Primary standard chemicals

What is the P in KHP Draw the structure of KHP. Tell why it is useful as a primary standard chemical. 

What is the name of the chemical often referred to as THAM or TRIS What is its structure It does not contain OFT ions, yet it is a base. Explain. Tell why it is useful as a primary standard chemical. 

Standard solution Potassium dichromate can be prepared as a primary-standard chemical by recrystallization from water and drying at 150°C. Its standard solutions, usually prepared by direct weight, are extraordinarily stable. Carey found that a 0.017 M solution did not change appreciably in titer in 24 years. Dichromate reacts less readily with organic matter than does permanganate and does not react with chloride in acid solutions in the cold at concentrations less than 3 M hydrochloric acid. 

Standard substances in clinical chemistry include primary standards, which can be obtained sufficiently pure to be used for the preparation of solutions by weighing or by reference to other definable physical characteristics (e.g., constant-boiling hydrochloric acid). Primary standard chemicals are available for acid-base reactions, precipitation reactions, oxidation-reduction reactions, etc. (V3), and are used in these various categories of analytical determination to validate the preparation of solutions of other chemical substances which cannot be obtained in a form suitable to meet the criteria demanded for a primary standard. Following their calibration in terms of a primary standard, these other chemieals can act as secondary standards. 

The criteria which a primary standard chemical substance should satisfy are fully stated in many textbooks (e.g., V3), and few compounds satisfactorily meet all these exacting requirements. Furthermore, the primary standards of quantitative inorganic analysis are, for the most part, made to take part in reactions occurring in aqueous protein-free solution during the calibration of secondary standards the conditions under which these secondary standardizations are performed are as nearly ideal as possible, and solutions are kept free from contaminants which might interfere with the stoichiometry of the reactions. 

The different grades of chemicals are listed on the back cover of the text. In general, only American Chemical Society (ACS) reagent-grade or primary standard chemicals should be used in the analytical laboratory. 

In addition to commercial producers, the National Institute of Standards and Technology supplies primary standard chemicals. NIST Special Publication 260 catalogs standard reference materials. (See http //ts.nist.gov/ts/htdocs/23Q/232/232.htm for information on the SRM program and lists of reference standards.) Reference standards are complex materials, such as alloys that have been carefully analyzed for the ingredients and are used to check or calibrate an analytical procedure. 

National Institute of Standards and Technology (NIST). The NIST is the source of many of the standards used in chemical and physical analyses in the United States and throughout the world. The standards prepared and distributed by the NIST are used to caUbrate measurement systems and to provide a central basis for uniformity and accuracy of measurement. At present, over 1200 Standard Reference Materials (SRMs) are available and are described by the NIST (15). Included are many steels, nonferrous alloys, high purity metals, primary standards for use in volumetric analysis, microchemical standards, clinical laboratory standards, biological material certified for trace elements, environmental standards, trace element standards, ion-activity standards (for pH and ion-selective electrodes), freezing and melting point standards, colorimetry standards, optical standards, radioactivity standards, particle-size standards, and density standards. Certificates are issued with the standard reference materials showing values for the parameters that have been determined. 

In titrimetry certain chemicals are used frequently in defined concentrations as reference solutions. Such substances are referred to as primary standards or secondary standards. A primary standard is a compound of sufficient purity from which a standard solution can be prepared by direct weighing of a quantity of it, followed by dilution to give a defined volume of solution. The solution produced is then a primary standard solution. A primary standard should satisfy the following requirements. 

A number of methods are available for following the oxidative behaviour of food samples. The consumption of oxygen and the ESR detection of radicals, either directly or indirectly by spin trapping, can be used to follow the initial steps during oxidation (Andersen and Skibsted, 2002). The formation of primary oxidation products, such as hydroperoxides and conjugated dienes, and secondary oxidation products (carbohydrides, carbonyl compounds and acids) in the case of lipid oxidation, can be quantified by several standard chemical and physical analytical methods (Armstrong, 1998 Horwitz, 2000). 

The history of reference materials is closely linked with the development of analytical chemistry. In the 19th Century all chemicals were, in comparison with those of today, of poor purity. Thus, for volumetric analysis suitable purified materials as primary standards had to be specified. One of the first examples was the recommendation of As(III) oxide by Gay-Lussac (1824) for this purpose. Somewhat later, Sorensen (1887) proposed criteria for the selection of primary chemical standards. These were further elaborated by Wagner (1903) at the turn of the last century. It is worthwhile mentioning that their criteria were quite similar to those used today. 

The application of electroanalysis in non-aqueous media to a certain analytical problem requires a well considered selection of the solvent together with a suitable electroanalytical method, which can be carried out on the basis of the solvent classes mentioned in Table 4.3 and of the related theories. The steps to be taken include the preparation of the solvent and the apparatus for the electroanalytical method proper, together with other chemicals, especially when the method includes titration. Much detailed information on the purification of the solvents and on the preparation of titrants and primary standards can be found in the references cited in Section 4.1 and in various commercial brochures1,84,85 and books17,86-89 we shall therefore confine ourselves to some remarks on points of major importance. 

They used the titration method of Tsunogai et al. [157]. The titrant solutions were standardised against calcium carbonate of primary standard quality (99.9975% purity) rather than zinc, and the EGTA (Eastman Chemicals) was used without further purification. 

It is important that a measurement made in one laboratory by a particular analyst can be repeated by other analysts in the same laboratory or in another laboratory, even where the other laboratory may be in a different country. We aim to ensure that measurements made in different laboratories are comparable. We are all confident that if we measure the length of a piece of wire, mass of a chemical or the time in any laboratory, we will get, very nearly, the same answer, no matter where we are. The reason for this is that there are international standards of length, mass and time. In order to obtain comparable results, the measuring devices need to be calibrated. For instance, balances are calibrated by using a standard mass, which can be traced to the primary mass standard (see also Chapter 5). The primary standard in chemistry is the amount of substance, i.e. the mole. It is not usually possible to trace all of our measurements back to the mole. We generally trace measurements to other SI units, e.g. mass as in 40 mg kg-1 or trace back to reference materials which are themselves traceable to SI units. 

The reported, 29Xe NMR chemical shifts. Values in italic were referenced to XeF2 in MeCN as primary standard. h The, 29Xe NMR chemical shifts were referenced to XeOF4 (24 °C) and extrapolated to -30 °C if measured at other temperature (53). c, 3C NMR 6 81.2 (d, 2J(C-2,Xe) = 69 Hz, C-2). 

For standardizing a base solution, primary standard grade potassium biphthalate is a popular choice. Also called potassium hydrogen phthalate, potassium acid phthalate, or simply KHP, it is the salt representing partially neutralized phthalic acid and is a monoprotic weak acid. The true formula is KHC8H404. Figure 5.8 shows the chemical structure of phthalic acid and KHP. The reaction with a base is as follows ... 

Modern-day chemical analysis can involve very complicated material samples—complicated in the sense that there can be many substances present in the sample, creating a myriad of problems with interferences when the lab worker attempts the analysis. These interferences can manifest themselves in a number of ways. The kind of interference that is most famihar is one in which substances other than the analyte generate an instrumental readout similar to the analyte, such that the interference adds to the readout of the analyte, creating an error. However, an interference can also suppress the readout for the analyte (e.g., by reacting with the analyte). An interference present in a chemical to be used as a standard (such as a primary standard) would cause an error, unless its presence and concentration were known (determinant error, or bias). Analytical chemists must deal with these problems, and chemical procedures designed to effect separations or purification are now commonplace. 

There is often some confusion between the terms standards and reference materials. Primary standards represent the top-tier of chemical standards and, in principle, provide a means of establishing the traceability of analytical data to the SI measurement units (e.g., the kilogram, mole, meter, and second). A limited number of pure chemicals are recognized as primary standards (and thus can constitute certified reference materials). Most certified reference materials are not of themselves primary standards rather, the property values assigned to them are traceable to primary standards where practical. 

Potassium hydrogen phthalate has many uses in analytical chemistry. It is a primary standard for standardization of bases in aqueous solutions. Its equivalent weight is 204.2. It also is a primary standard for acids in anhydrous acetic acid. Other applications are as a buffer in pH determinations and as a reference standard for chemical oxygen demand (COD). The theoretical COD of a Img/L potassium hydrogen phthalate is 1.176mg O2. 

Primary standards are stable chemical compounds that are available in high purity and which can be used to standardise the standard solutions used in titrations. Titrants such as sodium hydroxide or hydrochloric acid cannot be considered as primary standards since their purity is quite variable. So for instance sodium... 

Now consider a primary standard buffer containing 0.025 0 m KH2P04 and 0.025 0 m Na2HP04. Its pH at 25°C is 6.865 0.006.4 The concentration unit, m, is molality, which means moles of solute per kilogram of solvent. For precise chemical measurements, concentrations are often expressed in molality, rather than molarity, because molality is independent of temperature. Tabulated equilibrium constants usually apply to molality, not molarity. Uncertainties in equilibrium constants are usually sufficiently great so that the 0.3% difference between molality and molarity of dilute solutions is unimportant. 

The network at the top of the traceability system providing the primary standards for chemical measurements consists at present of four institutes as shown in Fig. 2. 

Keywords Amount of substance standards Chemical composition standards Traceability Third party assessment Primary reference materials... 

Present-day analytical laboratories are increasingly under pressure to supply objective evidence of their technical competence, of the reliability of their results and performance, and to seek formal certification or accreditation. This pressure may come from the laboratory s customers (e.g., industry and national bodies) but may also be due to scientific considerations. A QM system in place, validation of methods, uncertainty evaluation, the use of primary standards and CRMs, participation in ILCs, and PT, all serve to assure and demonstrate the quality of measurements. Compared to, say, 30 years ago, the stability of the equipment now available is much improved, and a greater range of RMs for method validation and calibration is accessible. Nevertheless, to achieve mutual (international) acceptance of various bodies of evidence for QA activities, a number of protocols have been developed. The most widely recognized protocols used in chemical measurements and testing are the ISO Guide 9000 2000, ISO/IEC 17025 2005, and OECD Guidelines for GLP, as well as its national and sector equivalents. 

In this scheme, the primary reference material is defined as a chemical substance of the highest (and known) purity, or a well-characterized substance in a matrix, This classification of materials is, however, fairly arbitrary. It is ideal when used in connection with standards characterized in terms of biological activity. Primary standards are thus the International Reference Preparations (IRP) produced by the World Health Organization (WHO). In this case the primary standard for a particular antibiotic is the WHO reference preparation which constitutes the unit of that antibiotic. When people wish to use it they have to prepare a large batch of samples calibrated to the primary. This is then called a secondary standard. However, for well-defined chemical parameters, the term certified reference material is preferred. 

Primary standard — (in titrimetry) A highly purified and chemically stable reagent that can be dissolved in the solvent of choice to serve as reference material for the -> titration of a proper analyte. A primary standard reagent must react rapidly, completely, and stoichiomet-rically with the analyte, as well as having a reasonably large molar mass [i]. 

Secondary standard — (in titrimetry) A chemically stable compound whose active agent contents have been established by its -> titration with a primary standard to be subsequently used as -> titrant [i]. 

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