Sealed Ampoules Research Articles

CRYSTAL STRUCTURE AND LUMINESCENT PROPERTIES OF RHENIUM CLUSTERS [{Re6(μ3-Q)8}(imz-[1,2-a]py)6]Br2

Octahedral rhenium cluster complexes of the composition [{Re6(μ3-Q)8}(imz-[1,2-a]py)6]Br2, where Q = S, Se, are obtained by the interaction of Csn[{Re6(μ3-Q8)}Br6] (n = 4 for Q = S; n = 3 for Q = Se) with an excess of imidazo-[1,2-а]pyridine in a sealed glass ampoule at 180 °С within two days. Both compounds are isostructural and crystallize in the trigonal space group $$R\bar{3}$$ . The crystal structure of the complexes represents three differently directed chains of [{Re6Q8}(imz-[1,2-a]py)6]2+ cations and bromine anions linked with each other by С–H⋯Br⋯H–C hydrogen bonds. The compounds obtained have pronounced luminescence with emission maxima at 652 nm and 678 nm for Q = S, Se respectively.

About Lanthanoid Fluoride Selenide Oxoselenotantalates with the Composition Ln3F2Se2TaO4 (Ln = La – Nd)

After solid‐state reactions of the light lanthanoid metals, their oxides and fluorides as well as selenium in sealed tantalum ampoules with sodium chloride as a fluxing agent at 850 °C for 8 days needle‐shaped single crystals of Ln3F2Se2TaO4 (Ln = La – Nd) were obtained. They crystallize in the orthorhombic space group Pnma analogous to La3F2Se2NbO4 with a = 1133–1120 pm, b = 400–393 pm and c = 1812–1778 pm (Ln = La – Nd) for Z = 4 as the first known quinary lanthanoid(III) oxoselenotantalates(V) with fluoride and selenide anions. The three crystallographically different Ln3+ cations are all surrounded by nine anions (O2–, F– and Se2–) each. Tantalum resides in an octahedral chalcogen coordination by forming trans‐vertex oxygen‐connected [TaO5Se]7– polyhedra, which build up chains 1∞{[TaOV2/2Ot3/1Set1/1]5–} along [010]. The sites of the four crystallographically different oxygen atoms and the two distinct fluoride anions were established by bond‐valence calculations. One fluorine and three oxygen atoms are surrounded tetrahedrally by cations, while another fluoride and oxide anion exhibit just triangular non‐planar coordination spheres. The two independent Se2– anions have five or six cationic neighbors.

Synergistic Effects during Physical Refining of Palm Oil to Mitigate the Formation of Monochloropropanediols

AbstractThe aim of this study is to assess the synergy of mitigating main chlorine sources in palm oil and the oil refining conditions in a lab‐scale physical refining process. Mitigation concepts including centrifugation and washing steps are integrated into the physical refining protocol and the MCPD levels in the fully refined oils are determined. The endogenous chlorine content of the crude oil and that of the bleaching clay is confirmed to predominantly impact MCPD formation in this refining process. Residual sediments are shown to induce up to 1 ppm MCPD in the fully refined oils. Residual chlorine content of bleaching clay is shown to increase MCPD content of the oil twofold. t‐Test statistical analysis confirms significant effect of centrifugation, phosphoric acid content, clay type and clay washing on the formation of MCPD. Centrifugation is shown to effectively reduce the chlorine source coming from the sediments, while clay washing is shown to effectively reduce the chlorine source coming from the bleaching clay. These mitigation effects are confirmed both in sealed ampoule tests and in deodorizer experiments.Practical Applications: A combined application of strong centrifugation and clay washing is recommended to potentially improve the MCPD content of physically refined palm oil.

The Solid Solution Eu1–xSrxAuIn

EuAuIn and SrAuIn (TiNiSi type structure, space group Pnma) form a complete solid solution Eu1–xSrxAuIn. Samples with x = 0.2, 0.4, 0.5, 0.6 and 0.8 were prepared by melting of the elements in sealed tantalum ampoules followed by slow cooling. The samples were characterized through Guinier powder patterns. The X‐ray data confirm Vegard type behavior. The crystal structures of Eu0.8Sr0.2AuIn and Eu0.5Sr0.5Au1.02In0.98 were refined from single‐crystal X‐ray diffraction data in order to confirm the Eu/Sr site occupancies. Temperature‐dependent magnetic susceptibility data confirm divalent europium. The Néel temperature linearly drops from 21.0 K for EuAuIn and long‐range magnetic ordering is still present in the x = 0.8 sample with TN = 4.1 K. Low‐field measurements indicate two successive magnetic ordering temperatures for all samples, resulting from a complex interplay of antiferromagnetic and ferromagnetic interactions, similar to the tetrelides EuMgX (X = Si, Ge, Sn). 151Eu Mössbauer spectra confirm the divalent ground state and show complex magnetic hyperfine field splitting at 6 K.

Sc14Co3.10In2.59 – the representative of the Lu14Co3In3 type with the smallest rare earth element

Abstract The scandium-rich phase Sc14Co3.10In2.59 has been synthesized by a direct reaction of the elements in a sealed tantalum ampoule in a high-frequency furnace. Single crystals were obtained by slow cooling of the product. The Sc14Co3.10In2.59 structure was refined from single-crystal X-ray diffractometer data: Lu14Co3In3 type, P42/nmc, a = 889.13(13), c = 2138.7(4) pm, wR2 = 0.0483, 1636 F 2 values, and 64 variables. Sc14Co3.10In2.59 completes the series of the rare earth metal-rich phases RE 14Co3In3. The structure refinement revealed defects on the Co1 site (84.7(5)% occupancy on 8g) and a mixed occupancy of 59.1(7)% In1/40.9(7)% Co3 on the 4c site. The structure is built up by a dense condensation of Co@Sc6 trigonal prisms and In2@InSc11 and In1/Co2@Co2Sc10 icosahedra. An interpenetration of the In2@InSc11 icosahedra leads to dumb-bell formation with an In2–In2 distance of 289 pm. The Sc14Co3.10In2.59 structure is stabilized by substantial Sc–Sc bonding (316–360 pm Sc–Sc).

Polymorphs of VO(PO3)2: synthesis and crystal structure refinement revisited

Abstract The monoclinic α-polymorph of (VIVO)(PO3)2 is obtained reproducibly by reaction of V2O5 and H3PO4 (85%) (Au crucible, 380 °C, 4 d). Its crystal structure was refined from X-ray single-crystal data [C2/c, Z = 4, a = 15.1038(7) Å, b = 4.193(2) Å, c = 9.573(9) Å, β = 126.45(3), R 1 = 0.052, wR 2 = 0.189 for 976 unique reflections with F o > 4σ(F o ), 48 variables]. A single-phase powder of the β-polymorph is obtained by the reaction of V2O5, H3PO4 (85%) and oxalic acid, evaporating the mixture, and subsequent annealing (porcelain crucible, 800 °C in air, 2 d). Single crystals of β-(VIVO)(PO3)2 were grown in a sealed silica ampoule with chlorine as mineralizer. The crystal structure of the orthorhombic (pseudo-tetragonal) β-polymorph was refined from X-ray single-crystal data [pseudo-merohedral twin, Fdd2, Z = 8, a = 15.536(2) Å, b = 15.586(2) Å, c = 4.2611(5) Å, R 1 = 0.032, wR 2 = 0.068 for 1072 unique reflections with F o > 4σ(F o ), 50 variables]. Earlier reports on a tetragonal polymorph with unusual geometric structure of the [(V≡O)O5] polyhedron are corrected.

The Triclinic Lanthanoid(III) Halide Oxidoarsenates(III) Sm3Cl2[As2O5][AsO3] and Tm3Br2[As2O5][AsO3

Pale yellow single crystals of the composition Ln3X2[As2O5][AsO3] (Ln = Tm for X = Br and Ln = Sm for X = Cl) were obtained via solid‐state reactions in the systems Ln2O3/As2O3 from sealed silica ampoules using different halides as fluxing agents. Sm3Cl2[As2O5][AsO3] and Tm3Br2[As2O5][AsO3] crystallize isotypically in the triclinic space group P1 with Z = 2 and cell parameters of a = 543.51(4) pm, b = 837.24(6) pm, c = 1113.45(8) pm, α = 90.084(2)°, β = 94.532(2)°, γ = 90.487(2)° for the samarium and a = 534.96(4) pm, b = 869.26(6) pm, c = 1081.84(8) pm, α = 90.723(2)°, β = 94.792(2)° γ = 90.119(2)° for the thulium compound. The isotypic crystal structure of both representatives exhibits three crystallographically different Ln3+ cations, each with a coordination number of eight. (Ln1)3+ and (Ln2)3+ are only coordinated by three oxygen atoms, whereas (Ln3)3+ shows additional contacts to halide anions in forming square [LnO4X4]9– antiprisms. All As3+ cations are surrounded by three oxygen atoms in the shape of isolated [AsO3]3– ψ1‐tetrahedra. They occur either isolated or condensed as pyroanionic [As2O5]4– units with a bridging oxygen atom. In both anions, non‐binding lone‐pair electrons are present at the As3+ cations with a pronounced stereochemically active function.

Solid solutions EuAu4Cd2−x Mg x with a remarkably stable ferromagnetic ground state

Abstract Samples of the solid solutions EuAu4Cd2−x Mg x were synthesized from the elements in sealed tantalum ampoules. The elements were reacted at a maximum temperature of 1273 K followed by slow cooling. For crystal growth, the polycrystalline samples were ground to powders, pressed to pellets and annealed again. All samples crystallize with the tetragonal YbAl4Mo2-type structure, space group I4/mmm. The solid solution extends up to x = 1 and the Cd/Mg substitution has only a minor influence on the lattice parameters. The samples have been characterized by powder X-ray diffraction and the structure of EuAu4Cd1.58(2)Mg0.42(2) was refined from single crystal X-ray diffractometer data: a = 715.46(14), c = 549.96(11) pm, wR2 = 0.0334, 180 F 2 values and 11 variables. The striking crystal chemical motifs of the EuAu4Cd2−x Mg x structures are Eu@Au12 and (Cd/Mg)@Au8(Cd/Mg)2 polyhedra and linear Cd/Mg chains in form of a tetragonal rod packing with distances of 275 pm for Cd/Mg–Cd/Mg. Temperature dependent magnetic susceptibility measurements of all samples from the solid solutions EuAu4Cd2−x Mg x revealed Curie–Weiss behavior and stable divalent europium. All samples are ordered ferromagnetically around T = 16 K, and magnetization isotherms at 3 K classify these materials as soft ferromagnets. It is remarkable that the structural Cd/Mg disorder within the chains does not influence the ferromagnetic ground state. The divalent nature of europium in these intermetallics was exemplarily studied for the EuAu4Cd1.4Mg0.6 sample by 151Eu Mössbauer spectroscopy. At 6 K the isomer shift is −9.95(4) mm s−1 and one observes full magnetic hyperfine field splitting with B hf = 27.1(1) T.

Solubilities of Magnesium and Cadmium Sulfates in Water at High Temperatures and Pressures

The solubilities of salts in the MgSO4–H2O and CdSO4–H2O systems are studied at 276–500°C using various methods (visual examination of phase transformations in water–salt mixtures in sealed quartz ampoules, collecting solution samples and performing chemical analysis, and measuring p–V–T dependences in an autoclave) to determine temperature dependence and classify the compounds as one the of two types (type 1 or type 2) according to the classification of inorganic salts. In the studied temperature range, the solubility of these salts is very low at pressures below 157 MPa and decreases when approaching the critical point of water. The systems under study are found to be classified as type 2 water–salt systems having the critical point (G = L – S) lying near the critical point of water. No separation of fluid into two liquid phases was detected at temperatures below 500°C and pressures below 157 MPa, thus indicating that the second critical point (L1 = L2 – S) has very high parameters. The resulting data can be used for elaborating methods for raw material processing.

Eu1\u2009\u2212\u2009xSrxAu4Cd2: a ferromagnetic solid solution with adjustable Curie temperature

Samples of the solid solution Eu1–xSrxAu4Cd2 (YbAl4Mo2 type, space group I4/mmm) with x = 0.2, 0.4, 0.6, and 0.8 were synthesized from the elements by annealing in sealed tantalum ampoules. The structures of Eu0.66Sr0.34Au4.12Cd1.88 and Eu0.22Sr0.78Au4.10Cd1.90 were refined from X-ray single crystal diffractometer data. Besides the expected Eu/Sr mixing on the 2a sites the diffraction data revealed also a small degree of Cd/Au mixing on the 4d sites of the cadmium chains. Temperature dependent magnetic susceptibility data show divalent europium and ferromagnetic ground states for all samples and a linear decrease of the Curie temperature from 16.3 K for EuAu4Cd2 to 2.9 K for Eu0.2Sr0.8Au4Cd2. Magnetization isotherms characterize the Eu1 − xSrxAu4Cd2 samples as soft ferromagnets. The divalent nature of europium is underpinned by 151Eu Mössbauer spectra. The decreasing Curie temperature goes along with a decreasing magnetic hyperfine field at 6 K.Graphic abstract

EuIrIn4 with LaCoAl4 Type Structure – Synthesis, Magnetic Properties, and 151Eu Mössbauer Spectroscopy

LaCoAl4 type EuIrIn4 was synthesized by induction‐melting of the elements in a sealed tantalum ampoule, followed by annealing of the sample in a high‐frequency or in a muffle furnace. The EuIrIn4 structure was refined from single‐crystal X‐ray diffraction data: Pmma, a = 860.65(3), b = 430.33(6), c = 757.65(7) pm, wR = 0.0748, 633 F2 values and 24 variables. The striking building units are iridium‐centered trigonal prisms of indium atoms, distorted bcc indium cubes and a pentagonal prismatic indium coordination of the europium atoms. Within the three‐dimensional [IrIn4]2– polyanionic network the Ir–In and In–In distances range from 260–288 pm and 306–332 pm, respectively. The divalent ground state of europium was manifested through magnetic [7.96(1) μB / Eu atom, TN = 7.9(1) K] and 151Eu Mössbauer spectroscopic data [δ = –10.54(2) mm·s–1; Bhf = 19.1(1) T at 6 K].

A brief visit to the BeCl2/ZnCl2 system and the prediction of a new polymorph of ZnCl2

Abstract Reactions of zinc chloride with beryllium chloride in the molar ratios of 1:1 and 3:2 at T = 300°C in sealed ampoules lead to the formation of the two compounds Be1− x Zn x Cl2 (x = 0.563(2) and 0.489(3), respectively). Their composition and crystal structures were evidenced by single crystal X-ray structure analysis. Both compounds crystallize isotypic to β-BeCl2 in the tetragonal space group I41/acd, No. 142, tI96, with a = 10.7548(1), c = 19.4656(5) Å, V = 2251.50(7) Å3, Z = 32 at T = 100 K for the first and a = 10.7511(3), c = 19.2335(10) Å, V = 2223.1(2) Å3, Z = 32 at T = 100 K for the second compound. The positions of the Be atoms are mixed-occupied by Zn atoms. The compounds were additionally characterized by powder X-ray diffraction and infrared spectroscopy. Plots according to Vegard’s law allowed for extrapolation towards a neat ZnCl2 phase that would crystallize in the β-BeCl2 structure, which is the ZnI2 structure type. Quantum chemical calculations have confirmed that such a ZnCl2 modification would represent a true local minimum.

Quaternary intermetallics RE 2Pt3Ga4In (RE=Y, Gd-Tm) – intergrowth structures of NdRh2Sn4 and TiNiSi related slabs

Abstract The quaternary gallium-rich intermetallic phases RE 2Pt3Ga4In with RE = Y and Gd-Tm were synthesized by arc-melting of the elements and subsequent annealing. Small single crystals were obtained by high-frequency annealing of the samples in sealed tantalum ampoules. The polycrystalline samples were characterized through their X-ray powder patterns. The RE 2Pt3Ga4In phases crystallize with a site ordering variant of the orthorhombic Y2Rh3Sn5 type, space group Cmc 21. The structures of Gd2Pt3Ga4In, Dy2Pt3Ga4.14In0.86, Er2Pt3Ga4.17In0.83 and Tm2Pt3Ga4.21In0.79 were refined from single-crystal X-ray diffraction data. The single crystals reveal small homogeneity ranges RE 2Pt3Ga4±xIn1±x. The striking geometrical structural building units are slightly distorted trigonal prisms around the three crystallographically independent platinum atoms: Pt1@RE 4Ga2, Pt2@RE 2Ga4 and Pt3@RE 2Ga2In2. Based on these prismatic building units, the RE 2Pt3Ga4In structures can be described as intergrowth variants of TiNiSi and NdRh2Sn4 related structural slabs. Temperature dependent magnetic susceptibility studies of Gd2Pt3Ga4In and Tb2Pt3Ga4In show Curie-Weiss behavior and the experimental magnetic moments confirm stable trivalent gadolinium respectively terbium. Gd2Pt3Ga4In and Tb2Pt3Ga4In order antiferromagnetically at T N = 15.8(1) and 26.0(1) K. Magnetization curves at 3 K show field-induced spin reorientations.

PHASE EQUILIBRIUM IN THE Cu2Se – SnSe2 – As2Se3 QUASITERNARY SYSTEM

77 alloys have been synthesized to study the interaction of the components in the Cu 2 Se –SnSe 2 – As 2 Se 3 quasi-ternary system. The synthesis was carried out by direct single-temperature method from high purity substances (Cu – 99.99 wt.%, Sn – 99.99 wt.%, Se – 99.9997 wt.%, As – 99.9999 wt.%) in evacuated and sealed quartz ampoules. The maximum temperature of the synthesis was 1170 K, homogenizing annealing was carried out at 510 K during 600 h. The obtained samples were investigated by X-ray analysis and differential thermal analysis. The isothermal section of the system at 510 K has been constructed based on the results of the X-ray analysis. The quasi-binary equilibria Cu 2 SnSe 3 – CuAsSe 2 ; Cu 2 GeSe 3 – As 2 Se 3 divide the quasi-ternary system into 3 subsystems: Cu 2 Se – Cu 2 SnSe 3 – CuAsSe 2 ; CuAsSe 2 – Cu 2 SnSe 3 – As 2 Se 3 and Cu 2 SnSe 3 – SnSe 2 – As 2 Se 3 . Solid solutions with large length are not formed, solubilities based on binary, ternary compounds are not more than 5 mol. %. The liquid surface projection of the Cu 2 Se – SnSe 2 – As 2 Se 3 quasi-ternary system has been built based on the literary and obtained results of investigations of the four polythermal sections and one phase diagram. The projection consists of the fields of primary crystallization of Cu 2 Se, Cu 2 SnSe 3 , SnSe 2 , As 2 Se 3 , CuAsSe 2 . They are separated by 8 monovariant curves and 9 nonvariant points. The Cu 2 SnSe 3 – As 2 Se 3 section is quasi-binary and it devides the investigated system into two subsystems: Cu 2 Se – Cu 2 SnSe 3 – As 2 Se 3 (I) and Cu 2 SnSe 3 – As 2 Se 3 – SnSe 2 (II). In the subsystem (I) two nonvariant processes take place:L U1 + Cu 2 Se ↔ Cu 2 SnSe 3 + CuAsSe 2 (peritectic) at 700 K and L E1 ↔ As 2 Se 3 + CuAsSe 2 + Cu 2 SnSe 3 (eutectic) at 600 К. In the subsystem (II) one nonvariant eutectic process L E2 ↔ As 2 Se 3 + Cu 2 SnSe 3 + SnSe 2 takes place at 610 К.

Estimation of Reactivity Ratios in the Copolymerization of Styrene and VeoVa‐10

AbstractThe styrene and vinyl neodecanoate copolymerization system shows a strong tendency to form two separate homopolymers. In order to improve the feeding strategies and hence the copolymer uniformity, it is necessary to know the reactivity ratios between these monomers. The error‐in‐variables‐method (EVM) is the most recommended mathematical procedure for estimating these parameters. Experiments on free‐radical copolymerization in solution in sealed ampoules are carried out to provide data for the conversion (via gravimetry) and fractional monomer compositions (via Fourier transform mid‐infrared (mid‐FT‐IR) spectroscopy). These data allow estimation of the reactivity ratios. EVM appropriately takes into account the experimental errors in the data and allows determination of the reactivity ratio values by the Mayo–Lewis model (r1 = 28.60 and r2 = 1.23). The convergence and robustness of the method decrease considerably with a larger discrepancy between the reactivity values.

Synthesis and characterization of semiconducting sinnerite (Cu6As4S9) thin films

Sinnerite (Cu6As4S9) is a semiconductor computed to have attractive optoelectronic properties, but little attention has been paid to its experimental synthesis and characterization. Here, the authors report the first synthesis of polycrystalline sinnerite thin films. By heating Cu3AsS4 nanoparticles in sealed ampoules with As2S2 powder, a phase transformation to Cu6As4S9 is achieved along with the formation of micronsized dense grains appropriate for device applications. The films display a bandgap of ~1.2 eV, significant photocurrent generation under simulated AM1.5 illumination, and carrier lifetimes nearing 1 ns, demonstrating the promise of sinnerite for use in photovoltaic applications.

SrIrIn6 – An Intergrowth of SrIrIn4 with Indium Slabs

The indium‐rich intermetallic compound SrIrIn6 was synthesized from the elements in a sealed tantalum ampoule at 1173 K, followed by slow cooling for crystal growth. SrIrIn6 crystallizes with a new structure type which was characterized by X‐ray powder and single crystal diffraction: Pmma, a = 852.34(2), b = 434.54(5), c = 1059.18(6) pm, wR2 = 0.0178, 884 F2 values, and 32 variables. The SrIrIn6 structure shows two basic building units: (i) Ir@In9 tricapped trigonal prisms (261–292 pm Ir–In) and (ii) distorted bcc In@In8 cubes (301 to 329 pm In–In). The strontium cations fill cages within the complex three‐dimensional [IrIn6] network and have coordination number 13 (Sr@In13) in form of a tricapped pentagonal prism. The SrIrIn6 structure can be described as a simple intergrowth variant of SrIrIn4 (LaCoAl4 type) with indium slabs. The crystal chemical similarities with the structures of SrIrIn4, SrIr2In8 and Eu3Ir2In15 are discussed.

Facile One‐step Synthesis of Zn1–xMnxSiN2 Nitride Semiconductor Solid Solutions via Solid‐state Metathesis Reaction

We report on the synthesis of the II‐IV‐N2 semiconductors ZnSiN2, MnSiN2, and the Zn1–xMnxSiN2 solid solutions by a one‐step solid‐state metathesis reaction. The successful syntheses were carried out by reacting the corresponding metal halides with stoichiometric amounts of silicon nitride and lithium azide in sealed tantalum ampoules. After washing out the reaction byproduct LiCl, powder X‐ray diffraction patterns were indexed with orthorhombic space group Pna21. Single phase products were obtained without applying external pressure and at a moderate reaction temperature of 700 °C. The resulting ZnSiN2 was found to consist of nano‐sized grains and needle‐shaped nano‐crystals. With increasing manganese content in the Zn1–xMnxSiN2 solid solution, we found the reaction product to be increasingly crystalline. Both the cell parameters and the bandgap values across the different compositions of the solid solutions change linearly. The sample Zn0.95Mn0.05SiN2 synthesized by means of solid‐state metathesis reaction is an intense red emitter with a broad emission maximum at λmax ≈ 619 nm when excited with ultraviolet light after annealing the sample at a pressure of 6 GPa and a temperature of 1200 °C.

CdTe synthesis and crystal growth using the high-pressure Bridgman technique

Abstract Efficient, safe and cost-effective synthesis of CdTe from elements is rather challenging in silica sealed ampoules due to the high vapor pressure of Cd. In this article, we report on the integrated synthesis and crystal growth of high-purity CdTe using the high pressure Bridgman (HPB) technique that is scalable to large volumes. The process lends itself for cost competitive industrial production of polycrystalline feedstock material for photovoltaics, sensors and electro-optic applications. Cadmium telluride (CdTe) crystals exceeding 1 kg in size were synthesized from elemental Cd and Te sources with purity comparable to state-of-the-art gamma ray detector crystals. In addition, synthesis of highly-doped CdTe feedstock for thin film photovoltaics applications demonstrating effective incorporation of group V (As, Sb) dopants was achieved at growth speeds of ~500 mm/hr. The technique may be applicable to produce other II-VI compounds with volatile components.

Determination of matrix composition of Ge-Se-Te chalcogenide glasses using the ICP-AES method

One of the most important stages of the high-purity chalcogenide glasses’ analytical control is the determination of matrix elements’ content with the uncertainty at the levels of 0.1–0.2 mol.%. The content of the macro-components may differ from the composition of the initial charge; therefore, an important task is the macro-composition determination of the final materials. This article describes the development of the technique for determining the matrix elements of high-purity Ge-Se-Te glasses in the range of germanium content from 10 to 35 mol. %, selenium and tellurium content from 20 to 50 mol. % with the expanded uncertainty within 0.01–0.2 mol. % (P = 0.95) using the inductively coupled plasma atomic emission spectrometry (ICP-AES). A simple technique for the preparation of primary calibration solutions from pure elementary Ge, Se and Te is proposed. The correctness of the analysis results is confirmed by comparing the calculated matrix composition of model glass samples, prepared by direct synthesis from high-purity simple substances in the sealed quartz glass ampoule, with the analysis results. The main advantage of the proposed analysis technique is the absence of the need for the reference samples identical to the analyzed material, which is especially important for determination of new materials’ matrix composition. The minimum sample mass for the determination of matrix elements is about 1 mg, which makes it possible to analyze not only bulk glass samples, but also fibers and expensive materials.