Abstract

The article is devoted to the development of a reference material of the sorption roperties of nanoporous zeolite, which ensures metrological traceability of measurement results to the State primary measurement standard of units for specific gas adsorption, specific surface area, specific pore volume, pore size, open porosity and gas permeability coefficient of solid substances and materials GET 210-2019.The paper presents the results of theoretical and experimental studies on optimizing the conditions of sample preparation (thermal training) of the reference material using the thermogravimetric method and differential scanning calorimetry, coupled with mass spectrometric detection of the evolved gases (TG-DSC–MS analysis). The results of establishing the metrological characteristics of the reference material are described, including standard uncertainty due to the method of determining the certified value, as well as standard uncertainties from heterogeneity and instability. The GSO 10734–2015 reference material of the sorption properties of nanoporous zeolite (Zeolite SO UNIIM) has certified metrological characteristics: specific surface area (500–1200) m2/g; specific pore volume (0.10.5) cm3/g; the predominant pore diameter (0.4–0.9) nm; specific argon adsorption (0.001–20.0) mol/kg.The reference material is designed to calibrate measuring instruments and to control accuracy of results of sorption characteristics of nanoporous materials measurements; it can be used to certify appropriate measurement procedures, to test measuring instruments and reference materials for type approval and other types of metrological control.

Highlights

  • Ɋɬɚɬɶɹ ɩɨɫɜɹɳɟɧɚ ɪɚɡɪɚɛɨɬɤɟ ɫɬɚɧɞɚɪɬɧɨɝɨ ɨɛɪɚɡɰɚ ɫɨɪɛɰɢɨɧɧɵɯ ɫɜɨɣɫɬɜ ɧɚɧɨɩɨɪɢɫɬɨɝɨ ɰɟɨɥɢɬɚ, ɨɛɟɫɩɟɱɢɜɚɸɳɟɝɨ ɦɟɬɪɨɥɨɝɢɱɟɫɤɭɸ ɩɪɨɫɥɟɠɢɜɚɟɦɨɫɬɶ ɪɟɡɭɥɶɬɚɬɨɜ ɢɡɦɟɪɟɧɢɣ ɤ Ƚɨɫɭɞɚɪɫɬɜɟɧɧɨɦɭ ɩɟɪɜɢɱɧɨɦɭ ɷɬɚɥɨɧɭ ɟɞɢɧɢɰ ɭɞɟɥɶɧɨɣ ɚɞɫɨɪɛɰɢɢ ɝɚɡɨɜ, ɭɞɟɥɶɧɨɣ ɩɨɜɟɪɯɧɨɫɬɢ, ɭɞɟɥɶɧɨɝɨ ɨɛɴɟɦɚ ɩɨɪ, ɪɚɡɦɟɪɚ ɩɨɪ, ɨɬɤɪɵɬɨɣ ɩɨɪɢɫɬɨɫɬɢ ɢ ɤɨɷɮɮɢɰɢɟɧɬɚ ɝɚɡɨɩɪɨɧɢɰɚɟɦɨɫɬɢ ɬɜɟɪɞɵɯ ɜɟɳɟɫɬɜ ɢ ɦɚɬɟɪɢɚɥɨɜ ȽɗɌ 210-2019. ȼ ɪɚɛɨɬɟ ɩɪɟɞɫɬɚɜɥɟɧɵ ɪɟɡɭɥɶɬɚɬɵ ɬɟɨɪɟɬɢɱɟɫɤɢɯ ɢ ɷɤɫɩɟɪɢɦɟɧɬɚɥɶɧɵɯ ɢɫɫɥɟɞɨɜɚɧɢɣ ɩɨ ɨɩɬɢɦɢɡɚɰɢɢ ɭɫɥɨɜɢɣ ɩɪɨɛɨɩɨɞɝɨɬɨɜɤɢ ɫɬɚɧɞɚɪɬɧɨɝɨ ɨɛɪɚɡɰɚ ɫ ɩɨɦɨɳɶɸ ɬɟɪɦɨɝɪɚɜɢɦɟɬɪɢɱɟɫɤɨɝɨ ɦɟɬɨɞɚ ɢ ɞɢɮɮɟɪɟɧɰɢɚɥɶɧɨ-ɫɤɚɧɢɪɭɸɳɟɣ ɤɚɥɨɪɢɦɟɬɪɢɢ, ɫɨɩɪɹɠɟɧɧɨɣ ɫ ɦɚɫɫ-ɫɩɟɤɬɪɨɦɟɬɪɢɱɟɫɤɢɦ ɞɟɬɟɤɬɢɪɨɜɚɧɢɟɦ ɜɵɞɟɥɹɸɳɢɯɫɹ ɝɚɡɨɜ (ɌȽ-ȾɋɄ-Ɇɋ-ɚɧɚɥɢɡ)

  • Ɉɩɢɫɚɧɵ ɪɟɡɭɥɶɬɚɬɵ ɭɫɬɚɧɨɜɥɟɧɢɹ ɦɟɬɪɨɥɨɝɢɱɟɫɤɢɯ ɯɚɪɚɤɬɟɪɢɫɬɢɤ ɫɬɚɧɞɚɪɬɧɨɝɨ ɨɛɪɚɡɰɚ, ɜɤɥɸɱɚɹ ɫɬɚɧɞɚɪɬɧɭɸ ɧɟɨɩɪɟɞɟɥɟɧɧɨɫɬɶ, ɨɛɭɫɥɨɜɥɟɧɧɭɸ ɫɩɨɫɨɛɨɦ ɨɩɪɟɞɟɥɟɧɢɹ ɚɬɬɟɫɬɨɜɚɧɧɨɝɨ ɡɧɚɱɟɧɢɹ, ɚ ɬɚɤɠɟ ɫɬɚɧɞɚɪɬɧɵɟ ɧɟɨɩɪɟɞɟɥɟɧɧɨɫɬɢ ɨɬ ɧɟɨɞɧɨɪɨɞɧɨɫɬɢ ɢ ɧɟɫɬɚɛɢɥɶɧɨɫɬɢ

  • The article is devoted to the development of a reference material of the sorption roperties of nanoporous zeolite, which ensures metrological traceability of measurement results to the State primary measurement standard of units for specific gas adsorption, specific surface area, specific pore volume, pore size, open porosity and gas permeability coefficient of solid substances and materials GET 210-2019

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Summary

DEVELOPMENT OF A REFERENCE MATERIAL OF NANOPOROUS ZEOLIT

The GSO 10734–2015 reference material of the sorption properties of nanoporous zeolite (Zeolite SO UNIIM) has certified metrological characteristics: specific surface area (500–1200) m2/g; specific pore volume (0.1 0.5) cm3/g; the predominant pore diameter (0.4–0.9) nm; specific argon adsorption (0.001–20.0) mol/kg. Для метрологического обеспечения данных измерений на практике во всем мире применяются стандартные образцы пористых веществ, которые охарактеризованы с применением одной из существующих моделей. На основе аттестованных значений удельной адсорбции газа от относительного давления газа возможно провести аттестацию интересующих величин (удельной поверхности, удельного объема и размера пор) с применением различных теорий, при этом отсутствует необходимость в проведении дополнительных экспериментальных исследований. ( ) ( ) порошка цеолита (Na86 ⎡⎣ AlO2 86 SiO2 106⎤⎦ ⋅xH2O), в связи с чем он и был выбран в качестве материала СО. Образeц был помещен в алюминиевый тигель (с крышкой), скорость нагрева 10 °С/мин в диапазоне (20–1000) °С (см. рис. 1)

Теоретические предпосылки
Удельная поверхность рассчитывается как
Po P
NA RT
Диаметр нм
Определение метрологических характеристик стандартного образца
Коэффициент газопроницаемости
Номер экземпляра СО
Расширенную неопределенность аттестованного значения оценим как
Аттестованная характеристика
ИНФОРМАЦИЯ ОБ АВТОРАХ

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