0000000000060992
AUTHOR
I. Pitkänen
Infrared evolved gas analysis during thermal investigation of lanthanum, europium and samarium carbonates
Abstract The characterisation of rare earth elements carbonates (REECs) was performed by thermal analysis (TG–DTG) combined with simultaneous infrared evolved gas analysis–Fourier transform infrared (EGA–FTIR) spectroscopy. The TG–DTG curves were obtained using the Perkin-Elmer PC series TGA-7 thermogravimetric analyser in the temperature range 25–800 °C both in dynamic air and nitrogen atmosphere. La 2 (CO 3 ) 3 · n H 2 O, Eu 2 (CO 3 ) 3 · n H 2 O and Sm 2 (CO 3 ) 3 · n H 2 O were analysed, the dehydration and decarbonation steps were investigated and the water content was calculated. The trace rare earth elements in lanthanum, europium and samarium carbonates were determined by Philips PU…
Comparison of two melting range analysis methods with lactitol monohydrate
Abstract In pharmacopoeia, the melting point is determined by a standard method with a melting point instrument. The melting point can also be determined with differential scanning calorimetry (DSC). In this study, the standard method and DSC method are compared for determining the melting range of lactitol monohydrate. The effect of initial temperature, grinding, and drying on the melting range of different lactitol monohydrate samples was studied by a melting point instrument. The melting point and melting enthalpy of the stable form of lactitol monohydrate was identified by DSC. The statistical analysis of the results is based on a t-test. All studied variables had a small effect on the …
Quantification of low levels of amorphous content in maltitol
A method for the quantification of low levels of amorphous content of maltitol with hyper-DSC (high speed DSC) was developed. The method is based on the fact that the change of specific heat ( � Cp) at the glass transition is linearly proportional to the amorphous content. Twelve synthetic mixtures with various degrees of crystalline and amorphous maltitol were prepared. � Cp was determined at both fictive and
X-ray powder diffraction pattern for lactitol and lactitol monohydrate
Diffraction patterns were recorded, and unit cell dimensions refined by the least-squares method, for lactitol and lactitol monohydrate. Refined unit cell parameters for lactitol are: a =7.622(1) Å, b = 10.764(2) Å, c = 9.375(1) Å, β= 108.25(1)° in space group P21, and those for lactitol monohydrate a =7.844(1) Å, b = 12.673(2) Å, c = 15.942(2) Å in space group P212121.
Melting behaviour of d-sucrose, d-glucose and d-fructose
The melting behaviour of d-sucrose, d-glucose and d-fructose was studied. The melting peaks were determined with DSC and the start of decomposition was studied with TG at different rates of heating. In addition, melting points were determined with a melting point apparatus. The samples were identified as d-sucrose, alpha-d-glucopyranose and beta-d-fructopyranose by powder diffraction measurements. There were differences in melting between the different samples of the same sugar and the rate of heating had a remarkable effect on the melting behaviour. For example, T(o), DeltaH(f) and T(i) (initial temperature of decomposition) at a 1 degrees Cmin(-1) rate of heating were 184.5 degrees C, 126…
Thermal and spectroscopic investigation of europium and samarium sulphates hydrates by TG-FTIR and ICP-MS techniques.
The investigation of europium(III) sulphate hydrate and samarium(III) sulphate hydrate was performed by thermal analysis (TG-DTG) and simultaneous infrared evolved gas analysis-Fourier transformed infrared (EGA-FTIR) spectroscopy. The TG, DTG and DTA curves were recorded at the 25-1400 degrees C in the dynamic air atmosphere by TG/DTA analyser. The infrared evolved gas analysis was obtained on the FTIR spectrometer. Eu(2)(SO(4))(3).nH(2)O (n=3.97) and Sm(2)(SO(4))(3).nH(2)O (n=8.11) were analysed, the dehydration and decomposition steps were investigated and the water content was calculated. The formation of different oxysulphates was studied. The trace rare earth elements in Eu and Sm sulp…
Crystal and molecular structure of anhydrous betaine, (CH3)3NCH2CO2
Abstract 1–Carboxy–N,N,N–trimethylmethanamanium inner salt or anhydrous betaine, (CH3)3NCH2CO2, FW=117.15 gmol −1 , crystallizes in the orthorhombic space group Pnma with a=14.544(2) A , b=6.859(3) A , c=6.131(1) A , V=611.7(3) A 3 , Z=4, D x =1.27 Mgm −3 , λ (MoK α )=0.71073 A , μ =0.091 mm −1 . The structure was resolved by direct methods and refined by least-square calculations to R=0.038 for 531 reflections. Observed changes in bond angles imply that there is a repulsion between nitrogen and oxygen. The melting point (measured at onset) is 570 K. FTIR spectra of anhydrous betaine and monohydrate were recorded. Clear differences were found between the two compounds based on infrared (i.r…
Thermoanalytical studies on sodium 1,2-naphthoqoinone oximesolfonates
Abstract Five sodium 1,2-nitrosonaphtholsulfonatea were prepared or purified and their thermal behaviour studied by TG, DTG and DSC. Pyrolysis MS technique was used to identify evolved gases and FTIR to characterize residuals. The water contents depended on preparation and conservation. The decomposition was analysed in three stages which can be formed by one or more steps. The final product was sodium sulfate in air at 530 °C and the mixture of carbon and sodium sulfide at 950 °C in nitrogen. The structure effects on decomposition is discussed.
Thermal and infrared spectroscopic characterization of historical mortars
Abstract The characterization of historical mortars was performed by thermal analysis (TG-DTG), simultaneous infrared spectroscopy (TG-FTIR) and inductively coupled plasma atomic emission spectrometry (ICP-AES). The samples were taken from St. John Church (Tartu, Estonia), built in the 13th–14th centuries. The analyses are important for the restoration of the church. In reality, mortar is a very difficult system, the lime is accompanied with different hydraulic components. TG-DTG analysis and FTIR methods can be used to identify various components of mortar and to observe the reactions associated with the controlled heating at 25–900°C in dynamic air and nitrogen atmosphere. The elemental c…
Analysis of archaeological samples and local clays using ICP-AES, TGâDTG and FTIR techniques
Abstract The spectrochemical and thermal analysis of different archaeological samples as bricks, terra-cotta and local clays were carried out. The concentration of major and minor elements of samples was determined by sequential inductively coupled plasma atomic emission spectrometry. The method was tested by determining Si, Al, Fe, Ca, Mg, Mn, Pb, Cu, Zn, Ti, Na and K in the standard solutions and reference material GXR-4. The precision of the determination (relative standard deviation) ranged from 0.4 to 1.54%. The clay minerals are the main materials for the production of bricks and terra-cotta figures. Thermogravimetric (TG) and differential (TG–DTG) analysis and Fourier transform infra…
X-ray powder diffraction pattern for glucopyranosylsorbitol and glucopyranosylmannitol dihydrate
X-ray powder data are given for glucopyranosylsorbitol, C12H24O11, and glucopyranosylmannitol dihydrate, C12H24O11 * 2H2O. Refined unit cell parameters for glucopyranosylsorbitol are: a=0.9124(4) nm, b=1.1336(5) nm, c=0.7232(3) nm, and β=91.23(4)° in space group P21 and those for glucopyranosylmannitol dihydrate are a=2.2579(15) nm, b=1.0016(5) nm, and c=0.7584(5) nm in space group P212121.
Crystal structure of lactitol (4-O-beta-D-galactopyranosyl-D-glucitol).
Abstract Lacitol, C 12 H 24 O 11 , is monoclinic, space group P 2 1 with cell dimensions a = 7.614(1), b = 10.757(1), c = 9.370(1) A, β = 108.19(1)°, and V = 729.0(1) A 3 ; Z = 2, D x = 1.57 Mg.m −3 , λ(Cu- K α ) = 1.5406 A, μ = 1.166 mm −1 , F (000) = 368, and T = 23°. The structure was solved by direct methods and refined by least-squares calculations to R = 0.048 for 1510 unique observed reflections. There are one intra- and eight inter-molecular hydrogen bonds in the structure. Bond lengths and angles accord well with the mean values of related structures. The galactopyranosyl ring has a chair conformation.
A new synthesis and crystal structure of n-(2-hydroxyethyl)succinimide
Abstract N-(2-Hydroxyethyl) succinimide was formed with 80 % yield in the reaction of 2-oxazolidinone with succinic anhydride at 210° C instead of polyesteramides obtained from N-substituted 2-oxazolidinones. The identification based on the crystal structure determination.
Thermoanalytical studies on phases of D-mannitol
Abstract D-mannitol exists in several polymorphic crystalline forms. The conditions of crystallization are not well-defined, and in some cases mixtures of the different forms are obtained. In the DSC study the different forms melted nearly at the same temperature (166±°C). The heat of fusion of the k form was lower than those of the other forms. With slow heating rate (2 ° C min ) the δ form changed to k between 140 and 165 °C. The crystallization of D-mannitol from the melt gave from one to seven peaks in the DSC between 95 and 126 °C depending on cooling rates and the amounts of sample.
Crystal structure and IR spectrum of 1-O-α-d-glucopyranosyl-d-mannitol–ethanol (2/1)
Abstract 1- O - α - d -Glucopyranosyl- d -mannitol–ethanol (2/1), (C 12 H 24 O 11 ) 2 –C 2 H 5 OH, crystallizes in the monoclinic space group P2 1 with unit cell dimensions a =11.4230(8) A, b =9.525(4) A, c =15.854(2) A, β =102.751(7)° and V =1682.4(7) A 3 , Z =2, D x =1.45 Mg m −3 , λ (Mo-K α )=0.71069 A, μ=0.128 mm −1 , F (000)=788 and T =293(2) K. The structure was solved by direct methods and refined by least-squares calculations on F 2 to R 1 =0.0371[ I >2 σ ( I )], and 0.0930 (all data, 3542 independent reflections, R int =0.021). There are two molecules of glucopyranosylmannitol (GPM) and one ethanol molecule in the asymmetric unit, and the glucopyranosyl ring adopts a chair conforma…
Thermal behaviour of anhydrous, dihydrate and (2/1) ethanol forms of 1-O-α-d-glucopyranosyl-d-mannitol
Abstract The melting points of anhydrous 1-O-α- d -glucopyranosyl- d -mannitol, 1-O-α- d -glucopyranosyl- d -mannitol dihydrate and a new compound, 1-O-α- d -glucopyranosyl- d -mannitol-ethanol (2/1) were determined using differential scanning calorimetry. The melting onset values were 169.2 (3), 104.3 (18) and 158.7 (9), respectively, and the melting peak values were 171.4 (5), 107.9 (15) and 160.1 (6), respectively. 1-O-α- d -glucopyranosyl- d -mannitol dihydrate and 1-O-α- d -glucopyranosyl- d -mannitol-ethanol (2/1) decompose to anhydrous form when heated at slow heating rates. According to TG-FTIR measurements, 1-O-α- d -glucopyranosyl- d -mannitol-ethanol (2/1) lost its ethanol in the…
Influence of drying to the structure of lactitol monohydrate
The purpose of this study is to find out the effect of the crystal water content on the crystal structure of lactitol monohydrate. Crystal water was removed by drying over silicagel at 40°C and by using phosphorus pentoxide as drying agent at 20°C. The amouts of water removals were identified by thermogravimetry, the melting points and the heat of fusions were calculated from the results of differential scanning calorimetry measurements and the structure of samples were identified by X-ray powder diffraction method. Over 23 w/w% of total water content could removed by gently drying until significant structural changes could be detected. The melting point of anhydrous lactitol obtained by dr…
Quantification of low levels of amorphous content in sucrose by hyperDSC.
A method was developed for the quantification of low levels of amorphous content in sucrose with hyperDSC. The method was based on the fact that the change of specific heat at the glass transition is linearly proportional to the amorphous content. It was found out that as annealing time increased, the glass transition temperature moved to a higher temperature and the change of specific heat increased. DeltaC(p) for annealed totally amorphous sucrose was 0.761+/-0.012 Jg(-1) degrees C(-1). Synthetic mixtures with various proportions of crystalline and amorphous sucrose were prepared. The following linear regression between DeltaC(p) and amorphous content was obtained: DeltaC(p)=0.0075x - 0.0…