Colorimetric

C22H23N3O9. An organic reagent used for the detection and estimation of aluminium. It is a brownish-red powder, soluble in water which gives a red lake with aluminium which can be estimated colorimetrically. It can also be used for detecting scandium and indium. 

M.p. 296 C. Accepts an electron from suitable donors forming a radical anion. Used for colorimetric determination of free radical precursors, replacement of Mn02 in aluminium solid electrolytic capacitors, construction of heat-sensitive resistors and ion-specific electrodes and for inducing radical polymerizations. The charge transfer complexes it forms with certain donors behave electrically like metals with anisotropic conductivity. Like tetracyanoethylene it belongs to a class of compounds called rr-acids. tetracyclines An important group of antibiotics isolated from Streptomyces spp., having structures based on a naphthacene skeleton. Tetracycline, the parent compound, has the structure ... 

Total sulfur M 07-052 Combustion in furnace and colorimetric analysis... 

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). 

Bismuth standard solution (quantitative color test for Bi) dissolve 1 g of bismuth in a mixture of 3 mL of concentrated HNO3 and 2.8 mL of H2O and make up to 100 mL with glycerol. Also dissolve 5 g of KI in 5 mL of water and make up to 100 mL with glycerol. The two solutions are used together in the colorimetric estimation of Bi. 

In the DPD colorimetric method for the free chlorine residual, which is reported as parts per million of CI2, the oxidizing power of free chlorine converts the colorless amine N,N-diethyl-p-phenylenediamine to a colored dye that absorbs strongly over the wavelength range of 440-580 nm. Analysis of a set of calibration standards gave the following results... 

Color-forming reactions Color generation Colorimeters Colorimetric methods... 

Reagents, Indicators, and Solutions. This section includes the specifications and testing methods for reagents to be used in the tests specified in the USP-NF, and directions for making the various indicator, buffer, colorimetric, test, and volumetric solutions used in the testing. Reagents for which ACS specifications exist are referenced to the ACS book (7). 

In view of the chromophoric character of the elemental iodine itself, many colorimetric methods have been proposed for the deterrnination of inorganic iodine (88—92). These methods use the visible portion of the spectmm in reading iodine concentrations. In the visible range the extinction coefficient for iodine is not high enough to be used for minute quantities of iodine in water and other solvents (93). Higher sensitivities have been reported for elemental iodine in potassium iodide solutions in the ultraviolet (93,94). 

Colorimetric. A sensitive method for the deterrnination of small concentrations of dissolved iron is the spectrophotometric deterrnination of the orange-red tris(1,10-phenanthroline)iron (IT) complex. Other substituted phenanthrolines can be even more sensitive. Only the inon(II) complexes of these Ligands are highly colored. The sample is first treated with an excess of reducing agent. The complexes are stable from pH 2 ndash 9 and analysis preferably is done at about pH 3.5. 

Titrations with dibutylamine [111-92-2] can also be used to determine the NCO content of isocyanates and prepolymers. Generally, an excess of amine in a suitable solvent such as chlorobenzene [108-90-7] is added to the sample. The resulting solution is allowed to react and the unreacted amine is back- titrated with dilute hydrochloric acid. For low NCO content levels, a colorimetric method is often used. The isocyanate-containing species is titrated with amine and the unreacted amine is deterrnined using malachite green [569-64-2]. 

Analytical and Test Methods. Colorimetric quaUtative tests for diketene are known but seldom used (131). Identification is by spectrometric methods. Diketene has typical ir absorption bands at - ISSO, 1855, and 1685 cm , and signals at 3.92 (t), 4.51 (m), and 4.87 (m) ppm in the H-nmr spectmm (CDCl ). Purity is routinely monitored by gc. Alternatively, diketene is quantitatively converted to acetoacetic derivatives which are assayed by standard methods. 

Colorimetric Method. A finely powdered sample treated with sulfuric acid, hydrobromic acid [10035-10-6] and bromine [7726-95-6] gives a solution that when adjusted to pH 4 may be treated with dithi one [60-10-6] ia / -hexane [110-54-3] to form mercuric dithi2onate [14783-59-6] (20). The resultant amber-colored solution has a color iatensity that can be compared against that of standard solutions to determine the mercury concentration of the sample. Concentrations below 0.02 ppm have been measured by this method. 

Phosphatase Test. The phosphatase [9001-78-9] test is a chemical method for measuring the efficiency of pasteurization. AH raw milk contains phosphatase and the thermal resistance of this enzyme is greater than that of pathogens over the range of time and temperature of heat treatments recognized for proper pasteurization. Phosphatase tests are based on the principle that alkaline phosphatase is able, under proper conditions of temperature and pH, to Hberate phenol [108-95-2] from a disodium phenyl phosphate substrate. The amount of Hberated phenol, which is proportional to the amount of enzyme present, is determined by the reaction of Hberated phenol with 2,6-dichloroquinone chloroimide and colorimetric measurement of the indophenol blue formed. Under-pasteurization as well as contamination of a properly pasteurized product with raw milk can be detected by this test. 

Protein Content. The protein content of milk can be determined using a variety of methods including gasometric, Kjeldahl, titration, colorimetric, and optical procedures (see Proteins). Because most of the techniques are too cumbersome for routine use in a dairy plant, payment for milk has seldom been made on the basis of its protein content. Dye-binding tests have been appHed to milk for determination of its protein content these are relatively simple to perform and can be carried out in dairy plant laboratories. More emphasis will be given to assessing the nutritional value of milk, and the dependence on fat content as a basis for payment will most likely change. 

Nickel also is deterrnined by a volumetric method employing ethylenediaminetetraacetic acid as a titrant. Inductively coupled plasma (ICP) is preferred to determine very low nickel values (see Trace AND RESIDUE ANALYSIS). The classical gravimetric method employing dimethylglyoxime to precipitate nickel as a red complex is used as a precise analytical technique (122). A colorimetric method employing dimethylglyoxime also is available. The classical method of electro deposition is a commonly employed technique to separate nickel in the presence of other metals, notably copper (qv). It is also used to estabhsh caUbration criteria for the spectrophotometric methods. X-ray diffraction often is used to identify nickel in crystalline form. 

Analytical and Test Methods. o-Nitrotoluene can be analyzed for purity and isomer content by infrared spectroscopy with an accuracy of about 1%. -Nitrotoluene content can be estimated by the decomposition of the isomeric toluene diazonium chlorides because the ortho and meta isomers decompose more readily than the para isomer. A colorimetric method for determining the content of the various isomers is based on the color which forms when the mononitrotoluenes are dissolved in sulfuric acid (45). From the absorption of the sulfuric acid solution at 436 and 305 nm, the ortho and para isomer content can be deterrnined, and the meta isomer can be obtained by difference. However, this and other colorimetric methods are subject to possible interferences from other aromatic nitro compounds. A titrimetric method, based on the reduction of the nitro group with titanium(III) sulfate or chloride, can be used to determine mononitrotoluenes (32). Chromatographic methods, eg, gas chromatography or high pressure Hquid chromatography, are well suited for the deterrnination of mononitrotoluenes as well as its individual isomers. Freezing points are used commonly as indicators of purity of the various isomers. 

A number of colorimetric methods are available (83) however, spectroscopic methods are generally preferred. 

Ozone can be analyzed by titrimetry, direct and colorimetric spectrometry, amperometry, oxidation—reduction potential (ORP), chemiluminescence, calorimetry, thermal conductivity, and isothermal pressure change on decomposition. The last three methods ate not frequently employed. Proper measurement of ozone in water requites an awareness of its reactivity, instabiUty, volatility, and the potential effect of interfering substances. To eliminate interferences, ozone sometimes is sparged out of solution by using an inert gas for analysis in the gas phase or on reabsorption in a clean solution. Historically, the most common analytical procedure has been the iodometric method in which gaseous ozone is absorbed by aqueous KI. 

Various colorimetric methods have been employed for measuring ozone residuals, although most of these ate susceptible to significant interferences (142). The indigo trisulfonate method (143), however, has been approved by the Standard Methods Committee of the American Pubfle Health Association (141) and the International Ozone Association for ozone residual measurement. 

There are many colorimetric methods used for trace analysis of peroxides using reagents such as ferrous ion, leuco base of methylene blue, yy -diphenylcarbohydrazide, titanium(IV), iodide ion, and Ai,A7-dimethyl- -phenylenediamine. The latter two are the most commonly used reagents... 

ISO 7724-1-1984, CIE Standards Colorimetric Observers Paints and Varnishes—Colorimetry, Part 1, Principles-, ISO 7724-2-1984, Part 2, Colour Measurement, ISO, Geneva, Swit2erland. 

Only slightly less accurate ( 0.3—0.5%) and more versatile in scale are other titration techniques. Plutonium maybe oxidized in aqueous solution to PuO " 2 using AgO, and then reduced to Pu" " by a known excess of Fe", which is back-titrated with Ce" ". Pu" " may be titrated complexometricaHy with EDTA and a colorimetric indicator such as Arsenazo(I), even in the presence of a large excess of UO " 2- Solution spectrophotometry (Figs. 4 and 5) can be utilized if the plutonium oxidation state is known or controlled. The spectrophotometric method is very sensitive if a colored complex such as Arsenazo(III) is used. Analytically usehil absorption maxima and molar absorption coefficients ( s) are given in Table 10. Laser photoacoustic spectroscopy has been developed for both elemental analysis and speciation (oxidation state) at concentrations of lO " — 10 M (118). Chemical extraction can also be used to enhance this technique. 

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. 

Contaminant by-products depend upon process routes to the product, so maximum impurity specifications may vary, eg, for CHA produced by aniline hydrogenation versus that made by cyclohexanol amination. Capillary column chromatography has improved resolution and quantitation of contaminants beyond the more fliUy described packed column methods (61) used historically to define specification standards. Wet chemical titrimetry for water by Kad Eisher or amine number by acid titration have changed Httle except for thein automation. Colorimetric methods remain based on APHA standards. 

Colorimetric and Fluorimetric Analysis. The functional groups of amino acids exhibit Htde absorption of uv light from 210 to 340 nm where uv absorption spectrometry is most conveniently conducted. Thus color or fluorescence formation reactions are employed for amino acid detection (128). 

The most widely appHed colorimetric assay for amino acids rehes upon ninhydrin-mediated color formation (129). Fluorescamine [38183-12-9] and (9-phthalaldehyde [643-79-8] are popular as fluorescence reagents. The latter reagent, ia conjunction with 2-mercaptoethanol, is most often used ia post-column detection of amino acids separated by conventional automated amino acid analysis. More recently, determiaation by capillary 2one electrophoresis has been developed and it is possible to determine attomole quantities of amino acids (130). 

More specifically, 2-aminophenol can be detected in solution using an iron(II) sulfate—hydrogen peroxide reagent (94). 3- Aminopheno1 has been analyzed colorimetrically by oxidation in base and subsequent extraction of a violet quinoneimide dye (95). A colorimetric method using... 

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