Reference standard material concentration determination

All instrumental analytical methods except coulometry (Chapter 15) require calibration standards, which have known concentrations of the analyte present in them. These calibration standards are used to establish the relationship between the analytical signal being measured by the instrument and the concentration of the analyte. Once this relationship is established, unknown samples can be measured and the analyte concentrations determined. Analytical methods should require some sort of reference standard or check standard. This is also a standard of known composition with a known concentration of the analyte. This check standard is not one of the calibration standards and should be from a different lot of material than the calibration standards. It is run as a sample to confirm that the calibration is correct and to assess the accuracy and precision of the analysis. Reference standard materials are available from government and private sources in many countries. Government sources include the National Institute of Standards and Technology (NIST) in the US, the National Research Council of Canada (NRCC), and the Laboratory of the Government Chemist in the UK. 

A number of analytical methods for the separation of organic mercury compounds use an initial extraction of the organic materials with an organic solvent. Klisenko and Shmigidina [83] then converted both the inorganic mercury held in the aqueous fraction and the organic mercury in the chloroform extract to dithizonate, separated the components on chromatographic columns, and determined the concentration of the various fractions by comparison with reference standards. This method is semi-quantitative at best. 

If a blank material, that is, the matrix of the test material without the analyte, can be analyzed a number of times, the limit of detection is often defined as three times the standard deviation of this blank determination. The limit of detection of the instrumental response is therefore yB + 3xB, where the subscript B refers to a blank determination. The corresponding concentration is then calculated from the calibration equation (equation 5.4), if it may be assumed that the equation is valid down to that concentration ... 

Linearity of a method should be established or a series of standards selected for use with non-linear-method calibration. This can be checked by preparing and analyzing serial dilutions of aqueous reference standard solutions, quality control materials, enzyme solutions, or commercially available materials for demonstrating linearity (again, these are designed for use in human medicine) and comparing the determined values with the theoretical values calculated for the dilutions. The serial dilutions used for linearity checks can also help establish the analytical sensitivity when defined as the minimal detectable change from one concentration to another. 

The traceability of the result of a measurement is defined as the property of the result whereby it can be related to stated references, usually national (NIST, NRC, etc.) or international (CSA and EU) standards, through an unbroken chain of comparisons all with stated uncertainties, e.g.. Figure 2.1. As applied to an analytical standard, distinct from a measurement of an unknown concentration, this concept implies that the purity of the standard has been determined by a traceable sequence of analytical steps, each with a known uncertainty, that permit comparison with a certified reference material (CRM) (Section 2.2.2) from a recognized supplier. This procedure results in a Certificate of Analysis, discussed in Section 2.2.2 for CRMs and also in Section 9.4.4c with respect to the analytical (reference)... 

Analysis of Standards The analysis of a standard containing a known concentration of analyte also can be used to monitor a system s state of statistical control. Ideally, a standard reference material (SRM) should be used, provided that the matrix of the SRM is similar to that of the samples being analyzed. A variety of appropriate SRMs are available from the National Institute of Standards and Technology (NIST). If a suitable SRM is not available, then an independently prepared synthetic sample can be used if it is prepared from reagents of known purity. At a minimum, a standardization of the method is verified by periodically analyzing one of the calibration standards. In all cases, the analyte s experimentally determined concentration in the standard must fall within predetermined limits if the system is to be considered under statistical control. 

NAA is a quantitative method. Quantification can be performed by comparison to standards or by computation from basic principles (parametric analysis). A certified reference material specifically for trace impurities in silicon is not currently available. Since neutron and y rays are penetrating radiations (free from absorption problems, such as those found in X-ray fluorescence), matrix matching between the sample and the comparator standard is not critical. Biological trace impurities standards (e.g., the National Institute of Standards and Technology Standard Rference Material, SRM 1572 Citrus Leaves) can be used as reference materials. For the parametric analysis many instrumental fiictors, such as the neutron flux density and the efficiency of the detector, must be well known. The activation equation can be used to determine concentrations ... 

Standardization. Standardization in analytical chemistry, in which standards are used to relate the instrument signal to compound concentration, is the critical function for determining the relative concentrations of species In a wide variety of matrices. Environmental Standard Reference Materials (SRM s) have been developed for various polynuclear aromatic hydrocarbons (PAH s). Information on SRM s can be obtained from the Office of Standard Reference Materials, National Bureau of Standards, Gaithersburg, MD 20899. Summarized in Table VII, these SRM s range from "pure compounds" in aqueous and organic solvents to "natural" matrices such as shale oil and urban and diesel particulate materials. 

The revised database holds over 23 000 analyte values for 660 measurands and 1670 reference materials produced by 56 different producers, from 22 countries. The database is restricted to natural matrix materials (i.e. made from naturally occurring materials, excluding calibration standards manufactured from pure chemicals). Information has been extracted from the relevant certificates of analysis, information sheets, and other reports provided by the reference material producers. As a general rule, the authors have only included in the compilation reference materials for which a certificate of analysis or similar documentation is on file. Information included in the survey is on values for measurands determined in reference materials, producers, suppliers, the cost of the materials, the unit size supplied, and the recommended minimum weight of material for analysis, if available. The new searchable database has been designed to help analysts to select reference materials for quality assurance purposes that match as closely as possible, with respect to matrix type and concentrations of the measurands of interest and their samples to be analyzed see Table 8.3. 

Accuracy of in vivo and in vitro measurements of americium is determined through the use of standard, certified radioactive sources with known concentrations of americium. The primary source of certified americium standards is the National Institute of Standards and Technology (NIST). Standard solutions are available for241 Am (SRM 4322, 40 Bq/g [1.1 nCi/g]) and 243Am (SRM 4332, 40 Bq/g [1.1 nCi/g]). Standard Reference Materials for human lung (SRM 4351) and human liver (SRM 4352) are also available from NIST. 

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