The determination of nitrate by infrared spectroscopy

Summary Nitrate may be determined by precipitation with nitron acetate and determination of the absorbance at 7.3 in a potassium bromide disc. The results are reproducible at milligram levels with a standard deviation of around ±5%. The presence of twice the amount of nitrite, perchlorate, bromate, chlorate, chromate, periodate or iodide has no significant effect on the determination.

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Zusammenfassung Nach Fällung mit Nitronacetat läßt sich Nitrat durch Messung der Absorption bei 7,3 in Kaliumbromid bestimmen. Die Resultate sind im Milligramm-Maßstab mit einer Standardabweichung von etwa ±5% reproduzierbar. Die gleichzeitige Anwesenheit der doppelten Menge Nitrit, Perchlorat, Bromat, Chlorat, Chromat, Perjodat oder Jodid hat keinen merklichen Einfluß auf die Bestimmung.

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Résumé On peut doser les nitrates par précipitation par l'acétate de nitron et mesure de l'absorption à 7,3 sur pastille en bromure de potassium. Les résultats sont reproductibles à l'échelle du milligramme avec une déviation standard de ±5% environ. La présence d'une quantité double de nitrites, perchlorates, bromates, chlorates, chromates, periodates ou iodures ne produit pas d'effet important sur le dosage.

     

Determination of hexacelsian by infrared spectroscopy

Hexacelsian has been determined by infrared spectroscopy with KBr discs and K(4)Fe(CN)(6) as internal standard. A KBr particle size of <40 mum gave better homogenization of the sample-KBr mixture than a particle size in the 40-70 mum range. For determinations of hexacelsian in synthetic samples containing amorphous phase or celsian, calibration curves were constructed. A least-squares fit yielded correlation coefficients of 0.998 and 0.997.     

Determination of nitrate in thorium,uranium and plutonium solutions

A potentiometric titration method and a conductometric titration method were standardized for the determination of nitrate in thorium, uranium and plutonium solutions in the range of 2–10 mg, and 15–30 mg, respectively, with a precision and accuracy of 2% in both cases. The results were compared with those of other methods like Devarda's alloy reduction method and volumetric titration method. The procedures standardized have been recommended for the determination of nitrate in heavy element solutions used for the preparation of oxide and mixed oxide microspheres by the sol-gel technique.     

Determination of water in furfural by infrared spectroscopy

The IR absorption band at 5250 cm^–1 is used to determine 0–5% water in furfural. The accuracy of the determination is not less than 5%. The method is suitable for any kind of furfural. The analytical results are unaffected by the presence of formic, acetic, and pyromucic acids, and methanol and ethanol.     

Determination of deuterium in organic compounds by infrared spectrophotometry

The Trenner-Arison-Walker method for the micro-analysis of deuterium in organic compounds involves oxidation of the compound with copper oxide in a sealed tube, collection of the water by vacuum distillation, and analysis of the water by infrared spectrophotometry. Experience in applying this technique to a variety of organic compounds in our laboratory has suggested a number of procedural modifications. These principally affect the methods of sample handling and water collection. Difficulties associated with temperature changes on the spectrophotometry of the deuterium-enriched water are overcome by differential analysis against natural-abundance water using a double-beam spectrophotometer.     

Determination of n-paraffinic structure in petroleum fraction by infrared spectroscopy

Summary The characteristic strong absorption infrared band near 720–725 cm^–1 of an open chain methylene group of the type (CH₂) _n (n = 4 or more) has been used to estimate the number of n-paraffinic methylene groups in an average molecule of saturates, urea adductables and non-adductables of various gas-oil and vacuum gas oil fractions. The method was developed by computing the average absorptivity at 725 cm^–1 of several pure n-paraffins (C₁₄-C₃₂). Although the interference due to the aromatic C — H band at 740 cm^–1 disturbs the estimation of shorter chains, it is seen from the data on adductables and non-adductables that the estimation can be done in long chain paraffins even in the presence of aromatics.

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Bestimmung von n-Paraffinstrukturen in Erdölfraktionen mit Hilfe der Infrarot-Spektroskopie

Zusammenfassung Die charakteristische starke IR-Absorptionsbande der paraffinischen Methylengruppe des Typs (CH₂) _n (n = 4 oder mehr) bei 720–725cm^–1 wurde zur Bestimmung der Anzahl von Methylengruppen in einem durchschnittlichen Molekül von gesättigten Kohlenwasserstoffen, Harnstoffprodukten sowie Nicht-Addukten verschiedener Gasöl- und Vakuum-Gasöl-Fraktionen benutzt. Das Verfahren wurde durch Berechnung der durchschnittlichen Extinktion bei 725 cm^–1 von mehreren reinen n-Paraffmen (C₁₄-C₃₂) entwickelt. Wenn auch die Bestimmung kürzerer Ketten durch die aromatische C — H-Bande bei 740 cm^–1 gestört wird, so ergibt sich doch aus den Werten für Addukte und Nicht-Addukte, daß die Bestimmung bei langkettigen Paraffinen selbst in Gegenwart von Aromaten durchgeführt werden kann.

     

二甲基二烯丙基氯化铵及其聚合物的红外光谱研究

对二甲基二烯丙基氯化铵（DMDAAC）不同聚合度的均聚物和它与丙烯酰胺的共聚物进行了结构分析，讨论了红外光谱吸收峰随聚合物特性粘度、单体的质量分数变化的规律及原因。结果表明，在均聚物中，随粘度的升高，峰位分别为1262cm^-1和678cm^-1处的碳氮键的伸缩与变形振动吸收峰增强；在共聚物中，当粘度不是很大时，粘度或单体的质量分数的升高都会使3017cm^-1处碳氢键的伸缩振动吸收峰增强。     

Determination of nitrite, sulphate, bromide and nitrate in human serum by ion chromatography

An ion chromatographic method has been developed for the determination of trace amounts of nitrite, sulphate, bromide and nitrate in human serum, using an ODS column dynamically coated with cetylpyridinium chloride. The anions studied were eluted with 1 mM citrate - 2.5% methanol (pH 6.5) as the mobile phase and detected by an ultraviolet detector. The interfering proteins in human serum were removed by an initial filtration through an ultrafilter-paper. The many inorganic and organic anions commonly found in serum had little effect on the determination of the four anions. Recoveries of nitrite, sulphate, bromide and nitrate in serum were 107-110, 94-106, 106-110 and 92-100%, respectively. The proposed method was also applied to human saliva and urine.     

Determination of atomic stress distribution in stressed polymers by infrared spectroscopy

An attempt was made to evaluate stresses on chemical bonds in axially stressed polymers from the shift of skeletal vibration frequencies in chain molecules. The maximum stress on chemical bonds was found to be at least ten times the average stress on the specimen.     

Prediction of phenolic compounds in red wine fermentations by visible and near infrared spectroscopy

Near infrared (NIR) spectroscopy was used to simultaneously predict the concentrations of malvidin-3-glucoside (M3G), pigmented polymers (PP) and tannins (T) in red wine. A total of 495 samples from 32 commercial scale red wine fermentations over two vintages using two grape varieties (Cabernet Sauvignon and Shiraz), and also including as additional variables two types of fermenters, two different yeasts, and three fermentation temperatures were used. Samples were scanned in transmission mode (400-2500 nm) using a monochromator instrument (NIRSystems6500). Calibration equations were developed from high performance liquid chromatography (HPLC) and NIR data using partial least squares (PLS) regression with internal cross validation. Using PLS regression, very good calibration statistics (R_cal²>0.80) were obtained for the prediction of M3G, PP and T with standard deviation (S.D.)/standard error in cross validation (SECV) ratio (residual predictive deviation, RPD)) ranging from 1.8 to 5.8. It was concluded that near infrared spectroscopy could be used as rapid alternative method for the prediction of the concentration of phenolic compounds in red wine fermentations.     

Determination of calcium in organometallic compounds by atomic absorption spectroscopy

A simple and relatively rapid procedure for the estimation of calcium in organometallic compounds is described. The oxygen filled flask for decomposition of the organic sample and AAS determination of the metal in aqueous medium without any effect of the organic portion of the molecule or solvent is recommended. The results of calcium determination in a lubricant obtained by different combustion procedures and different final determinations are also compared.     

Determination of organosilicon compounds in water by atomic absorption spectroscopy

Summary An extraction technique is described for the determination of ppm concentrations of both hydrophobic and hydrophilic methylsiloxane compounds in water, based on a single extraction with a mixed solvent of (11) l-pentanol and methyl isobutyl ketone followed by the determination of the silicone compounds extracted into the mixed solvent by atomic absorption spectroscopy. The method is applicable over the concentration range 0.3–30 ppm Si. Standard deviation in the case of 10 ppm Si is 0.313.

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Bestimmung von siliciumorganischen Verbindungen in Wasser mit Hilfe der Atomabsorptions-Spektralphotometrie

Zusammenfassung Zur Bestimmung von ppm-Konzentrationen an hydrophoben und hydrophilen Methylsiloxanverbindungen im Wasser wird ein Extraktionsverfahren beschrieben. Hierbei wird nach einfacher Extraktion mit l-Pentanol/Methylisobutylketon (11) das Silicium im Extrakt mit Hilfe der AAS bestimmt. Der erfaßbare Konzentrationsbereich liegt bei 0,3–30 ppm Si. Die Standardabweichung beträgt bei 10 ppm Si 0,313.

     

Determination of uranium and plutonium in plutonium based fuels by sequential amperometric titration

A method is described for the sequential determination of uranium and plutonium in plutonium bearing fuel materials. Uranium and plutonium are reduced to U(IV) and Pu(III) with titanous chloride and then titrated with dichromate to two end points which are detected amperometrically using two polarized platinum electrodes. Uranium-plutonium solutions of known concentrations containing plutonium in the proportions of 4, 30, 50, and 70% were analyzed with precisions better than 0.3%, maintaining the amounts of plutonium per aliquot in the range of 2–10 mg. No significant bias could be detected. Several samples of (U, Pu)O₂ and (U, Pu)C were analyzed by this procedure. The effects of iron, fluoride, oxalic acid and mellitic acid on the method were also studied.     

Determination of chloride, nitrate, sulphate and total sulphur in environmental samples by single-column ion chromatography

The analytical performance characteristics of a single-column ion chromatography system are reported. The data were obtained by using conductivity detection as well as by an indirect ultraviolet technique. The method has been applied to the determination of Cl(-), NO(3)(-) and SO(4)(2-) in samples of rain, sewer water, and soil-pore water. Also described are two methods which allow ion Chromatographic analysis of CaS0(4)-extractable nitrate in soils, and total sulphur in soils, marine sediments and plant tissue.     

Determination of tacticity in poly(vinyl chloride) by infrared spectroscopy

From the temperature dependence of infrared spectra of poly(vinyl chloride) samples prepared by different methods, the intensity of the band at 690 cm.¹ (proportional to the number of isotactic diads in the sample), as well as that of the tacticity-independent C? H stretching band, was found to be independent of the crystallinity of the sample. These lines were therefore applied for the tacticity determination in poly(vinyl chloride), measured in the form of KBr pellets. The numerical tacticity value was obtained from the known values of absorbance coefficients of SCH and SHH type C? Cl stretching bands in solution, and from the shape of the spectrum.     

Determination of total sterols in brown algae by Fourier transform infrared spectroscopy

A procedure is proposed for the determination of the total amount of sterols in brown algae Bifurcaria bifurcata, Cladostephus hirsitus, Dictyota dichotoma and Cystoseira sedoides, globally determined as fucosterol, which is the major sterol contained in these algae. The method involves the use of cholesterol as reference standard and a correction factor of 1.259 ± 0.003, which represents the ratio between the slopes of calibration lines obtained from fucosterol and cholesterol. The method provides precise and accurate results for the IR analysis of real samples.     

Determination of ascorbic acid in pharmaceutical preparations by near infrared reflectance spectroscopy

We developed a method for determination of ascorbic acid in pharmaceutical preparations containing various excipients by using near infrared diffuse reflectance spectroscopy and two different calibration methods, viz. stepwise multiple linear regression (SMLR) and partial least-squares (PLS) regression, which provided comparable results and resulted in prediction errors of 1-2%. However, the PLS method provided somewhat better results with the more complex samples.