for atomic absorption analysis should be collected and stored in acid (HN0 3 ) 

 rinsed polyethylene bags or jars. Glass jars used for collecting or stor- 

 ing samples should be covered with Teflon or aluminum-lined lids. All 

 glassware should be meticulously cleaned by one of several available acid- 

 washing techniques (Goda 1970, Chesler et al . 1976), or an equivalent proce- 

 dure involving high temperature (about 500°C) bakeouts in an annealing oven. 

 A representative sample of each lot of cleaned glassware should be tested 

 for contamination by gas chromatographic analysis of pentane washes. The 

 pentane washes should be analyzed using both a flame ionization detector 

 and an electron capture detector. These results should be recorded as docu- 

 mentation of the cleanliness of the glassware used in sample collection and 

 storage. Detection of squalene in the pentane washes usually indicates the 

 presence of fingerprints on the inside of the glassware. Sample collection 

 gear should be cleaned prior to use by detergent washing followed by rinsing 

 with appropriate organic solvents. Sampling gear should also be thoroughly 

 rinsed with water or some other appropriate solvent and air dried between 

 collections of replicate samples in the field. 



Sample presentation by freezing has general applicability because it 

 does not involve the use of chemical preservatives. The expansion of water 

 at temperatures below 4°C must, however, be considered when samples contain- 

 ing large amounts of water are frozen in glass containers. For instance, 

 glass jars containing water or wet sediment samples should be filled to no 

 more than half their capacity if they are to be stored below C. Freezing 

 glass sample jars on their sides further reduces the possibility of breakage 

 due to ice expansion (Chesler et al. 1976). 



As indicated previously, collection methods for a variety of sample types 

 are outlined in Table 4. Included in this table are methods of sample 

 preservation, estimated sample sizes required for analysis, equipment re- 

 quired for sample collection, and pertinent comments related to the collec- 

 tion of each sample type. Although not indicated under the Method of 

 Preservation heading, all samples should be stored in the dark to prevent 

 photodecomposition prior to analysis. 



ANALYTICAL SAFEGUARDS 



Spill investigation technology has not yet reached the point of standard- 

 ization. It is unlikely that there will ever be a single analytical technique 

 applicable to all spill situations. It is, however, possible to standardize 

 analytical techniques for certain classes of compounds, such as petroleum 

 hydrocarbons, that are often spilled or dumped into the environment. Stan- 

 dardization of analytical methods is desirable from a legal standpoint because 

 data obtained using standard methods carry with them the implication, often 

 undeserved, of a high level of reliability. Scientifically, and also legally 

 if the point is pursued, all analytical results, whether obtained by standard 

 methods or not, should be accompanied by quality assurance data that specifi- 

 cally indicate their reliability. Data reliability expressed in terms of 



190 



