Quantifying uncertainty in the measurement of arsenic in suspended particulate matter by Atomic Absorption Spectrometry with hydride generator.

Arsenic is the toxic element, which creates several problems in human being specially when inhaled through air. So the accurate and precise measurement of arsenic in suspended particulate matter (SPM) is of prime importance as it gives information about the level of toxicity in the environment, and preventive measures could be taken in the effective areas. Quality assurance is equally important in the measurement of arsenic in SPM samples before making any decision. The quality and reliability of the data of such volatile elements depends upon the measurement of uncertainty of each step involved from sampling to analysis. The analytical results quantifying uncertainty gives a measure of the confidence level of the concerned laboratory. So the main objective of this study was to determine arsenic content in SPM samples with uncertainty budget and to find out various potential sources of uncertainty, which affects the results. Keeping these facts, we have selected seven diverse sites of Delhi (National Capital of India) for quantification of arsenic content in SPM samples with uncertainty budget following sampling by HVS to analysis by Atomic Absorption Spectrometer-Hydride Generator (AAS-HG). In the measurement of arsenic in SPM samples so many steps are involved from sampling to final result and we have considered various potential sources of uncertainties. The calculation of uncertainty is based on ISO/IEC17025: 2005 document and EURACHEM guideline. It has been found that the final results mostly depend on the uncertainty in measurement mainly due to repeatability, final volume prepared for analysis, weighing balance and sampling by HVS. After the analysis of data of seven diverse sites of Delhi, it has been concluded that during the period from 31st Jan. 2008 to 7th Feb. 2008 the arsenic concentration varies from 1.44 ± 0.25 to 5.58 ± 0.55 ng/m3 with 95% confidence level (k = 2).

Monitoring the trace metals concentration in rice by flame atomic absorption spectrometer and inductively coupled plasma atomic emission spectrometer.

The objective of this study was to monitor the concentration of trace metals in rice. Eight different commercial rice samples were collected from retail market and among these samples Fe, Cd, Cr and Zn metal concentrations were determined by using Flame Atomic Absorption Spectrometer (FAAS) and Inductively Coupled Plasma Atomic Emission Spectrophotometer (ICP-AES). The powdered rice samples were digested by wet chemical method. The analytical results obtained by both the instruments were found comparable. The accuracy of the method has been confirmed by analyzing Certified Reference Material CRM No. 10-b of National Institute for Environmental Studies (NIES). The concentrations of Fe, Cd, Cr and Zn in different brands were found in the range of 15.4 +/- 1.1 to 57.7 +/- 2.5 mg/kg, 0.08 +/- 0.03 to 0.39 +/- 0.05 mg/kg, 0.16 +/- 0.03 to 0.58 +/- 0.08 mg/kg and 7.3 +/- 0.3 to 18.6 +/- 0.5 mg/kg respectively. The standard deviation of the measurements has been calculated for Fe, Cd, Cr and Zn in six replicates of each sample and was found to be less than +/- 3% by the method proposed.

Selective masking and demasking for the stepwise complexometric determination of aluminium, lead and zinc from the same solution.

BACKGROUND: A complexometric method based on selective masking and de-masking has been developed for the rapid determination of aluminium, lead and zinc from the same solution in glass and glass frit samples. The determination is carried out using potassium cyanide to mask zinc, and excess disodium salt of EDTA to mask lead and aluminium. The excess EDTA was titrated with standard Mn(II)SO(4 )solution using Erichrome Black-T as the indicator. Subsequently selective de-masking agents - triethanolamine, 2,3-dimercaptopropanol and a formaldehyde/acetone mixture - were used to determine quantities of aluminium, lead and zinc in a stepwise and selective manner. RESULTS: The accuracy of the method was established by analysing glass certified reference material NBS 1412. The standard deviation of the measurements, calculated by analysing five replicates of each sample, was found to be less than 1.5% for the method proposed. CONCLUSION: The novelty of the method lies in its simplicity and accuracy afforded by there not being a need for a prior separation or instrumentation. The proposed method was found to be highly selective for the precise determination of aluminum, zinc and lead in the routine analysis of glass batch and allied materials.

Stepwise complexometric determination of aluminium, titanium and iron concentrations in silica sand and allied materials.

BACKGROUND: This study aimed at measuring the quantities of Al, Ti and Fe in silica sand and allied materials employing a complexometric method in the same analyte and a stepwise indirect titration with EDTA. The method involves the complexation of Al, Ti and Fe with excess EDTA and the selective de-complexation of TiO-EDTA and Al-EDTA complexes with tartaric acid and NaF respectively. In addition to its simplicity, rapidity and accuracy, the proposed method does not require the use of a separation technique or any sophisticated instrumentation. RESULTS: Each of the test samples were analyzed five times using the proposed method. The method's accuracy was confirmed by analyzing the US National Institute of Standards and Technology's (NIST) Standard Reference Materials (SRM) 81a, 89 and IPT SRM 61 using the procedure proposed, in addition to analyzing Ti and Fe levels by spectrophotometry and that of Al by complexometry. CONCLUSION: The study shows that there is good agreement between the proposed and existing methods. The standard deviations of the measurements were calculated by analyzing five replicates of each sample, and were found to be less than 1.5% in our method.

Synthesis, X-ray crystal structure, anti-fungal and anti-cancer activity of [Ag2(NH3)2(salH)2] (salH2=salicylic acid).

[Ag(2)(NH(3))(2)(salH)(2)] (salH(2)=salicylic acid) was synthesised from salicylic acid and Ag(2)O in concentrated aqueous NH(3) and the dimeric Ag(I) complex was characterised using X-ray crystallography. The complex is centrosymmetric with each metal coordinated to a salicylate carboxylate oxygen and to an ammonia nitrogen atom in an almost linear fashion. The two [Ag(NH(3))(salH)] units in the complex are linked by an Ag-Ag bond. Whilst metal-free salH(2) did not prevent the growth of the fungal pathogen Candida albicans [Ag(2)(NH(3))(2)(salH)(2)], [Ag(2)(salH)(2)] and some simple Ag(I) salts greatly inhibited cell reproduction. SalH(2), [Ag(2)(NH(3))(2)(salH)(2)] [Ag(2)(salH)(2)] and AgClO(4) produced a dose-dependent cytotoxic response against the three human derived cancer cell lines, Cal-27, Hep-G2 and A-498, with the Ag(I)-containing reagents being the most effective.