Methods Quantitative determination

UNI 8490-7 1984 Aqueous dispersions of polymers and copolymers. Test methods Quantitative determination of plasticizer in dispersions of homo- and copolymers of vinyl acetate. 

Carius method The quantitative determination of S and halogens in covalent (organic) compounds by complete oxidation of the compound with cone, nitric acid and subsequent estimation of precipitated AgX or BaS04. 

A method for determining the SO, content of oleum is described in the author s Text Book 0/ Quantitative Inorganic Analysis Theory and Practice, Second Edition, 1951, p. 263 (Longmans, Green and Co. Ltd.). 

Aminothiazole present in urine or blood plasma forms a colored Schiff base when 5-nitrofurfural is added the colorimetric analysis of the Schiff base allows the quantitative determination of this thiazole (1571). The Schiff base may also be dosed by polarographic of spectro-photometric methods (1572). 

Perhaps the most common type of problem encountered in the analytical lab is a quantitative analysis. Examples of typical quantitative analyses include the elemental analysis of a newly synthesized compound, measuring the concentration of glucose in blood, or determining the difference between the bulk and surface concentrations of Cr in steel. Much of the analytical work in clinical, pharmaceutical, environmental, and industrial labs involves developing new methods for determining the concentration of targeted species in complex samples. Most of the examples in this text come from the area of quantitative analysis. 

A spectrophotometric method for the quantitative determination of Pb + levels in blood yields an Sjtand of 0.474 for a standard whose concentration of lead is 1.75 ppb. How many parts per billion of Pb + occur in a sample of blood if Ssamp is 0.361 ... 

A second spectrophotometric method for the quantitative determination of Pb + levels in blood gives a linear normal calibration curve for which... 

A third spectrophotometric method for the quantitative determination of the concentration of in blood yields an Sjamp of 0.193 for a 1.00-mL sample of blood that has been diluted to 5.00 mb. A second 1.00-mL sample is spiked with 1.00 )J,L of a 1560-ppb Pb + standard and diluted to 5.00 mb, yielding an Sspike of 0.419. Determine the concentration of Pb + in the original sample of blood. 

A fifth spectrophotometric method for the quantitative determination of the concentration of Pb + in blood uses a multiple-point standard addition based on equation 5.6. The original blood sample has a volume of 1.00 mb, and the standard used for spiking the sample has a concentration of 1560 ppb Pb +. All samples were diluted to 5.00 mb before measuring the signal. A calibration curve of Sjpike versus Vj is described by... 

A sixth spectrophotometric method for the quantitative determination of Pb + levels in blood uses CQ+ as an internal standard. A standard containing 1.75 ppb Pb + and 2.25 ppb CQ+ yields a ratio of Sa/Sis of 2.37. A sample of blood is spiked with the same concentration of Cu +, giving a signal ratio of 1.80. Determine the concentration of Pb + in the sample of blood. 

Yang, M. J. Orton, M. L. Pawliszyn, J. Quantitative Determination of Caffeine in Beverages Using a Combined SPME-GC/MS Method, /. Chem. Educ. 1997, 74,... 

Before we are in a position to discuss the viscosity of polymer melts, we must first give a quantitative definition of what is meant by viscosity and then say something about how this property is measured. This will not be our only exposure to experimental viscosity in this volume—other methods for determining bulk viscosity will be taken up in the next chapter and the viscosity of solutions will be discussed in Chap. 9—so the discussion of viscometry will only be introductory. Throughout we shall be concerned with constant temperature experiments conducted under nonturbulent flow conditions. 

The assessment of the contribution of a product to the fire severity and the resulting hazard to people and property combines appropriate product flammabihty data, descriptions of the building and occupants, and computer software that includes the dynamics and chemistry of fires. This type of assessment offers benefits not available from stand-alone test methods quantitative appraisal of the incremental impact on fire safety of changes in a product appraisal of the use of a given material in a number of products and appraisal of the differing impacts of a product in different buildings and occupancies. One method, HAZARD I (11), has been used to determine that several commonly used fire-retardant—polymer systems reduced the overall fire hazard compared to similar nonfire retarded formulations (12). 

The preferred method of determining water in glycerol is by the Kad Fischer volumetric method (18). Water can also be determined by a special quantitative distillation in which the distilled water is absorbed by anhydrous magnesium perchlorate (19). Other tests such as ash, alkalinity or acidity, sodium chloride, and total organic residue are included in AOCS methods (13,16,18). 

The fermentation-derived food-grade product is sold in 50, 80, and 88% concentrations the other grades are available in 50 and 88% concentrations. The food-grade product meets the Vood Chemicals Codex III and the pharmaceutical grade meets the FCC and the United States Pharmacopoeia XK specifications (7). Other lactic acid derivatives such as salts and esters are also available in weU-estabhshed product specifications. Standard analytical methods such as titration and Hquid chromatography can be used to determine lactic acid, and other gravimetric and specific tests are used to detect impurities for the product specifications. A standard titration method neutralizes the acid with sodium hydroxide and then back-titrates the acid. An older standard quantitative method for determination of lactic acid was based on oxidation by potassium permanganate to acetaldehyde, which is absorbed in sodium bisulfite and titrated iodometricaHy. 

Quantitative Analysis of All llithium Initiator Solutions. Solutions of alkyUithium compounds frequentiy show turbidity associated with the formation of lithium alkoxides by oxidation reactions or lithium hydroxide by reaction with moisture. Although these species contribute to the total basicity of the solution as determined by simple acid titration, they do not react with allyhc and henzylic chlorides or ethylene dibromide rapidly in ether solvents. This difference is the basis for the double titration method of determining the amount of active carbon-bound lithium reagent in a given sample (55,56). Thus the amount of carbon-bound lithium is calculated from the difference between the total amount of base determined by acid titration and the amount of base remaining after the solution reacts with either benzyl chloride, allyl chloride, or ethylene dibromide. 

X-Ray Methods. In x-ray fluorescence the sample containing mercury is exposed to a high iatensity x-ray beam which causes the mercury and other elements ia the sample to emit characteristic x-rays. The iatensity of the emitted beam is directly proportional to the elemental concentration ia the sample (22). Mercury content below 1 ppm can be detected by this method. X-ray diffraction analysis is ordinarily used for the quaUtative but not the quantitative determination of mercury. 

Thermal decomposition of perchlorate salts to chloride, followed by the gravimetric determination of the resulting chloride, is a standard method of determining quantitatively the concentration of perchlorates. Any chlorates that are present in the original sample also break down to chloride. Thus results are adjusted to eliminate errors introduced by the presence of any chlorides and chlorates in the original sample. 

Ion-specific electrodes can be used for the quantitative determination of perchlorates in the parts per million (ppm) range (109) (see Electro ANALYTICAL techniques). This method is linear over small ranges of concentration, and is best appHed in analyzing solutions where interferences from other ionic species do not occur. 

The fire assay, the antecedents of which date to ancient Egypt, remains the most rehable method for the accurate quantitative determination of precious metals ia any mixture for concentrations from 5 ppm to 100%. A sample is folded iato silver-free lead foil cones, which are placed ia bone-ash cupels (cups) and heated to between 1000 and 1200°C to oxidize the noimoble metals. The oxides are then absorbed iato a bone-ash cupel (ca 99%) and a shiny, uniformly metaUic-colored bead remains. The bead is bmshed clean, roUed fiat, and treated with CP grade nitric acid to dissolve the silver. The presence of trace metals ia that solution is then determined by iastmmental techniques and the purity of the silver determined by difference. 

Colorimetric Methods. Numerous colorimetric methods exist for the quantitative determination of carbohydrates as a group (8). Among the most popular of these is the phenol—sulfuric acid method of Dubois (9), which rehes on the color formed when a carbohydrate reacts with phenol in the presence of hot sulfuric acid. The test is sensitive for virtually all classes of carbohydrates. Colorimetric methods are usually employed when a very small concentration of carbohydrate is present, and are often used in clinical situations. The Somogyi method, of which there are many variations, rehes on the reduction of cupric sulfate to cuprous oxide and is appHcable to reducing sugars. 

It is important to note that simulated distillation does not always separate hydrocarbons in the order of their boiling point. For example, high-boihng multiple-ring-type compounds may be eluted earher than normal paraffins (used as the calibration standard) of the same boiling point. Gas chromatography is also used in the ASTM D 2427 test method to determine quantitatively ethane through pentane hydrocarbons. 

Catechin and epicatechin are two flavanols of the catechin family. They are enantiomers. The capillary zone electrophoresis (CE) methods with UV-detection were developed for quantitative determination of this flavanols in green tea extracts. For this purpose following conditions were varied mnning buffers, pH and concentration of chiral additive (P-cyclodextrin was chosen as a chiral selector). Borate buffers improve selectivity of separation because borate can make complexes with ortho-dihydroxy groups on the flavanoid nucleus. 

In report separately discuss the peculiarities of determination of the anion composition of the solid solutions, that conditioned by ability of diphosphate anion to destruction in water solutions. In given concrete case by most acceptable method of control of the diphosphate anion in the hydrated solid solutions is a traditional method of the quantitative chromatography on the paper. Methodical ways which providing of minimum destruction of the diphosphate anion in the time of preparation of the model to analysis (translation in soluble condition) and during quantitative determination of the P.,0, anion are considered. 

Uranium and thorium are the first members of natural radioactive chain which makes their determination in natural materials interesting from geochemical and radioecological aspect. They are quantitatively determined as elements by spectrophotometric method and/or their radioisotopes by alpha spectrometry. It is necessary to develop inexpensive, rapid and sensitive methods for the routine researches because of continuous monitoring of the radioactivity level. 

Over the last seventeen year s the Analytical center at our Institute amassed the actual material on the application of XRF method to the quantitative determination of some major (Mg, Al, P, S, Cl, K, Ti, Mn, Fe) and trace (V, Cr, Co, Ni, Zn, Rb, Sr, Y, Zr, Nb, Mo, Ba, La, Ce, Pb, Th, U) element contents [1, 2]. This paper presents the specific features of developed techniques for the determination of 25 element contents in different types of rocks using new Biaiker Pioneer automated spectrometer connected to Intel Pentium IV. The special features of X-ray fluorescence analysis application to the determination of analyzed elements in various types of rocks are presented. The softwai e of this new X-ray spectrometer allows to choose optimal calibration equations and the coefficients for accounting for line overlaps by Equant program and to make a mathematic processing of the calibration ai ray of CRMs measured by the Loader program. 

This is a very important and well tested method for the quantitative determination of loading of Fmoc protected compounds particularly that of Fmoc (fluorenylmethoxycarbonyl) amino acids on solid support. Fmoc groups can... 

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