Quality Specifications and Analysis

Various concentrations and purities of aqueous ammonia are on the market. Mostly, the concentration is 25-30% NH3 and the iron content less than 10 ppm. Shipping in pressure vessels is necessary for ammonia contents above 25 % because of its elevated vapor pressure. For more stringent purity requirements for aqueous ammonia, the containers should be made of seawater-resistant aluminum (magnesium alloyed) or austenitic steels. 

Analysis. Ammonia is readily detectable in air in the range of a few parts per million by its characteristic odor and alkaline reaction. Specific indicators, such as Nessler s reagent (Hgf in KOH), can detect ammonia in a concentration of 1 ppm. For the quantitative determination of ammonia in air, synthesis gas, and aqueous solutions, individual (manual) and continuous (recorded) analyses can be made (for a measure- 

Normally, the water content of liquid ammonia is determined volumetrically as the ammonia-containing residue on evaporation or gravimetrically by fully vaporizing the ammonia sample and absorbing the water on KOH. 

The oil content of liquid ammonia can be tested gravimetrically by first evaporating the ammonia liquid and then concentrating the ether extract of the residue. Iron, aluminum, calcium (ammonia catalyst) and other impurities can then be determined in the ether-insoluble residue. 

The inert gas content is analyzed volumetrically after the vaporized ammonia has been absorbed in water. Then the inert gas composition is analyzed chromatographi-cally. 

International, technical specifications for chromium oxide pigments are defined in ISO 4621 (1986), they must have a minimum Cr2Oa content of 96 wt%. 

Various grades are defined according to their particle fineness as measured by the residue on a 45-pm sieve grade 1, 0.01 % residue (max.) grade 2, 0.1 % (max.) and grade 3, 0.5% (max.). 

ISO 4621 (1986) also specifies analytical methods. Usually, analysis of chromium and the byproducts is preceded by melting with soda and sodium peroxide. The content of water-soluble or acid-soluble chromium is becoming important from the toxicological and ecological point of view. It is determined according to DIN 53 780 with water, or according to ISO 3856, part 1 with 0.1 mol/L hydrochloric acid. 

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Hall, K.R., Yarborough, L, Lindsay, R., Kilmer, J., Fling, W., Calculation of Gross Heating Value for a Saturated Gas from Compositional Analysis, International Congress of Gas Quality—Specification and Measurement of Physical and Chemical Propeties of Natural Gas, Gronigen, The Netherlands (1986), April. 

This proliferation in the use of color additives was soon recognized as a threat to the public s health. Of particular concern were the practices of adding poisonous colorants to food, and of using dyes to hide poor quality or to add weight or bulk to certain items. References 5-14 provide additional information on the history of food colorants and their regulation. Reference (15) provides more information regarding the applications, properties, specifications, and analysis of color additives, as well as methods for the determination of colorants in products. 

There will be a continued need for enantiospecific methods of preparation and analysis, not only to ensure the quality of the final drug substance and reference materials, but also to control starting materials used for their manufacture, and key intermediates during synthesis. Likewise, specific and sensitive bioanalytical methods will be required to follow the fate of individual enantiomers after their administration. 

Quality control tests are intended to detect produced materials which deviate from manufacturing specifications, and thus may result in questionable performance. The materials are usually subjected to spectrographic analysis which is the primary quality control check. The exposure tests are necessarily of short duration (hours or days), in which the test conditions attempt to reflect the environment of operation, for example using artificial seawater for a marine application. Since a property that is reproducible and indicative of a consistent quality anode is all that is required, there is no attempt to mirror, except in the crudest fashion, current density profiles. 

In a modern industrialised society the analytical chemist has a very important role to play. Thus most manufacturing industries rely upon both qualitative and quantitative chemical analysis to ensure that the raw materials used meet certain specifications, and also to check the quality of the final product. The examination of raw materials is carried out to ensure that there are no unusual substances present which might be deleterious to the manufacturing process or appear as a harmful impurity in the final product. Further, since the value of the raw material may be governed by the amount of the required ingredient which it contains, a quantitative analysis is performed to establish the proportion of the essential component this procedure is often referred to as assaying. The final manufactured product is subject to quality control to ensure that its essential components are present within a pre-determined range of composition, whilst impurities do not exceed certain specified limits. The semiconductor industry is an example of an industry whose very existence is dependent upon very accurate determination of substances present in extremely minute quantities. 

The nature of the performance metric, y, is determined by the characteristics of the specific process under analysis. Since we are particularly interested in analyzing situations where y is related to product or process quality, it is quite common to find systems where a categorical variable y is chosen to classify and evaluate their performance. This may happen due to the intrinsic nature of y (e.g., it can only be measured and assume qualitative values, such as good, high, and low ), or because y is derived from a quantization of the values of a surrogate continuous measure of performance (e.g., y = good if some characteristic z of the product has value within the range of its specifications, and y= bad, otherwise). 

Unfortunately these and other existing quality control procedures do not answer aU problems. There remains a clear need for development of PCR reference materials that win provide information both on quality and quantity levels. For quality the reference materials should be host-specific and PCR primers, for positive control, may correspond to host specific house keeping genes e.g. b-actin. For quantitative analysis, fluorescence dyes in specific primers might be used in order to measure accurately the amount of DNA present. Such practices, and other as yet un-realized procedures, will be needed to achieve reliable results in the quantification of DNA analysis. 

The use of reference samples for method calibration and development/validation occurred hand-in-hand with the development of all modern instrumental methods of analysis. In fact, the two developments are intimately linked with one another. As already noted, G-i and W-i (Fairbaim et al. 1951 Stevens i960) illustrate first instance of reference samples specifically developed for calibration purposes. Following that, the use of BCR-i as a reference sample throughout the lunar program (Science 1970) is a prime illustration of the quality assurance and method validation applications in large-scale inter-laboratory measurement programs. 

Sample preparation consists of homogenization, extraction, and cleanup steps. In the case of multiresidue pesticide analysis, different approaches can have substantially different sample preparation procedures but may employ the same determinative steps. For example, in the case of soil analysis, the imidazolinone herbicides require extraction of the soil in 0.5 M NaQH solution, whereas for the sulfonylurea herbicides, 0.5M NaOH solution would completely decompose the compounds. However, these two classes of compounds have the same determinative procedure. Some detection methods may permit fewer sample preparation steps, but in some cases the quality of the results or ruggedness of the method suffers when short cuts are attempted. For example, when MS is used, one pitfall is that one may automatically assume that all matrix effects are eliminated because of the specificity and selectivity of MS. 

Capillary HPLC-MS has been reported as a confirmatory tool for the analysis of synthetic dyes [585], but has not been considered as a general means for structural information (degradant identification, structural elucidation or unequivocal confirmation) positive identification of minor components (trace component MW, degradation products and by-products, structural information, thermolabile components) or identification of degradation components (MW even at 0.01 % level, simultaneous mass and retention time data, more specific and much higher resolution than PDA). Successful application of LC-MS for additive verification purposes relies heavily and depends greatly on the quality of a MS library. Meanwhile, MB, DLI, CF-FAB, and TSP interfaces belong to history [440]. 

If one wishes to predict the future of additive analysis in polymers, it is relevant to consider the prospects of further evolution of polymeric and additive materials the influence of legislation and environment instrumental developments and currently unsolved problems. It then becomes clear that additive analysis stands a fair chance remaining in use for some time, certainly in a strongly competitive environment, which will require improved product design specifications, quality assurance and research for new applications. As ideal production environments are rare, customer complaints will also require continuous attention. Government regulations are another reason for continuous analytical efforts. 

The purpose of this monograph, the first to be dedicated exclusively to the analytics of additives in polymers, is to evaluate critically the extensive problemsolving experience in the polymer industry. Although this book is not intended to be a treatise on modem analytical tools in general or on polymer analysis en large, an outline of the principles and characteristics of relevant instrumental techniques (without hands-on details) was deemed necessary to clarify the current state-of-the-art of the analysis of additives in polymers and to accustom the reader to the unavoidable professional nomenclature. The book, which provides an in-depth overview of additive analysis by focusing on a wide array of applications in R D, production, quality control and technical service, reflects the recent explosive development of the field. Rather than being a compendium, cookery book or laboratory manual for qualitative and/or quantitative analysis of specific additives in a variety of commercial polymers, with no limits to impractical academic exoticism (analysis for its own sake), the book focuses on the fundamental characteristics of the arsenal of techniques utilised industrially in direct relation... 

The second question concerns the quality of the chemical control, directed more at the chemical analysis proper and its procedure. Important factors here are sufficient specificity and accuracy together with a short analysis time. In connection with accuracy, we can possible consider the quantization of the analytical information obtainable. For instance, from the above example of titration, if we assume for the pH measurement an accuracy of 0.02, an uncertainty remains of 0.04 over a total range of 14.0, which means a gain in information of n1 = 14.0/0.04 = 350 (at least 8 bits) with an accuracy of 5% as a mean for the titration end-point establishment of both acids, the remaining uncertainty of 1% over a range of 2 x 100% means a gain in information of n2 = 200 (at least 7 bits), so that the two-dimensional presentation of this titration represents a quantity of information I = 2log nx n2 = 15 bits at least. 

Laboratory analysis provides data that will be used as the basis for decision-making. The data require that the analysis of samples in laboratories meets specific quality assurance and quality control (QA/QC) requirements. 

Quality assurance (QA) is a generic term for all activities required to maintain quality in analytical results. These include laboratory management structures and sample documentation procedures, as well as the more practical sample preparation and analysis requirements (as described above). The ISO (International Organization for Standardization) develops standards across a wide range of areas, from screw threads to banking cards. The majority of ISO standards are specific to certain areas they are documented agreements containing technical specifications or precise criteria to be used... 

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