0000000000012466
AUTHOR
Rose Matilainen
Determination of SiO 2 in lime mud by gravimetry
A simple and rapid method for the determination of SiO2 in lime mud used in current sulfate pulping practice is reported. The lime mud samples are treated three times with 2.5 mL of 6 mol/L hydrochloric acid. The samples are nearly evaporated to dryness two times and the third time to complete dryness. To determine the exact SiO2 content of the residue, it is treated with an excess of concentrated hydrofluoric acid and a little hydrochloric acid, and the silica is expelled as volatile silicon tetrafluoride. The sample treatments take about 1.5 h and the heating periods take a total of about 3.5 h. The SiO2 results were evaluated by analyzing National Institute of Standards and Technology St…
Determination of Calcium in Certain Fertilizers by Inductively Coupled Plasma Atomic Emission Spectrometry: Studies of Some Spectral and Interelement Effects at Different Wavelengths
Abstract Four analytical wavelengths (393.366, 396.847, 317.933, and 422.673 nm) were used to determine Ca in 2 fertilizers by inductively coupled plasma atomic emission spectroscopy (ICP-AES). Matrix effects were studied by adding to real fertilizer solutions fertilizer elements that are known or believed to interfere with Ca determination. Matrix effects were calculated by multiple linear regression. Interference was caused by S, K, or B. At 422.673 nm, the interference of B and K is a spectral effect, and at 396.847 and 317.933 nm, the interference of S and K is an interelement effect. At 393.366 nm, no linear interference was found. The best wavelength for determining Ca in fertilizers …
A new ionic liquid dimethyldinonylammonium bromide as a flow modifier for the simultaneous determination of eight carboxylates by capillary electrophoresis.
Two new methods of capillary zone electrophoresis based on aqueous phosphate running buffers with UV spectrophotometric detection were developed and optimized for the determination of eight carboxylates as copper complexes. Metalcomplexes are negatively charged, so measurements were made as anion analyses with flow reversal in the capillary. Two flow modifiers were used: a common tetradecyltrimethylammonium bromide (TTAB) and a new ionic liquid dimethyldinonylammonium bromide (DMDNAB). The methods were compared to each other. Better separation was achieved with DMDNAB as the flow modifier. Method development was done using a fused silica capillary (61 cm x 50 microm i.d.). Optimization was …
Optimization of instrumental parameters for improving sensitivity of single particle inductively-coupled plasma mass spectrometry analysis of gold
Single particle inductively-coupled plasma mass spectrometry (spICP-MS) is a promising technique for analysis of engineered nanoparticles, whose utilization has increased substantially over the past years. Optimization of instrumental conditions is, however, crucial to improve the sensitivity and precision of nanoparticle (NP) detection. In this study, the influence of ICP-MS instrumental parameters (nebulizer gas flow, plasma radiofrequency-power and sampling depth) on the signal intensity of gold in spICP-MS was evaluated using dispersions of Au NPs and a solution of dissolved gold. The interaction effects of the main factors were found to have a significant effect on the signal intensity…
Solid phase extraction materials as a key for improving the accuracy of silver nanoparticle characterization with single-particle inductively coupled plasma mass spectrometry in natural waters through dissolved silver removal
The accurate characterization of silver nanoparticles (Ag NPs) in environmental samples is crucial for understanding the potential impact of these materials on the environment and human health. Single-particle inductively coupled plasma mass spectrometry (spICP-MS) is one of the few techniques available for quantifying NPs at environmentally relevant concentrations. However, the spICP-MS detection of Ag NPs can be interfered with coexisting dissolved analyte causing high background signals, which mask NP signals leading to a significant bias in NP characterization. In this paper, a simple sample pre-treatment procedure for efficient removal of dissolved silver in natural waters is proposed …
Iron Determination in Fertilizers by Inductively Coupled Plasma Atomic Emission Spectrometry: Study of Spectral and Interelement Effects at Different Wavelengths
Abstract Four analytical wavelengths of iron (238.204, 239.562, 259.940, and 240.488 nm) were tested for determination of Fe in fertilizers by inductively cou pled plasma atomic emission spectroscopy (ICP AES). Variations in measurements were caused by the changing interference pattern at different wave lengths evaluated by multiple linear regression. Thus, results obtained with different wavelengths are not comparable. Ca, P, and K were typical ele ments causing interference in almost all examined Fe wavelengths. Wavelength Fe II 238.204 nm is the best wavelength for determination of Fe in fertiliz ers by ICP-AES. Method accuracy is ± 8% at the ex amined Fe levels in fertilizers.
Determination of Magnesium in Fertilizers by Inductively Coupled Plasma Atomic Emission Spectrometry: Studies of Some Spectral and Interelement Effects at Different Wavelengths
Abstract Four analytical wavelengths of magnesium were tested for determination of Mg from fertilizers by inductively coupled plasma atomic emission spectroscopy (ICP-AES): 202.528, 285.213, and 383.826 nm (Mg I) and 279.553 (Mg II). The effects of fertilizer matrix elements on Mg determination were examined by adding matrix elements to fertilizer solutions. Multiple linear regression calculations proved a valuable technique for evaluating the effects of matrix elements on Mg determination. The observed interferences at Mg wavelengths may be both spectral and interelement. Interelement effects were typically caused by Na, K, and Ca, and spectral effects, by P, Fe, and S. The best wavelength…
Fighting carbon loss of degraded peatlands by jump-starting ecosystem functioning with ecological restoration
Degradation of ecosystems is a great concern on the maintenance of biodiversity and ecosystem services. Ecological restoration fights degradation aiming at the recovery of ecosystem functions such as carbon (C) sequestration and ecosystem structures like plant communities responsible for the C sequestration function. We selected 38 pristine, drained and restored boreal peatland sites in Finland and asked i) what is the long-term effect of drainage on the peatland surface layer C storage, ii) can restoration recover ecosystem functioning (surface layer growth) and structure (plant community composition) and iii) is the recovery of the original structure needed for the recovery of ecosystem f…
Reconstruction of undergraduate analytical chemistry laboratory course
The Analytical chemistry laboratory course at the Department of Chemistry at the University of Jyväskylä was reconstructed due to problems in the traditional arrangement, structure and contents of the course. The purposes of the reform were: to increase student-centered activity, co-operation and inquiry-based learning; to strengthen the connections to real-life; to develop students’ critical-thinking skills; and to decrease the number of drop-outs during the course. The reconstructed course includes independent laboratory work tasks and a research project. The results of the projects are presented in a course seminar. All of the laboratory experiments are done in groups of 8-10 students un…
Student experiences of project-based learning in an analytical chemistry laboratory course in higher education
Abstract This study describes students’ experiences in project-based learning (PjBL) incorporated as part of a revised undergraduate analytical chemistry laboratory course. We examined which phases were the easiest as well as the most challenging and what student skills developed during the research project. The research data were collected between 2016 and 2018 via two questionnaires. They were analyzed both quantitatively and qualitatively. One questionnaire focused on the whole course (in 2016–2018, n = 127) of which only the answers on the research project questions were analyzed. The other questionnaire focused on only the research project (in 2018, n = 42). Based on the results of our…
Application of 3D printed scavengers for improving the accuracy of single-particle inductively coupled plasma mass spectrometry analyses of silver nanoparticles by dissolved silver removal
The determination of silver nanoparticles (Ag NPs) with single-particle inductively coupled plasma mass spectrometry can be severely interfered with coexisting dissolved silver causing high background signals, which can lead to inaccurate quantification of NP size and particle concentration. In this paper, chemically active and reusable 3D printed scavengers are applied for highly efficient dissolved silver removal in Ag NP dispersions, allowing more accurate determination of particle concentration and size. Selective laser sintering was used for constructing the porous 3D scavengers constituting of polystyrene used as a supporting material and ion-exchange material SiliaBond Tosic acid (TA…
The effects of long-term drainage and subsequent restoration on water table level and pore water chemistry in boreal peatlands
Summary Degradation by drainage threatens biodiversity and globally important peatland ecosystem functions such as long-term carbon sequestration in peat. Restoration aims at safeguarding peatland values by recovering natural hydrology. Long-term effects of drainage and subsequent restoration, especially related to within-site variation of water table level and pore water chemistry, are poorly known. We studied hydrological variation at 38 boreal Sphagnum peatland sites (pristine, drained and restored) in Finland. The average water table level was significantly lower at Drained than Pristine sites especially near the ditches. We also observed large pore water chemical differences between Dr…
Separation of chelating agents as copper complexes by capillary zone electrophoresis using quaternary ammonium bromides as additives in N-methylformamide
This study presents the use of quaternary ammonium bromides as additives in N-methylformamide (NMF) for the separation and quantification of chelating agents as copper complexes by capillary zone electrophoresis (CZE). The new quaternary ammonium bromides were synthesized in our laboratory and used for the first time for CZE applications performed in NMF media. The methods were developed and optimized for determination of six chelating agents (trans-1,2-diaminocyclohexane-N,N,N',N'-tetraacetic acid (CDTA), diethylenetriaminepentaacetic acid (DTPA), ethylenediaminetetraacetic acid (EDTA), N-(2-hydroxyethyl)ethylenediamine-N,N',N'-triacetic acid (HEDTA), nitrilotriacetic acid (NTA) and trieth…
The determination of certain major and minor elements in geological samples by inductively coupled plasma atomic emission spectrometry. Some interference problems with the analysis of geological standard reference materials and nutrition supplements
Direct ICP-AES measurements of the digested geological standard reference material samples yielded the wrong information about their composition. The differences between certified and measured concentrations of the samples were due to the complicated sample matrix. The measured concentrations can be successfully corrected by using a multiple linear regression technique. The correction is based on the multiple regression line calculated from the analytical results at synthetic mixtures of matrix elements, where concentrations varied on five levels. There were no significant (P = 0.05) differences between certified and measured concentrations in standard reference materials after the correcti…
Simultaneous determination of As, Cd, Cr and Pb in aqua regia digests of soils and sediments using electrothermal atomic absorption spectrometry and fast furnace programs
A method was developed for the simultaneous multi-element determination of As, Cd, Cr and Pb in aqua regia digests of soils and sediments using an electrothermal atomic absorption spectrometer with a transversely heated graphite atomizer and longitudinal Zeeman-effect background correction. A fast furnace program with no pyrolysis stage or chemical modifier was used, and the total duration of the time-temperature program of the graphite furnace was 45 s. The method detection limits calculated from blank samples were 9.5 μg l−1, 0.18 μg l−1, 6.2 μg l−1 and 2.5 μg l−1 for As, Cd, Cr and Pb, respectively. Sample preparation procedures are briefly described. The accuracy of the method was confi…
Determination of alternative and conventional chelating agents as copper(II) complexes by capillary zone electrophoresis—The first use of didecyldimethylammonium bromide as a flow reversal reagent
Abstract A capillary zone electrophoresis (CZE) method for analyzing 11 chelating agents [β-alaninediacetic acid (β-ADA), trans-1,2-diaminocyclohexane- N , N , N ′, N ′-tetraacetic acid (CDTA), diethylenetriaminepentaacetic acid (DTPA), ethylenediaminetetraacetic acid (EDTA), N -(2-hydroxyethyl)ethylenediamine- N , N ′, N ′-triacetic acid (HEDTA), N -(2-hydroxyethyl)iminodiacetic acid (HEIDA), iminodiacetic acid (IDA), methylglycinediacetic acid (MGDA), nitrilotriacetic acid (NTA), 1,3-diaminopropane- N , N , N ′, N ′-tetraacetic acid (PDTA) and triethylenetetraaminehexaacetic acid (TTHA)] as negatively charged copper(II) complexes has been established. Both conventional and alternative che…
Quantitative determination of the main aliphatic carboxylic acids in wood kraft black liquors by high-performance liquid chromatography-mass spectrometry.
The versatile characterization of organic material and especially of the significant aliphatic hydroxy acids in black liquor is of great importance, for example, in monitoring the progress of the kraft pulping process. This paper describes a simple high-performance liquid chromatographic separation method with atmospheric-pressure chemical ionization mass spectrometry (HPLC-APCI-MS) which was developed for the rapid quantitative analysis of these acids, mainly formed as the alkaline degradation products of feedstock carbohydrates. The fraction of carbohydrate degradation products is mainly composed of hydroxy monocarboxylic and volatile acids (formic and acetic acids) along with lesser amou…
Example of a technique for evaluation of interferences caused by complicated sample matrix elements in ICP-AES determination
An example of a useful and rapid procedure for the evaluation of interferences caused by complicated sample matrices in inductively coupled plasma atomic emission spectrometry (ICP-AES) is described. Using simple acid-base standards, all the elements investigated were determined separately in complicated matrices with satisfactory results. Multiple linear regression was used to calculate the linear correction coefficients for each matrix element analyzed. Good analytical results improved still further when this correction method was used.
Determination of Boron in Fertilizers by Inductively Coupled Plasma-Atomic Emission Spectrometry: Studies of Some Spectral Interferences at Different Wavelengths
Abstract The most sensitive analytical wavelengths of boron cannot be used in the determination of boron in fertilizers by inductively coupled plasma-atomic emission spectrometry because of spectral interference by potassium, phosphorus, and iron. For the 4 wavelengths of boron investigated, it was noticed that, at the same wavelength, the pattern of spectral interference changes according to fertilizer composition. The spectral interference patterns at the 4 analytical boron wavelengths were studied by adding matrix elements typically found in fertilizers to real fertilizer samples. When levels of added matrix elements correlate less than 0.2 to each other, the effect of added matrix eleme…
Determination of Sulfur in Fertilizers by Inductively Coupled Plasma-Atomic Emission Spectrometry: Spectral and Interelement Effects at Various Wavelengths
Abstract Three analytical wavelengths (180.731,182.037, and 182.625 nm) were tested for determination of sulfur in 2 fertilizers by inductively coupled plasmaatomic emission spectrometry (ICP-AES). Variable S results at 182.037 nm were caused by a downward sloping background shift (Fe line at 181.851 nm) during measurement of the sample solutions. At 182.625 nm an emission peak doublet, 182.619/182.635 nm, was observed from which the instrument selected the measurement peak. A shift from calibrated peak 182.619 nm to noncalibrated peak 182.635 nm occurred when the S/B ratios were ≤22-31 in the fertilizer samples examined. For the 3 wavelengths of S investigated, the pattern of spectral and …
Optimization of the gravimetric determination method of nickel as dimethylglyoximate for nickel raw materials
The method parameters of an almost one century old method for analyzing nickel as dimethylglyoximate were critically examined for the analysis of nickel raw materials and many of the method parameters were observed to have a significant effect on the Ni recovery. Thus, because the Ni precipitation method parameters vary a lot in analytical literature and also in practice, the obtained Ni results by different methods are not comparable. During this study it was found that the double precipitation worked out perfectly in eliminating the effects of impurity elements. The residual Ni content in the filtrates should also be measured to obtain accurate and precise Ni results. In complexing the im…
Improving sensitivity in simultaneous determination of copper carboxylates by nonaqueous capillary electrophoresis
Abstract A new method of nonaqueous capillary electrophoresis (NACE) with UV spectrophotometric detection was developed and optimized for the simultaneous determination of seven carboxylates (trans-1,2-diaminocyclohexane-N,N,N′,N′-tetraacetic acid (CDTA), diethylenetriaminepentaacetic acid (DTPA), ethylenediaminetetraacetic acid (EDTA), N-(2-hydroxyethyl)ethylenediamine-N,N′,N′-triacetic acid (HEDTA), nitrilotriacetic acid (NTA), 1,3-diaminopropane-N,N,N′,N′-tetraacetic acid (PDTA) and triethylenetetraaminehexaacetic acid (TTHA)) as copper complexes. The method development was carried out by using a fused silica capillary. Background electrolyte (BGE) was optimized and the best separation a…
Determination of low-molecular-mass aliphatic carboxylic acids and inorganic anions from kraft black liquors by ion chromatography.
An ion chromatographic (IC) method with suppressed conductivity detection (CD) was developed and validated for the quantitative determination of several low-molecular-mass aliphatic mono- and dicarboxylic acids as their carboxylate anions together with some inorganic anions (chloride, sulfate, and thiosulfate) from kraft black liquors. To confirm the identification of some carboxylate anions which lack commercial model substances, a qualitative IC method with suppressed electrospray ionization mass spectrometry (ESI-MS) was also developed. The separations were performed on an IonPac AS 11-HC anion-exchange column operated at 25 degrees C within 25 min by a gradient elution with aqueous pota…