Colorimetric procedure

Chemical Analysis. Chemical impurities commonly analyzed include Na20, Fe202, and Si02. The hydroxide is first dissolved in boiling concentrated HQ. Atomic absorption methods have replaced older colorimetric procedures. 

Several colorimetric procedures for fluoride are available, but it is usually desirable to distill the sample from concentrated sulfuric acid prior to analysis to eliminate interferences. One method is based upon bleaching a dye formed by the reaction of zirconium and sodium 2-(p-sulfophenylazo)-l,8-dihydroxy-3,6-naphthalenedisulfonate (SPADNS reagent) (28). 

Colorimetric procedures are often used to determine copper in trace amounts. Extraction of copper using diethyldithiocarbamate can be quite selective (60,62), but the method using dithhone is preferred because of its greater sensitivity and selectivity (50—52). Atomic absorption spectroscopy, atomic emission spectroscopy, x-ray fluorescence, and polargraphy are specific and sensitive methods for the deterrnination of trace level copper. 

The choice of a colorimetric procedure for the determination of a substance will depend upon such considerations as the following. 

Reproducibility. The colorimetric procedure must give reproducible results under specific experimental conditions. The reaction need not necessarily represent a stoichiometrically quantitative chemical change. 

The colorimetric procedure has been applied to each of the fractions isolated from the partition column. The response to the color test has allowed an accurate prediction of the general type of infrared spectra ultimately found. The color test has also been applied to fractions collected from the gas chromatograph. Of the major responses observed when the pyrethrum mixture is passed through the chromatograph, three of the components respond to the color test. At least two other pyrethrin-like compounds of long retention and small quantity also give the color test. No infrared data are available on these. 

While the colorimetric procedure has not found wide application as a quantitative method, it has proved its worth as a diagnostic tool. 

Colorimetric procedures used In steroid assays are often subject to drug Interference. In the determination of 17-Ketosterolds by the Zimmerman reaction, drugs with the 17-Keto basic structure such as ascorbic acid, morphine and reserplne will cause Increased values. In the determination of 17,21 -dlhydroxysterolds by the Porter-Sllber reaction the dlhydroxy-acetone chain Is the reactive unit. Drugs like meprobamate, chloral hydrate, chloropromazlne and potassium Iodide will Interfere with this reaction and cause elevated values. In the colorimetric determination of vanlllylmandellc acid (VMA) by a dlazo reaction, drugs like methocarbamol and methyl dopa cause... 

Micro amounts of sulfur in polymer are usually determined by oxygen flask combustion, sodium peroxide fusion in a metal bomb followed by titration [30], pyroluminescence [36] or ICP-AES. An oxygen flask combustion photometric titration procedure capable of determining total sulfur in polymers in amounts down to 50 ppm was reported. The repeatability of the sulfur determination in polyolefins in the oxygen flask is 40% at 50 ppm level, improving to 2% at the 1 % level [21]. Crompton [31] has also combined Schoniger flask combustion with a colorimetric procedure for the determination of phosphorous in polymers in various concentration ranges (0.01 to 2%, 2 to 13%). 

A colorimetric procedure is described for the determination of small amounts of Compound 118 (1,2,3,4,10,10-hexa-chloro - 1,4,4a,5,8,8a - hexahydro - 1,4,.5,8 - dimethano-naphthalene). Reaction with phenyl azide to form a di-hydrotriazole derivative and subsequent treatment with diazotized dinitroaniline in strongly acid medium produce an intense red color. Amounts of the insect toxicant of 10 to 40 micrograms in the final 10-ml. aliquot are readily determined with a spectrophotometer. Commonly used insect toxicants do not interfere. 

This colorimetric procedure is applicable to the estimation of Compound 118 in cow s urine. 

This method was developed as a second independent method to complement the usual colorimetric procedure in the determination of a certified concentration of dissolved silica in a seawater reference material. Ion exclusion affords a separation of the dissolved silica not only from major seawater cations but also from potentially interfering anions. The detection unit limit, conservatively estimated at 2.3 ng/g Si (0.08. im), is superior to that achievable by direct analysis using inductively coupled plasma emission spectrometry. 

Bond and Willis 2") have determined ammonia in mitrochondria samples after separation by distillation. The enhancement of zirconium absorption by the ammonia is measured. This is more rapid than colorimetric procedures. 

The precision of absorption measurements depends upon the degree of sophistication of the instrumentation and on the chemical species involved, both of which can affect the apparent validity of the Beer-Lambert law. Where a single absorbing species exhibiting a broad flat maximum is to be determined, adequate results can often be achieved with a simple filter-photometer. In the visible region, this technique is known as colorimetry. The inherent disadvantage of colorimetric procedures using simple filter instruments with a broad bandpass lies in the invalidation of the Beer-Lambert law and the lack of compatibility between results from different... 

Blood samples were centrifuged at 1000 x g for 20 min at 0-4°. Ionized calcium levels were immediately determined in serum and urine samples using a calcium ion-selective electrode (Ionetics, Inc., Costa Mesa, CA) urine volumes were recorded. The remaining serum and urine were aliquoted for various analyses and stored at -40°. Serum insulin was analysed by radioimmunoassay (Amersham Corp., Arlington Heights, IL). Serum levels of total calcium, phosphorus and creatinine as well as urine creatinine were determined by colorimetric procedures using an automated analyzer (Centrifichem, Baker Instruments Corp., Pleasantville, NY). Glomerular filtration rates (GFR) were calculated from serum and urine creatinine data GFR = urine creatinine/serum creatinine. 

The fluorimetric methods often offer improved specificity and sensitivity over colorimetric procedures and the quantitative assays for the aromatic amino acids tyrosine and phenylalanine illustrate this point. 

Dimethylbiguanide may be estimated by colorimetric procedures based on its reaction with diacetyl in presence of a-naphthol (618), or a modified Sakaguchi (343, 508) and other (46) reactions. 

Colorimetric Procedures and Chemical Lists for Water and Wastewater Analysis", Hatch Chemical Co., Ames, Iowa, 1971. "Standard Methods for the Examination of Water and Waste-water", 14th ed., American Public Health Assoc., Inc., New York, 1975. 

Weiss and MacDonald (87) recently reviewed methods for determination of ionophore antibiotics. lonophores approved for use in animal agriculture in the U.S. are lasalocid, monensin, and salinomycin. An HPLC ( ) and GLC-MS ( ) procedure have been described for lasalocid. For other ionophores, TLC-bioautography is the preferred procedure because of lack of any useful UV absorbance. However, a few TLC colorimetric procedures have been described for monensin residues in tissues (90-92). 

The "impact compound that provides the primary stimulus for fruit character in the raspberry is the ketone, l-(p-hydroxphenyl)-3-butanone 11). Other important flavour contributors are cw-3-hexen-l-ol, a - and p - ionones, and a - irone (72, 13). In R. arcticus the characteristic aroma is considered to be from mesifiirane (70). It has, however, been reported that steam distillates of raspberries can be assessed for aroma content using a colorimetric procedure and 80% of aroma is accounted for by geraniol, nerol, linalool, a - terpineol and die ionones (13). 

Providing no other acidic species are present and water has been used as the absorption medium in either the 02 flask or pyrohydrolytic tube decomposition, the acidimetric titration of hydrogen fluoride is the simplest. Unfortunately this is often not the case, so one of the other finishes such as colorimetry and titrimetry has to be used. One of the best colorimetric procedures employs Ce-Alizarin complexone reagent5 which changes from wine red to dark blue in the presence of fluoride ion. The color takes a while to develop fully, but it is very reliable. 

---