Analytical specifications for

Table 12. Chemical Compositions and Analytical Specifications for Chromate Corrosion Inhibiting Pigments...

The design equations can be used in a simple computer program to report the basic data and print the column and analytical specifications for any particular analysis carried out on a specified liquid chromatograph. The program is written In the Microsoft Quick Basic language that can be used on... 

TABLE 1.6 Analytical Specifications for Coal from Selected U.S. Mines"... 

HPLC analytical specification for I (<8 ppm) was introduced. The sum of detectable contaminant peaks eluting prior to Trp was reduced to <100 ppm and the sum of those eluting after Trp was reduced to <300 ppm. This case, more than any other, has served to reinforce the FDA s position on the vital importance of building quality into process operations. 

The API Assay, the Assay of Impurities and Product Stability. The central independent analytical research and quality control unit is responsible for the analytical release of both the API and the formulated drug product for the drug development programs. The central independent QC unit provides all the analytical data needed to build the analytical specification for the IND. It is recognized by those involved that the IND is a relatively raw document compared with the later NDA, which is built on data from a more developed process situation, using more refined analytical techniques. 

Qualifying a third party requires that detailed synthesis, analytical, and GMP information are provided to the third party. This is usually passed to the third party in a technology transfer package (see later). Eventually the third party is registered in the NDA as a supplier who has committed to meet an agreed analytical specification. For materials well back in the synthesis and for raw materials, including solvents, one may need no more than basic analytical release information—appearance, identity, purity (sometimes it may be necessary to set limits on specific impurities). 

Table 6.8. Analytical specifications for turmeric (whole and powder).

Increasing Analyte Specificity for Mass Spectral Images Alternative Source Options for Mass Spectral Imaging 14.6 Conclusions... 

Increasing Analyte Specificity for Mass Spectral Images... 

Ah initio trajectory calculations have now been performed. However, these calculations require such an enormous amount of computer time that they have only been done on the simplest systems. At the present time, these calculations are too expensive to be used for computing rate constants, which require many trajectories to be computed. Semiempirical methods have been designed specifically for dynamics calculations, which have given insight into vibrational motion, but they have not been the methods of choice for computing rate constants since they are generally inferior to analytic potential energy surfaces fitted from ah initio results. 

To examine a sample by inductively coupled plasma mass spectrometry (ICP/MS) or inductively coupled plasma atomic-emission spectroscopy (ICP/AES) the sample must be transported into the flame of a plasma torch. Once in the flame, sample molecules are literally ripped apart to form ions of their constituent elements. These fragmentation and ionization processes are described in Chapters 6 and 14. To introduce samples into the center of the (plasma) flame, they must be transported there as gases, as finely dispersed droplets of a solution, or as fine particulate matter. The various methods of sample introduction are described here in three parts — A, B, and C Chapters 15, 16, and 17 — to cover gases, solutions (liquids), and solids. Some types of sample inlets are multipurpose and can be used with gases and liquids or with liquids and solids, but others have been designed specifically for only one kind of analysis. However, the principles governing the operation of inlet systems fall into a small number of categories. This chapter discusses specifically substances that are normally liquids at ambient temperatures. This sort of inlet is the commonest in analytical work. 

The AGS Book. The ACS book, Feagent Chemicals—zA.CS Specifications, estabhshes a standard of quahty for reagents to be used in precise analytical work, for which purpose it contains both specifications and testing methods for some 350 reagent chemicals. 

The physical techniques used in IC analysis all employ some type of primary analytical beam to irradiate a substrate and interact with the substrate s physical or chemical properties, producing a secondary effect that is measured and interpreted. The three most commonly used analytical beams are electron, ion, and photon x-ray beams. Each combination of primary irradiation and secondary effect defines a specific analytical technique. The IC substrate properties that are most frequendy analyzed include size, elemental and compositional identification, topology, morphology, lateral and depth resolution of surface features or implantation profiles, and film thickness and conformance. A summary of commonly used analytical techniques for VLSI technology can be found in Table 3. 

The general analytical chemistry of manganese is discussed elsewhere (162—167). A review covering more modem techniques, specifically for manganese dioxide, has also been pubUshed (168). A series of analytical techniques and procedures have been developed to study the metaboHc fate of manganese (169,170). 

Quality Control. Reproducible production of perfumes requires careful quality control of all materials used as well as the compounding process itself. The use of analytical tools has iacreased over the years with their availability, but there can be no substitute for organoleptic evaluation. The human nose is far more sensitive than any analytical instmment for certain materials, yet it is also quite limited as a quantitative tool and is subject to fatigue. There are also weU-documented examples of specific anosmias ia iadividuals, ie, iaability to smell certain odor types, which is somewhat analogous to color-blindness. 

Manufacturing, analytical, and quaUty control procedures are thus estabhshed. Specifications for taw and in-process materials, as well as for final products per USP/NF and in-house standards are also determined. Process and formula vaUdation assures that each technological procedure in manufacture accomplishes its purpose most efficiently, eg, blending times for powdered mixtures in tableting, and that each formula ingredient is present in optimal concentrations (12). Thus, it serves to ensure process control (qv), reproducibiUty, and content uniformity. 

Analytical and Test Methods. Ash in isophthahc acid refers to the residue left after combustion of the sample. Ash consists of oxides of trace metals that are deterrnined individually by atomic absorption or inductively coupled plasma. A Kad Fischer titration is specific for the water content. 

Specifications for sulfuric acid vary rather widely. Exceptions include the federal specifications for "Sulfuric Acid, Technical" and "Sulfuric Acid, Electrolyte (for storage batteries)" and the Food Chemicals Codex specification for sulfuric acid, frequentiy called food-grade acid (although industrywide, "food-grade" is nonspecific). Very Httie has been done to estabUsh industry-wide analytical standards in the United States, except for development of the ASTM analytical methods, designated as E223-88 and summarized in Table 12. 

Measurement and specification of nitrates or other nitrogen oxide compounds in sulfuric acid is a complex subject. The difficulty occurs because nitrogen oxides are usually present both as nitrous and nitric compounds, predominantiy in the nitrous form. Hence, analytical procedures specific for nitrates only do not give a complete analysis. 

Tar. Before the development of gas chromatography (gc) and high pressure Hquid chromatography (hplc), the quantitative analyses of tar distillate oils involved tedious high efficiency fractionation and refractionation, followed by identification or estimation of individual components by ir or uv spectroscopy. In the 1990s, the main components of the distillate fractions of coal tars are deterrnined by gc and hplc (54). The analytical procedures included in the specifications for tar bulk products are given in the relevant Standardi2ation of Tar Products Tests Committee (STPTC) (33), ISO (55), and ASTM (35) standards. 

An excellent overview of vitamin analytics is available (13). Specifications for the vitamins are available for food use (14) and pharmaceutical use (15). 

Both nicotinic acid and nicotinamide have been assayed by chemical and biological methods. Owing to the fact that niacin is found in many different forms in nature, it is important to indicate the specific analyte in question. For example, if biological assay procedures are used, it is necessary to indicate whether the analysis is to determine the quantity of nicotinic acid or if niacin activity is the desired result of the analysis. If nicotinic acid is desired, then a method specific for nicotinic acid should be used. If quantitation of niacin activity is the desired outcome, then all compounds (bound and unbound) which behave like niacin will assay biologically for this substance (1). 

There are several comprehensive reviews of analytical methods for vitamin K (19,20). Owiag to the preseace of a aaphthoquiaoae aucleus, the majority of analytical methods use this stmctural feature as a basis for analysis. Several identity tests such as its reaction with sodium bisulfite or its uv spectmm exploit this characteristic. Although not specific, titrimetric, polarographic, and potentiometric methods have also been used (20). 

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