Method For Determination Of Chlorine Research Articles

Novel method for chlorine determination in biofuel lipid feedstock by coupling a total sample introduction system (hTISIS) to an inductively coupled plasma tandem mass spectrometry (ICP-MS/MS)

BackgroundChlorine concentrations above 1 mg kg−1 in lipid feedstocks for biofuel production can generate corrosion issues in the different refining units as well as catalyst deactivation by clogging or fouling. To reach accurate analyses by inductively coupled plasma (ICP) techniques at low concentration levels, dilution in organic solvents rises as a simpler and more straightforward sample preparation methodology than conventional sample decomposition procedures (e.g., microwave-assisted acid digestion). However, matrix effects and the impact of the Cl chemical form on the signal must be overcome to obtain accurate results. ResultsIn this work, the high temperature torch integrated sample introduction system (hTISIS) operated at 350 °C is coupled to an inductively coupled plasma tandem mass spectrometry (ICP-MS/MS) for the determination of Cl in lipid biofuel feedstock samples diluted in xylene and these results are compared with those reported by a conventional sample introduction system. Under optimal conditions of the hTISIS-ICP-MS/MS configuration, matrix effects are efficiently overcome (recovery values ranged from 101 to 104%) as well as the effect of the Cl chemical form on the signal for 6 organochloride compounds. Thus, an external calibration approach can be set to carry out the quantification of this element in real samples. The method is successfully validated, obtaining a good agreement in the Cl concentration reported in a standard reference material (SRM NIST 1634c) and also by comparing the concentration results obtained by external calibration and standard addition approaches in two biofuel feedstock samples. Significance and noveltyThe hTISIS coupled to an ICP-MS/MS system is used for the first time to overcome not only matrix effects but also the impact of the Cl chemical form in biofuel feedstock samples. This novel method, with a limit of quantification (LOQ) of 7.1 μg kg−1, give access to an accurate Cl determination in all kind of lipid feedstocks for clean fuel production.

Determination of Chlorine in Crude Oil Emulsified via the MgCl Molecule by HR‑CS MAS

A method for chlorine determination in crude oil samples, through the formation of MgCl molecule, by high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS) was developed and is described in this paper. The use of this molecule for chlorine determination in crude oil has not been reported up to now. Measures were carried out at the wavelength 377.010 nm and the samples were submitted to a simple treatment as emulsion, whose composition was optimized applying a simplex-centroid experimental design. Magnesium was used as molecule forming agent at the concentration of 10 g L-1, at least 500 times higher than the concentration of chlorine. This excess is required to ensure the molecule formation of all content of Cl present in the sample. Chemical modifier Pd was used and improved greatly the signal intensities. Optimized pyrolysis and vaporization temperatures, applied for determination, were 800 and 2300 °C, respectively. Accuracy was evaluated through analysis of certified reference materials, NIST 1848 and NIST 1634c, and addition and recovery tests with recoveries between 92 and 117%. Limits of detection and quantification were 3.0 and 9.0 µg g-1, respectively. The method was applied to eight crude oil samples.

A new method for chlorine determination in commercial pet food after decomposition by microwave-induced combustion

A new method for commercial pet food decomposition using microwave-induced combustion was developed for further determination of chlorine by ion selective electrode.

Heavy crude oil sample preparation by pyrohydrolysis for further determination.

In this work, a method for chlorine determination in heavy crude oil using pyrohydrolysis for sample decomposition was developed. Chlorine was determined using ion chromatography (IC), inductively coupled plasma optical emission spectrometry (ICP OES) and inductively coupled plasma mass spectrometry. In this case an ICP-MS spectrometer equipped with a dynamic reaction cell (DRC-ICP-MS) was used. Heavy crude oil samples were homogenized and placed on a quartz holder, which was then introduced into the pyrohydrolysis apparatus. Nitric acid (0.2 mL) was used to assist the decomposition of the sample. Solutions with different concentrations of ammonium hydroxide were evaluated to collect the volatile chloride produced using pyrohydrolysis. A 0.75 mol L-1 ammonium hydroxide solution was chosen in view of the better accuracy achieved. Best precision and accuracy were obtained by heating the sample for 10 min up to 1000 °C. The limits of quantification (LOQs, 10σ) of chlorine measured by IC, ICP OES and DRC-ICP-MS were 4.5, 48 and 3.6 µg g-1, respectively. A sample amount of 300 mg and final volume of 20 mL were taken into account to calculate the LOQs. The relative standard deviation (RSD) was lower than 5% (4 replicates). Accuracy was evaluated by analysis of certified reference material (NIST 1634c) and comparison with the results obtained using the ASTM D6470 method. In both cases the results obtained using pyrohydrolysis were in agreement. The proposed method was suitable for heavy crude oil decomposition and chlorine determination by IC, ICP OES and DRC-ICP-MS. Three samples per hour can be processed using a simple and low-cost pyrohydrolysis apparatus. The pyrohydrolysis procedure is easy to perform, which is very attractive for routine analysis of crude oil, a very complex matrix. According to the authors' knowledge this is the first application of pyrohydrolysis for heavy crude oil sample preparation.

Determinação espectrofotométrica em fluxo de cloro em água usando célula de longo caminho óptico e multicomutação

A multicommuted method for determination of chlorine in water samples using a 100-cm cell was developed. In this method, orto-Tolidine reacts with chlorine and the product was monitored at 438 nm. The analytical curve for chlorine was linear in concentration range from 1.34x10-6 to 2.01x10-5 mol L-1 with a detection limit of 9.40x10-8 mol L-1. A sampling rate of 45 h-1and a RSD of 1.0 % (n = 15) were obtained. The method was applied with success for chlorine determination in six water samples.

A Sensitive Extracto-Photometric Method for Determination of Residual Chlorine in Greywater

A new photometric method for chlorine determination based on the oxidative transformation of iodide to iodine and subsequent extraction in ethyl acetate has been developed. The effects of several chemical variables (pH, ionic strength, and iodide concentration) have been studied. Characteristics of the method were linear range 0-0.6 mg C12/L, limit of detection 5 microg Cl2/L, and coefficient of variation 0.6%. The method has been applied to greywater without previous sample treatment.

Determination of chlorine in atmosphere by kinetic spectrophotometry

A kinetic method for determination of chlorine in air was described in the present work. The method based on fading of methyl orange (MO) containing solution in air absorption process. A determination limit of 2.64 μg L −1 was found. With the present method, chlorine concentration could be determined in several minutes with convenient manipulation. As concentration variation of methyl orange in the absorption solution did not affect the experimental results, fabrication and preservation of the stock absorption is also convenient. The present method is promising in monitoring chlorine concentration in atmosphere.

Determination of chlorine and bromine in automotive shredder residues by oxygen bomb and ion chromatography.

An analytical procedure, oxygen bomb combustion-ion chromatography (IC), has been developed for the determination of total chlorine in Automotive Shredder Residues (ASR). Samples of these residues are fired under elevated oxygen pressure (30 atm) and the combustion products are transferred into a Na2CO3/NaHCO3 absorbent solution containing 1% of H2O2; the chlorine contents are then evaluated by ion chromatography. The use of the non-suppressed IC determination with a conductivity detector provides a rapid, sensitive and selective method for chlorine determination in ASR, allowing determinations of this heteroatom at levels below 1% in the presence of bromine and sulfur. Moreover, the proposed method allows the simultaneous determination of chlorine, bromine and sulfur which are potential environmental hazards.

Colorimetric method for determination of chlorine with 3,3′,5,5′-tetramethylbenzidine

A new method is developed for the calorimetric determination in water of chlorine (free and combined) with 3,3′,5,5′-tetramethylbenzidine. The procedure proposed achieves a detection limit of 2 ng/ml and its sensitivity is greater than that of the methods used at present.

An ion-selective electrode method for determination of chlorine in geological materials

A method is presented for the determination of chlorine in geological materials, in which a chloride-selective ion electrode is used after decomposition of the sample with hydrofluoric acid and separation of chlorine in a gas-diffusion cell. Data are presented for 30 geological standard materials. The relative standard deviation of the method is estimated to be better than 8% for amounts of chloride of 10 μg and greater.

Bestimmung geringer Chlor-konzentrationen nach der methylorange-methode

Due to the minimum value of 0.3μg C1 2 absolute, the Methyl orange method for determination of Chlorine is suitable for the measurement in the emission concentration range. By means of careful selection, the graphic method is accurate. NO, NO 2, H 2S, HCl and HF have no effect on the measurement. The standard deviation is in the order of 2.4% relative, or ±0.05 μg Cl 2/ m 3 absolute.

An Accurate Rapid Method for the Quantitative Determination of Chlorine in the Urine; A Critical Study of the Short Methods in Vogue

An Accurate Rapid Method for the Quantitative Determination of Chlorine in the Urine; A Critical Study of the Short Methods in Vogue