Sample Analytical Report

The FDA Guidance document (FDA 2001) provides a good model for analytical reports in general. Flowever, since the publication of that document additional details are commonly addressed (Viswanathan 2007). Table 10.8 was drawn from these publications and although the documents specifically address reporting requirements for bioanalyt-ical analysis in support of drug development studies, they provide an excellent overview of the requirements for a analytical report in general. 

---

A validation report that describes overall conduct of the validation, and includes all of the relevant tables needed to support the interpretation of results and final conclusions, should be written prior to initiating sample analysis. The report should be assigned a unique identification number that can be used as a reference in the sample analytical report. A cover page should contain, at a minimum, the name and address of the laboratory and the report and amendment number (if applicable). A signature page that includes, at a minimum, the author(s), reviewer(s) and laboratory management should also be included. 

Table 10.8 Minimum requirements of the sample analytical report...

Mass Sample (g) True Mass of Analyte (g) Proportional Error (%) Mass of Analyte Determined (g) Percent Analyte Reported (%w/w)... 

Finally, we have seen that the detection limit is a statistical statement about the smallest amount of analyte that can be detected with confidence. A detection limit is not exact because its value depends on how willing we are to falsely report the analyte s presence or absence in a sample. When reporting a detection limit, you should clearly indicate how you arrived at its value. 

In preceding chapters we have indicated which tools are nowadays being used routinely or currently are under development. General trends are higher sensitivity, more information, and faster and further automation. Automatic analyses are nice (sample in, report out), but interactive analysis tools are better. It is not realistic to expect the need for more analyses. Some future needs are more reliable quantitation, reference materials and simplification of data management. A particular problem in additive analysis concerns accuracy and traceability. In many cases, extractable rather than total concentration is determined. There are still many quantitative analytical methods waiting to be developed. It is here that the field will advance. Table 10.31 lists some proposed (r)evolutionary developments in polymer/additive analysis. 

No specific information was found on the releases of diisopropyl methylphosphonate to soil. However, diisopropyl methylphosphonate has been detected in soils at the RMA (Williams et al. 1989). Concentrations of diisopropyl methylphosphonate in live surface soil samples at the RMA ranged from <0.05 to 0.24 mg/kg (Williams et al. 1989). Concentrations of diisopropyl methylphosphonate in surface soil samples measured during the Remedial Investigation/Feasibility Study (RI/FS) at RMA ranged from less than the analytical limit of 0.114 mg/kg to 11 mg/kg (Ebasco Services 1991). The most recent sampling conducted in 1995 indicated the concentrations of diisopropyl methylphosphonate in the onpost surface soil samples were less than the analytical reporting limit of 0.342 mg/kg (D.P. Associates 1995). 

In 1997, concentrations of diisopropyl methylphosphonate in onpost groundwater samples at the RMA ranged from less than the analytical reporting limit of 0.2 g/L to 1,500 g/L (USGS 1998). Concentrations of diisoproply methylphosphonate in onpost surface water samples at the RMA ranged from less than the analytical reporting limit of 0.2 g/L to 0.581 g/L. 

The most recent onpost sediment sampling occurred in 1990. All concentrations of diisopropyl methylphosphonate in sediment samples measured during the RI at RMA were less than the analytical reporting limits, which ranged from 0.05 mg/kg to 1.0 mg/kg (Ebasco Services Inc. 1992). Diisopropyl methylphosphonate has not been detected in sediment samples near the RMA. The most recent sampling for diisopropyl methylphosphonate occurred in 1990 and all the results were less than the analytical reporting limit of 1.0 mg/kg (Harding Lawson Associates 1992). 

Analytical methods for determining disulfoton in environmental samples are reported in Table 6-2. The steps included in the methods are solvent extraction, purification and fractionation, and gas chromatographic analysis. Other analytical techniques, including capillary gas chromatography with mass selective detection (Stan 1989), high-performance liquid chromatography with either mass spectrometric (MS) or MS-MS detection (Betowski and Jones 1988), have been used to determine disulfoton in environmental samples. 

Of these, the fluorescence approach described by Thompson and Reynolds [17] and modified by Thompson and Godden [18] has proved to be the most sensitive. Godden and Stockwell [12] have described a specific fluorescence system tailored for mercury determination in more detail. P.S. Analytical has developed a fuUy automated system from these initial developments to measure mercury produced from the samples, to quantify the data and provide precise analytical reports, using an IBM compatible computer and custom software. 

Hammersma,. W. and Reynolds, S. L., Field Test Sampling/Analytical Strategies and Implementation Cost Estimates Coal Gasification and Flue Gas Desulfurization. U. S. Environmental Protection Agency Report, EPA-600/2-76-093b, NTIS No. PB 254-166/AS (4/76). 

The DMHP used in these tests was procured from Shell Development Corporation or made at Edgewood. Analytic information on the test material is not available, but some Edgewood-prepared samples were reported to have a purity of 98%. 

Work continued in 1960-1963 in the Ohio Range (formerly called the Central Range of the Horlick Mountains) to procure coal for accurate analysis. Samples of outcrop coal and one excellent sample of coal from an adit opened in one bed were collected. Coal samples were taken in 1959 by John J. Mulligan (31) at Mount Gran in the vicinity of Frank Debenham and McKenzie Taylor s old Mount Suess locality. The following season Mulligan (32) sampled coal farther inland in the Willett Range. Brown and Taylor (6) published an analytic report on coal from the Theron Mountains in 1961. 

Deposit sample analysis and report interpretation. A minimum of 1 to 2 ounces (25 to 50 grams approximately) is usually required for analysis. Precise details are required concerning the point of sampling from the cooling system, also the date, time, and any relevant operating information and observations. Deposit samples are almost always dried before any further analytical work is undertaken and the results are typically scaled to 100% dried material. (A comparison of visual observations, from the time and place of sampling, with subsequent analytical reports, can provide valuable experience for evaluating similar problems in the future.)... 

The raw data and the hardcopy analytical results for original analysis and all reanalyses become part of the sample file. They are maintained as a permanent analytical record and may become part of a data package deliverable to the client. The sample and laboratory QC sample results are transferred into the LIMS for the generation of final analytical reports. 

Common conventions for reporting of environmental sample analytical results are as follows ... 

All activities and factual findings during the inspection period are reported in the Preliminary Findings (PF, for all inspections except CWDF) or monthly Interim Report (IR, for continuous monitoring CWDF inspections) (see CWC VA Part II Paragraph 60). An inspection report includes annexes concerning samples taken and analytical results. As part of these Annexes, an on-site Analytical Report is attached, which consists of... 

Analytical method the complete process used to determine an analyte or analytes in a sample. The analytical method documents all the individual steps in the process from sampling to reporting the results. 

The Handbook has been divided into six main parts of which the first four address the logical progression of an analytical measurement from obtaining a sample to reporting the result. Clearly there are many ways in which such a complex process can be divided but the authors believe that it is helpful to both students and practising analysts to address it in tenns of ... 

---