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.