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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