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Appendix B
5/20/2009
9
7.
REAGENTS AND STANDARDS
7.1.
Purity of Water
– Unless otherwise indicated, references to water shall be
understood to mean reagent water conforming to ASTM Specification D 1193, Type
I.
7.2.
Purity of Reagents
– Reagent grade chemicals shall be used in all tests. Unless
otherwise indicated, it is intended that all reagents shall conform to the specifications
of the Committee on Analytical Reagents of the American Chemical Society, where
such specifications are available. Other grades may be used, provided it is first
ascertained that the reagent is of sufficiently high purity to permit its use without
lessening the accuracy of the determination.
7.3.
Acetanilide, 99.9% + purity
, C
8
H
9
NO (CASRN 103-84-4) - Primary standard
7.4.
Blanks
– Three blanks are used for the analysis. Two blanks are instrument related.
The instrument zero response (ZN) is the background response of the instrument
without sample holding devices such as capsules and sleeves. The instrument blank
response (BN) is the response of the instrument when the sample capsule, sleeve and
ladle are inserted for analysis without standard or sample. The BN is also the
laboratory reagent blank (LRB) for standards and sediment or other weighed
samples. The LRB for water samples includes the sleeve, ladle and a precombusted
filter without standard or sample. These blanks are subtracted from the uncorrected
instrument response used to calculate concentration. The third blank is the
laboratory fortified blank (LFB.) For sediment or other weighed sample analysis, a
weighed amount of acetanilide or other standard is placed in an aluminum capsule
and analyzed. For aqueous samples, a weighed amount of acetanilide or other
standard is placed on a glass fiber filter the same size as used for sample filtration,
and analyzed.
7.5.
Quality Control Sample (QCS)
– For this procedure, the QCS can be any assayed
and certified sediment or particulate sample which is obtained from an external
source. BCSS-1 from the National Research Council of Canada is used by this
laboratory.
8.
SAMPLE COLLECTION, PRESERVATION AND STORAGE
8.1.
Water Sample Collection
– Samples collected for PNC analysis from fresh,
estuarine and coastal waters are normally collected from a boat or pier using one of
two methods; hydrocast or submersible pump systems. Follow the recommended
sampling protocols associated with the method used. Whenever possible,
immediately filter the samples as described in Section 11.1.1. Store the filtered
sample in an aluminum foil pouch and freeze at -20°C or store in a low temperature
(47
o
C) drying oven after drying at 47
o
C ± 2°C, until use. If storage of the unfiltered
water sample is necessary, place the sample into a clean bottle and store at 4°C until
filtration is performed. Dry samples in a low temperature (47
o
C+/-2
o
C) drying oven
prior to analysis.
8.2. The volume of water sample collected will vary with the type of sample being
analyzed. Table 1, see 8.3.2., provides a guide for a number of matrices of interest.
If the matrix cannot be classified by this guide, collect 1 L of water from each site.