Simultaneous Ultraviolet Spectrophotometric Determination of Nitrate and Nitrite in Water

Abstract

A rapid and accurate method for the direct simultaneous determination of nitrate and nitrite is proposed. The method is applied to the determination of nitrate and nitrite in rainwater and wastewater without preliminary separation. The determinations are performed by a CPA matrix method with ultraviolet spectrophotometric detection. The results obtained are in agreement with those obtained by conventional methods for the determination of nitrate and nitrite.     

Simultaneous determination of iron, cobalt, nickel and copper by UV-visible spectrophotometry with multivariate calibration

A method for the simultaneous spectrophotometric determination of the divalent ions of iron, cobalt, nickel and copper based on the formation of their complexes with 1,5-bis(di-2-pyridylmethylene) thiocarbonohydrazide (DPTH) is proposed. The resolution of quaternary mixtures of these metallic ions was accomplished by several chemometric approaches. A comparative study of the results obtained for simultaneous determinations in mixture by using principal component regression (PCR) and partial least-squares regression (PLS-1 and PLS-2) for absorbance, first-derivative and second-derivative data is presented. In general, the best recovery values are obtained by the PLS-2 method for absorbance data. This procedure allows the simultaneous determination of the cited ions in alloys and biological materials Good reliability of the determination was proved.     

Simultaneous determination of rifampicin and isoniazid by continuous-flow chemiluminescence with artificial neural network calibration

In this paper a continuous-flow chemiluminescence (CL) system with artificial neural network calibration is proposed for simultaneous determination of rifampicin and isoniazid. This method is based on the different kinetic spectra of the analytes in their CL reaction with alkaline N-bromosuccinimide as oxidant. The CL intensity was measured and recorded every second from 1 to 300 s. The data obtained were processed chemometrically by use of an artificial neural network. The experimental calibration set was 20 sample solutions. The relative standard errors of prediction for both analytes were approximately 5%. The proposed method was successfully applied to the simultaneous determination of rifampicin and isoniazid in a combined pharmaceutical formulation.     

混合线性分析-分光光度法同时测定微量锌、镉、汞

提出了以2－（5－溴－2－吡啶偶氮）－5－二乙氨基酚为显色剂分光光度法同时测定锌、镉、汞的新方法。由于在可见区3种络合物的吸收光谱具有相似的特征和严重重叠,本文采用混合线性分析进行光谱分辨,各组分的纯光谱则用最小二乘法从校正集中求出。讨论了显色条件,波长选择,纯光谱的确定和吸光度加合性等因素对测定的影响。方法具有简单,快速,准确等优点。已成功地应用于混合试样中锌、镉、汞的同时测定,并与同条件下偏最小二乘法的计算结果进行了对比。     

Simultaneous determination of dapsone and pyrimethamine by derivative spectrophotometry in pharmaceutical formulations

A simple and fast method was developed for the simultaneous determination of dapsone and pyrimethamine by first-order digital derivative spectrophotometry. Acetonitrile was used as a solvent to extract the drugs from the pharmaceutical formulations, and the samples were subsequently evaluated directly by digital derivative spectrophotometry. The simultaneous determination of both drugs was performed by the zero-crossing method at 249.4 and 231.4 nm for dapsone and pyrimethamine, respectively. The best signal-to-noise ratio was obtained when the first derivative of the spectrum was used. The linear range of determination for the drugs was from 6.6 x 10(-7) to 2.0 x 10(-4) and from 2.5 x 10(-6) to 2.0 x 10(-4) mol/L for dapsone and pyrimethamine, respectively. The excipients of commercial pharmaceutical formulations did not interfere in the analysis. Chemical and spectral variables were optimized for determination of both analytes. A good level of repeatability, 0.6 and 1.7% for dapsone and pyrimethamine, respectively, was observed. The proposed method was applied for the simultaneous determination of both drugs in pharmaceutical formulations.     

Simultaneous determination of lead, nickel, tin and copper in aluminium-base alloys using slurry sampling by electrical discharge and multielement ETAAS

The simultaneous multielement determination of Pb, Sn, Ni and Cu in aluminium alloys by electrothermal atomic absorption spectrometry (ETAAS) was performed by a quick method using slurry sampling. The metallic colloidal slurries were obtained by an electrical discharge operated in liquid medium. In this work, the effects of aluminium were evaluated and the results show that it causes a strong retention of Pb, Ni and Cu at low pyrolysis temperatures which is overcome by employing high pyrolysis temperatures. Aluminium also significantly improves the thermal stabilisation of Pb and Sn, it being possible to reach pyrolysis temperatures of 1100 and 1300 °C, respectively. Such stabilisation indicates that the performance of aluminium as a matrix modifier for Pb is better than that obtained using phosphate and magnesium nitrate without substantial changes of the figures of merit. The effects of aluminium on the atomisation characteristics of the elements and those coming from the simultaneous multielement determination on the figures of merit of the elements are also discussed. In this work, a calibration procedure involving a matrix matching method with aqueous aluminium standards is proposed as a simple and efficient way to solve the inconveniences originated by the aluminium matrix. The proposed method was applied to the simultaneous multielement determination of several aluminium-base alloy standards giving results well within the recommended values.     

High-performance liquid chromatographic determination of tocopherols in infant formulas

A method for the simultaneous determination of alpha-tocopherol acetate and alpha-, delta-, and gamma-tocopherols by normal-phase high-performance liquid chromatography (HPLC) with a fluorescent detector in infant formula is proposed. The values obtained in the determination of the analytical parameters: linearity, precision, limit of detection and accuracy (analysis of a standard reference material, SRM 1846), confirm the quality of the method. The proposed method is useful for the determination of alpha-, delta-, and gamma-tocopherols and alpha-tocopherol acetate in infant formulas at a low cost and in a total time of 2 h.     

分光光度法同时测定多元素的研究 : 以CPA-矩阵法计算混合体系中Mo、W、Ti三元素的含量

本文将CPA-矩阵法用于光度分析中同时对多元素的测定, 确定了在SAF为显色剂、DTMAB为胶束增敏剂的配合体系中以CPA-矩阵法计算Mo、W、Ti三元素含量的各种最佳实验条件, 建立了在该体系中同时测定互相干扰的Mo、W、Ti三元素的分光光度法. 总结了进行多组份测定时选择分析波长的四项原则, 并依此确定了6个测定波长: 510、512、514、516、518、520nm为Mo、W、Ti三元素的测定波长. 依本文建立的方法, 通过对任意含量配比的三元素混合试样进行测定结果极为满意, 方法具有稳定、准确、简便、快速和经济等特点, 便于推广应用.     

Simultaneous kinetic spectrophotometric determination of cephalexin and trimethoprim in pharmaceutical preparation and human urine with the aid of chemometrics

A procedure for the simultaneous kinetic spectrophotometric determination of cephalexin and trimethoprim was described. It was based on the different reaction rate of oxidation of these compounds with yellow ammonium cerous （Ⅳ） sulfate in acidic medium and colorless cerous （Ⅲ） sulfate was produced. The overlapped kinetic data was quantitatively resolved by the use of chemometric methods, partial least squares （PLS）, principal component regression （PCR） and radial basis function-artificial neural network （RBF-ANN）. The proposed method was also applied to the simultaneous determination of cephalexin and trimethoprim in pharmaceutical preparation and human urine with satisfied results, which compared well with those obtained by HPLC.     

Determination of odorous mixed chloro-bromoanisoles in water by solid-phase micro-extraction and gas chromatography-mass detection

A headspace-solid-phase micro-extraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) method has been proposed for the simultaneous determination of odorous trihalogenated anisoles in water. Parameters affecting efficiency of HS-SPME procedure, such as the selection of the SPME coating, extraction time, temperature and ionic strength were optimized. The commercially available polydimethylsiloxane (PDMS 100 microm) fiber appears to be the most suitable for the simultaneous determination of these compounds. Run-to-run precision with relative standard deviations (R.S.D.s) between 5 and 15% were obtained for most of the compounds except for 2,5-dicloro-6-bromo-anisole, 2,3-dibromo-6-chloroanisole, pentachloro- and pentabromoanisole (>20%). The method was linear over two orders of magnitude, and detection limits were compound dependent and ranged from 0.03 ng/L for 2,4,6-trichloroanisole to 0.25 ng/L for 2,3-dibromo-6-chloroanisole. The HS-SPME-GC-MS procedure was tested using real samples and relatively good standard deviations were obtained when using p-iodoanisole as internal standard for quantification. This is the first time that the individual identification of odorous trihalogenated chloro-bromoanisoles has been reported, being HS-SPME-GC-MS a suitable method for simultaneous determination of these compounds in water at concentration levels below their odor limit of detection.     

Simultaneous determination of nitrite and nitrate in potato and water samples using negative electrospray ionization ion mobility spectrometry

Nowadays, nitrite and nitrate ions are analyzed in biological samples using laborious and expensive methods; such as HPLC, CE, MS-MS. In this work, the simultaneous analysis of nitrite and nitrate ions was conducted by electrospray ionization-ion mobility spectrometry (ESI-IMS), without using any complicated or laborious derivitization step. Ion mobility spectrometry with low cost, inexpensive maintenance and very fast analysis makes an attractive technique for the simultaneous determination of these ions in foodstuff and drinking water samples. The analyte interference was systematically investigated for binary mixture analysis. The obtained results provided detection limits of 3.8 and 4.7 μg/L for nitrite and nitrate, respectively. A linear dynamic range of about 2 orders of magnitude, and relative standard deviations below 5% were obtained by the proposed method for the analysis of both ions. Also, the proposed method was used to analyze various real samples of potato and drinking water samples, and the obtained results confirmed the capability of negative ESI-IMS for the simultaneous detection of nitrite and nitrate.     

New computational approach for the simultaneous photometric determination of catalysts and activators

A new method for the simultaneous kinetic determination of catalysts and activators was developed on the basis of a mathematical model. The parameters and variables are optimized from experimental data obtained by application of a multiple standard-addition method and use of the Gauss-Newton and Simplex method, both of which provide identical results. The proposed method was applied to the simultaneous photometric determination of Mn(II) and Pb(II) on the basis of their catalytic and activating effects, respectively, on the oxidation of Tiron by hydrogen peroxide. Data were both acquired and processed with the aid of software developed by the authors. The linear determination range achieved was 1.00-5.00 ng/ml Mn(II) and 200-800 ng/ml Pb(II). Experimental readings were made at 450 nm with a fibre optics detector. The most serious interference with the method was posed by Cr(III).     

Simultaneous determination of N-unsubstituted and N-substituted nitroazoles and criteria for their identification-III Chromatographic separation and polarographic determination of halo-nitroimidazoles

Methods for identifying and determining halo-nitroimidazoles appearing together during synthetic processes, regardless of the preparation methods, are proposed. Polarographic determination can be used in all synthetic processes when halo-nitroimidazoles have been obtained by nitration of the halo-imidazoles. When the halo-nitroimidazoles have been obtained from 5(4)-halo-4(5)-nitroimidazoles by substitution of the imino hydrogen atom, and when only one N-substituted derivative has been obtained in a reaction mixture, simultaneous polarographic determination of both compounds is possible, but only when an alkaline medium is used as supporting electrolyte. In some cases, simultaneous polarographic determination of all three compounds present in a reaction mixture during N-substitution processes [one 5(4)-halo-4(5)-nitroimidazole and two N-substituted isomers] is also possible with alkaline supporting electrolyte. Explanations are given of the phenomena on which the simultaneous polarographic determination is based. When simultaneous polarographic determination cannot be used to determine the amount of each polarographically-active compound present in a reaction mixture, the compounds can be separated chromatographically and then determined individually by polarography.     

比光谱导数分光光度法同时测定微量磷和砷

采用比光谱导数法对严重重叠的砷钼酸和磷钼酸与乙基罗丹明Ｂ的缔合物的吸收光谱进行数据解释。结果表明，此法不需分离和掩蔽而能实现对微量砷和磷的同时测定，探讨了显色条件，测定波长及求导计算时波长间距的选择等问题，应用于合成样品和水样的分析。     

Simultaneous Determination of Gallic Acid and Folic Acid in Fruit Juice Samples Using Square Wave Voltammetry at Electrochemically Pretreated Carbon Paste Electrode

An efficient sensor was developed for the simultaneous determination of gallic and folic acid in juice samples using an electrochemically pretreated carbon paste electrode. The electrode was characterized by CV and EIS. The electrochemical behavior of GA and FA was evaluated by CV and SWV. The electrode exhibited high electrocatalytic activity towards GA and FA due to high surface area. Under the optimized condition, linear plots in the ranges of 0.08–13 μM and 0.1 to 15 μM were obtained for GA and FA, respectively. The proposed method was successful for the simultaneous determination of GA and FA in juice samples with satisfactory recovery.     

A Sensitive Sensor Based on CuTSPc and Reduced Graphene Oxide for Simultaneous Determination of the BHA and TBHQ Antioxidants in Biodiesel Samples

A novel and sensitive electrochemical sensor was developed for the simultaneous determination of the butylated hydroxyanisole (BHA) and tert‐butylhydroquinone (TBHQ) antioxidants in biodiesel samples employing the differential pulse voltammetry (DPV). In this sense, a glassy carbon electrode (GCE) modified with copper (II) tetrasulfonated phthatocyanine immobilized on reduced graphene oxide (CuTSPc/rGO) allowed the detection of BHA and TBHQ at potentials lower than those observed at unmodified electrodes. The sensor was characterized by cyclic voltammetry (CV) and linear scan voltammetry (LSV). After optimization of the experimental parameters, the analytical curves for simultaneous determination of BHA and TBHQ by DPV technique demonstrated an excellent linear response from 0.1 to 500 µmol L^?1 with detection limit of 0.045 µmol L^?1 for TBHQ and 0.036 µmol L^?1 for BHA. Finally, the proposed method was successfully applied in the simultaneous determination of BHA and TBHQ in six biodiesel samples, and the results obtained were found to be similar to those obtained using the HPLC method with agreement at 95 % confidence level.     

Application of spectral beta-correction method and partial least squares for simultaneous determination of V(IV) and V(V) in surfactant media

Simultaneous determination of V(IV) and V(V) was performed by application of partial least squares when the calibration matrix was obtained using beta-correction spectra. Two reaction between V(IV) and V(V) and Pyrogallol Red as a ligand in presence of cethyltrimethylammoniumbromide (CTAB) media has been investigated and applied to the simultaneous spectrophotometric determination of these species. The parameters controlling behavior of the system were investigated and optimum conditions selected. Determinations were made over the concentration range 0.6-4.50 microg ml-1 of V(IV) and 0.3-5.50 microg ml-1 of V(V). Applying this method to simultaneous determination of these metal ions in several real samples with total relative standard error less than 5% validated the proposed method.     

模式空间变换技术解析多组份光谱重叠体系及其在食用色素同时？…

采用模式空间变换技术使多组份光谱重叠体系中各组份得到有效地分离从而达到部分或所有组份定性及定量的目的。方法分辨效果好,定性定量结果可靠。无论光谱重叠程度如何,只要光谱间存在一定的差异即可得到较好的结果。将该方法用于人工合成食用色素多组份体系中各组份的同时测定,获得了较好的结果。     

Simultaneous determination of calcium and magnesium by using a flow-injection system with simultaneous injection of two sample plugs and a masking agent plug

A flow-injection system is described for the simultaneous determination of calcium and magnesium with simultaneous injection of two sample plugs and a masking agent plug and with a single detector. The system utilizes the simultaneous injection of an ethylene glycol-bis(2-aminoethylether)-N,N,N',N'-tetra-acetic acid plug and two small sample plugs into the same carrier stream and which are merged downstream with 3,3'-bis[N,N-bis(carboxymethyl)aminomethyl)]-o-cresolphthalein solution for spectrophotometric determination of calcium and magnesium. The results for the analysis of natural waters by the proposed method correspond well with those obtained by the conventional titration method with ethylenediaminetetra-acetic acid, and showed good reproducibility. The rate of analysis is about 15 samples/hr.     

Analysis of odorous trichlorobromophenols in water by in-sample derivatization/solid-phase microextraction GC/MS

The simultaneous determination of several odorous trichlorobromophenols in water has been carried out by an in-sample derivatization headspace solid-phase microextraction method (HS-SPME).The analytical procedure involved their derivatization to methyl ethers with dimethyl sulfate/NaOH and further HS-SPME and gas chromatography-mass spectrometry (GC/MS) determination. Parameters affecting both the derivatization efficiency and headspace SPME procedures, such as the selection of the SPME fiber coating, derivatization–extraction time and temperature, were studied. The commercially available polydimethylsiloxane (PDMS) 100 μm and Carboxen-polydimethylsiloxane-divinylbenzene (CAR-PDMS-DVB) fibers appeared to be the most suitable for the simultaneous determination of these compounds. The precision of the HS-SPME/GC/MS method gave good relative standard deviations (RSDs) run-to-run between 9% and 19% for most of them, except for 2,5-diCl-6-Br-phenol, 2,6-diCl-3-Br-phenol and-2,3,6-triBr-phenol (22%, 25% and 23%, respectively). The method was linear over two orders of magnitude, and detection limits were compound dependent but ranged from 0.22 ng/l to 0.95 ng/l. The results obtained for water samples using the proposed SPME procedure were compared with those found with the EPA 625 method, and good agreement was achieved. Therefore, the in-sample derivatization HS-SPME/GC/MS procedure here proposed is a suitable method for the simultaneous determination of odorous trichlorobromophenols in water.