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Development of an extraction procedure and analysis of electrostatically stabilized silanates from aqueous solutions Cover

Development of an extraction procedure and analysis of electrostatically stabilized silanates from aqueous solutions

Open Access
|Sep 2020

Figures & Tables

Figure 1

Structures of analyzed compounds: a) 1-(N-morpholiniomethyl)spirobi(1-sila-2,5-dioxacyclopentan-3-on)at (72), b) 1-(N-morpholiniomethyl)spirobi(1-sila-2,5-dioxa-4-methylcyclopentan-3-on)at (73), c) 1-(N-morpholiniomethyl) spirobi(1-sila-2,5-dioxa-4-(i-propyl)cyclopentan-3-on)at (79)
Structures of analyzed compounds: a) 1-(N-morpholiniomethyl)spirobi(1-sila-2,5-dioxacyclopentan-3-on)at (72), b) 1-(N-morpholiniomethyl)spirobi(1-sila-2,5-dioxa-4-methylcyclopentan-3-on)at (73), c) 1-(N-morpholiniomethyl) spirobi(1-sila-2,5-dioxa-4-(i-propyl)cyclopentan-3-on)at (79)

Figure 2

Structure of a compound used in terminating electrolyte 4,4’-bis[(1-morpholiniomethyl)spirobi(1-sila-2,5-dioxacyclopentan-3-on)at]
Structure of a compound used in terminating electrolyte 4,4’-bis[(1-morpholiniomethyl)spirobi(1-sila-2,5-dioxacyclopentan-3-on)at]

Figure 3

Chemical structures of bonded stationary phases used in the study: a) octadecyl, b) octyl, c) phenylpropyl stationary phases
Chemical structures of bonded stationary phases used in the study: a) octadecyl, b) octyl, c) phenylpropyl stationary phases

Figure 4

Isotachophoregram of the mixture of 1-(N-morpholiniomethyl)spirobi(1-sila-2,5-dioxacyclopentan-3-on)at (72), 1-(N-morpholiniomethyl)spirobi(1-sila-2,5-dioxa-4-methylcyclopentan-3-on)at (73), 1-(N-morpholiniomethyl) spirobi(1-sila-2,5-dioxa-4-(i-propyl)cyclopentan-3-on)at (79)
Isotachophoregram of the mixture of 1-(N-morpholiniomethyl)spirobi(1-sila-2,5-dioxacyclopentan-3-on)at (72), 1-(N-morpholiniomethyl)spirobi(1-sila-2,5-dioxa-4-methylcyclopentan-3-on)at (73), 1-(N-morpholiniomethyl) spirobi(1-sila-2,5-dioxa-4-(i-propyl)cyclopentan-3-on)at (79)

Optimum conditions for isotachophoretic separation of a mixture 1-(N-morpholiniomethyl)spirobi(1-sila-2,5-dioxacyclopentan-3-on)at (72), 1-(N-morpholiniomethyl)spirobi(1-sila-2,5-dioxa-4-methylcyclopentan-3-on)at (73), 1-(N-morpholiniomethyl)spirobi(1-sila-2,5-dioxa-4-(i-propyl)cyclopentan-3-on)at (79)

Considered parameters
StageTime (s)Intensity (μA)Comp (10 mV)Conductometric detector
150800
27012050
320900X
42505050
53251200X

Characteristic of the applied analytical method

AnalyteLinearity

determination coefficient above 0.9987

(μg l−1)
Coefficient of variation

n = 6, the samples were analyzed twice

(%)
Limit of detection

calculated from the limit of identification and coefficients of the calibration curve

(LOD) (μg l−1)
Limit of quantification

LOQ = 3.3 x LOD

(LOQ) (μg l−1)
Recovery

the sample was enriched with 4 ml of a solution containing 2 μg fil-1 of the examined ion, n = 6

(%)
(72)3.1–50.43.0–4.22.27.391 ± 5
(73)2.8–49.63.2–4.52.16.992 ± 3
(79)2.9–51.32.8–4.12.37.692 ± 4

Mean recovery values [1-(N-morpholiniomethyl)spirobi(1-sila-2,5-dioxacyclopentan-3-on)at (72), 1-(N-morpho liniomethyl)spirobi(1-sila-2,5-dioxa-4-methylcyclopentan-3-on)at (73), 1-(N-morpholiniomethyl)spirobi(1-sila-2,5-dioxa-4-(i-propyl)cyclopentan-3-on)at (79)] obtained on the columns used in the study (n = 5)

Type of extraction columnMean recovery values and SD (%)
(72)(73)(79)
RP Si–C1885.3 ± 4.284.7 ± 3.985.1 ± 3.5
RP Si–C882.2 ± 4.382.9 ± 4.983.7 ± 4.6
RP Si–FP89.3 ± 3.991.3 ± 3.693.9 ± 4.1

Common parameters of optimal (72), (73) and (79) separation and determination by the isotachophoresis method

Parameters of the method
UV filter (nm)200
High Voltage Limit (kV)12
Sample rate (smp s−1)50
Polarity+ cations
DOI: https://doi.org/10.1515/ohs-2020-0022 | Journal eISSN: 1897-3191 | Journal ISSN: 1730-413X
Language: English
Page range: 247 - 254
Submitted on: Feb 21, 2020
Accepted on: Apr 9, 2020
Published on: Sep 25, 2020
Published by: University of Gdańsk
In partnership with: Paradigm Publishing Services
Publication frequency: 4 issues per year

© 2020 Joanna Jabłońska, Mariusz Kluska, Nikolai Erchak, Stanisław Popiel, published by University of Gdańsk
This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 License.