Titration gravimetric

A sample of the suspension can then be taken and titrated separately with a double beam spectrophotometer, the reference being the initial solution. The optical density of the solution at X = 650 mn is actually proportional to the amount of S produced in the experiment. This was checked by a gravimetric titration of the precipitate which served as a standard for the optical method. The experience was repeated at all the injection points indexed on Figures 2 and 3. The amount of precipitate is simply additive from one experiment to the next. These amounts (Cg = 10- to 10 2 moles. m 3 per experiment) are very small as compared to the concentration of reactants. CQ can thence be identified to (Ba +)0 and it is not necessary to readjust the reactant concentration as long as the number of sucessive injections does not exceed about ten. It can be noticed from [4] that precipitation is facilitated by the presence of pre-existing precipitate. 

A matter of practical importance in nonaqueous titrimetry is that, when volumetric equipment is used, errors should be prevented that arise from solvent volatility and from characteristics of viscosity and surface tension that differ from those of water. Temperature coefficients of expansion are often about six times that of water, so careful control of temperature is needed when volumes are being measured. Gravimetric titration techniques are recommended, since they avoid most of these volumetric problems. Details of a gravimetric technique using a syringe have been given. ... 

Because the coefficients of expansion for most nonaqueous solvents are high compared with water, the technique of gravimetric titration is attractive. Precise titrations can be performed in this way with small volumes of titrant and sample. End points can be obtained potentiometrically or with visual indicators such as ferroin and diphenylamine. 

Parallel method comparisons are used to establish the validity of a new method developed for five organic pharmaceutical compovmds, food colors, and color additives. The standard methods such as the Japanese Standard Food Additives and Japanese Standard of Cosmetic Ingredients method, based on volumetric and gravimetric titration, have been used to establish new methods developed for the determination of I, Cl, Br, and SO4 in food colors. The results obtained indicate good agreement in both accuracy and precision for procedures based on the oxygen flask method as compared with the standard methods. In addition to anion elemental analysis, method validation has also been carried out for metal analysis such as that of Ce(III), Th(IV), and U(VI), with the results showing acceptable limits of variation. 

Gravimetric titration. A solution of NaOH was standardized by titration of a known quantity of the primary standard, potassium hydrogen phthalate ... 

Addition of silver nitrate to a solution of a chloride in dilute nitric acid gives a white precipitate of silver chloride, AgCl, soluble in ammonia solution. This test may be used for gravimetric or volumetric estimation of chloride the silver chloride can be filtered off, dried and weighed, or the chloride titrated with standard silver nitrate using potassium chromate(VI) or fluorescein as indicator. 

Time, Cost, and Equipment Acid-base titrations require less time than most gravimetric procedures, but more time than many instrumental methods of analysis, particularly when analyzing many samples. With the availability of instruments for... 

Industrial Hquid chlorine is routinely analy2ed for moisture, chlorine, other gaseous components, NCl, and mercury foUowing estabHshed procedures (10,79). Moisture and residue content in Hquid chlorine is determined by evaporation at 20°C foUowed by gravimetric measurement of the residue. Eree chlorine levels are estimated quantitatively by thiosulfate titration of iodine Hberated from addition of excess acidified potassium iodide to the gas mixture. 

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. 

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. 

Another step in laboratory automation to be achieved is the conversion of standard chemical procedures such as titrations or thermal gravimetric analysis, into unit laboratory operations. A procedure could then be selected from these laboratory operations by an expert system and translated by the system to produce a set of iastmctions for a robot. The robot should be able to obey specific iastmctions, such as taking a specified sample aliquot and titrating it using a specified reagent. 

Although gravimetric methods have been used traditionally for the determination of large amounts of tellurium, more accurate and convenient volumetric methods are favored. The oxidation of teUurium(IV) by ceric sulfate in hot sulfuric acid solution in the presence of chromic ion as catalyst affords a convenient volumetric method for the determination of tellurium (32). Selenium(IV) does not interfere if the sulfuric acid is less than 2 N in concentration. Excess ceric sulfate is added, the excess being titrated with ferrous ammonium sulfate using o-phenanthroline ferrous—sulfate as indicator. The ceric sulfate method is best appHed in tellurium-rich materials such as refined tellurium or tellurium compounds. 

Zirconium is often deterniined gravimetrically. The most common procedure utilizes mandelic acid (81) which is fairly specific for zirconium plus hafnium. Other precipitants, including nine inorganic and 42 organic reagents, are Hsted in Reference 82. Volumetric procedures for zirconium, which also include hafnium as zirconium, are limited to either EDTA titrations (83) or indirect procedures (84). X-ray fluorescence spectroscopy gives quantitative results for zirconium, without including hafnium, for concentrations from 0.1 to 50% (85). Atomic absorption determines zirconium in aluminum in the presence of hafnium at concentrations of 0.1—3% (86). 

Specifications, Analysis, and Toxicity. Dicyandiamide is identified quaHtatively by paper chromatography and quantitatively by ultraviolet spectrometry of the chromatogram. More commonly, total nitrogen analysis is used as a purity control or the dicyandiamide is converted by hydrolysis to guanylurea, which is determined gravimetrically as the nickel salt (50). Methods based on the precipitation of silver dicyandiamide picrate are sometimes used (51). Dicyandiamide can also be titrated with tetrabutylammonium hydroxide ia pyridine solution. Table 4 gives a typical analysis of a commercial sample. Dicyandiamide is essentially nontoxic. It may, however, cause dermatitis. 

Ln(II) in LnFj Ln(II) were determined after samples dissolution in H PO in the presence of a titrated solution of NFI VO, which excess was titrated with the Fe(II) salt. It was found that dissolution of the materials based on CeF CeFj in H PO does not change the oxidation state of cerium, thus phosphate complexes of Ce(III, IV) can be used for quantitative spectrophotometric determination of cerium valence forms. The contents of Ln(II, III) in Ln S LnS may be counted from results of the determination of total sulfur (determined gravimetric ally in BaSO form) and sum of the reducers - S and Ln(II) (determined by iodometric method). 

The analysis of low-melting alloys such as Wood s metal is greatly simplified by complexometric titration, and tedious gravimetric separations are avoided. The alloy is treated with concentrated nitric acid, evaporated to a small volume, and after dilution the precipitated tin(IV) oxide is filtered off heavy metals adsorbed by the precipitate are removed by washing with a known volume of standard EDTA solution previously made slightly alkaline with aqueous... 

Unique methods based on new principles have been developed within the past 10 years. Threonine (27,28,249) is oxidized by lead tetraacetate or periodic acid to acetaldehyde, which is determined by photometric analysis of its p-hydroxydiphenyl complex or iodometric titration of its combined bisulfite. Serine is oxidized similarly to formaldehyde, which is determined gravimetrically (207) as its dimedon (5,5-dimethyldihydro-resorcinol) derivative or photometric analysis (31) of the complex formed with Eegriwe s reagent (l,8-dihydroxynaphthalene-3,5-disulfonic acid). It appears that the data obtained for threonine and serine in various proteins by these oxidation procedures are reasonably accurate. [Block and Bolling (26) have given data on the threonine and serine content of various proteins. ]... 

The quantitative analysis procedure involves gravimetric detn of the HMX on a moisture-free basis after benzene extraction of, and differential detn of TNT. Moisture content is detd by conductometric titration of sample in an acetic-sulfuric acid suspension. Acetone insoluble matter is determined gravimetrically... 

It was found that chlorides, chlorates, and nitrates interfere by forming in sol ppts (Ref 6). Later it was found that w sol perchlorates could be analyzed gravimetrically by pptn of the perchlorate ion as tetraphenylarsonium perchlorate (Ksp at 20° = 2.60 0.14 x 10"9). The ppt can be (Tried at 105° and weighed directly (Ref 16). Still more recently a specific perchlorate ion electrode has been developed (Ref 17) which can be used for the potentiometric titration of the perchlorate ion using a soln of tetraphenylarsonium chloride as the titrant (Ref 15). Tetra-phenylphosphonium chloride has been similarly used, but the corresponding Sb compd is too insol in w for practical use (Ref 8), For routine assay of perchlorates for use by the armed forces, a Na carbonate fusion procedure is described in Mil Specs MlL-A-23946 (19 Aug 1964) MIL-A-23948 (19 Aug 1964) (see also under Ammonium Perchlorate). The tetraphenylarsonium chloride procedure has also been proposed for use in Mil Specs (Ref 11)... 

Footnotes to Table 3 a—by K permanganate titration b—gravimetrically by loss in wt after heating c— gravimetrically by exposure of a sample to 75% RH... 

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