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itriolage, a heinous crime committed with intention to disfigure a person has come into view as an extremely brutal gender-based crime especially against young women in India and also another part of world mainly in South Asia over the past few years. India is facing an alarming situation of crime against women such as rape, domestic violence, dowry deaths etc. In recent year’s cases of vitriolage are on the rise in India. By understanding the gravity of crime, section 326A and 326B was incorporated in the prevailing Indian Penal Code and came into effect from 3 February 2013. Forensic Science Laboratory, Delhi receives a number of cases pertaining to acid attacks every year. We present here five such cases which were received for forensic examination. The exhibits were analyzed using Ion Chromatography apart from classical tests in order to strengthen the forensic reports and play vital role in conviction of the accused. This paper encompasses the necessity and importance of controlled samples treated with the quality of water used in analysis, importance of packing of exhibits and role of investigating agencies/police in collection of exhibits, which play crucial role in proving the sanctity of the forensic examination.

The global incidence of high fluoride levels in groundwater and its role in various health complications necessitate the development of effective methods for its reduction to sustainable limits. Thus, this study proposed an electrocoagulation technology of fluoride removal from groundwater. The groundwater having 4 mg/L fluoride was collected at 70 m depth from Khalra village (31.3955°N, 74.6211°E), Tarn Taran district, Punjab, India. Analysis of fluoride concentration was carried out using ion-chromatography. The central composite design (CCD) was employed to optimize the effect of treatment time and current density. Permissible fluoride concentration (1.5 mg/L) in drinking water was achieved at pH 7.4, treatment time 37 min, and current density 40 A/m² using aluminum electrodes with 1.64 kWh/m³ of energy consumption. The fluoride removal follows the pseudo-first-order kinetic model. Negative values of zeta potential indicated OH– surface exchange mechanism of fluoride. Boehmite AlO(OH) formation in sludge was confirmed using X-ray diffraction. Fourier-transform infrared spectroscopy and Raman spectroscopy of sludge revealed that complex formation between aluminum hydroxide/oxyhydroxide and fluoride is crucial for removal. [ABSTRACT FROM AUTHOR]

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Alternaria leaf blight is major fungal disease of summer groundnut, causes significant loss of haulm and pod yield. Aims of this study were to understand the role of metabolites and phenylpropanoid related enzymes in Alternaria leaf blight resistance and to find out metabolic marker for disease resistance. Alternaria leaf blight resistant (GPBD4 and CS186) and susceptible genotypes (GG2 and TPG41) of groundnut were grown in pots during rabi-summer 2015. Groundnut plants were infected with Alternaria alternata (Fr.) Keissler at 40 days after sowing. 5 days after infection, upper second leaves were collected from both control and infected plants for analysis. A total of 67 metabolites comprising sugars, sugar alcohols, amino acids, organic acids, fatty acids, sterols and phenolic were identified using gas chromatography–mass spectrometry (non-targeted metabolomics). Constitutive levels of alpha-d-galactoside, d-mannitol, d-erythropentitol, glycine, and hexadecanoic acid were observed higher in resistant genotypes compared to susceptible genotypes. Moreover, arabinofuranose, cinnamic acid, 2-butendioic acid, and linoleic acid were observed only in resistant genotypes at both control and infected stage. In susceptible genotypes myo-inositol, glucose and fructose content was increased after infection with pathogen while decreased in resistant genotypes. Resistant genotypes had higher constitutive level of cinnamic and salicylic acid compared to susceptible genotypes. Non-infected leaves of resistant genotypes also had higher activities of phenylalanine ammonia lyase and tyrosine ammonia lyase activities. Our results suggest that metabolites specifically present in resistant genotypes impart defense mechanism against Alternaria pathogen and can be used as bio-marker for screening of germplasm. [ABSTRACT FROM AUTHOR]

The addition of oxidants for disinfecting water can lead to the formation of potentially carcinogenic compounds referred to as disinfection byproducts (DBPs). Haloacetic acids (HAAs) are one of the most widely detected DBPs in US water utilities and some of them are regulated by the US Environmental Protection Agency (USEPA). The present study developed a method to analyze all the compounds in the USEPA method 557 (nine HAAs, bromate and dalapon) plus four potentially more toxic iodinated HAAs in water by coupling ion chromatography with tandem mass spectrometry (IC–MS/MS). This aqueous direct injection method has significant advantages over traditional GC methods, which require a derivatization and sample extraction that are laborious, time-consuming, and can negatively impact reproducibility. The method developed in this study requires half the time of the current USEPA method 557 on IC–MS/MS while including more compounds and achieving sub-μg/L level method detection limits (MDLs) for all 15 target analytes. The single laboratory lowest concentration minimum reporting level (LCMRL) has also been determined in reagent water, which ranged from 0.011 to 0.62 μg/L for the analytes. The mean recoveries of the analytes during matrix spike recovery tests were 77–125% in finished drinking water and 81–112% in surface water. This method was then applied to untreated, chlorinated, and chloraminated groundwater and surface water samples. Bromate and 9 HAAs were detected at different levels in some of these samples. [ABSTRACT FROM AUTHOR]

Age of individual uranium-plutonium (U/Pu) mixed particles with various U/Pu atomic ratios (1-70) were determined by inductively coupled plasma mass spectrometry. Micron-sized particles were prepared from U and Pu certified reference materials. The Pu reference was stored for 4-6 years since the last purification (July 14, 2008). The Pu purification age was obtained from the Am/Pu ratio which was calculated from the product of three measured ratios of Pu and Am isotopes in the eluted fractions. These ratios were measured by a high-resolution inductively coupled plasma mass spectrometer equipped with a desolvation system. Femto-gram to pico-gram quantities of Am, U, and Pu in a sample solution were sequentially separated on a small anion-exchange column. The Am/Pu ratio was accurately determined by spiking pure Am into the sample solution. The average determined age for the particles for the five independent U/Pu ratios was in good agreement with the expected age with high accuracy (difference age 0.27 years) and high precision (standard deviation 0.44 years). The described analytical technique can serve as an effective tool for nuclear safeguards and environmental radiochemistry. [Figure not available: see fulltext.] [ABSTRACT FROM AUTHOR]

The distinct reactivities of Mo and Re in oxic versus anoxic waters make these elements ideally suited for use as redox proxies. However, their full exploitation as geochemical tracers requires that their chemical transformations in sulfidic water be well understood. While thermodynamic data have been used to predict Mo and Re speciation within sulfidic waters, these predictions remain unsubstantiated because effective methodologies for separating the thiomolybdate (Mo VI O x S 4 − x 2 − ) and thioperrhenate (Re VII O x S 4 − x − ) anions within natural settings have yet to be developed. Anion exchange chromatography (AEC) is often employed to provide separation of environmentally important anions. For example, thiometalates of As and Sb have been quantified in sulfidic geothermal waters using AEC coupled with inductively coupled plasma mass spectrometry (ICP-MS). Unfortunately, AEC methods are incapable of separating the thiomolybdate or thioperrhenate anions due to the extreme retention these thiometalates experience on AEC columns. Because reverse phase ion pair chromatography (RP-IPC) offers greatly diminished retention times, we have developed RP-IPC methods that are capable of separating all stable thiomolybdates and thioperrhenates within 40 min. An isocratic method provides effective separation of the thiomolybdates. Thioperrhenates and mixtures of the thiomolybdates and thioperrhenates require gradient methods. Addition of p-cyanophenol (p-CP) to the eluent markedly reduces thiometalate retention and facilitates their separation. Our efforts could lead in the near future to coupling RP-IPC with ICP-MS or multi-collector ICP-MS for characterizing Mo and Re speciation in natural sulfidic waters as well as potential fractionation among Mo and Re isotopes during speciation changes. [ABSTRACT FROM AUTHOR]

A new, highly sensitive and reliable two-dimensional matrix elimination ion chromatography (IC) method was developed for simultaneous detection of bromate, chlorite and five haloacetic acids. This method combined the conventional IC in first dimension with capillary IC in the second dimension coupled with suppressed conductivity detection. The first dimension utilizes a high capacity column to partially resolve matrix from target analytes. By optimizing the cut window, the target analytes were selectively cut and trapped in a trap column through the use of a six-port valve, while the separated matrix were diverted to waste. The trapped target analytes were delivered on to the capillary column for further separation and detection. Temperature programming was used to improve selectivity in second dimension column to obtain complete resolution of the target analytes. Compared to the performance of one-dimensional IC, the two-dimensional approach resulted in a significant increase in sensitivity for all target analytes with limit of detection ranging from 0.30 to 0.64 μg/L and provided more reliable analysis due to second column confirmation. Good linearity was obtained for all the target analytes with correlation coefficients >0.998. The proposed method was successfully applied to the determination of oxyhalides and haloacetic acids in various matrices with recoveries ranging from 90 to 116% and RSD less than 6.1%. The method allows direct injection of samples and the use of columns with different selectivity, thus significantly reduces the level of false positive results. The method is fully automated and simple, making it practical for routine monitoring of water quality. The satisfactory results also demonstrated that the two-dimensional matrix elimination method coupled with capillary IC is a promising approach for detection of trace substances in complex matrices. [ABSTRACT FROM AUTHOR]

Background The majority of studies examining anionic composition in human saliva have focused on inorganic anions only, and accompanying organic anion concentration has often been overlooked in the development of artificial salivas. The purpose of this study was to examine the major organic anionic species profile of human saliva, with a view to gaining further insight into human salivary chemistry. Methods Unstimulated whole saliva was collected from 11 healthy volunteers over a period of 18 months. Samples were subjected to ion chromatography for detection and quantification of organic and inorganic anions. Results Among organic anions, acetate was predominant (0.24 ± 0.38 mmol/l), with lactate (0.01 ± 0.04 mmol/l), propionate (0.03 ± 0.07 mmol/l), and formate (0.02 ± 0.03 mmol/l) detected at lower levels. Acetate, propionate, and formate were detected in at least 80% of the saliva samples. Positive partial correlations were found between phosphate and sulfate (r = 0.510, p-value = 1.545 × 10 − 4 ), and between propionate and acetate (r = 0.836, p-value = 7.510 × 10 − 14 ). Conclusion Organic anionic species were consistently detected at low levels in saliva samples collected longitudinally over a period of 18 months. These salivary components must be considered in order to understand saliva chemistry, and should not be neglected during the continuing development of artificial salivas. [ABSTRACT FROM AUTHOR]

The reduction of vanadate (+V) in the presence of 3-mercaptopropionic acid was studied using a chromatographic method for the determination of vanadate (+V) versus vanadyl (+IV) species. Ion chromatography was combined with spectrophotometric investigation of the absorption properties of the solution. The chromatographic method for the separation of vanadate (+V) and vanadyl (+IV) was carried out with an anion exchange column. In the initial reaction mixture containing vanadate (+V) and 3-mercaptopropionic acid, ethylenediaminetetraacetic acid – EDTA was added in an excessive amount relative to the concentration of reactants in the solution. After the ligand exchange reaction, the added EDTA terminates the reduction, allowing redox speciation in the solutions. A strong pH dependence of the reduction rates in the investigated solution was observed. The vanadate reduction seems to proceed in 2 steps: 1) formation of the intermediate vanadate (+V)-thioester; 2) reduction reaction and formation of the vanadyl (+IV)-thiol complex. The obtained results strongly suggest that the reaction of vanadate (+V)-thioester formation is proton catalyzed. It was observed that the overall reduction rates are pH dependent due to the complex vanadate (+V) solution speciation and changes in the ionic form of 3-mercaptopropionic acid. Synopsis: Ion Chromatography results show decrease of vanadate (+V) – EDTA and increase of vanadyl (+IV) - EDTA signal. Reduction is fast in the initial 120 min of reaction. Afterward, no signal intensity changes are observed indicating reaction termination. Vanadate reduction is pH dependent with higher reduction rates at lower pH values. [Display omitted] • Vanadate – V(+V) is easily reduced by biological thiols at lower pH values. • V(+V) reduction is slower at high pH value due to V(+V)-thioester formation. • V(+V) and vanadyl – V(+IV) form complexes with 3–mercaptopropionic acid. • Thiols-induced V(+V) reduction is successfully detected by ion chromatography. [ABSTRACT FROM AUTHOR]

The levels of the anions fluoride (F), bromide, chloride, nitrate, and sulphate were measured in 51 underground water samples, collected from 33 places in West Bengal, India, using the ion-chromatographic method. The F concentrations were within tolerable limits except for the villages of Kapileswar, Haringhata, (1.24 mg/L); Palta, 24 Parganas (North), (1.75 mg/L); Rondia, near Panagarh, (1.61 mg/L); Midnapore (1.38 mg/L); Hijli (1.08 mg/L); and Laxmanpur, Purulia, (1.06 mg/L). The ground water samples of these villages, were found, in general, to be alkaline in nature. The F concentrations appeared to be related to the physiographic and geological nature of the soils. A forensic investigation into the death of a 25-yr-old male from sodium fluoride overdose, resulting in F levels in the gastric contents and blood of 35.05 and 4.341 mg/L, respectively, is also noted. [ABSTRACT FROM AUTHOR]

Highlights: [•] Ion chromatography–inductively coupled plasma mass spectrometry method for iron. [•] Redox speciation analysis of iron. [•] Carryover assessment using isotopically enriched analyte analogs. [•] Systematic identification and elimination of carryover. [•] Determination of iron species in real sample with mass balance. [Copyright &y& Elsevier]

A method based on ion-chromatography has been developed for determination of Cs and Sr in high level waste (HLW) without matrix separation. The acidity of HLW (3 M HNO) was decreased to 0.01 M by addition of NaOH. Chromatographic separation of Cs and Sr in presence of bulk Na has achieved using methane sulphonic acid as mobile phase in isocratic and gradient mode. The calibration plot was linear for the concentration range of 0.5-12 mg/L for Cs and 0.025-6 mg/L for Sr with regression coefficients close to 1. RSD obtained for Cs and Sr was 1 and 5 % respectively. Detection limit calculated as 3(S/N) was found to be 20 μg/L for Cs and 30 μg/L for Sr. The standard addition procedure was used to validate the developed method. The samples received from PREFRE, Tarapur and WIP, BARC were analyzed by the new method and the results are presented. [ABSTRACT FROM AUTHOR]

An ion chromatographic (IC) method has been developed for determination of trace levels of halide impurities in various types of ionic liquids (ILs). The advantage of this method is that all relevant halide species can be measured in a single chromatographic analysis. Separation of halides was performed on a Dionex AS9-HC column using an eluent consisting of 20 mM NaOH and 10% ( v/v) acetonitrile, delivered at 1.5 mL min−1. Using this eluent, fluoride, chloride and bromide were well resolved from each other, but iodide was co-eluted with tetrafluoroborate (BF) present as a counter-anion in tetrafluoroborate-based ILs. The same eluent was also used successfully for the determination of halides in highly hydrophobic ILs, such as those based on bis-(trifluoromethanesulfonyl)imide (TFSI−) and bis-perfluoroethylsulfonylimide (BETI−). In this case, 50% ( v/v) acetonitrile aqueous was needed to dissolve the sample before injection, and this did not adversely affect the separation. Detection limits in the measured solution were 0.1, 0.2 and 1.0 ppm for chloride, bromide and iodide, respectively, by conductivity detection, and 0.02 ppm for iodide by UV detection. [ABSTRACT FROM AUTHOR]

The formation of Cr(VI) in Cr(III) tanned leather, in neutral and alkaline solution, has been demonstrated by means of crossed experiments using different pH buffers, ethylenediaminetetraacetic acid as Cr(III) complexing agent and NaCl solutions. According to the found results the composition of the extracting solution suitable to extract Cr(VI) amount present in leather was pH 4.4 (which is also the tanned leather natural pH) and 5% NaCl (w/v). Interferences coming from coloured compounds have been eliminated with suitable SPE cartridges. A new protocol for the analysis of Cr(VI) based on ion chromatography and a diphenylcarbazide post-column reaction has been implemented. The use of a large volume injection loop (500 μl) allowed to obtain a very low quantification limit (0.15 mg kg-1) despite the low amount of leather extracted (0.2 g with respect to 2.0 g used by the IUC 18 official method). Evidence of the transient nature of Cr(VI) in leather requires using the external calibration procedure for the correct quantification of the species. [Copyright &y& Elsevier]

Selected trace transition metal ions have been determined in an FIA/HPLC hyphenated system using on-line preconcentration on cellulose functionalised sorbent Cellex P. For HPLC separation ion-pair chromatography was employed with spectrophotometric detection at 510 nm using post-column derivatisation with PAR. Favourable kinetic conditions of sorption and elution as well as optimisation of hyphenated system allowed to obtain detection limits at sub-μg L−1 level at 25 min preconcentration time. The developed method was employed for determination of Co(II), Ni(II), Cd(II) and Mn(II) in river water with reasonable agreement of obtained results with electrothermal AAS determination. [Copyright &y& Elsevier]

Retention behavior of anions and cations on anion-exchangers modified with dextran sulfate has been investigated. Retention of anions was remarkably reduced by the modification, and the retention factor decreased with decreasing eluent concentration when sodium sulfate was used as the eluent. Cations were also retained on the modified stationary phase, and alkali and alkaline-earth metal ions were separated using copper sulfate or tris(2,2′-bipyridyl)ruthenium chloride as eluent. The size of the dextran sulfate strongly affected the retention behavior of analyte ions. [ABSTRACT FROM AUTHOR]

• Disinfection by products monitored to fulfil Drinking water directive revision. • Haloacetic acids (HAAs) are determined together with oxyhalides by IC-MS/MS. • Disproportionate concentrations of oxyhalides do not affect accurate HAA analysis. • In drinking water, the method satisfies the recovery limits set EPA. • A tool to check control measures in water treatment, distribution and storage. According to the recent proposal released by the European Commission for the revision of the 98/83/EC Directive, water suppliers will be requested to monitor the nine bromine- and chlorine congeners of haloacetic acids, HAAs, as well as the oxyhalides chlorite and chlorate, as disinfection by-products (DBPs) originated during the potabilization process. In this work, we propose a direct-injection method based on ion chromatography and mass spectrometric detection for the determination of the mentioned DBPs as well as bromate (already included in the 98/83/EC), implemented also for the following emerging HAAs monoiodo-, chloroiodo- and diiodo-acetic acids. The method was optimized to include the fifteen compounds in the same analytical run, tuning the chromatographic (column and gradient) and detection conditions (suppression current, transitions, RF lens settings and collision energies). To avoid matrix effect and to manage the instrumental conditions, optimization was performed directly in drinking water matrix. The method quantitation limits satisfy the new limits imposed by the future directive and range from 0.08 μg/L (monobromoacetic acid) to 0.34 μg/L (trichloroacetic acid). The performance of the method was checked along different strategic sampling points of three potabilization plants serving the city of Turin (Italy), including intermediate treatments and finished waters. Recovery was checked according to the ±30% limit of acceptability set by EPA regulations. The effect of disproportionate concentrations of chlorite and chlorate in respect to HAAs on HAA signals was studied; this aspect is underestimated in literature. The method is routinely applied by the potabilization plant of the city of Turin to confirm the effectiveness of all control measures in abstraction, treatment, distribution and storage. This study represents the first example in Italy of development and use of a cutting-edge technique for HAAs analysis along the potabilization processes. [ABSTRACT FROM AUTHOR]

A highly sensitive and selective ion-chromatographic procedure with UV detection at 227 nm was developed for the determination of trace amounts of iodide. The procedure utilizes 0.1 M NaOH as eluent, which enables the determination of 1–100 μg I−1 I− with a precision of ca. 6%. 1000-fold amounts of other anions such as fluoride, chloride, phosphate, sulphate, bromide, nitrite and nitrate do not interfere. The method has been applied to determine iodide in sea water samples from the Indian coast. [ABSTRACT FROM AUTHOR]

Ion-chromatography, a relatively new technique in analytical chemistry, has already shown great promise toward solving complex trace analysis problems, in particular the speciation and quantitation of anions. It is especially attractive to the field of microanalysis. The method of sample preparation, however, is crucial in order to realize this capacity. Existing microanalytical methods nearly always must be modified to be compatible with ion-chrornatography, and often, more extensive sample cleanup is required than is needed for "single species" methods. These considerations have been applied to the determination of chloride and bromide in waste oil, and to the analysis of oyster tissue. Pretreatment with polystyrene resin and ion-exchange resin is discussed.