Highly Selective and Sensitized Spectrophotometric Determination of Iron (III) Following Potentiometric Study

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Article
Highly Selective and Sensitized Spectrophotometric Determination of Iron (III) Following Potentiometric Study
Ardeshir Shokrollahi, Mehrorang Ghaedi *, Hamid Reza Rajabi
Chemistry Department Yasouj University Yasouj Iran 75914-353
email: Mehrorang Ghaedi (m_ghaedi@mail.yu.ac.ir)
*Correspondence to Mehrorang Ghaedi, Chemistry Department Yasouj University Yasouj Iran 75914-353, Tel.Fax. (+98)-741-2223048
setDOI("ADOI=10.1002/adic.200790067")
Abstract
A simple, selective and sensitized spectrophotometric method for determination of trace amounts of Fe3+ ion in tap and waste water solutions has been described. The spectrophotometric determination of Fe3+ ion using Ferron in the presence of N,N-Dodecytrimethylammonium bromide (DTAB) has been carried out. The Beer's law is obeyed over the concentration range of 0.05-2.6 g mL-1 of Fe3+ ion with the relative standard deviation (RSD %) <0.2 % and the molar absorptivity of complexes in pH 3.5 is 3.8×103 L mol-1 cm-1.
Potentiometric pH titration has been used for prediction of protonation constants of ferron, and evaluating its stoichiometry and respective stability constant with Fe3+ ion. As it is obvious the most likely species of ferron alone and its complexes are LH (log=7.64), LH2 (logK=10.52), LH3 (logK=11.74) and ML2 (log= 23.68), ML3 (log= 23.68), ML3H (log= 23.68), ML3H2 (log= 23.68) and ML(OH)2 (log=23.68) respectively.

Rapid Spectrophotometric Determination of Zirconium(IV)

Rapid Spectrophotometric Determination of Zirconium(IV) with 2,2,3,4-tetrahydroxy–3 -sulpho–5-chloroazobenzene in Alloys
A. Ali HÜSEYİNLİ,1†Fitnat KÖSEOĞLU,2 and Ülkü Dilek UYSAL1
1† Anadolu University, Faculty of Sciences, Department of Chemistry, 26470, Eskişehir, Turkey (E-mail: ahuseyin@anadolu.edu.tr)
2 Gazi University, Gazi Education Faculty, Teknikokullar, 06500, Ankara, Turkey
New o,o/–monoazo reagents have been synthesized using pyrogallol and 2-aminophenol-6-sulphonic acid or its derivatives. Spectrophotometric properties of the complexes formed by the reaction of synthesized monoazo reagents with Zr4+ have been investigated. According to the results it is found that the most sensitive and selective ligand for the Zr4+ is 2,2/,3,4-tetrahydroxy–3/-sulpho–5/-chloroazobenzene (tetrahydroxyazon SCl) and it was used for the direct spectrophotometric determination of Zr4+ion. Tetrahydroxyazon SCl reagent forms a red complex with Zr4+ ion in acidic media up to pH 6. The complex formation is fast and its absorbance reaches to a level immediately where remains constant for more than three days. The metal (M):ligand (L) ratio of the formed complex is 1:1 and the optimal wavelength of the
complex is 496 nm. Under optimum conditions Zr4+ ion acts in accordance with the Beer law at an ion concentration range of 0.08-3.20 μg/mL. The molar absorptivity was found as 34500 Lmol-1cm-1. The determination of Zr4+ was not interfered by Cu2+, Cd2+, Pb2+, Ni2+, Cr3+, Zn2+, Bi3+, U6+, Th4+, Al3+, Be2+, Co2+, Mn2+, Hg2+, halides, phosphates, sulfates, thiocyanides, urea, tartrate, ascorbic acid etc. This method is highly sensitive, selective, very rapid and a simple technique. It has been successfully applied to the determination of Zr4+ ion in an aluminum based certified alloys.

[PDF] Rapid Spectrophotometric Determination of Zirconium(IV) with 2,2 ...

Tungsten and Cobalt in Workplace Atmospheres (ICP Analysis)

Related Information: Chemical Sampling - Tungsten (as W) Insoluble Compounds, Tungsten (as W) Soluble Compounds, Cobalt, Metal, Dust & Fume (as Co)
Method Number: ID-213
Matrix: Air

Analytical Procedure:
The MCE filter is subjected to a sequence of digestion steps using ammonium hydroxide (aqueous ammonia), water, hydrochloric acid, nitric acid, and phosphoric acid. The resulting solution is analyzed by aspiration into the argon stream of an inductively coupled plasma atomic emission spectrometer (ICP-AES).

Articles

An Extractive Spectrophotometric Method of Determination of Molybdenum(VI) Using 3-Hydroxy-2-(4-methoxyphenyl)-6-methyl-4H-chromen-4-one

Abstract
3-Hydroxy-2-(4-methoxyphenyl)-6-methyl-4H-chromen-4-one (HL) behaved as a sensitive spectrophotometric reagent for molybdenum(VI). The metal ion formed a yellow complex with the reagent in acetic acid medium. The complex was extractable into 1,2-dichloroethane and the absorbance values remained unchanged for more than one week. Spectral data showed the formation of 1 : 2 species with λ_max value at 411 nm. Beer’s law was obeyed over the concentration range of 0—2.3 ppm. The molar absorptivity and Sandell’s sensitivity were calculated to be 5.61 × 10⁴ dm³ mol⁻¹ cm⁻¹ and 0.0017 μg Mo cm⁻² respectively, at 411 nm. The effect of as many as 41 cations and 28 anions and complexing agents was studied. Out of these only Sn(II), Ce(IV), citrate, oxalate, disodium dihydrogen ethylenediaminetetraacetate, and hydrogen peroxide interfered seriously. For ten replicate determinations of 1 μg Mo cm⁻³ the standard deviation was 0.008 with a relative mean error of ±0.09%. The method is simple, selective, precise and rapid. It has been applied satisfactorily to the determination of molybdenum in steels, waters and flue dust samples.



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Elemental analysis, Intertek USA

Method Summaries

Carbon, Hydrogen & Nitrogen (CHN)

• Standard Conditions
• Combustion Additive
• Optimum Combustion Conditions

Oxygen (O)

• Pyrolysis

Sulfur,Chlorine,Bromine & Iodine (S,Cl,Br & I)

Colormetric Titration

• Bromine
• Chlorine
• Sulfur

Ion Chromatography

• Bromine
• Chlorine
• Sulfur

Inductively Coupled Plasma

• Sulfur

Fluorine (F)

• Ion Specific Electrode
• Ion Chromatography

Inductively Coupled Plasma - Optical Emission Spectroscopy (ICP-OES)

• Individual Elements

  Inorganics

  Inductively Coupled Plasma Optical Emission Spectrometry(ICP-OES)/Inorganic Elements

  Supported Elements

  This analysis is suitable for the following elements; Ag, Al, As, Au, B, Ba, Be, Bi, Ca, Cd, Ce, Co, Cr, Cu, Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf, Hg, Ho, In, Ir, K, La, Li, Lu, Mg, Mn, Mo, Na, Nb, Nd, Ni, Os, P, Pb, Pd, Pr, Pt, Re, Rh, Ru, S, Sb, Sc, Se, Si, Sn, Sr, Ta, Tb, Th, Ti, Tl, Tm, U, V, W, Y, Yb, Zn, and Zr. The elements Hg, Os and S may be analyzed by special arrangement with the laboratory. Solid samples requiring lower limits of detection must use ICPMS in most cases. Cesium can only be measured by ICPMS.
• Semi Quantitative Scan

  Inorganics

  Inductively Coupled Plasma Optical Emission Spectrometry(ICP-OES)/Semi Quantitative Scan of Inorganic Elements

  Supported Elements

  This analysis is suitable for the following elements; Ag, Al, As, Au, B, Ba, Be, Bi, Ca, Cd, Ce, Co, Cr, Cu, Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf, Hg, Ho, In, Ir, K, La, Li, Lu, Mg, Mn, Mo, Na, Nb, Nd, Ni, Os, P, Pb, Pd, Pr, Pt, Re, Rh, Ru, S, Sb, Sc, Se, Si, Sn, Sr, Ta, Tb, Th, Ti, Tl, Tm, U, V, W, Y, Yb, Zn, and Zr. The elements Hg, Os and S may be analyzed by special arrangement with the laboratory. Solid samples requiring lower limits of detection must use ICPMS in most cases. Cesium can only be measured by ICPMS.

Inductively Coupled Plasma - Mass Spectroscopy (ICP-MS)

• Individual Elements

  Inorganics

  Inductively Coupled Plasma Mass Spectrometry(ICP-Ms).
  Inorganic Elements

  Supported Elements

  This analysis is suitable for the following elements; Ag, Al, As, Au, B, Ba, Be, Bi, Ca, Cd, Ce, Co, Cr, Cs, Cu, Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf, Hg, Ho, In, Ir, K, La, Li, Lu, Mg, Mn, Mo, Na, Nb, Nd, Ni, Os, P, Pb, Pd, Pr, Pt, Re, Rh, Ru, S, Sb, Sc, Se, Si, Sn, Sr, Ta, Tb, Th, Ti, Tl, Tm, U, V, W, Y, Yb, Zn, and Zr. The elements Hg, Os and S may be analyzed by special arrangement with the laboratory. Cesium can only be measured by ICPMS.
• Semi Quantitative Scan

  Inorganics

  Inductively Coupled Plasma Mass Spectrometry(ICP-Ms)/Semi Quantitiative Scan of Inorganic Elements

  Supported Elements

  This analysis is suitable for the following elements; Ag, Al, As, Au, B, Ba, Be, Bi, Ca, Cd, Ce, Co, Cr, Cs, Cu, Dy, Er, Eu, Fe, Ga, Gd, Ge, Hf, Hg, Ho, In, Ir, K, La, Li, Lu, Mg, Mn, Mo, Na, Nb, Nd, Ni, Os, P, Pb, Pd, Pr, Pt, Re, Rh, Ru, S, Sb, Sc, Se, Si, Sn, Sr, Ta, Tb, Th, Ti, Tl, Tm, U, V, W, Y, Yb, Zn, and Zr. The elements Hg, Os and S may be analyzed by special arrangement with the laboratory. Cesium can only be measured by ICPMS.

Flame Atomic Absorption Spectroscopy (FLAA)

• Individual Elements

  Flame Atomic Absorption Spectroscopy or emission.(FLAA) Inorganic Elements

  Supported Elements

  This analysis is suitable for the following elements; Al, Ag, Ba, Bi, B, Ca, Cd, Cr, Co, Cu, Ga, K, Fe, Pb, Li, Mg, Mn, Mo, Na, Ni, Pd, Pt, Rh, Ru, Sb, Se, Si, Sn, Ti, V and Zn. Other elements may be analyzed by special arrangement with the laboratory. The technique is best used for alkali metals. Solid samples requiring lower limits of detection must use either GFAA, ICP or ICPMS depending on the element.

Graphite Furnace Atomic Absorption (GFAA)

• Individual Elements

  Graphite furnace atomic absorption.(GFAA) Inorganic Elements

  Supported Elements

  This analysis is suitable for the following elements; Al, Ag, Ba, Bi, Cd, Cr, Co, Cu, Ga, Fe, Pb, Li, Mn, Mo, Ni, Pd, Pt, Rh, Ru, Se, Si, Sb, Sn, Ti, V and Zn. Other elements may be analyzed by special arrangement with the laboratory. Solid samples requiring lower limits of detection must use either ICP or ICPMS depending on the element.

Cold Vapor Atomic Absorption (CVAA)

• Individual Elements

  Cold Vapor Flame atomic absorption (CVAA)/Inorganic Elements

  Supported Elements

  This analysis is suitable for Hg. Other elements (As, Sb, Se) may be analyzed by special arrangement with the laboratory.

Ion Chromatography (IC)

• Individual Anions

  IC

  Anions/Inorganic Anions

  Supported Elements

  Fluoride (F^-), Chloride (Cl^-), Bromide (Br^-), Sulfate (SO₄2^-), Phosphate (PO₄3^-), Nitrate (NO₃^-), and Nitrite (NO₂^-)
• Anion Scan

  IC

  Anions/Inorganic Scan

  Supported Elements

  Fluoride (F^-), Chloride (Cl^-), Bromide (Br^-), Sulfate (SO₄2^-), Phosphate (PO₄3^-), Nitrate (NO₃^-), and Nitrite (NO₂^-)
• Trifluoroacetate (TFA)
• Methanesulfonate (MSA)
• Individual Cations

  IC

  Cations/Inorganic Cations

  Supported Elements

  Cations (m⁺): Sodium (Na⁺), Potassium (K⁺), Lithium (Li⁺), and Ammonium (NH₄⁺)
• Cation Scan

  IC

  Cations/Inorganic Scan

  Supported Elements

  Cations (m⁺): Sodium (Na⁺), Potassium (K⁺), Lithium (Li⁺), and Ammonium (NH₄⁺)
• Acetate
• High Performance Liquid Chromatography (HPLC)
• Liquid Chromatography - Mass Spectrometry (LC-MS)
• Residual Solvents

  GC

  Fid/Known Compounds

  Supported Elements

  This analysis is suitable for samples containing residual solvents at levels ranging from trace amounts (typical 0.01% quantitation limit using 100 mg sample size) to a relative high percentage.
• Gas Chromatography (GC)

  General Gas Chromatography

  Supported Elements

  This analysis is suitable for samples containing residual solvents at levels ranging from trace amounts (typical 0.01% quantitation limit using 100 mg sample size) to a relative high percentage.
• Gas Chromatography - Mass Spectrometry (GC-MS)

  Gas Chromatography - Mass Spectrometry

  Supported Elements

  This analysis is suitable for identification of unknown residual solvents at levels ranging from trace amounts (typical 0.05% quantitation limit using 100 mg sample size) to a relative high percentage.
• Mass Spectrometry (MS)

  MS

  General/Unknown Compounds

  Supported Elements

  This analysis is suitable for structure elucidation of unknown compounds.
• Thermal Gravimetric Analysis (TGA)

Spectroscopy

• Fourier Transform Infrared Spectroscopy (FT-IR)

  FTIR

  /FTIR

  Supported Elements

  This analysis consists of acquiring the infrared spectrum of a given compound. The spectrum is indicative of the vibrations between atoms in the molecule. Therefore, it can be used to identify the structure of a molecule.
• Optical Rotation (OR)
• Ultraviolet and Visible Spectroscopy (UV-Vis)

  UVvis

  UVvis

  Supported Elements

  This analysis consists of acquiring the ultraviolet and visible spectrum of a given compound. The spectrum is indicative of electron transitions between the orbitals in the molecule. Therefore, it can be used to identify the structural features of a molecule.

Water Determination

• Coulometric Karl Fischer

  Water Determination

  Karl Fischer/Coulometric Titration

  Supported Elements

  This analysis is suitable for samples containing water at levels ranging from trace amounts (typical 0.1% detection limit) to very large amounts.
• Volumetric Karl Fischer

  Water Determination

  Karl Fischer/Volumetric Titration

  Supported Elements

  This analysis is suitable for samples containing water at high levels, 0.5% to 10%. Additionally, a large amount of sample is usually required for accurate results. For smaller sample sizes and lower detection limits use Coulometric Karl Fischer titration.

Ashing

• Micro Ash

  Micro Ash

  Supported Elements

  This analysis is suitable for samples requiring a detection limit of <0.1%.> Residue on Ignition.
• Micro Residue on Ignition (ROI)

  Residue on Ignition

  Supported Elements

  This analysis is suitable for samples requiring a detection limit of <0.1%.> Residue on Ignition.
• Melting Point
• Total Organic Carbon (TOC)

  TOC

  Organic Carbon

  Supported Elements

  Carbon (<1000ppm)>

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Extractive Spectrophotometric Determination of Tungsten(VI) Using 3-Hydroxy-2-(2'-Thienyl)-4-OXO-4H-1- Benzopyran

Abstract
A simple, rapid, highly sensitive and selective spectrophotometric method for the determination of tungsten(VI) in trace amounts is developed using 3- hydroxy-2-(2'-thienyl)-4-oxo-4H-1-benzopyran (HTB) as a reagent for the complexation of metal ion and extracting the 1:2 (metal:ligand) complex into dichloromethane from 0.2 M HCl solution. It obeys Beer's law in the range 0-2.8 g Wml^-1 with molar absorptivity and Sandell's sensitivity at 415 nm as 6.45 x 10⁴ L mol^-1cm^-1 and 0.0029 g W(VI) cm^-2, respectively. The method is free from the interference of a large number (39) of elements and handles satisfactorily the analysis of various samples of varying complexity.

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Performance and frequency of use of NAA and other techniques during the certification of two new Polish CMRs prepared by INCT

Abstract
Two new candidate reference materials of biological origin, viz. Tea Leaves (INCT-TL-1) and Mixed Polish Herbs (INCT-MPH-2), were prepared, and world-wide interlaboratory comparison involving over 100 laboratories was organised with the aim to certify these materials for the content of possibly great number of trace elements. In this paper a preliminary analysis of the contribution of various analytical techniques to the certification of the new reference materials is presented and discussed with the emphasis on the role played by neutron activation analysis (NAA). The potential significance of “very accurate methods” by radiochemical NAA in the certification process is pointed out. An attempt is made to compare the outcome of the present intercomparison with those formerly organised by INCT as well as with some earlier IAEA intercomparisons in order to demonstrate similarities, differences and trends in the use of the various analytical techniques in trace analysis as a function of time.


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