Sulfur Analysis of Air Pollution Samples Containing Sulfuric Acid with a Vacuum X-Ray Fluorescence Spectrometer

1975 ◽  
Vol 19 ◽  
pp. 427-434
Author(s):  
K. T. Knapp ◽  
R. L. Bennett ◽  
R. B. Kellogg

Vacuum x-ray fluorescence spectrometers are used routinely in our laboratory to analyze automotive exhaust particulate emissions. However, a problem has developed in the analyses of samples collected from cars equipped with catalytic converters. The catalytic converters which were developed to decrease the carbon monoxide and unburned hydrocarbon emissions from auto exhausts, also produce sulfuric acid through the oxidation of part of the SO2 emissions. The sulfuric acid aerosol which is collected with the particulate emissions causes problems in the use of a vacuum spectrometer. If the samples are analyzed as , collected, the sulfuric acid would be pumped off the collection filters resulting in the loss of sulfur from the samples and contamination of the spectrometer. A technique was needed to fix the sulfuric acid so that it would remain on the filters. Exposure of the samples to ammonia gave the needed stability. Details of the technique in cluding standard preparation procedures are described. The results obtained with samples exposed to ammonia at various concentrations and periods of time are presented.

2018 ◽  
Vol 42 (1) ◽  
pp. 80-92 ◽  
Author(s):  
Sérgio Henrique Godinho Silva ◽  
Elen Alvarenga Silva ◽  
Giovana Clarice Poggere ◽  
Luiz Roberto Guimarães Guilherme ◽  
Nilton Curi

ABSTRACT Portable X-ray fluorescence spectrometer (pXRF) has been recently adopted by the Soil Science community for uses in both field and laboratory, obtaining the total content of several chemical elements in a few seconds. Sulfuric acid digestion is an expensive and time-consuming laboratory analysis that provides contents of Fe2O3, Al2O3, SiO2, TiO2 and P2O5, important for soil studies. Due to few pXRF studies in tropical soils, this work aimed to compare contents of Fe2O3, Al2O3, SiO2, TiO2 and P2O5 obtained by pXRF with sulfuric acid digestion results, and to evaluate the effects of varying forms of preparing soil samples and scanning with pXRF on the resulting values in Brazilian soils. Soils were scanned in five conditions in-field (in situ) and in laboratory, evaluating varying sample preparation methods, particle sizes and soil moisture. Four pXRF scanning operational modes were tested. Linear regressions were adjusted between results of pXRF and sulfuric acid digestion. Equations were validated with an independent set of samples. Statistical analyses compared the methods of preparing the samples. Adequate linear models reached R2 of 0.99 and 0.89 for Fe2O3 and TiO2, respectively. Validation promoted R2 greater than 0.97 and RMSE and ME close to zero for both oxides. Statistical differences of pXRF results were found among the methods of preparing samples. pXRF spectrometer has great potential to obtain Fe2O3 and TiO2 content rapidly and economically with high correspondence with laboratory results of sulfuric acid digestion analysis. Varying methods of preparing the samples promote differences in the results of pXRF.


2012 ◽  
Vol 9 (4) ◽  
pp. 379 ◽  
Author(s):  
Piotr Nowinski ◽  
Vernon F. Hodge ◽  
Shawn Gerstenberger

Environmental context Rock surfaces are often covered with a dark coating called desert varnish that can capture and retain air pollutants. A field portable X-ray fluorescence spectrometer was used for direct non-destructive analysis of varnished rocks in the fallout zones of two coal-fired power plants. At one power plant where tracer studies had been carried out, the highest concentration of elements including Cr, As, Pb and Zn in the rock varnish samples, coincides with the peak tracer concentration locations. AbstractDesert varnish samples were collected near two coal-fired power plants to determine if the varnish contained a record of recent air pollution. Samples were collected: (1) in the fallout patterns of the shuttered Mohave Power Plant (MPP), located in Laughlin, NV; and (2) near the operating Reid-Gardner Power Plant (RGPP), just east of Las Vegas, NV. Small pieces of varnished rocks were analysed by field portable X-ray fluorescence spectroscopy (FPXRF). Results were obtained for 15 elements: Cr, Mn, Fe, Co, Ni, Cu, Zn, As, Se, Rb, Sr, Zr, Mo, Hg and Pb. The FPXRF data indicate that the elements commonly found in fly ash from coal-fired power plants (e.g. Cr, Zn, As and Pb) had significantly higher concentrations in the rock coatings in relation to the unvarnished substrate rock. For one of the power plants, where tracer plume studies had been carried out, the highest concentrations in the desert varnish coincided with the peak tracer concentration locations. Thus, these elements in desert varnish hold promise for identifying those geographical regions affected by nearby power plants. However, additional samples are required to demonstrate unequivocally that the power plants are indeed the sources of these elements. Overall, it is apparent that desert varnish can be utilised as a passive environmental monitor to investigate recent air pollution (past 20–30 years) and that FPXRF can be used as a surveying tool to obtain multi-element data from a large number of samples.


1975 ◽  
Vol 19 ◽  
pp. 393-402 ◽  
Author(s):  
Roy L. Bennett ◽  
Jack Wagman ◽  
Kenneth T. Knapp

The design and application of a newly-developed Siemens multichannel wavelength x-ray fluorescence spectrometer that has been specially adapted to the needs of the Environmental Protection Agency for rapid analysis of particulate samples is described. The system consists of sixteen fixed-wavelength spectrometers which are optimized for sixteen pre-selected elements and a computer-operated scanning channel which is used to determine additional elements that might be desired on a given sample. A minicomputer operates the instrument and custom-designed sample changer and processes the data.Requirements for standards suitable for air pollution samples and the approaches used for the preparation of thin layer standards are discussed. Sensitivities, detection limits for elements of interest in air pollution, and the relative merits of aerosol filter types for x-ray fluorescence analysis have been determined. The system has been used to measure the elemental composition of a large number of samples from stationary source emissions, mobile sources, and ambient air.


2012 ◽  
Vol 560-561 ◽  
pp. 678-681
Author(s):  
Li Fen Yang ◽  
Bin Xiang ◽  
Liang Hui Ke

The component and contents of scale sample on the graphite heat exchanger were analyzed by ED-XRF( Energy dispersive X-ray fluorescence spectrometer) and the component and contents of spent acid unconcentrated and concentrated were measured by AAS(atomic absorption spectrometer).In addition, the phase structure of scale sample was tested by XRD(X-ray diffraction) and the simulation experiment of spent acid concentrating was carried out to study the scaling mechanism in the laboratory. The results show that the main components of scale were Ca, Ti and Fe. The scaling might be induced by settlement of Ti oxide, and then Ca and Fe precipitate rapidly.


1982 ◽  
Vol 26 (4) ◽  
pp. 257-261 ◽  
Author(s):  
M Öblad ◽  
P Standzenieks ◽  
E Selin ◽  
J Dubois

Author(s):  
N.M. Novikovskii ◽  
◽  
V.M. Raznomazov ◽  
V.O. Ponomarenko ◽  
D.A. Sarychev ◽  
...  

Author(s):  
Z.B. Baktybaeva ◽  
R.A. Suleymanov ◽  
T.K. Valeev ◽  
N.R. Rahmatullin ◽  
E.G. Stepanov ◽  
...  

Introduction. High density of oil-producing and refining facilities in certain areas of Bashkortostan significantly affects the environment including ambient air quality in residential areas. Materials and methods. We analyzed concentrations of airborne toxicants (sulfur and nitrogen oxides, nitrogen and carbon oxides, hydrogen sulfide, ammonia, xylenes, toluene, phenol and total suspended particles) and population health status in the cities of Ufa, Sterlitamak, Salavat, Blagoveshchensk, and the Tuymazinsky District in 2007–2016. Pearson's correlation coefficients (r) were used to establish possible relationships between medico-demographic indicators and air pollution. Results. Republican fuel and energy enterprises contributed the most to local air pollution levels. Gross emissions from such enterprises as Bashneft-Ufaneftekhim and Bashneft-Navoil reached 43.69–49.77 thousand tons of pollutants per year. The levels of some air pollutants exceeded their maximum permissible concentrations. Elevated concentrations of ammonia, total suspended particles, nitrogen dioxide, and carbon monoxide were registered most frequently. High rates of congenital abnormalities, respiratory diseases in infants (aged 0-1), general mortality and morbidity of the population were observed in some oil-producing and refining areas. The correlation analysis proved the relationship between the concentration of carbon monoxide and general disease rates in adults based on hospital admissions (r = 0.898), general incidence rates in children (r = 0.957), and blood disease rates in infants (r = 0.821). Respiratory diseases in children correlated with nitrogen dioxide emission levels (r = 0.899). Conclusions. Further development of oil-producing, petrochemical and oil-refining industries should be carried out taking into account socio-economic living conditions of the population.


2013 ◽  
Vol 248-249 ◽  
pp. 159-166 ◽  
Author(s):  
Gudny Okkenhaug ◽  
Gijs D. Breedveld ◽  
Terje Kirkeng ◽  
Marit Lægreid ◽  
Trond Mæhlum ◽  
...  

2021 ◽  
Vol 80 (Suppl 1) ◽  
pp. 1422.3-1423
Author(s):  
T. Hoffmann ◽  
P. Oelzner ◽  
F. Marcus ◽  
M. Förster ◽  
J. Böttcher ◽  
...  

Background:Interstitial lung disease (ILD) in inflammatory rheumatic diseases (IRD) is associated with increased mortality. Moreover, the lung is one of the most effected organs on IRD. Consequently, screening methods were required to the detect ILD in IRD.Objectives:The objective of the following study is to evaluate the diagnostic value of lung function test, chest x-ray and HR-CT of the lung in the detection of ILD at the onset of IRD.Methods:The study is designed as a case-control study and includes 126 patients with a newly diagnosed IRD. It was matched by gender, age and the performance of lung function test and chest x-ray. The sensitivity and specificity were verified by crosstabs and receiver operating characteristic (ROC) curve analysis. The study cohort was divided in two groups (ILD group: n = 63 and control group: n = 63). If possible, all patients received a lung function test and optional a chest x-ray. Patients with pathological findings in the screening tests (chest x-ray or reduced diffusing capacity for carbon monoxide (DLCO) < 80 %) maintained a high-resolution computer tomography (HR-CT) of the lung. Additionally, an immunological bronchioalveolar lavage was performed in the ILD group as gold standard for the detection of ILD.Results:The DLCO (< 80 %) revealed a sensitivity of 83.6 % and specificity of 45.8 % for the detection of ILD. Other examined parameter of lung function test showed no sufficient sensitivity as screening test (FVC = Forced Vital Capacity, FEV1 = Forced Expiratory Volume in 1 second, TLC = Total Lung Capacity, TLCO = Transfer factor of the Lung for carbon monoxide). Also, a combination of different parameter did not increase the sensitivity. The sensitivity and specificity of chest x-ray for the verification of ILD was 64.2 % versus 73.6 %. The combination of DLCO (< 80 %) and chest x-ray showed a sensitivity with 95.2 % and specificity with 38.7 %. The highest sensitivity (95.2 %) and specificity (77.4 %) was observed for the combination of DLCO (< 80 %) and HR-CT of the lung.Conclusion:The study highlighted that a reduced DLCO in lung function test is associated with a lung involvement in IRD. DLCO represented a potential screening parameter for lung manifestation in IRD. Especially patients with suspected vasculitis should receive an additional chest x-ray. Based on the high sensitivity of DLCO in combination with chest x-ray or HR-CT for the detection of ILD in IRD, all patients with a reduced DLCO (< 80%) should obtained an imaging of the lung.Disclosure of Interests:None declared


2001 ◽  
Vol 79 (3) ◽  
pp. 263-271
Author(s):  
Paul K Baker ◽  
Michael GB Drew ◽  
Deborah S Evans

Reaction of [WI2(CO)3(NCMe)2] with two equivalents of 1-phenyl-1-propyne (MeC2Ph) in CH2Cl2, and in the absence of light, gave the bis(1-phenyl-1-propyne) complex [WI2(CO)(NCMe)(η2-MeC2Ph)2] (1) in 77% yield. Treatment of equimolar quantities of 1 and NCR (R = Et, i-Pr, t-Bu, Ph) in CH2Cl2 afforded the nitrile-exchanged products, [WI2(CO)(NCR)(η2-MeC2Ph)2] (2-5) (R = Et (2), i-Pr (3), t-Bu (4), Ph (5)). Complexes 1, 2, and 5 were structurally characterized by X-ray crystallography. All three structures have the same pseudo-octahedral geometry, with the equatorial sites being occupied by cis and parallel alkyne groups, which are trans to the cis-iodo groups. The trans carbon monoxide and acetonitrile ligands occupy the axial sites. In structures 1 and 2, the methyl and phenyl substituents of the 1-phenyl-1-propyne ligands are cis to each other, whereas for the bulkier NCPh complex (5), the methyl and phenyl groups are trans to one another. This is the first time that this arrangement has been observed in the solid state in bis(alkyne) complexes of this type.Key words: bis(1-phenyl-1-propyne), carbonyl, nitrile, diiodo, tungsten(II), crystal structures.


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