Magnesium gravimetric analysis

For a precipitate used in gravimetric analysis magnesium ammonium phosphate has a rather high solubility (0.1 g dm 3 in water at 20°C). Hence solution volumes should be kept as low as possible and the precipitate must be filtered from cold solution. Furthermore, the solution composition must be carefully controlled to ensure the maintenance of conditions of... 

The checkers noted a delay in the formation of solid magnesium dihydride, which did not begin to precipitate until nearly all the lithium tetrahydridoaluminate(l —) had been added, t The diethyl ether was determined by difference in the gravimetric analysis. 

Although preliminary separations may be required, in other instances the precipitation step in gravimetric analysis is sufficiently selective that other separations are not required. The pH is important because it often influences both the solubility of the analytical precipitate and the possibility of interferences from other substances. For example, calcium oxalate is insoluble in basic medium, but at low pH the oxalate ion combines with the hydrogen ions to form a weak acid. 8-Hydroxy-quinoline (oxine) can be used to precipitate a large number of elements, but by controlling pH, we can precipitate elements selectively. Aluminum ion can be precipitated at pH 4, but the concentration of the anion form of oxine is too low at this pH to precipitate magnesium ion. 

Apparatus for determining the empirical formula of magnesium oxide (by gravimetric analysis)... 

Various other reagents are also useful for gravimetric analysis, for example dimethylglyoxime (a) for nickel and oxine (b) for aluminum and magnesium (Fig. 2(a) and (b)). 

Referee Methods. The American Society for Testing Materials (ASTM) has collected a series of standard referee methods for the analysis of magnesium and its alloys (78). These methods are accurate over a larger range of concentration than the production methods, but are time consuming ia thek apphcation. The methods are based on potentiometric titration, photometric methods, or gravimetric methods. The photometric methods are most common and are relatively straightforward. 

Vol. 3 Photometric Determination of Traces of Metals. Fourth Edition Part I General Aspects. By E. B. Sandell and Hiroshi Onishi Part IIA Individual Metals, Aluminum to Lithium. By Hiroshi Onishi Part IIB Individual Metals, Magnesium to Zirconium. By Hiroshi Onishi Vol. 4 Organic Reagents Used in Gravimetric and Volumetric Analysis. By John F. Flagg (out ofprint)... 

Basic magnesium phosphates may be characterized by x-ray and thermo-gravimetric analyses and elemental analysis. Magnesium may be determined... 

Analytical methods employed in soil chemistry include the standard quantitative methods for the analysis of gases, solutions, and solids, including colorimetric, titrimetric, gravimetric, and instrumental methods. The flame emission spectrophotometric method is widely employed for potassium, sodium, calcium, and magnesium barium, copper and other elements are determined in cation exchange studies. Occasionally arc and spark spectrographic methods are employed. 

A standard wet chemical analysis (ASTM D-811) is available for determination of aluminum, barium, calcium, magnesium, potassium, silicon, sodium, tin, and zinc. The procedure involves a series of chemical separations with specific elemental analysis performed by using appropriate gravimetric or volumetric analyses. 

Phosphorus can serve as a benehcial adjunct or as a deleterious agent. There are several test methods for the determination of phosphorus. In addition to the three test methods described here, reference should also be made to multielement analysis methods such as inductively coupled plasma atomic emission spectroscopy (ICPAES) (ASTM D-4951, ASTM D-5185) and X-ray fluorescence (XRF) (ASTM D-4927, ASTM D-6443) described above in this guide. Phosphorus can also be determined by a photometric procedure (IP 148) or by a test method (ASTM D-1091) in which the organic material in the sample is destroyed, phosphorus in the sample is converted to phosphate ion by oxidation with sulfuric acid, nitric acid, and hydrogen peroxide, and the magnesium pyrophosphate is determined gravimetrically. Another method (ASTM D-4047, IP 149) in which the phosphorus is converted to quinoline phosphomolybdate is also available. 

A crystalline precipitate of magnesium ammonium phosphate hexahydrate (struvite) is produced when other magnesium salts are added with ammonia to weakly basic or neutral phosphate solutions (5.39). The ignition of this salt to give the pyrophosphate forms the basis of a gravimetric method of analysis for P (Chapter 14.1). 

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