std Dev

Within Run 6.703157175 0.670315718 0.81872811 1.01
Between Run 25.62678391 2.847420435 1.043337126 1.28
Total 32.32994109 1.326223238 1.63
Quality material 2
1 440 441 441 0.01971216 0.01971216 388149.3973
2 438 442 440 5.180858822 5.180858823 387377.3403
3 463 475 469 36.91170025 36.91170025 439699.5345
4 467 475 471 15.31469956 15.31469956 444254.7323
5 459 464 461 5.49527364 5.49527364 425566.2263
6 451 462 456 30.26210121 30.26210121 416335.9725
7 465 470 467 6.777431222 6.777431223 437032.3742
8 447 458 453 28.33965225 28.33965225 409658.0369
9 456 463 459 12.16788806 12.16788806 421794.3971
10 452 461 457 22.49747192 22.49747192 417219.8407

Within Run 325.9335782 32.59335782 5.709059276 1.25
Between Run 2106.524048 234.0582275 10.03655493 2.19
Total 2432.457626 11.54667886 2.52
72 of 138
Metals - Urine
NHANES 2019-2020
Precision

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: tin
Quality material 1
1 1.57 1.53 1.55 0.000535923 0.000535923 4.800970845
2 1.60 1.59 1.59 2.25625E-05 2.25625E-05 5.063516645
3 1.39 1.23 1.31 0.00638401 0.00638401 3.442688
4 1.57 1.54 1.55 0.000211703 0.000211703 4.815235445
5 1.53 1.52 1.53 8.01025E-05 8.01025E-05 4.655826125
6 1.71 1.77 1.74 0.001020803 0.001020803 6.036770045
7 1.50 1.42 1.46 0.001365303 0.001365303 4.257653805
8 1.69 1.78 1.74 0.00170569 0.00170569 6.02878088
9 1.53 1.54 1.53 6.241E-05 6.241E-05 4.70508488
10 1.58 1.57 1.57 8.281E-05 8.281E-05 4.95936018
Rel Std Dev

Within Run 0.02294263 0.002294263 0.047898466 3.08
Between Run 0.27467865 0.03051985 0.118797279 7.63
Total 0.29762128 0.128090033 8.23
Quality material 2
1 19.2 19.0 19.1 0.009379922 0.009379922 726.3956701
2 19.2 19.4 19.3 0.00811801 0.00811801 743.2517235
3 20.7 19.7 20.2 0.27499536 0.27499536 816.5810369
4 19.4 19.6 19.5 0.00430336 0.00430336 759.6890163
5 19.3 19.0 19.2 0.02951524 0.02951524 733.751432
6 20.9 21.3 21.1 0.04235364 0.04235364 887.1398664
7 18.8 18.1 18.4 0.121138803 0.121138803 678.043995
8 20.4 20.9 20.7 0.044163022 0.044163022 853.6092211
9 19.3 19.0 19.1 0.016939023 0.016939023 732.9050694
10 19.0 19.5 19.3 0.06275025 0.06275025 744.648077

Within Run 1.22731326 0.122731326 0.35033031 1.79
Between Run 11.8779888 1.319776534 0.773642426 3.95
Total 13.10530206 0.849266701 4.34
73 of 138
Metals - Urine
NHANES 2019-2020
Precision

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: thallium
Quality material 1
1 0.176 0.178 0.177 1.69E-06 1.69E-06 0.06272882
2 0.169 0.166 0.168 1.96E-06 1.96E-06 0.05631368
3 0.172 0.174 0.173 0.000001 0.000001 0.05958152
4 0.172 0.167 0.169 4.2025E-06 4.2025E-06 0.057426605
5 0.167 0.166 0.167 6.25E-08 6.25E-08 0.055477805
6 0.174 0.179 0.177 7.84E-06 7.84E-06 0.06237512
7 0.177 0.171 0.174 8.41E-06 8.41E-06 0.06034338
8 0.181 0.182 0.182 3.6E-07 3.6E-07 0.0658845
9 0.177 0.179 0.178 1.69E-06 1.69E-06 0.06343922
10 0.175 0.167 0.171 1.64025E-05 1.64025E-05 0.058516205
Rel Std Dev

Within Run 0.000087235 8.7235E-06 0.002953557 1.70
Between Run 0.000423495 4.70549E-05 0.004377867 2.52
Total 0.00051073 0.005281025 3.04
Quality material 2
1 2.43 2.45 2.44 7.921E-05 7.921E-05 11.9072
2 2.42 2.44 2.43 5.329E-05 5.329E-05 11.79911042
3 2.47 2.48 2.47 4.761E-05 4.761E-05 12.24531072
4 2.40 2.39 2.39 3.54025E-05 3.54025E-05 11.44380641
5 2.43 2.41 2.42 5.776E-05 5.776E-05 11.6982845
6 2.48 2.51 2.49 0.000287303 0.000287303 12.43458581
7 2.43 2.47 2.45 0.000418202 0.000418202 12.04668613
8 2.47 2.49 2.48 8.37225E-05 8.37225E-05 12.27551701
9 2.44 2.45 2.45 7.056E-05 7.056E-05 11.95800608
10 2.45 2.51 2.48 0.00085849 0.00085849 12.310722

Within Run 0.0039831 0.00039831 0.019957705 0.81
Between Run 0.018263652 0.002029295 0.028556826 1.17
Total 0.022246752 0.034839666 1.42
74 of 138
Metals - Urine
NHANES 2019-2020
Precision

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: tungsten
Quality material 1
1 0.217 0.217 0.217 4E-08 4E-08 0.09409122
2 0.229 0.223 0.226 7.84E-06 7.84E-06 0.10206162
3 0.222 0.226 0.224 3.8025E-06 3.8025E-06 0.100217645
4 0.223 0.215 0.219 1.33225E-05 1.33225E-05 0.095878205
5 0.224 0.224 0.224 6.25E-08 6.25E-08 0.100128125
6 0.224 0.234 0.229 2.401E-05 2.401E-05 0.10460738
7 0.222 0.227 0.225 8.41E-06 8.41E-06 0.1008005
8 0.229 0.218 0.224 3.19225E-05 3.19225E-05 0.099949205
9 0.232 0.217 0.225 5.476E-05 5.476E-05 0.1008005
10 0.216 0.217 0.217 9E-08 9E-08 0.09383112
Rel Std Dev

Within Run 0.00028852 0.000028852 0.005371406 2.41
Between Run 0.000281552 3.12836E-05 0.001102623 0.50
Total 0.000570072 0.005483409 2.46
Quality material 2
1 3.83 3.87 3.85 0.00032041 0.00032041 29.60805152
2 3.89 3.96 3.92 0.001145823 0.001145823 30.80732513
3 4.03 4.06 4.04 0.00038809 0.00038809 32.72243202
4 3.91 3.99 3.95 0.001636202 0.001636203 31.25637113
5 3.96 3.99 3.98 0.000270603 0.000270602 31.62112813
6 3.89 3.97 3.93 0.00156816 0.00156816 30.9605805
7 3.91 3.89 3.90 0.00011881 0.00011881 30.43248128
8 3.93 3.99 3.96 0.00082369 0.00082369 31.410738
9 3.92 3.87 3.90 0.000529 0.000529 30.34516608
10 3.93 4.01 3.97 0.001652423 0.001652423 31.51306661

Within Run 0.01690642 0.001690642 0.041117417 1.04
Between Run 0.052449562 0.005827729 0.045481244 1.15
Total 0.069355982 0.061312197 1.56
75 of 138
Metals - Urine
NHANES 2019-2020
Precision

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: uranium
Quality material 1
1 0.0165 0.0175 0.0170 0.00000025 0.00000025 0.000578
2 0.0160 0.0174 0.0167 4.9E-07 4.9E-07 0.00055778
3 0.0175 0.0158 0.0167 7.225E-07 7.225E-07 0.000554445
4 0.0166 0.0159 0.0163 1.225E-07 1.225E-07 0.000528125
5 0.0164 0.0167 0.0166 2.25E-08 2.25E-08 0.000547805
6 0.0181 0.0185 0.0183 4E-08 4E-08 0.00066978
7 0.0165 0.0169 0.0167 4E-08 4E-08 0.00055778
8 0.0170 0.0183 0.0177 4.225E-07 4.225E-07 0.000623045
9 0.0164 0.0164 0.0164 0 0 0.00053792
10 0.0165 0.0168 0.0167 2.25E-08 2.25E-08 0.000554445
Rel Std Dev

Within Run 4.265E-06 4.265E-07 0.00065307 3.87
Between Run 7.0605E-06 7.845E-07 0.000423084 2.51
Total 1.13255E-05 0.000778139 4.61
Quality material 2
1 0.388 0.395 0.392 1.296E-05 1.296E-05 0.3065445
2 0.387 0.397 0.392 2.45025E-05 2.45025E-05 0.307720125
3 0.399 0.391 0.395 1.98025E-05 1.98025E-05 0.311971005
4 0.390 0.392 0.391 1.5625E-06 1.5625E-06 0.305683805
5 0.383 0.381 0.382 8.1E-07 8.1E-07 0.29138978
6 0.450 0.470 0.460 0.000101003 0.000101003 0.423292005
7 0.400 0.399 0.400 9E-08 9E-08 0.31936032
8 0.410 0.422 0.416 3.481E-05 3.481E-05 0.34594562
9 0.382 0.382 0.382 1.225E-07 1.225E-07 0.291618845
10 0.391 0.394 0.392 2.1025E-06 2.1025E-06 0.308034005

Within Run 0.00039553 0.000039553 0.006289118 1.57
Between Run 0.009639722 0.00107108 0.02271043 5.68
Total 0.010035252 0.023565157 5.89
76 of 138
Metals - Urine
NHANES 2019-2020
C. Stability
Stability
The initial measurement can be from the same day for all stability experiments.
Freeze and thaw stability = Assess for a minimum of 3 freeze-thaw cycles; conditions should mimic intended sample handling conditions
Describe condition: Three times frozen at ≤-70°C and then thawed (3 freeze-thaw cycles) to room temperature.
Bench-top stability = Assess short-term stability for length of time needed to handle study samples (typically at room temperature)
Describe condition: Original samples stored capped at room temperature for 1 day prior to preparation and analysis.
Processed sample stability = Assess short-term stability of processed samples, including resident time in autosampler
Describe condition: Processed samples (ready for instrument analysis) stored capped at room temperature for 1 day prior to analysis.
Long-term stability = Assess long-term stability that equals or exceeds time between date of first sample collection and date of last sample analysis
Describe condition: Samples stored at ≤-70°C for 2 years.
All stability sample results should be within ±15% of nominal concentration

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: antimony
Quality material 1
Initial Three freeze- Initial Bench-top Initial Processed Initial Long-term
measurement thaw cycles measurement stability measurement sample stability measurement stability
Replicate 1 0.159 0.170 0.155 0.171 0.169 0.168 0.178 0.160
Replicate 2 0.175 0.153 0.168 0.165 0.162 0.165 0.163 0.178
Replicate 3 0.156 0.174 0.165 0.173 0.159 0.168 0.152 0.167
Mean 0.1629 0.165733333 0.1627 0.1694 0.163333333 0.167176667 0.1643 0.1682

% difference from
-- 1.7 -- 4.1 -- 2.4 -- 2.4
initial measurement
Quality material 2
Replicate 1 4.36 4.49 4.38 4.40 4.49 4.48 0.621 0.572
Replicate 2 4.32 4.54 4.50 4.42 4.48 4.51 0.581 0.615
Replicate 3 4.36 4.57 4.43 4.41 4.49 4.49 0.578 0.606
Mean 4.348166667 4.534233333 4.4361 4.4102 4.486291 4.494525667 0.593316667 0.5978667

% difference from
-- 4.3 -- -0.6 -- 0.2 -- 0.8
initial measurement
77 of 138
Metals - Urine
NHANES 2019-2020
Stability

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: barium
Quality material 1
measurement thaw cycles measuremen stability measuremen sample measuremen stability
Replicate 1 1.54 1.56 1.52 1.50 1.50 1.51 1.28 1.24
Replicate 2 1.54 1.54 1.50 1.48 1.54 1.52 1.20 1.26
Replicate 3 1.55 1.53 1.53 1.46 1.46 1.51 1.15 1.26
Mean 1.544333333 1.544433333 1.519466667 1.4786333 1.4993 1.512152667 1.21 1.253333333

% difference from initial
-- 0.0 -- -2.7 -- 0.9 -- 3.6
measurement
Quality material 2
measurement thaw cycles measuremen stability measuremen sample measuremen stability
Replicate 1 13.9 13.9 13.4 13.2 13.6 13.6 6.62 6.54
Replicate 2 13.9 13.8 13.5 13.2 13.6 13.7 6.41 6.49
Replicate 3 13.9 13.9 13.4 13.1 13.4 13.5 6.38 6.32
Mean 13.88103333 13.84966667 13.4244 13.1541 13.55066667 13.593224 6.47 6.45

% difference from initial
-- -0.2 -- -2.0 -- 0.3 -- -0.3
measurement
78 of 138
Metals - Urine
NHANES 2019-2020
Stability

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: beryllium
Quality material 1
Replicate 1 0.410 0.415 0.425 0.422 0.446 0.451 0.357 0.381
Replicate 2 0.418 0.408 0.426 0.411 0.438 0.439 0.387 0.400
Replicate 3 0.419 0.428 0.428 0.402 0.412 0.429 0.374 0.404
Mean 0.4159 0.417033333 0.426333333 0.4117 0.432172667 0.439729333 0.372666667 0.395

% difference from
-- 0.3 -- -3.4 -- 1.7 -- 6.0
initial measurement
Quality material 2
Replicate 1 7.21 7.35 7.20 7.08 7.39 7.42 5.15 5.08
Replicate 2 7.36 7.32 7.37 7.14 7.41 7.32 5.01 5.05
Replicate 3 7.23 7.43 7.28 7.03 7.36 7.36 5.04 5.14
Mean 7.2679 7.367366667 7.282166667 7.0840667 7.388 7.363674667 5.066666667 5.09

% difference from
-- 1.4 -- -2.7 -- -0.3 -- 0.5
initial measurement
79 of 138
Metals - Urine
NHANES 2019-2020
Stability

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: cadmium
Quality material 1
Replicate 1 0.213 0.228 0.205 0.183 0.244 0.221 0.159 0.148
Replicate 2 0.229 0.215 0.216 0.193 0.238 0.227 0.168 0.158
Replicate 3 0.233 0.230 0.206 0.187 0.225 0.231 0.126 0.163
Mean 0.224766667 0.224033333 0.208866667 0.1876333 0.235674333 0.226079 0.150783333 0.1563

% difference from
-- -0.3 -- -10.2 -- -4.1 -- 3.7
initial measurement
Quality material 2
Replicate 1 5.97 6.13 6.05 5.95 6.08 5.81 1.45 1.53
Replicate 2 5.93 6.02 6.11 6.03 6.08 5.80 1.34 1.55
Replicate 3 5.98 6.17 6.04 6.00 6.18 5.83 1.56 1.58
Mean 5.9609 6.107466667 6.0673 5.9932667 6.115733333 5.812911667 1.4479 1.5531167

% difference from
-- 2.5 -- -1.2 -- -5.0 -- 7.3
initial measurement
80 of 138
Metals - Urine
NHANES 2019-2020
Stability

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: cesium
Quality material 1
Replicate 1 4.04 3.99 3.99 3.92 4.00 4.07 4.62 4.47
Replicate 2 4.03 4.02 3.98 3.92 3.98 4.00 4.46 4.46
Replicate 3 4.02 3.99 4.02 3.89 4.00 4.07 4.36 4.45
Mean 4.0291 3.997766667 3.995833333 3.9128 3.989866667 4.045862333 4.479483333 4.4607333

% difference from
-- -0.8 -- -2.1 -- 1.4 -- -0.4
initial measurement
Quality material 2
Replicate 1 13.7 13.6 13.6 13.4 13.5 13.9 12.9 12.3
Replicate 2 13.8 13.6 13.6 13.4 13.6 13.8 12.4 12.3
Replicate 3 13.8 13.7 13.5 13.4 13.4 13.8 12.1 12.1
Mean 13.74476667 13.63736667 13.5593 13.388767 13.499 13.83860167 12.49213333 12.217567

% difference from
-- -0.8 -- -1.3 -- 2.5 -- -2.2
initial measurement
81 of 138
Metals - Urine
NHANES 2019-2020
Stability

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: cobalt
Quality material 1
Replicate 1 0.430 0.442 0.434 0.444 0.290 0.277 0.548 0.487
Replicate 2 0.446 0.426 0.429 0.430 0.283 0.279 0.502 0.473
Replicate 3 0.433 0.435 0.437 0.448 0.299 0.284 0.471 0.481
Mean 0.436266667 0.434233333 0.433466667 0.4406333 0.290753333 0.279975667 0.507 0.4804333

% difference from
-- -0.5 -- 1.7 -- -3.7 -- -5.2
initial measurement
Quality material 2
Replicate 1 4.25 4.23 4.25 4.40 4.33 4.18 2.45 2.47
Replicate 2 4.27 4.23 4.22 4.46 4.29 4.19 2.42 2.44
Replicate 3 4.25 4.29 4.27 4.39 4.28 4.21 2.41 2.47
Mean 4.253533333 4.247933333 4.244766667 4.4142667 4.300316667 4.192304667 2.428116667 2.4589333

% difference from
-- -0.1 -- 4.0 -- -2.5 -- 1.3
initial measurement
82 of 138
Metals - Urine
NHANES 2019-2020
Stability

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: lead
Quality material 1
Replicate 1 0.425 0.438 0.446 0.442 0.449 0.449 0.408 0.387
Replicate 2 0.436 0.435 0.434 0.429 0.437 0.438 0.373 0.395
Replicate 3 0.427 0.437 0.444 0.424 0.439 0.439 0.401 0.402
Mean 0.429566667 0.436633333 0.4409 0.4317 0.441903 0.442067 0.394283333 0.39465

% difference from
-- 1.6 -- 0.5 -- 0.0 -- 0.1
initial measurement
Quality material 2
Replicate 1 6.42 6.59 6.57 6.52 6.78 6.84 2.82 2.85
Replicate 2 6.44 6.60 6.65 6.60 6.73 6.76 2.87 2.77
Replicate 3 6.48 6.57 6.60 6.54 6.73 6.85 2.87 2.81
Mean 6.450066667 6.588733333 6.605466667 6.5559 6.747133667 6.818445 2.850166667 2.8100333

% difference from
-- 2.1 -- -0.8 -- 1.1 -- -1.4
initial measurement
83 of 138
Metals - Urine
NHANES 2019-2020
Stability

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: manganese
Quality material 1
Replicate 1 5.92 6.14 5.02 4.53 5.05 4.83 0.670 0.767
Replicate 2 5.26 5.26 4.94 4.68 5.06 4.86 0.779 0.835
Replicate 3 5.04 5.16 5.08 4.87 4.97 4.84 0.720 0.741
Mean 5.4087 5.5198 5.010266667 4.694333333 5.027030333 4.840263 0.722716667 0.7809833

% difference from
-- 2.1 -- -6.3 -- -3.7 -- 8.1
initial measurement
Quality material 2
Replicate 1 7.16 7.17 7.09 6.62 7.11 6.80 2.84 2.98
Replicate 2 7.10 7.04 7.05 6.60 7.13 6.74 2.48 3.05
Replicate 3 7.27 7.06 7.06 6.63 7.18 6.77 3.47 2.82
Mean 7.175233333 7.092233333 7.067633333 6.618433333 7.1398 6.770702 2.92895 2.94785

% difference from
-- -1.2 -- -6.4 -- -5.2 -- 0.6
initial measurement
84 of 138
Metals - Urine
NHANES 2019-2020
Stability

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: molybdenum
Quality material 1
Replicate 1 43.3 44.1 44.3 44.4 44.0 43.9 36.6 39.1
Replicate 2 44.4 45.3 43.6 43.8 43.6 43.9 38.3 39.2
Replicate 3 43.4 44.7 44.4 43.5 43.7 43.7 36.7 40.1
Mean 43.67926667 44.68183333 44.13593333 43.908467 43.766426 43.81701333 37.22275 39.438933

% difference from
-- 2.3 -- -0.5 -- 0.1 -- 6.0
initial measurement
Quality material 2
Replicate 1 115 118 115 117 117 117 124 131
Replicate 2 115 118 117 118 117 116 129 132
Replicate 3 116 119 117 118 116 116 127 133
Mean 115.6496333 118.705 116.3135333 117.75673 116.5516927 116.5613597 126.6666667 132

% difference from
-- 2.6 -- 1.2 -- 0.0 -- 4.2
initial measurement
85 of 138
Metals - Urine
NHANES 2019-2020
Stability

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: platinum
Quality material 1
Replicate 1 0.158 0.159 0.174 0.168 0.163 0.174 0.086 0.100
Replicate 2 0.163 0.160 0.156 0.174 0.165 0.179 0.090 0.089
Replicate 3 0.156 0.159 0.163 0.165 0.162 0.169 0.120 0.091
Mean 0.1593 0.159233333 0.1644 0.1689 0.163121667 0.173892667 0.098666667 0.09333333

% difference from
-- 0.0 -- 2.7 -- 6.6 -- -5.4
initial measurement
Quality material 2
Replicate 1 1.31 1.33 1.33 1.38 1.37 1.47 0.840 0.770
Replicate 2 1.32 1.34 1.34 1.40 1.35 1.43 0.840 0.870
Replicate 3 1.33 1.36 1.36 1.41 1.34 1.47 0.960 1.100
Mean 1.322066667 1.345133333 1.344966667 1.39656667 1.351881 1.457321 0.88 0.91333333

% difference from
-- 1.7 -- 3.8 -- 7.8 -- 3.8
initial measurement
86 of 138
Metals - Urine
NHANES 2019-2020
Stability

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: strontium
Quality material 1
Replicate 1 82.4 84.6 84.3 83.6 80.3 81.5 74.0 78.9
Replicate 2 82.7 85.0 83.8 83.9 80.0 81.3 79.9 80.8
Replicate 3 82.3 85.1 84.8 83.3 79.9 80.8 79.3 84.2
Mean 82.46663333 84.88183333 84.31546667 83.601567 80.061069 81.21443467 77.72816667 81.317417

% difference from
-- 2.9 -- -0.8 -- 1.4 -- 4.6
initial measurement
Quality material 2
Replicate 1 439 447 443 446 484 502 151 160
Replicate 2 438 446 448 451 490 507 165 168
Replicate 3 438 450 445 448 481 507 165 171
Mean 438.0983333 447.3991667 445.5601333 448.31793 485.361542 505.4178297 160.3333333 166.33333

% difference from
-- 2.1 -- 0.6 -- 4.1 -- 3.7
initial measurement
87 of 138
Metals - Urine
NHANES 2019-2020
Stability
Long-term stability = Assess long-term stability that equals or exceeds time between date of first sample collection and date of last sample anal

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: tin
Quality material 1
measurement thaw cycles measurement stability measurement sample measurement stability
Replicate 1 1.66 1.76 1.67 1.67 1.78 1.80 2.43 2.34
Replicate 2 1.65 1.78 1.58 1.60 1.81 1.82 2.57 2.57
Replicate 3 1.70 1.78 1.61 1.60 1.78 1.81 2.33 2.75
Mean 1.670833333 1.774 1.621366667 1.6237667 1.792863 1.8084913 2.44375 2.5564167

% difference from
-- 6.2 -- 0.1 -- 0.9 -- 4.6
initial measurement
Quality material 2
measurement thaw cycles measurement stability measurement sample measurement stability
Replicate 1 20.6 22.1 19.6 20.1 19.7 21.4 15.1 14.7
Replicate 2 20.6 21.9 19.9 20.0 20.2 21.7 15.3 15.2
Replicate 3 20.9 22.2 19.7 19.8 20.1 21.5 14.7 15.1
Mean 20.6902 22.07023333 19.73306667 19.943367 20.00045233 21.554953 15.01686667 15.005433

% difference from
-- 6.7 -- 1.1 -- 7.8 -- -0.1
initial measurement
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Stability

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: thallium
Quality material 1
Replicate 1 0.164 0.179 0.158 0.176 0.177 0.167 0.176 0.169
Replicate 2 0.170 0.179 0.158 0.176 0.178 0.164 0.168 0.167
Replicate 3 0.166 0.185 0.166 0.175 0.176 0.166 0.173 0.173
Mean 0.166733333 0.180733333 0.160733333 0.1754333 0.177317 0.165768667 0.172116667 0.16955

% difference from
-- 8.4 -- 9.1 -- -6.5 -- -1.5
initial measurement
Quality material 2
Replicate 1 2.38 2.51 2.47 2.50 2.59 2.53 0.450 0.466
Replicate 2 2.38 2.50 2.56 2.55 2.54 2.54 0.464 0.459
Replicate 3 2.43 2.51 2.52 2.53 2.57 2.56 0.464 0.466
Mean 2.397 2.507466667 2.513033333 2.5271667 2.565997 2.54564 0.459566667 0.4635333

% difference from
-- 4.6 -- 0.6 -- -0.8 -- 0.9
initial measurement
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Stability

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: tungsten
Quality material 1
Replicate 1 0.225 0.230 0.237 0.231 0.230 0.235 0.118 0.146
Replicate 2 0.210 0.230 0.214 0.218 0.235 0.223 0.144 0.156
Replicate 3 0.220 0.235 0.229 0.236 0.237 0.221 0.167 0.168
Mean 0.218133333 0.2314 0.226233333 0.2280667 0.234200667 0.226324333 0.14275 0.1564833

% difference from
-- 6.1 -- 0.8 -- -3.4 -- 9.6
initial measurement
Quality material 2
Replicate 1 3.88 4.09 3.96 3.87 4.09 3.91 0.874 0.922
Replicate 2 3.91 4.06 4.05 3.92 4.02 3.89 0.890 0.932
Replicate 3 3.94 4.03 3.91 3.94 4.07 3.94 0.913 0.952
Mean 3.909266667 4.058066667 3.9719 3.9103333 4.059864333 3.910938 0.892316667 0.9350333

% difference from
-- 3.8 -- -1.6 -- -3.7 -- 4.8
initial measurement
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Stability

Method #: 3018
Matrix: Urine
Units: µg/L
Analyte: uranium
Quality material 1
Replicate 1 0.0170 0.0179 0.0164 0.0156 0.0174 0.0190 0.0175 0.0185
Replicate 2 0.0176 0.0197 0.0174 0.0164 0.0170 0.0182 0.0191 0.0178
Replicate 3 0.0168 0.0196 0.0163 0.0162 0.0164 0.0182 0.0180 0.0193
Mean 0.017133333 0.019066667 0.0167 0.0160667 0.016942333 0.018501333 0.018166667 0.0185333

% difference from
-- 11.3 -- -3.8 -- 9.2 -- 2.0
initial measurement
Quality material 2
Replicate 1 0.413 0.447 0.388 0.390 0.406 0.445 0.115 0.117
Replicate 2 0.409 0.448 0.396 0.392 0.411 0.455 0.123 0.117
Replicate 3 0.409 0.445 0.384 0.384 0.415 0.454 0.117 0.123
Mean 0.410033333 0.4464 0.389466667 0.3887 0.410969667 0.451063 0.118233333 0.1187167

% difference from
-- 8.9 -- -0.2 -- 9.8 -- 0.4
initial measurement
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D. Analytical Sensitivity and Specificity

LOD, specificity and fit for intended use
Method name: Multi-elements in urine by ICP-UCT-MS

Method #: 3018
Matrix: Urine
Units: µg/L
Interferences Accuracy, precision, LOD,

Limit of Detection successfully checked in specificity and stability meet
(LOD) at least 50 human performance specifications
Analytes samples for intended use
barium (Ba) 0.084 Yes Yes
beryllium (Be) 0.020 Yes Yes
cadmium (Cd) 0.055 Yes Yes
cobalt (Co) 0.024 Yes Yes
cesium (Cs) 0.13 Yes Yes
manganese (Mn) 0.068 Yes Yes
molybdenum (Mo) 0.45 Yes Yes
lead (Pb) 0.022 Yes Yes
platinum (Pt) 0.0063 Yes Yes
antimony (Sb) 0.018 Yes Yes
tin (Sn) 0.20 Yes Yes
strontium (Sr) 3.2 Yes Yes
thallium (Tl) 0.017 Yes Yes
tungsten (W) 0.015 Yes Yes
uranium (U) 0.0024 Yes Yes
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17. Appendix B. Ruggedness testing results

A. Ruggedness parameter Test #1: RF Power.
Ruggedness Table 1. Parameter test 1 (Ba, Be, Cd, Co). Impact of RF power changes on observed results.
ID RF power tested* Ba (µg/L) Be (µg/L) Cd (µg/L) Co (µg/L)
characterized mean 0.76 0.69 0.32 0.42

(±2SD range) (0.65 - 0.86) (0.59 - 0.79) (0.28 - 0.36) (0.38 - 0.47)
LU-04310_UMP3_e
1150W 0.67 0.62 0.28 0.39
1450W 0.70 0.66 0.31 0.32
1600W 0.75 0.75 0.33 0.42

(±2SD range) (4.54 - 5.24) (4.48 - 6.07) (1.47 - 1.78) (1.66 - 2.09)
HU-04311_UMP3_e
1150W 4.93 5.75 1.6 1.96
1450W 5.55 5.28 1.75 1.67
1600W 4.85 5.82 1.58 1.90
* Test performed 3/24/2010 by Denise Tevis using ELAN DRC-2N.
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Ruggedness Table 2. Parameter test 1 (Cs, Mo, Pb, Tl). Impact of RF power changes on observed results.
ID RF power tested* Cs (µg/L) Mo (µg/L) Pb (µg/L) Pt (µg/L)

(±2SD Range) (2.25 - 2.51) (18.6 - 20.0) (0.37 - 0.48) (0.07 - 0.13)
LU-04310_UMP_e
1150W 2.13 ¥ 17.2 ** 0.42 0.09
1450W 2.32 18.9 0.41 0.09
1600W 2.42 18.8 0.43 0.10
characterized mean 9.82 136 2.95 0.85

(±2SD Range) (9.03 - 10.6) (131 - 142) (2.82 - 3.08) (0.71 - 1.00)
HU-04311_UMP_e
1150W 9.62 136 3.03 0.93
1450W 10.56 133 2.89 1.02
1600W 9.55 135 3.05 1.08 #
* Test performed 3/23/2011 by Denise Tevis using ELAN DRC-2N. ¥ Low in one pool only and was within
expected precision of method from default setting result. ** Low result in one pool only (3SD range =
18.2 – 20.4). # Result at 1600W within expected precision of result at default method setting.
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Ruggedness Table 3. Parameter test 1 (Sb, Tl, W, U). Impact of RF power changes on observed results.
ID RF power tested* Sb (µg/L) Tl (µg/L) W (µg/L) U (µg/L)

(±2SD Range) (0.17 - 0.21) (0.17 - 0.19) (0.19 - 0.24) (0.011 - 0.016)
LU-04310_UMP_e
1150W 0.21 0.16 0.19 0.017 α
1450W 0.16 0.19 0.22 0.014
1600W 0.20 0.18 0.22 0.017 α

(±2SD Range) (0.60 - 0.71) (0.55 - 0.61) (0.90 - 0.99) (0.115 - 0.141)
HU-04311_UMP_e
1150W 0.69 0.59 0.90 0.153 α
1450W 0.61 0.57 0.93 0.126
1600W 0.66 0.60 0.91 0.150 α
* Test performed 3/23/2011 by Denise Tevis using ELAN DRC-2N. α Results within expected precision of
the method of result at default setting (3 SD).
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Ruggedness Table 4. Parameter test 1 (Mn, Sn, and Sr). Impact of RF power changes on observed results.
ID RF power tested* Mn (µg/L) Sn (µg/L) Sr (µg/L)
characterized mean 1.37 2.2

NYDOH UE09-05‡ (±2SD Range) (1.55 -1.19) (2.0-2.8)
1150W 1.22 2.9
1450W 0.98 2.8
1600W 1.30 3.0
characterized mean 31.1 61

(±2SD Range) (26.3 -35.9) (55.0 - 67.0)
NYDOH UE09-06‡
1150W 29.4 67.4
1450W 23.8 68.5
1600W 30.0 66.7
characterized mean 12.3 54.6 110

(±2SD Range) (10.9 - 13.7) (51.9 - 57.3) (104 -116)
Seronorm Trace
Elements Urine§
1150W 10.4 62.3 113
1450W 8.46 62.3 111
1600W 10.5 61.4 111
* Tests performed 3/23/2011 by Denise Tevis using ELAN DRC-2N. §Purchased from Sero AS, Billingstad,
Norway. ‡ Purchased from Wadsworth Center, New York State Department of Health
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B. Ruggedness parameter test #2: UCT mode cell gas flow rate.
Ruggedness Table 5. Parameter test 2 (Cd, Mn, Ir). Impact of cell gas flow rate changes on observed results.
Sample ID Cell gas flow rate (units) Mn (µg/L)

55 NYDOH target value (µg/L)
Low (0.88) 3.23
3.24
UE18-15 Normal (1.1) 3.25
(2.43 – 4.05)
High (1.32) 3.24
Sample ID Cell gas flow rate (units) 111
Cd (µg/L) NYDOH target value (µg/L)
Low (2.16) 4.48
4.42
UE18-12 Normal (2.4) 4.53
(3.42 – 5.42)
High (2.88) 4.82
Sample ID Cell gas flow rate (units) 59
Co (µg/L) NYDOH target value (µg/L)
Low (2.8) 1.69
1.73
UE18-12 Normal (3.5) 1.70
(0.23 – 3.23)
High (4.2) 1.72
* Results collected March 2019 on NexION 2000_B
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B. Ruggedness parameter test #3: UCT voltages.
Ruggedness Table 6. Parameter test 3 (Cd and Mn). Impact of DRC RPq changes on observed results.
Sample ID UCT condition (units) Mn (µg/L)

55 NYDOH target value (µg/L)
RPq reduced (0.6) 2.37
2.4
UE18-09 RPq normal (0.75) 2.04
(1.8 – 3.2)
RPq elevated (0.9) 1.99
111
Cd (µg/L)
RPq reduced (0.66) 5.38
5.23
UE18-09 RPq normal (0.82) 5.63
(4.23 – 6.23)
RPq elevated (0.9) 6.39
59
Co (µg/L)
KED reduced (2 V) 2.43
2.5
UE18-09 KED normal (3 V) 2.41
(1.0 – 4.0)
KED elevated (4 V) 2.42
* Results collected in March 2019 on NexION-K and NexION 2000_D
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C. Ruggedness parameter test #4: stability of sample preparations.
1. Three separate run sets (A, B, and C) were prepared at one sitting from the same
starting materials. Set ‘A’ was analyzed immediately per the assumption of the
method. Set’s ‘B’ and ‘C’ were stored at ambient temperature for 24 and 48
hours, respectively before analysis. “Junk urine samples (20) were analyzed
between the beginning and ending QC of each run, making each a normal length
run. All other method parameters were kept per method.
1) On day two, a fresh run set (“D”) was prepared and analyzed immediately for
comparison to results from set “B” (Run 2 of the day. Results not shown).
2) On day three, another fresh run set (“E”) was prepared and analyzed immediately for
comparison to results from set “C” (Run 2 of the day. Results not shown).
Ruggedness Table 7. Parameter test 4 (Ba, Be, Cd, Co). Stability of sample preparations.
time from preparation to
ID Ba (µg/L) Be (µg/L) Cd (µg/L) Co (µg/L)
analysis *
(±2SD range) (0.65 - 0.86) (0.59 - 0.79) (0.28 - 0.36) (0.38 - 0.47)
LU-04310_UMP3_e
freshly prepared 0.70 0.66 0.32 0.32
24 hours 0.70 0.69 0.31 0.42
48 hours 0.86 0.67 0.31 0.43

(±2SD range) (4.54 - 5.24) (4.48 - 6.07) (1.47 - 1.78) (1.66 - 2.09)
HU-04311_UMP3_e
24 hours 4.66 5.76 1.57 1.94
48 hours 5.12 5.49 1.67 1.84
* Test begun 3/23/11 by Denise Tevis using ELAN DRC-2N.
Ruggedness Table 8. Parameter test 4 (Cs, Mo, Pb, Pt, Sb, Tl, W, U). Stability of sample preparations.

ID Cs (µg/L) Mo (µg/L) Pb (µg/L) Pt (µg/L)
analysis
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LU-04310_UMP_e (±2SD range) (2.25 - 2.51) (18.6 - 20.0) (0.37 - 0.48) (0.07 - 0.13)

24 hours 2.35 19.2 0.44 0.11
48 hours 2.30 19.0 0.46 0.10
characterized mean 9.82 136 2.95 0.85
HU-04311_UMP_e
(±2SD range) (9.03 - 10.6) (131 - 142) (2.82 - 3.08) (0.71 - 1.00)
freshly prepared 10.6 133 2.89 1.02

24 hours 9.36 134 3.08 1.03
48 hours 10.0 132 3.04 1.12 *
ID Sb (µg/L) Tl (µg/L) W (µg/L) U (µg/L)
analysis
LU-04310_UMP_e
(±2SD range) (0.17 - 0.21) (0.17 - 0.19) (0.19 - 0.24) (0.011 - 0.016)

24 hours 0.19 0.18 0.21 0.013
48 hours 0.19 0.19 0.22 0.014
HU-04311_UMP_e
(±2SD range) (0.60 - 0.71) (0.55 - 0.61) (0.90 - 0.99) (0.115 - 0.141)

24 hours 0.65 0.60 0.90 0.128
48 hours 0.69 0.59 0.90 0.126
* Test begun 3/23/11 by Denise Tevis using ELAN DRC-2N. ** Results within expected precision of the method of
result at fresh preparation.
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Ruggedness Table 9. Parameter test 4 (Mn, Sn, Sr). Stability of sample preparations.
Parameter test 4 results (Table 3 of 3). All concentrations in µg/L.

ID Mn (µg/L) Sn (µg/L) Sr (µg/L)
analysis*
characterized mean 1.37 2.2
NYDOH UE09- NYDOH UE09-
(±2SD range) (1.55 -1.19) (2.0-2.8)

freshly prepared 0.98 2.8
05‡
24 hours 1.26 2.6

48 hours 1.47 2.6
characterized mean 31.1 61
(±2SD range) (26.3 -35.9) (55.0 - 67.0)
freshly prepared 23.8 68.5
06‡
24 hours 30.6 62.8

48 hours 31.9 61.4
characterized mean 12.3 54.6 110

Seronorm Trace
Elements Urine§
(±2SD range) (10.9 - 13.7) (51.9 - 57.3) (104 -116)

freshly prepared 8.47 62.3 111
24 hours 10.9 57.5 ** 112
48 hours 10.4 58.3 ** 114
* Test begun 3/23/11 by Denise Tevis using ELAN DRC-2N. §Purchased from Sero AS, Billingstad, Norway.
‡ Purchased from Wadsworth Center, New York State Department of Health. ** Results within expected
precision of the method of result at default setting
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D. Ruggedness parameter test #5: impact of extra dilutions.
Ruggedness Table 10. Parameter test 5. Impact of extra dilutions.
Ba Be Cd Co Cs Mn
initial conc (µg/L) 297 98 various 149 252 96
observed concentrations normalized to ‘no extra dilution’ result
no extra dilution 1.00 ± 0.02 1.00 ± 0.04 1.00 1.00 ± 0.02 1.00 ± 0.02 1.00 ± 0.03
2x dilution 1.00 ± 0.00 1.00 ± 0.01 1.06 ± 0.07 0.99 ± 0.01 0.99 ± 0.01 1.02 ± 0.01
4x dilution 1.09 ± 0.07
5x dilution 0.99 ± 0.00 1.01 ± 0.01 0.99 ± 0.00 0.98 ± 0.00 1.03 ± 0.01
10x dilution 0.98 ± 0.00 1.00 ± 0.01 1.09 ± 0.05 0.98 ± 0.00 0.97 ± 0.00 1.03 ± 0.00
20x dilution 0.97 ± 0.00 1.01 ± 0.00 1.11 ± 0.08 0.98 ± 0.00 0.97 ± 0.00 1.05 ± 0.00
Mo Pb Pt Sb Sn Sr
initial conc (µg/L) 1885 various** 137 98 325 1816
observed concentrations normalized to ‘no extra dilution’ result
no extra dilution 1.00 ± 0.02 1.00 1.00 ± 0.01 1.00 ± 0.02 1.00 ± 0.05 1.00 ± 0.03
2x dilution 0.97 ± 0.00 1.03 1.00 ± 0.01 1.00 ± 0.00 1.00 ± 0.02 0.92 ± 0.01
4x dilution 1.05
5x dilution 0.94 ± 0.00 1.09 0.99 ± 0.00 1.01 ± 0.00 1.00 ± 0.01 0.90 ± 0.00
10x dilution 0.92 ± 0.00 1.08 0.94 ± 0.00 1.00 ± 0.00 0.97 ± 0.01 0.88 ± 0.00
20x dilution 0.90 ± 0.00 1.09 0.89 ± 0.00 0.97 ± 0.00 0.95 ± 0.00 0.87 ± 0.00
Tl* U W
initial conc (µg/L) 25-115 43 99
observed concentrations
normalized to ‘no extra dilution’ result
no extra dilution 1.00 1.00 ± 0.06 1.00 ± 0.01
2x dilution 1.01 ± 0.01 1.00 ± 0.03 0.98 ± 0.01
5x dilution 1.04 ± 0.01 1.01 ± 0.01 0.96 ± 0.00
10x dilution 1.07 ± 0.01 1.01 ± 0.01 0.96 ± 0.00
20x dilution 1.09 ± 0.05 1.02 ± 0.00 0.95 ± 0.00
18. Appendix C
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Table 1. Instrument and method parameters.

Instrument: PerkinElmer NexION 300D/350D or NexION 2000 ICP-MS
Autosampler: ESI SC4 autosampler with FAST sample introduction system
Optimization (conditions) window parameters
RF power 1600W
plasma gas flow (Ar) 15 L/min
auxiliary gas flow (Ar) 1.2 L/min
nebulizer gas flow (Ar) ~0.90 – 1.0 L/min
(optimized as needed for sensitivity)
ion lens voltage(s) AutoLens (optimized as needed for sensitivity)
AFV, QRO, CRO, CPV, Optimized per instrument by service engineer, or advanced
discriminator threshold user.
Parameters of x-y alignment, nebulizer gas flow, AutoLens voltages, mass calibration, dual
detector calibration, and detector voltages are optimized regularly. Optimization file name =
default.dac.
Configurations window parameters
cell gas changes pause times Pressurize delay (From Standard to UCT mode) = 30
Exhaust delay (From UCT mode to Standard mode) = 30
Flow delay (gas changes while in UCT mode) = 30
Channel delay (channel change in UCT mode) = 30
File names & directories
Method file names CDC_DLS3018_15 element_urblk.mth
CDC_DLS3018_15 element_aqblk.mth
Dataset Create a new dataset subfolder each day. Name as “2011-
0718” for all work done on July 18, 2011
Sample file Create for each day’s work
Report file name See Figure 9 in Appendix C.
For sample results printouts
cdc_quant comprehensive.rop
For calibration curve information

CDC_Quant Comprehensive (calib curve info).rop
Tuning Default.tun
Optimization Default.dac
Calibration N/A
Polyatomic polyatomic.ply
Report options template CDC_Database Output.rop
(transferring results to the Report Format Options: select only “Use Separator”
database) File Write Option: Append
Report File name: include date, instrument, and group being
analyzed in file name (i.e. 2012-0311b_NexION-A_HM-
0364.txt)
Method parameters
Method parameters: timing page (see Figure 2 and Figure 3 and in Appendix C)
sweeps/reading 40
readings/replicate 1
replicates 3
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enable QC checking On
isotopes monitored Group 1 (use 103Rh as an internal standard)
and internal standard associations 9Be (9.0122), 88Sr (87.9056) ,98Mo (97.9055), 103Rh
(exact mass) (102.905), 118Sn (117.902), 121Sb (120.904), 133Cs (132.905),
138
Ba (137.905)
Group 2 (use 193Ir as an internal standard)

184
W (183.951), 193Ir (192.963), 195Pt (194.965), 205
Tl
(204.975), 208Pb (207.977), 238U (238.05)
Group 3 : (use 193Ir as an internal standard)

55
Mn (54.9381) and 193Ir (192.963)
Group 4: (use 193Ir as an internal standard)

Cd (110.904) and 193Ir (192.963)
111
Group 5: (use 103Rh as an internal standard)

59
Co (58.9332) and 103Rh (102.905)
3018 can be performed analyzing only a subset of analytes

and the appropriate internal standards.
dwell times 30 ms for 88Sr,98Mo, 118Sn,103Rh (vented mode and KED
mode), 121Sb, 133Cs, 138Ba, 184W, 193Ir (vented mode and DRC
mode), 205Tl, and 208Pb
100 ms for 9Be, 55Mn,, 111Cd, 195Pt, and 238U
150 ms for 59Co
scan mode Peak Hopping for all isotopes (1 MCA channel)
cobalt analysis UCT channel, gas NexION 300D/350D
(pressure), and gas flow rate • Channel B
• Helium (15 ± 5 psig delivery pressure)
• Typically 3.5 mL/min
NexION 2000
• Channels B or C
• Helium (25 ± 2 psig delivery pressure)
• Typically 3.5 “units” in the software (these channels
are pressure-flow controlled, not mass-flow controlled)
cadmium analysis UCT channel, NexION 300D/350D
gas (pressure), and gas flow rate • Channel B
• Oxygen (15 ± 5 psig delivery pressure)
• Typically 1.75 (1.4 – 2.1) mL/min
NexION 2000
• Channel B or C
• Typically 2.4 (2.16-2.88) “units” in the software (these
channels are pressure-flow controlled, not mass-flow
controlled)
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manganese analysis UCT channel, NexION 300D/350D

gas (pressure), and gas flow rate • Channel B
• Typically 0.8 (0.64 – 0.96) mL/min
NexION 2000
• Channel B or C
• Typically 1.1 (0.88 – 1.32) “units” in the software (these
channels are pressure-flow controlled, not mass-flow
controlled)
RPa 0 for all isotopes
RPq Standard Mode: 0.25 for all standard mode isotopes
KED mode: 0.25 for all KED mode isotopes
DRC Mode (Cd group): Default 0.82* for 111Cd and 193Ir.
Default 0.75* for 55Mn and 193Ir. Use the same RPq for each
element in a group.
(* Optimize per instrument, and periodically verified)
Method parameters: processing page (see Figure 4 in Appendix C)
detector mode Dual
process spectral peak N/A
Autolens On
isotope ratio mode Off
enable short settling time Off
blank subtraction After internal standard
measurement units cps
process signal profile N/A
Method parameters: equations page (see Figure 5 in Appendix C)

equations On 208Pb, use “+ Pb 206 + Pb 207”
On 238U, use “+ U 235”
Method parameters: calibration page (see Figure 6 in Appendix C)

calibration type external standard
curve type weighted linear
sample units “µg/L” or “ppb”
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calibration standard Be: 0.1, 0.3, 1, 3, 10

concentrations (µg/L) Sr: 6, 18, 60, 180, 600
Mo: 3, 9, 30, 90, 300
Sn: 0.3, 0.9, 3, 9, 30
Sb: 0.08, 0.24, 0.8, 2.4, 8
Cs: 0.2, 0.6, 2, 6, 20
Ba: 0.2, 0.6, 2, 6, 20
W: 0.06, 0.18, 0.6, 1.8, 6
Pt: 0.025, 0.075, 0.25, 0.75, 2.5
Tl: 0.04, 0.12, 0.4, 1.2, 4
Pb: 0.1, 0.3, 1, 3, 10
U: 0.005, 0.015, 0.05, 0.15, 0.5
Cd: 0.08, 0.24, 0.8, 2.4, 8
Mn: 0.1, 0.3, 1, 3, 10
Co: 0.075, 0.225, 0.75, 2.25, 7.5
Method parameters: sampling page (see Figure 7 and Figure 8 in Appendix C)

“peristaltic pump On
under computer control”
autosampler If using ESI autosampler
tray Autosampler Type: AS-93plus
port Tray Name: esi.try
sampling device Sampling Device: None
If using other autosampler

Refer to autosampler user guide.
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sample flush FAST defaults for all 15 elements

NexION 300 / 350
• 10s at 6 rpm (standard ICP-MS peristaltic pump)
• 10s at 3 rpm (ESI DXi peristaltic pump)
NexION 2000
• 10s at 17.3 rpm (ESI DXi peristaltic pump)
FAST defaults for a 3 element subset

NexION 300 / 350
• 3.5s at 6 rpm (standard ICP-MS peristaltic pump)
• 3.5s at 3 rpm (ESI DXi peristaltic pump)
NexION 2000
• 3.5s at 24 rpm (standard ICP-MS peristaltic pump)
• 3.5s at 17.3 rpm (ESI DXi peristaltic pump)
FAST defaults for a single element subset

NexION 300 / 350
NexION 2000
Can be optimized as needed to adequately fill the FAST loop.

As a matter of lab practice, set this time to equal the loop
fill time in the ESI FAST program. As long as the combined
time of sample flush + read delay is equal to the time
required for signal to reach stability, analytical
measurement will be good.
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read delay Default for all 15 elements or down to a 3 element subset

NexION 300 / 350
NexION 2000
Default for a single element subset

NexION 300 / 350
• 20s at 3rpm (ESI DXi peristaltic pump)
NexION 2000
Can be optimized as needed to reach signal stability before

beginning analysis. As a matter of lab practice, set this time
equal to the total time required for the signal to reach
stability minus the loop fill time. As long as the combined
time of sample flush + read delay is equal to the time
required for signal to reach stability, analytical
measurement will be good.
wash Default for all 15 elements or down to a 3 element subset
NexION 300 / 350
NexION 2000
Default for a single element subset

NexION 300 / 350
• 20s at 3rpm (ESI DXi peristaltic pump)
NexION 2000
Can be optimized to allow for changes in FAST loop rinsing

(must be greater than total time of steps in FAST program
after the initial “on rinse” command).
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extended wash For sample concentrations greater than these, setup the
(via ICP-MS software ICP-MS software’s ‘QC checking’ feature to “Wash for X and
QC checking) continue.” See Figure 10in Appendix C.
Analyte Conc. Extended Rinse Time

Be 300 µg/L 200s
Sr 18000 µg/L 200s
Mo 900 µg/L 200s
Sn 90 µg/L 200s
Sb 24 µg/L 200s
Cs 60 µg/L 200s
Ba 600 µg/L 200s
W 18 µg/L 200s
Pt 75 µg/L 200s
Tl 12 µg/L 200s
Pb 300 µg/L 200s
U 1.5 µg/L 200s
Cd 24 µg/L 200s
Mn 30 µg/L 200s
Co 225 µg/L 200s
autosampler locations of blanks For calibration curve (points to urine blank)
and standards CDC_DLS3018_15 element 5 calib_urblk.mth
By default (but can be customized), urine blank, 102;
calibration stds, 103-107.
For QC & patient sample (points to aqueous blank)

CDC_DLS3018_15 element 5 calib_aqblk.mth
By default (but can be customized), aqueous blank, 149.
FAST parameters: See Figure 11 through Figure 18 in Appendix C for details

configuration file default.sc
(saved at C:\Program Files\ESI\ESI-SC\
OR at C:\Users\Public\ESI\ESI SC)
FAST programs cdc_dls3018_15element_loop3.0ml_scfast_QCen.txt
others will be needed for different loop sizes and

subsets of elements
cdc_DLS3018_15element_3mL_SCFAST_noQCen.txt
used for NexION 2000
Potential emergency response modifications:
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Cadmium, cobalt, and manganese: These elements can be tested in vented mode when the
primary purpose is to identify acute exposures. Set DRC or
KED gas flow to 0, RPq to 0.25, and group the elements
with the vented mode analysis of the internal standard
typically used. Use information from Section 2 about
magnitude of interference that may be present in vented
mode during interpretation of results.
Non-FAST If the FAST sample introduction system is not available on
sample introduction system: any instruments, the method can still be implemented, but
these settings will need to be optimized in the ICP-MS
software (and ESI software, if present).
• Sample flush: Set so that solution reaches nebulizer.

• Read delay: Set for best reproducibility of replicate
measured intensities.
• Wash: Set to prevent significant carry-over from one
sample to the next.
• If using ESI autosampler without FAST, disable FAST in
the ESI software before running analysis.
Table 2. Suggested maximum analyte concentrations for base urine.

Analyte Concentration (µg/L)
Be 0.5
Co 0.25
Mo 30
Sb 0.2
Cs 3
Ba 2
W 0.2
Pt 0.25
Tl 0.2
Pb 0.75
U 0.03
Cd 0.25
Mn 0.1
Sr 80
Sn 3
Table 3. Multi-element stock standard concentrations.

stock calibration stock calibration
standard conc. (mg/L) standard conc. (mg/L)
High Purity Standards High Purity Standards

analyte
Item # SM-2107-037 Item # SM-2107-037
Solution A Solution B
(5% HNO 3 ) (5% HNO 3 , 1% HF, 0.5% HCl)

Be 200
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Co 150
Mo 6000
Sb 160
Cs 400
Ba 400
W 120
Pt 50
TI 80
Pb 200
U 10
Cd 160
Sr 12,000
Sn 600
Mn 200
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Table 4. Preparation of multi-element intermediate stock calibration standard.

volume of flask (mL) 100
volume of spike of
5
stock standard A (mL)*
volume of spike of
5
stock standard B (mL)*
concentrations (mg / L)
Be 10
Co 7.5
Mo 300
Sb 8
Cs 20
Ba 20
W 6
Pt 2.5
TI 4
Pb 10
U 0.5
Cd 8
Sr 600
Sn 30
Mn 10
*If preparing from HPS # SM-2107-037, both stock solutions A and B need to be spiked into
the flask
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Table 5. Preparation of multi-element intermediate working standards.

standard # 0 1 2 3 4 5
flask vol. (mL) 0 500 200 100 100 100
vol. spike of
int. stock std. 0 0.050 0.060 0.100 0.300 1.00
(mL)
concentrations (µg/L) ‡
1 3 10 30 100
Be 0
(0.1) ‡ (0.3) ‡ (1.0) ‡ (3.0) ‡ (10.0) ‡
0.75 2.25 7.5 22.5 75
Co 0
(0.075) ‡ (0.225) ‡ (0.75) ‡ (2.25) ‡ (7.5) ‡
30 90 300 900 3000
Mo 0
(3.0) ‡ (9.0)‡ (30) ‡ (90) ‡ (300) ‡
0.8 2.4 8 24 80
Sb 0
(0.08) ‡ (0.24) ‡ (0.8) ‡ (2.4) ‡ (8.0) ‡
2 6 20 60 200
Cs 0
(0.2) ‡ (0.6) ‡ (2.0) ‡ (6.0) ‡ (20) ‡
2 6 20 60 200
Ba 0
(0.2) ‡ (0.6) ‡ (2.0) ‡ (6.0) ‡ (20) ‡
0.6 1.8 6 18 60
W 0
(0.06) ‡ (0.18) ‡ (0.6) ‡ (1.8) ‡ (6.0) ‡
0.25 0.75 2.5 7.5 25
Pt 0
(0.025) ‡ (0.075) ‡ (0.25) ‡ (0.75) ‡ (2.5) ‡
0.4 1.2 4 12 40
TI 0
(0.04) ‡ (0.12) ‡ (0.4) ‡ (1.2) ‡ (4.0) ‡
1 3 10 30 100
Pb 0
(0.1) ‡ (0.3) ‡ (1.0) ‡ (3.0) ‡ (10) ‡
0.05 0.15 0.5 1.5 5
U 0
(0.005) ‡
(0.015) ‡
(0.05) ‡
(0.15) ‡
(0.5) ‡
0.8 2.4 8 24 80
Cd 0
(0.08) ‡ (0.24) ‡ (0.8)‡ (2.4) ‡ (8.0) ‡
60 180 600 1800 6000
Sr 0
(6.0) ‡ (18.0) ‡ (60)‡ (180)‡ (600)‡
3 9 30 90 300
Sn 0
(0.3) ‡ (0.9) ‡ (3.0)‡ (9.0)‡ (30)‡
1 3 10 30 100
Mn 0
(0.1) ‡ (0.3) ‡ (1.0) ‡ (3.0) ‡ (10) ‡
‡ A further 1:10 dilution occurs when added to base urine. Enter concentrations in parentheses into the ICP-
MS software (method window, calibration page).
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Table 6. Acceptable ways to perform two consecutive analytical runs, bracketing with bench quality
control samples.
setup 1 setup 2 (typical)
Run #1 Run #1
calibrators calibrators
low bench QC low bench QC
high bench QC high bench QC
patient samples patient samples
Run #2
Run #2 calibrators
patient samples patient samples
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Table 7. A typical SAMPLE/BATCH window.

AS sample id measurements action method
location*
236 UCTstability1 Run sample ....15elem_urblk.mth
Continue UCT stability samples . . .
236 UCTstability12£ Run sample ....15elem_urblk.mth
101 3018 UrBlkChk Wash1 Run blank, standards, and ....15elem_urblk.mth
sample **
113 3018 UrBlkChk Wash2 Run sample ....15elem_urblk.mth
114 3018 UrBlkChk1 Run sample ....15elem_urblk.mth
115 3018 UrBlkChk2 Run sample ....15elem_urblk.mth
150 3018 AQBLK Run blank and sample ¥ ....15elem_aqblk.mth
136 L Bench QC Run sample ....15elem_aqblk.mth
160 H Bench QC Run sample ....15elem_aqblk.mth
301 Sample 1 Run sample ....15elem_aqblk.mth
135 L Bench QC Run sample ....15elem_aqblk.mth
159 H Bench QC Run sample ....15elem_aqblk.mth
* The exact autosampler positions of QCs and patient samples do not have to be those shown above. QC
samples do not have to be run in the order of low, then high, then elevated.
** When executing this row, the ICP-MS will first analyze the urine blank (standard 0) at AS position 102,
then standards 1-5 at autosampler positions 102-107, then the “UrBlkChk wash1” sample at A/S position
101. The sampling information about AS positions 103-107 are stored in the “urblk” method file and can
be customized.
¥ When executing this row, the ICP-MS will first analyze the aqueous blank at AS position 149, then the
“AQBlkChk” at AS position 150. The sampling information about AS positions 149 is stored in the “aqblk”
method file and can be customized.
£ A larger number of UCT stability samples will need to be analyzed to make this stability period 1-1.5 hrs
when measuring only Cd, Mn or Co (50 measurements ~ 1hour).
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Table 8. Preparation of samples, working standards, and QC materials.

Base AQ intermediate Patient or Total
Water Diluent **
Dilution ID urine working QC urine Volume
(µL) (µL)
(µL) standard (µL) sample (µL) (µL)
working
calibrators 9,000
- 900 x 1 100 x 1 - 10,000
(S0-S5) and (4,500 x 2)*
UrBlkChk (S0)
AQ blank 1000 x 1 - - - 9,000 10,000
(4,500 x 2)*
patient urine or
- - - 500 x 1 4,500 x 1 5,000
urine-based QC
patient urine 9,000
500 x 1 - - 500 x 1 10,000
2x dilution H (4,500 x 2)*
patient urine 9,000
800 x 1 - - 200 x 1 10,000
patient urine 9,000
900 x 1 - - 100 x 1 10,000
patient urine 4,750 45,000
- - 250 x 1 50,000
20x dilution H (950 x 5) (7,500 x 6)*
NOTE: These directions are written with the expectation of a 10,000 µL syringe on the left side and a
1,000 µL syringe on the right side of the benchtop automatic pipette. If a different total volume is
prepared, adjust the volumes for each component proportionally.
** By splitting the dispense step of diluent into two or more portions, liquids pulled up into the right
pipette tip are flushed out more completely. For example, when preparing a working calibrator dilution,
do the preparation in two steps: in step 1, dispense 4500 µL diluent + 100 µL; in step 2, dispense 4500 µL
diluent + 900 µL base urine to prepare a 10 mL total volume dilution.
H
Extra dilution is performed on urine samples whose concentration is greater than the concentration of
the highest calibrator listed in Table 9 of Appendix C. Any extra dilution within these limits can be
prepared as long as the 9:10 ratio of diluent to total dilution volume is maintained. Use of the lowest
possible dilution level is preferred to minimize differences between the calibrators and the samples (i.e.
2x dilution is preferred over 5x if 2x is sufficient to dilute analyte into the documented linearity range).
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Table 9. Reportable range concentrations (µg/L).

Analyte Limit of Detection High Maximum Reportable Range
(LOD)* Calibrator Extra Dilution** Upper Boundary
Be 0.084 10 20 200
Co 0.020 7.5 20 150
Sr 0.055 600 2 1200
Mo 0.024 300 10 3000
Sn 0.13 30 20 600
Sb 0.068 8 20 160
Cs 0.45 20 20 400
Ba 0.022 20 20 400
W 0.0063 6 20 120
Pt 0.018 2.5 10 25
Tl 0.20 4 5 20
Pb 3.2 10 4 40
U 0.017 0.5 20 10
Cd 0.015 8 2 16
Mn 0.0024 10 20 200
*Re-evaluated periodically (2+ years) or at significant method changes. LODs shown were
calculated 4/29/2019.
**See ruggedness test 5 in Appendix B for supporting validation data.
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Table 10. Boundary concentrations for urine concentrations (µg/L).

Range Highest Concentration
1st upper 2nd upper
Maximum Validated for
analyte boundary boundary
(“Lim Rep Delta”) † Washout
(“1UB”) * (“2UB”) **
0.3 µg/L for values <3 µg/L
Be 0.2 0.4 300
10% of value at ≥3 µg/L
3 µg/L for values <30 µg/L
Sr 400 800 18,000
Mo 293.5 587 9,000
Sn 25 50 900
Sb 0.8 1.6 240
Cs 16.5 33 600
Ba 17.1 34.2 600
W 1.38 2.76 180
Pt 0.2 0.4 75
TI 0.62 1.24 120
Pb 7.8 15.6 300
0.03 µg/L for values <0.3 µg/L
U 0.277 0.554 15
10% of value at ≥0.3 µg/L
Cd 2.54 5.08 240
Mn 4 8 300
Co 2.83 5.66 225
* Typically, the 1UB threshold is based on percentiles of non-weighted, non-creatinine corrected concentration
results from NHANES. In the absence of that data, these boundaries can be based on normal ranges reported in
the literature. The concentrations assigned to these boundaries is determined by study protocol but default
concentrations are listed in this table.
**Typically the 2nd upper boundary (2UB) is set to 2x the 1UB. The concentrations is determined by study protocol
but default concentrations are listed in this table.
† Range maximum is the range of the three replicate readings for a single sample analysis. This value is also called
the “Lim RepDelta” in the database which handles data for the Inorganic and Radiation Analytical Toxicology Branch.
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Table 11. Reference ranges for urine concentrations (from the Fourth National Report on Exposure to
Environmental Chemicals [8]). All results in µg/L.
survey geometric
analyte 50th 75th 90th 95th N
years mean
Be 09-10* ≤ 0.072 ≤ 0.072 ≤ 0.072 ≤ 0.072 ≤ 0.072 2848
Sr 15-16 85.5 96.3 161 235 299 3061
Mo 15-16 35.4 38.6 68.6 107 137 3060
Sn 15-16 0.495 0.470 1.05 2.42 4.36 3060
Sb 15-16 0.047 0.046 0.080 0.137 0.201 3061
Cs 15-16 3.92 4.19 6.29 8.93 11.0 3061
Ba 15-16 1.15 1.21 2.26 3.89 5.59 3061
W 15-16 0.068 0.068 0.136 0.263 0.390 3060
Pt 09-10* ≤ 0.009 ≤ 0.009 ≤ 0.009 0.009 0.016 2847
Tl 15-16 0.153 0.161 0.255 0.362 0.435 3061
Pb 15-16 0.284 0.290 0.520 0.960 1.26 3061
U 15-16 0.005 0.005 0.010 0.018 0.031 3061
Cd 15-16 0.129 0.131 0.289 0.616 0.909 3061
Mn 15-16 ≤ 0.13 ≤ 0.13 0.140 0.220 0.300 3061
Co 15-16 0.414 0.434 0.687 1.06 1.53 3061
*Indicates the latest cycle years the element was measured in the National Health and Nutrition
Examination Survey (NHANES).
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Figure 1. Configuration for liquid handling using FAST sample introduction

Below shows the correct connections to the 6-port FAST valve. The two diagrams show the
differences in liquid flow directions when the valve changes from “Load” to “Inject” This change
is internal to the valve. The shift of the valve cannot be seen, but it can be heard, and felt (with
hand on the valve). The light indicators on the actuator body also indicate the valve position.
The connections to the valve are color-coded (see Section 7.a.i).
Enable the FAST program in the ESI software before running the method, but optimizations can
be done in either FAST or non-FAST mode.
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Figure 2. NexION 2000 Syngistix v2.4 method screen shots (timing page)
.
Figure 3. NexION 300D/350D Syngistix v2.3 method screen shots (timing page)
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Figure 4. NexION (300/350/2000) Syngistix v2.4 method screen shots (processing page)
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Figure 5. NexION (300/350/2000) Syngistix v2.4 method screen shots (equation page)
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Figure 6. NexION (300/350/2000) Syngistix v2.3 method screen shots (calibration page)
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Figure 7. NexION 2000 Syngistix v2.4 method screen shots (sampling page)
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Figure 8. NexION 300D/350D Syngistix v2.3 method screen shots (sampling page)
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Figure 9. NexION (300/350/2000) Syngistix v2.4 method screen shots (report page)
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Figure 10. NexION (300/350/2000) Syngistix v2.3 method screen shots (QC / Sample page)
Not all elements shown in bottom table, see Table 1 of Appendix C “Extended Washout”.
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Figure 11. ESI SC4 autosampler screen shots (main page).

Additional flush times and “Max Rinse Time” are default, but can be optimized for best
reduction of elemental carry-over between samples. Tray types can be changed to allow for
different volumes of diluted sample digests. ‘FAST control’ must be enabled before start of
method, but does not need to be used in instrument optimization (pre-analysis) steps. Rinse
and additional flush times for eliminating carry-over from one sample to the next while using
the minimum amount of rinse solution.
A rinse time of 0 causes the probe to only dip into the station, but spends no time there.
Additional flush times can be optimized to keep the rinse station full while not using too much
rinse solution. The inner diameter size of the tubing providing the rinse solution to the rinse
station determines how quickly the station will fill. Various sizes are available for purchase or
can be made in the laboratory.
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Figure 12. ESI SC4 autosampler screen shots (5x12 rack setup window).
Settings are approximate. To be sure the loop is filled, set the probe to go close to the bottom
of the cup, but not touch. Optimize retraction speed for least droplet splatter.
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Figure 13. ESI SC4 autosampler screen shots (50mL tube rack setup window).
Settings are approximate. To be sure the loop is filled, set the probe to go close to the bottom
of the cup, but not touch. Optimize retraction speed for least droplet splatter.
Figure 14. ESI SC4 autosampler screen shots (rinse station rack setup window).
Settings are approximate. Optimize down height for best probe cleaning, and retraction speed
for least droplet splatter.
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Figure 15. ESI SC4 autosampler screen shots (“Configure” page).

“High Speed” option is to only be used for ‘High Speed’ models of the SC4 (look for “HS” in
serial number). Speeds and accel / decel values can be optimized per analyst preference and to
minimize droplet splatter off of probe.
Figure 16. ESI SC4 autosampler screen shots used (“Communication” page).
Communication ports will differ depending on available ports on instrument control computer.
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Figure 17. ESI SC4 autosampler screen shots (“FAST” page).

Timer A can be optimized to achieve proper filling of loop with diluted sample. Timers B – H
control rinsing the loop after analysis and can be optimized for eliminating carry-over from one
sample to the next while using the minimum amount of rinse solution. See Figure 3g and 3h for
the entire program.
Manually clicking the “Load” button prior to starting analysis will ensure the position of the
actuator is always the same at the beginning of the analysis.
Manually clicking the “Vacuum On” button prior to starting the analysis will help initial sample
uptake to be consistent.
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Figure 18. Entire ESI SC4 autosampler “FAST” program.

Line Event Action Parameters Parameter Units
1 On Probe Down Vacuum1 On
2 On Probe Down Load1
3 Probe In Sample Timer A 11 seconds
4 Timer A Expires Inject1
5 Timer A Expires Move Rinse
6 Rinse Completed Probe Up
7 On Rinse Vacuum1 On
8 On Rinse Probe Down
9 On Rinse Load1
10 On Rinse Timer B 4 seconds
11 Timer B Expires Inject1
12 Timer B Expires Timer C 4 seconds
13 Timer B Expires Probe Up
14 Timer B Expires A2 On
15 Timer C Expires Probe Down
16 Timer C Expires Load1
17 Timer C Expires Timer D 4 seconds
18 Timer D Expires Probe Up
19 Timer D Expires Timer E 4 seconds
20 Timer D Expires A2 Off
21 Timer E Expires Probe Down
22 Timer E Expires Timer F 4 seconds
23 Timer F Expires Probe Up
24 Timer F Expires Timer G 4 seconds
25 Timer G Expires Probe Down
26 Timer G Expires Timer H 4 seconds
27 Timer H Expires Move Next
NOTE: “Probe in Sample” time will need to be optimized for the appropriate number of
elements being analyzed (e.g. 1, 8, 15, etc…) and to ensure no air gaps remain in the loop after
filling. Typical times are 8–15 seconds for a 3mL loop (15 elements), 6–10 seconds for a 2mL
loop (e.g. 8 element subset), 4–6 seconds for a 1mL loop (e.g. 3 element subset), or 3-5 seconds
for a 0.5 mL loop (e.g. 1 element). Customized loop sizes can be created. Fill times need to be
optimized per instrument setup.
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Figure 19. Flow chart for handling an elevated result.
no Report the first analytically

Result > 1UB
valid result.
yes
no Repeat elevated result for

> 2UB? confirmation, and report the
first analytically valid result.
yes
Repeat elevated result for
no confirmation, and report the
> S5?
first analytically valid result
as >2UB.
yes
> highest Repeat elevated result for

concentration no confirmation by dilution in
validated for duplicate, and report the first
washout? analytically valid result as >2UB.
yes
Repeat elevated result for confirmation
by dilution in duplicate, and report the
first analytically valid result as >2UB.
run verified in
no
control for Confirm by re-analysis the results for the
low conc 2 samples immediately following the
samples? elevated sample. Report first analytically
valid result when it is confirmed within
±10% or ±3SD of the low bench QC,
whichever is larger.
yes
repeat elevated result for

confirmation by dilution in
duplicate, and report the first
analytically valid result as >2UB
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19. Appendix D: Help Sheets

Reagent Preparation Help Sheets, page 1 of 2
mg/L = ppm, µg/L = ppb, and µg/mL = ppm
Rinse Solution – 4 L
(5.0% (v/v) HNO 3 , 0.002% Triton X-100)
1. Partially fill a 4 liter bottle with 18 Mohm∙cm water.
2. Add 4 mL of the 2% Triton X-100™ / 5% (v/v) nitric-acid intermediate stock solution.
3. Carefully add 200 mL of concentrated HNO 3 .
4.
4. Add enough >18 Mohm∙cm water to bring to 4 liter mark.
5. Mix well by gently inverting several times.
6. Label appropriately and store at ambient temperature.
7.
Sample Diluent/Carrier Solution – 2 L

(2.0% (v/v) HNO 3 , 10 µg/L Ir and Rh)
1. Partially fill a 2 liter bottle with 18 MΩ∙cm water.
2. Add 40 mL concentrated HNO 3 .
3. Add 500 µL of the 40 µg/mL Rh and Ir internal standard solution.
4. Add enough 18 Mohm∙cm water to bring to 2 liter mark.
Intermediate Internal Standard Solution – 200 mL

(2.0% (v/v) HNO 3 , 40 µg/mL Ir and Rh)
1. Partially fill a 200 mL volumetric flask with 18 Mohm∙cm water.
2. Add 4 mL of concentrated HNO 3 .
3. Add 8 mL of 1,000 µg/mL Rh standard.
4. Add 8 mL of 1,000 µg/mL Ir standard.
5. Add enough 18 Mohm∙cm water to bring to 200 mL mark.
2% Triton X-100 in 5% (v/v) HNO 3 – 2 L

1. Partially fill a 2 liter bottle with 18 Mohm∙cm water.
3. Add 40 mL of Triton X-100.
5. Add a clean Teflon magnetic stirring bar and stir on stirrer until dissolved.
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Reagent Preparation Help Sheets, page 2 of 2

0.5% (v/v) HNO 3
2% (v/v) HNO 3
5% (v/v) HNO 3
UCT Stability Solution – 200 mL

1. Add 180 mL of diluent to 250 mL bottle.
2. Add 18 mL of human urine to bottle.
3. Add 2 mL of Standard 2 to bottle.
Daily Performance Solution (1 µg/L) in 2% (v/v) HNO 3

1. Partially fill a 1 liter volumetric flask with 18 Mohm∙cm water.
2. Add 1 mL of High Purity Standard: SM-2107-018.
Dual Detector Solution

1. Partially fill a 50 mL polypropylene tube with 2% (v/v) HNO 3 .
2. Add 100 µL of 100 µg/mL High Purity Standard: SM-2107-053.
3. Add 10 µL of any additional 1,000 µg/mL single element stock standard, if required.
4. Dilute to the 50 mL mark with 2% (v/v) HNO 3 .
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Laboratory Procedure Manual: Urine Multi-Elements in Urine by ICP-UCT-MS 3018.7

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Laboratory Procedure Manual

Analytes: Antimony, Barium, Beryllium, Cadmium,

Method: Multi-elements in urine by ICP-UCT-MS

Method No: 3018.7

As performed by: Inorganic and Radiation Analytical Toxicology

Contact: Mr. Jeffery M. Jarrett

James L. Pirkle, M.D., Ph.D.

Important Information for Users

Public Release Data Set Information

This method file describes measurements of UM_K.

1. Summary of test principle and clinical relevance

2. Limitations of method; interfering substances and conditions

Accuracy and precision of this method can be critically impacted by elemental

Specificity tests indicated that at there is no observable impact on observed cadmium

3. Procedures for collecting, storing, and handling specimens; criteria for

B. Criteria for specimen rejection:

Improper collection procedures or collection devices can contaminate the urine by

5. Instrument and material sources

B. Sources for ICP-MS parts & consumables

1. Screws (for hyper skimmer cone): PerkinElmer part # 09919737 (PerkinElmer,

www.perkinelmer.com) or equivalent (such as part # V75-010, O-rings West, Seattle, WA,

1) NexION 300D/350D: PerkinElmer part # N8145013 (PerkinElmer, Shelton, CT,

C. Sources for ICP-MS maintenance equipment and supplies:

D. Sources for general laboratory consumable supplies:

E. Sources of chemicals, gases, and regulators:

stainless steel Swagelok connector. Like part # GEORG/KCYCFR/ORS2/540 (Georgia Valve

6. Preparation of reagent and materials

4) Add 8,000 µg of rhodium (e.g. 8 mL of 1,000 µg/mL Rh stock standard).

1) Collection of urine: Collect urine anonymously by placing screened containers and / or

(iv) Homogeneity testing: After dispensing, check homogeneity of analyte

1) Base urine in diluent (1 + 9): In a 50 mL lot screened or acid-washed polypropylene

1) Base urine in diluent (1 + 9): In a 50 mL lot screened or acid-washed polypropylene

3) Base urine in diluent (1 + 9) + 400 µg/L K: In a 50 mL lot screened or acid-washed

1) Base urine in diluent (1 + 9): In a 50 mL lot screened or acid-washed polypropylene

M. For dual detector calibration:

1) Partially fill a 50 mL lot screened or acid-washed polypropylene tube with 2% (v/v)

2) Add a 0.1 mL of 100 ug/mL special mix standard.

B. Perform, evaluate and report a run:

1) Power on the computer, printer, and autosampler, and instrument computer

4) Daily pre-ignition maintenance checks: Perform and document daily maintenance

1) Thaw urine samples; allow them to reach ambient temperature.

(c) Comparison with other instruments.

1) Electronic records: Transfer data electronically to the laboratory information system.

1) Elevated concentrations: Refer to Figure 19 in Appendix C for flowchart.

2) Unacceptable reproducibility: If the range of the three replicate readings (maximum

9. Routine equipment maintenance and data backups

10. Reporting thresholds

11. Method calculations

13. Method Performance Documentation

14. Summary Statistics and QC Graph

2019-2020 Summary Statistics and QC Chart

Start End Standard Coefficient of

2019-2020 Summary Statistics and QC Chart

Start End Standard Coefficient of

2019-2020 Summary Statistics and QC Chart

Start End Standard Coefficient of

2019-2020 Summary Statistics and QC Chart

Start End Standard Coefficient of

2019-2020 Summary Statistics and QC Chart

Start End Standard Coefficient of

2019-2020 Summary Statistics and QC Chart

Start End Standard Coefficient of