METHOD 200.
DETERMINATION OF TRACE ELEMENTS IN WATERS AND WASTES BY INDUCTIVELY COUPLED
PLASMA - MASS SPECTROMETRY
3.0 DEFINITIONS
3.1 Calibration Blank - A volume of reagent water acidified with the same acid matrix as in the
calibration standards. The calibration blank is a zero standard and is used to calibrate the ICP
instrument (Section 7.6.1).
3.2 Calibration Standard (CAL) - A solution prepared from the dilution of stock standard
solutions. The CAL solutions are used to calibrate the instrument response with respect to
analyte concentration (Section 7.4).
3.3 Dissolved Analyte - The concentration of analyte in an aqueous sample that will pass
through a 0.45 μm membrane filter assembly prior to sample acidification (Section 11.1).
3.4 Field Reagent Blank (FRB) - An aliquot of reagent water or other blank matrix that is placed
in a sample container in the laboratory and treated as a sample in all respects, including
shipment to the sampling site, exposure to the sampling site conditions, storage, preservation,
and all analytical procedures. The purpose of the FRB is to determine if method analytes or
other interferences are present in the field environment (Section 8.5).
3.5 Instrument Detection Limit (IDL) - The concentration equivalent to the analyte signal which
is equal to three times the standard deviation of a series of 10 replicate measurements of the
calibration blank signal at the selected analytical mass(es). (Table 1).
3.6 Internal Standard - Pure analyte(s) added to a sample, extract, or standard solution in
known amount(s) and used to measure the relative responses of other method analytes that
are components of the same sample or solution. The internal standard must be an analyte that
is not a sample component (Sections 7.5 and 9.4.5).
3.7 Laboratory Duplicates (LD1 and LD2) - Two aliquots of the same sample taken in the
laboratory and analyzed separately with identical procedures. Analyses of LD1 and LD2 indicates
precision associated with laboratory procedures, but not with sample collection, preservation,
or storage procedures.
3.8 Laboratory Fortified Blank (LFB) - An aliquot of LRB to which known quantities of the
method analytes are added in the laboratory. The LFB is analyzed exactly like a sample, and its
purpose is to determine whether the methodology is in control and whether the laboratory is
capable of making accurate and precise measurements (Sections 7.9 and 9.3.2).
3.9 Laboratory Fortified Sample Matrix (LFM) - An aliquot of an environmental sample to which
known quantities of the method analytes are added in the laboratory. The LFM is analyzed
exactly like a sample, and its purpose is to determine whether the sample matrix contributes
bias to the analytical results. The background concentrations of the analytes in the sample
matrix must be determined in a separate aliquot and the measured values in the LFM corrected
for background concentrations (Section 9.4).
3.10 Laboratory Reagent Blank (LRB) - An aliquot of reagent water or other blank matrices that
are treated exactly as a sample including exposure to all glassware, equipment, solvents,
reagents, and internal standards that are used with other samples. The LRB is used to determine
if method analytes or other interferences are present in the laboratory environment, reagents,
or apparatus (Sections 7.6.2 and 9.3.1).
3.11 Linear Dynamic Range (LDR) - The concentration range over which the instrument
response to an analyte is linear (Section 9.2.2).
3.12 Method Detection Limit (MDL) - The minimum concentration of an analyte that can be
identified, measured, and reported with 99% confidence that the analyte concentration is
greater than zero (Section 9.2.4 and Table 7).
3.13 Quality Control Sample (QCS) - A solution of method analytes of known concentrations
which is used to fortify an aliquot of LRB or sample matrix. The QCS is obtained from a source
external to the laboratory and different from the source of calibration standards. It is used to
check either laboratory or instrument performance (Sections 7.8 and 9.2.3).
3.14 Solid Sample - For the purpose of this method, a sample taken from material classified as
either soil, sediment or sludge.
3.15 Stock Standard Solution - A concentrated solution containing one or more method
analytes prepared in the laboratory using assayed reference materials or purchased from a
reputable commercial source (Section 7.3).
3.16 Total Recoverable Analyte - The concentration of analyte determined either by "direct
analysis" of an unfiltered acid preserved drinking water sample with turbidity of <1 NTU
(Section 11.2.1), or by analysis of the solution extract of a solid sample or an unfiltered aqueous
sample following digestion by refluxing with hot dilute mineral acid(s) as specified in the
method (Sections 11.2 and 11.3).
3.17 Tuning Solution - A solution which is used to determine acceptable instrument
performance prior to calibration and sample analyses (Section 7.7).
3.18 Water Sample - For the purpose of this method, a sample taken from one of the following
sources: drinking, surface, ground, storm runoff, industrial or domestic wastewater.
.Typical Analytical Sequence
No. Solution Its meaning
1 SB Standard blank
2 CS 1 Calibration standard 1
3 CS 2 Calibration standard 2
4 CS 3 Calibration standard 3
5 CS 4 Calibration standard 54
6 ICV Initial calibration
verification
7 CCV تحضير تركيز منContinuing calib.
غير باتش استاندرverification
calibration curve
8 MB 1 Digested DI Method blank 1
9 MB 2 Method blank 2
10 MB 3 Method blank 3
11 Sample 1
12 Sample 1 with FAP Fortified analytical portion
بعد الهضم نضيف تركيز
MSD
13 Sample 2
14 LFB Spike and Laboratory fortified blank
digest
15 SB 1-2% HNO3 Standard blank
16 Sample 3
17 Sample 4
18 Sample 5
19 Sample 5 (MD) method
Duplicate
(digestion)
20 Sample 6
21 Sample 7
22 Sample 8
23 Sample 9
24 Sample 10
25 CCV- for control
chart
26 SB Standard blank
No Title Frequency intervals Equipment name
Recovery With validation ICP-MS
Verification Every Batch
Method blank Every Batch
Laboratory Fortified Every Batch
Blank (LFB) For
Control Chart
Control Chart Every 30 batch
According of PT
PT
Program
Uncertainty One per year
Calibration Every Batch