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Esbensen K.H.,Geological Survey of Denmark | Esbensen K.H.,University of Aalborg | Ramsey C.A.,Envirostat Inc.
Journal of AOAC International | Year: 2015

Quality control (QC) is a systematic approach for estimating and minimizing significant error contributions to the measurement uncertainty from the full sampling and analysis process. Many types of QC measures can be implemented; the three dealt with here are primary sampling reproducibility, sample processing reproducibility, and contamination. Sampling processes can be subject to QC by applying a replication experiment, used either from the top by replication of the entire sampling/ preparation/analysis process, or in a hierarchical fashion successively at each subsequent sampling stage. The analytical repeatability is necessarily always included in either alternative. The replication experiment results in a quality index, the Relative Sampling Variability, which is used to assess the total error associated with the full field-to-analysis pathway. Contamination can occur at essentially all locations in the sampling regimen in the food/feed realm, affecting sample containers, sampling tools, sample processing equipment, environmental conditions, and sampling personnel. QC events to determine contamination should always be included where appropriate, but is of most concern for low concentration and/or volatile analytes. It is also of key importance in the development of new sampling protocols or carried-over protocols intended for use on new types of materials/lots than the ones for which they were originally developed. We here establish a first practical framework for QC as applied to the sampling context. Source


Wagner C.,Ostpreussenring 46 | Ramsey C.A.,Envirostat Inc.
Journal of AOAC International | Year: 2015

The lack of a sound scientific sampling approach results in unknown data quality and ultimately indefensible decisions. Sampling Quality Criteria (SQC) need to be correctly defined and made explicit to ensure that sampling protocols are representative and fit-for-purpose. The systematic approach to representative sampling framework is the only approach that can ensure development of reliable and representative sampling protocols under all circumstances for all application scenarios. Source


Ramsey C.A.,Envirostat Inc.
Journal of AOAC International | Year: 2015

Sampling agricultural soils for contaminants is relatively new. Existing standard sampling protocols used for the evaluation of soil nutrients are likely insufficient for contaminants. The main reasons are the very low analyte levels and differences in heterogeneity between nutrients and contaminants. To evaluate the adequacy of existing sampling protocols or to develop new protocols, a systematic scientific approach is needed. This approach begins with the development of the Sample Quality Criteria followed by a realistic understanding of the properties of the material to be sampled, most notably its heterogeneity. The Sample Quality Criteria and material properties are inputs into the Theory of Sampling. With these inputs, the Theory of Sampling can be used to determine the specifics of the sampling protocol (e.g., mass, number of increments, tool selection) that must be implemented to control error to reliably estimate the concentration of the analyte(s) of interest. Development of sampling protocols in this manner will ensure sample representativeness and therefore improve data equivalency among various parties involved. This is the only way to provide a sound technical basis for defensible decision making to ensure increased safety of food and feed, specifically with respect to contaminants in agricultural soils. Source


Ramsey C.A.,Envirostat Inc. | Wagner C.,Ostpreussenring 46
Journal of AOAC International | Year: 2015

The concept of Sample Quality Criteria (SQC) is the initial step in the scientific approach to representative sampling. It includes the establishment of sampling objectives, Decision Unit (DU), and confidence. Once fully defined, these criteria serve as input, in addition to material properties, to the Theory of Sampling for developing a representative sampling protocol. The first component of the SQC establishes these questions: What is the analyte(s) of concern? What is the concentration level of interest of the analyte(s)? How will inference(s) be made from the analytical data to the DU? The second component of the SQC establishes the DU, i.e., the scale at which decisions are to be made. On a large scale, a DU could be a ship or rail car; examples for small-scale DUs are individual beans, seeds, or kernels. A well-defined DU is critical because it defines the spatial and temporal boundaries of sample collection. SQC are not limited to a single DU; they can also include multiple DUs. The third SQC component, the confidence, establishes the desired probability that a correct inference (decision) can be made. The confidence level should typically correlate to the potential consequences of an incorrect decision (e.g., health or economic). The magnitude of combined errors in the sampling, sample processing and analytical protocols determines the likelihood of an incorrect decision. Thus, controlling error to a greater extent increases the probability of a correct decision. The required confidence level directly affects the sampling effort and QC measures. Source


Walsh M.R.,U.S. Army | Walsh M.E.,U.S. Army | Ramsey C.A.,Envirostat Inc. | Brochu S.,Defence Research and Development Canada | And 2 more authors.
Journal of Hazardous Materials | Year: 2013

The insensitive high-explosive PAX-21 was the first of its kind fielded in an artillery munition by the United States military. This formulation contains three main components: RDX, dinitroanisole, and ammonium perchlorate (AP). In March 2012, detonation tests were conducted on PAX-21 60. mm mortar rounds to determine the energetic residues resulting from high-order and blow-in-place (BIP) detonations. Post-detonation residues were sampled and analyzed for the three main PAX-21 components. Concentrations of RDX and dinitroanisole in the samples were quite low, less than 0.1% of the munitions' original organic explosive filler mass, indicating high order or near high order detonations. However, disproportionately high concentrations of AP occurred in all residues. The residues averaged 15% of the original AP following high-order detonations and 38% of the original AP mass following the BIP operations. There was no correlation between AP residues and the RDX and dinitroanisole. Perchlorate readily leached from the detonation residues, with over 99% contained in the aqueous portion of the samples. Use of these rounds will result in billions of liters of water contaminated above drinking water perchlorate limits. As a result of this research, PAX-21 mortar rounds are currently restricted from use on US training ranges. © 2013. Source

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