7.2. Chemical Analysis
The documentation for nonradiological analyses is contained in the ESH-DA Chemistry
Laboratory Procedure Manual. All samples for NPDES and groundwater are collected and
analyzed in accordance with EPA regulations found in 40 CFR Part 136,26 EPA-600/4-84-017,35
and SW-846.9
Standard Reference Materials (SRM), traceable to the NIST, exist for most inorganic analyses
(see Table 7.3). These are replaced annually. Detection limits are determined with techniques
listed in Report SW-8469 and are listed in Table 7.4. In general, the detection limit is the
measure of the variability of a standard material measurement at 5 to 10 times the instrument
detection limit as measured over an extended time period. Recovery of inorganic metals, as
determined by "spiking" unknown solutions, must be in the range of 75% to 125%. The
precision, as determined by analysis of duplicate samples, must be within 20%. These
measurements must be made on at least 10% of the samples. Comparison samples for organic
constituents were formerly available from the EPA, but are now commercially available under
the Cooperative Research and Development Agreement (CRADA) that exists between the EPA
and commercial laboratories. In addition, standards are available that are certified by the
American Association for Laboratory Accreditation, under a memorandum of understanding with
the EPA. Many of these standards were used in this work. At least one standard mixture is
analyzed each month; the results for 1995 are shown in Table 7.5 for VOCs and Table 7.6 for
SVOCs. The recoveries listed are those required by the respective methods.
TABLE 7.3
Reference Materials Used for
Inorganic Analysis |
Reference Materiala |
Constituent |
HPS-10002-2 |
Antimony |
HPS-10003-1 |
Arsenic |
HPS-10004-1 |
Barium |
HPS-10005-1 |
Beryllium |
HPS-10008-1 |
Cadmium |
HPS-100012-1 |
Chromium |
HPS-100013-1 |
Cobalt |
HPS-100014-1 |
Copper |
HPS-100026-1 |
Iron |
HPS-100028-1 |
Lead |
HPS-100032-1 |
Manganese |
HPS-100033-1 |
Mercury |
HPS-100036-1 |
Nickel |
HPS-100049-1 |
Selenium |
HPS-100051-1 |
Silver |
HPS-100065-1 |
Vanadium |
HPS-100068-1 |
Zinc |
NIST-SRM 3181 |
Sulfate |
NIST-SRM 3182 |
Chloride |
NIST-SRM 3183 |
Fluoride |
a HPS = High Purity Standards,
Inc.; NIST-SRM = National
Institute of Standards and
Technology - Standard Reference
Materials. |
TABLE 7.4
Limit of Detection for Metal Analysis |
|
Limits of Detection
mg/L |
Constituent |
AAa |
ICPb |
Antimony |
0.0025 |
- |
Arsenic |
0.0025 |
0.110 |
Barium |
- |
0.015 |
Beryllium |
0.00015 |
0.025 |
Boron |
- |
0.080 |
Cadmium |
0.0001 |
0.040 |
Chromium |
0.020 |
0.060 |
Cobalt |
- |
0.025 |
Copper |
0.010 |
0.045 |
Hexavalent Chromiumc |
0.006 |
- |
Iron |
0.020 |
0.025 |
Lead |
0.0005 |
0.110 |
Manganese |
0.015 |
0.020 |
Mercury |
0.0001 |
- |
Nickel |
0.020 |
0.040 |
Selenium |
0.0025 |
0.090 |
Silver |
0.0010 |
0.110 |
Thallium |
0.0015 |
0.145 |
Vanadium |
- |
0.055 |
Zinc |
0.005 |
0.015 |
a AA = Atomic Absorption Spectroscopy.
b ICP = Inductively Coupled Plasma - Atomic
Emission Spectroscopy.
c Coulometric measurement. |
TABLE 7.5
Quality Check Sample Results: Volatile Analyses, 1995 |
Compound |
Recoverya
(%) |
Quality Limits
(%) |
Benzene |
111 |
73-126 |
Bromobenzene |
96 |
76-133 |
Bromodichloromethane |
90 |
101-138 |
Bromoform |
87 |
57-156 |
Butylbenzene |
94 |
71-125 |
sec-Butylbenzene |
98 |
71-145 |
t-Butylbenzene |
112 |
69-134 |
Carbon Tetrachloride |
96 |
86-118 |
Chlorobenzene |
99 |
80-137 |
Chloroform |
106 |
68-120 |
o-Chlorotoluene |
103 |
81-146 |
p-Chlorotoluene |
97 |
73-144 |
1,2-Dibromo-3-chloropropane |
93 |
36-154 |
Dibromochloromethane |
84 |
68-130 |
1,2-Dibromoethane |
100 |
75-149 |
Dibromomethane |
101 |
65-143 |
1,2-Dichlorobenzene |
112 |
59-174 |
1,3-Dichlorobenzene |
101 |
84-143 |
1,4-Dichlorobenzene |
99 |
58-172 |
1,1-Dichloroethane |
108 |
71-142 |
1,2-Dichloroethane |
100 |
70-134 |
1,1-Dichloroethene |
111 |
18-209 |
cis-1,2-Dichloroethene |
87 |
85-124 |
trans-1,2-Dichloroethene |
108 |
67-141 |
1,2-Dichloropropane |
99 |
19-179 |
1,3-Dichloropropane |
100 |
73-145 |
1,1-Dichloropropene |
87 |
71-133 |
Ethyl Benzene |
106 |
84-130 |
Isopropylbenzene |
100 |
70-144 |
4-Isopropyltoluene |
100 |
72-140 |
Methylene Chloride |
121 |
D-197 |
n-Propylbenzene |
128 |
78-139 |
1,1,1,2-Tetrachloroethane |
96 |
88-133 |
Tetrachloroethene |
111 |
84-132 |
Toluene |
94 |
81-130 |
1,1,1-Trichloroethane |
94 |
68-149 |
1,1,2-Trichloroethane |
89 |
70-133 |
Trichloroethene |
99 |
91-135 |
1,2,3-Trichloropropane |
113 |
50-158 |
1,2,4-Trimethylbenzene |
105 |
80-144 |
1,3,5-Trimethylbenzene |
97 |
76-142 |
o-Xylene |
100 |
79-141 |
p-Xylene |
108 |
74-138 |
Note: D denotes the compound was detected.
a Average of two determinations. |
TABLE 7.6
Quality Check Sample Results:
Semivolatile Analyses, 1995 |
Compound |
Recoverya
(%) |
Quality Limits
(%) |
2-Fluorophenolb |
57.2 |
21-100 |
Phenol-d5b |
49.3 |
10-94 |
Phenol |
49.9 |
17-100 |
2-Chlorophenol |
92.5 |
36-120 |
1,4-Dichlorobenzene |
53.7 |
37-106 |
n-Nitroso-n-Propyl Amine |
58.7 |
24-198 |
Nitrobenzene-d5b |
61.0 |
35-114 |
1,2,4-Trichlorobenzene |
62.2 |
57-129 |
4-Chloro-3-Methylphenol |
101.0 |
41-128 |
2-Fluorobiphenylb |
82.2 |
43-116 |
Acenaphthene |
88.8 |
47-145 |
2,4-Dinitrotoluene |
91.7 |
48-127 |
2,4,6-Tribromophenolb |
93.1 |
10-123 |
Pentachlorophenol |
95.2 |
38-152 |
Pyrene |
95.4 |
70-100 |
Terphenyl-d14b |
67.2 |
33-141 |
a Average of three determinations.
b Required surrogates. |
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