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, " EPA-600/4-
84-01726, and SW-846.27
Standard Reference Materials (SRM), traceable to the NIST, exist for most inorganic
analyses (see Table 7.4). These are replaced annually. Detection limits are determined
with techniques listed in Report SW-846 27 and are listed in Table 7.5. In general, the
detection limit is the measure of the variability (6) of a standard material measurement
at 5-10 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 12 %. 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) which exists between the EPA and commercial laboratories. In addition,
standards are available which are certified by the American Association for Laboratory
Accreditation, under a memorandum of understanding with the EPA. Many of these
standards are used in this work. At least one standard mixture is analyzed each month
and the results for 1994 are shown in Table 7.6 for volatile organic compounds and
Table 7.7 for semivolatiles. The recoveries listed are those required by the respective
methods.
TABLE 7.4
Reference Materials Used for Inorganic Analysis
____________________________________________________________
Reference Material Constituent
____________________________________________________________
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
______________________________________________________________
HPS = High Purity Standards, Inc.
NIST-SRM = National Institute of Standards and Technology
- Standard Reference Materials.
TABLE 7.5
Limit of Detection for Metal Analysis
_____________________________________________________
Limits of Detection
Milligrams/Liter
Constituent AA* ICP**
_____________________________________________________
Arsenic 0.0020 0.110
Barium - 0.015
Beryllium 0.0001 0.025
Cadmium 0.0001 0.040
Chromium 0.020 0.060
Cobalt 0.020 0.025
Copper 0.010 0.045
Hexavalent Chromium 0.006 -
Iron 0.040 0.025
Lead 0.0010 0.110
Manganese 0.010 0.020
Mercury 0.0001 -
Nickel 0.020 0.040
Silver 0.0010 0.110
Thallium 0.0030 0.145
Vanadium - 0.055
Zinc 0.010 0.015
_____________________________________________________
*AA Atomic Absorption Spectroscopy.
**ICP Inductively Coupled Plasma - Atomic Emission
Spectroscopy.
TABLE 7.6
Quality Check Sample Results, Volatile Analyses, 1994
__________________________________________________________________
Percent Percent
Compound Recovery Quality Limits
__________________________________________________________________
Benzene 101 73-126
Bromobenzene 101 76-133
Bromodichloromethane 98 101-138
Bromoform 76 57-156
Butylbenzene 108 71-125
sec-Butylbenzene 108 71-145
t-Butylbenzene 112 69-134
Carbon Tetrachloride 101 86-118
Chlorobenzene 108 80-137
Chloroform 103 68-120
o-Chlorotoluene 111 81-146
p-Chlorotoluene 107 73-144
1,2-Dibromo-3-chloropropane 117 36-154
Dibromochloromethane 89 68-130
1,2-Dibromomethane 113 75-149
Dibromomethane 99 65-143
1,2-Dichlorobenzene 121 59-174
1,3-Dichlorobenzene 116 84-143
1,4-Dichlorobenzene 118 58-172
1,1-Dichloroethane 92 71-142
1,2-Dichloroethane 119 70-134
1,1-Dichloroethene 127 18-209
cis-1,2-Dichloroethene 99 85-124
trans-1,2-Dichloroethene 114 67-141
1,2-Dichloropropane 125 19-179
1,3-Dichloropropane 93 73-145
1, 1-Dichloropropene 92 71-133
Ethyl Benzene 100 84-130
Isopropylbenzene 101 70-144
4-Isopropyltoluene 105 72-140
Methylene Chloride 89 D-197
n-Propylbenzene 108 78-139
1, 1, 1,2-Tetrachloroethane 94 88-133
Tetrachloroethene 108 84-132
Toluene 99 81-13O
1, 1, 1 -Trichloroethane 90 68-149
1, 1,2-Trichloroethane 119 70-133
Trichloroethene 100 91-135
1,2,3-Trichloropropane 120 50-158
1,2,4-Trimethylbenzene 105 80-144
1,3,5-Trimethylbenzene 109 76-142
o-Xylene 100 79-141
p-Xylene 108 74-138
_____________________________________________________________
Note: D denotes the compound was detected.
TABLE 7.7
Quality Check Sample Results, Semivolatile Analyses, 1994
__________________________________________________________
Percent Percent
Compound Recoverya Quality Limits
__________________________________________________________
2-Fluorophenolb 62.1 21-100
Phenol-d5b 42.6 10-94
Phenol 43.1 17-100
2-Chlorophenol 78.7 36-120
1,4-Dichlorobenzene 82.1 37-106
n-Nitroso-n-Propyl Amine 61.6 24-198
Nitrobenzene-d5b 85.9 35-114
1 2,4-Trichlorobenzene 92.0 57-129
4-Chloro-3-Methylphenol 89.3 41-128
2-Fluorobiphenylb 68.0 43-116
Acenaphthene 126.0 47-145
4-Nitrophenol 65.2 13-107
2,4-Dinitrotoluene 126.0 48-127
2,4,6-Tribromophenolb 88.6 10-123
Pentachlorophenol 107.0 38-152
Pyrene 90.2 70-100
Terphenyl-dl4b 99.9 33-141
_________________________________________________________
a Average of three determinations.
b Required surrogates.