Application of liquid chromatography/quadrupole time-of-flight mass spectrometry (LC-QqTOF-MS) in the environmental analysis

This paper gives an overview of the potentials of liquid chromatography-hybrid quadrupole time-of-flight mass spectrometry (LC-QqTOF) in the environmental analysis. Examples of applications of QqTOF instruments for target analysis of pharmaceuticals and pesticides are presented and discussed, as well as applications aimed on the identification of unknown compounds present in environmental waters or on the elucidation of structures of biodegradation and photodegradation products. Specific issues such as uncertainty of mass measurement and quantitative performances are discussed in details.     

Recent applications of atomic spectroscopy coupled with magnetic solid-phase extraction techniques for heavy metal determination in environmental samples: A review

Atomic spectroscopy is the most popular approach to determine the presence of heavy metals in the environment. Heavy metals are potentially toxic and have various negative effects on many living organisms, including humans. With the rapid increase in the variety of industries and human activities, large amounts of heavy metals are released into the atmosphere, water, and soil. Heavy metal analysis of environmental samples is very important for determining the exposure limits. Environmental samples are highly complex matrices, and various sample preparation techniques have been developed for the extraction of heavy metals from them, including magnetic solid-phase extraction (MSPE). The use of MSPE in heavy metal analysis has recently gained significant attention owing to a number of advantages. MSPE technique overcomes main issues such as phase separation, handling, and column packing. The use of magnetic adsorbents in sample preparation has grown over the past few years, making MSPE a promising technique for sample preparation. The objective of this review article is to provide the latest applications of MSPE coupled with atomic spectroscopy for heavy metal determination in environmental samples. In addition, new magnetic adsorbents and their analytical merits are emphasized.     

Analysis of the thermal decomposition of commercial vegetable oils in air by simultaneous TG/DTA

This work presents a study of the thermal decomposition of commercial vegetable oils and of some of their thermal properties by termogravimetry (TG), derivative termogravimetry (DTG) and by differential thermal analysis (DTA). Canola, sunflower, corn, olive and soybean oils were studied. A simultaneous SDT 2960 TG/DTA from TA Instruments was used, with a heating rate of 10 K min^-1 from 30 to 700°C. A flow of 100 mL min^-1 of air as the purge gas was used in order to burnout the oils during analysis to estimate their heat of combustion. From the extrapolated decomposition onset temperatures obtained from TG curves, it can be seen that corn oil presents the highest thermal stability (306°C), followed by the sunflower one (304°C). Olive oil presents the lowest one (288°C). The heat of combustion of each oil was estimated from DTA curves, showing the highest value for the olive oil. Except for corn oil, which presents a significantly different thermal decomposition behavior than the other oils, a perfect linear correlation is observed, with negative slope, between the heat of combustion of an oil and its respective extrapolated onset temperature of decomposition in air. This revised version was published online in August 2006 with corrections to the Cover Date.     

The role of anhydrous zinc nitrate in the thermal decomposition of the zinc hydroxy nitrates Zn5(OH)8(NO3)2·2H2O and ZnOHNO3·H2O

The steps associated with the thermal decomposition of Zn₅(OH)₈(NO₃)₂·2H₂O and ZnOHNO₃·H₂O are re-examined. Previous reports have suggested that Zn₅(OH)₈(NO₃)₂·2H₂O decomposes to ZnO via two intermediates, Zn₅(OH)₈(NO₃)₂ and Zn₃(OH)₄(NO₃)₂ whereas ZnOHNO₃·H₂O has been reported to decompose to ZnO via a Zn₃(OH)₄(NO₃)₂ intermediate. In this study, we demonstrate using TG, mass spectral analysis of evolved gases and in situ variable temperature powder X-ray diffraction analysis that, in fact, in the decomposition of Zn₅(OH)₈(NO₃)₂·2H₂O an anhydrous zinc nitrate intermediate is also involved. We, additionally, show that the decomposition of ZnOHNO₃·H₂O to ZnO also involves the formation of an anhydrous zinc nitrate intermediate. The anhydrous zinc nitrate formed in both cases is poorly crystallised and this observation may explain why this phase could not be observed by PXRD analysis in the previous studies.     

Critical comparison of radiometric and mass spectrometric methods for the determination of radionuclides in environmental, biological and nuclear waste samples

The radiometric methods, alpha (α)-, beta (β)-, gamma (γ)-spectrometry, and mass spectrometric methods, inductively coupled plasma mass spectrometry, accelerator mass spectrometry, thermal ionization mass spectrometry, resonance ionization mass spectrometry, secondary ion mass spectrometry, and glow discharge mass spectrometry are reviewed for the determination of radionuclides. These methods are critically compared for the determination of long-lived radionuclides important for radiation protection, decommissioning of nuclear facilities, repository of nuclear waste, tracer application in the environmental and biological researches, these radionuclides include ³H, ¹⁴C, ³⁶Cl, ⁴¹Ca, ^59,63Ni, ^89,90Sr, ⁹⁹Tc, ¹²⁹I, ^135,137Cs, ²¹⁰Pb, ^226,228Ra, ²³⁷Np, ²⁴¹Am, and isotopes of thorium, uranium and plutonium. The application of on-line methods (flow injection/sequential injection) for separation of radionuclides and automated determination of radionuclides is also discussed.     

Characterization of carbon nanotubes and analytical methods for their determination in environmental and biological samples: A review

In the present paper, a critical overview of the most commonly used techniques for the characterization and the determination of carbon nanotubes (CNTs) is given on the basis of 170 references (2000–2014). The analytical techniques used for CNT characterization (including microscopic and diffraction, spectroscopic, thermal and separation techniques) are classified, described, and illustrated with applied examples. Furthermore, the performance of sampling procedures as well as the available methods for the determination of CNTs in real biological and environmental samples are reviewed and discussed according to their analytical characteristics. In addition, future trends and perspectives in this field of work are critically presented.     

A new cleanup method of dioxins in sediment using large volume injection gas chromatography online coupled with liquid chromatography

A new cleanup method was developed and validated for the determination of polychlorinated dibenzo-p-dioxins and polychlorinated dibenzofurans (PCDD/Fs) in sediment. The sample extract was first treated with sulfuric acid and then cleaned up by a large volume injection gas chromatography online coupled with liquid chromatography (LVI-GC-LC) system. PCDD/Fs in the extract were separated by a GC column (DB-5), selected cut, cool trapped and transferred to a LC column (alumina). The fraction of PCDD/Fs eluted from the alumina column was collected and concentrated for the instrumental analysis. Under the optimized conditions, LVI-GC-LC method achieved the recoveries of 57–102% for 2,3,7,8-substituted PCDD/Fs, which met the requirements of US Environmental Protection Agency (EPA) Method 1613 and were better than those obtained using the conventional multistep column cleanup method. Meanwhile, compared with the conventional method, the limit of detection (LOD) values of 2,3,7,8-substituted PCDD/Fs cleaned up by LVI-GC-LC method were decreased due to the high-efficiency removal of interferents. These results suggested that the LVI-GC-LC cleanup method was a promising alternative to the multistep cleanup procedure for the determination of dioxins in environmental samples.