Development of an extraction procedure and analysis of electrostatically stabilized silanates from aqueous solutions
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Sep 25, 2020
About this article
Article Category: Research Article
Published Online: Sep 25, 2020
Page range: 247 - 254
Received: Feb 21, 2020
Accepted: Apr 09, 2020
DOI: https://doi.org/10.1515/ohs-2020-0022
Keywords
© 2020 Faculty of Oceanography and Geography, University of Gdańsk, Poland
This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 4.0 International License.
Figure 1
Figure 2
![Structure of a compound used in terminating electrolyte 4,4’-bis[(1-morpholiniomethyl)spirobi(1-sila-2,5-dioxacyclopentan-3-on)at]](https://sciendo-parsed.s3.eu-central-1.amazonaws.com/647264ce215d2f6c89dc6936/j_ohs-2020-0022_fig_002.jpg?X-Amz-Algorithm=AWS4-HMAC-SHA256&X-Amz-Content-Sha256=UNSIGNED-PAYLOAD&X-Amz-Credential=AKIA6AP2G7AKOUXAVR44%2F20250912%2Feu-central-1%2Fs3%2Faws4_request&X-Amz-Date=20250912T005714Z&X-Amz-Expires=3600&X-Amz-Signature=69f8548334f2ced581bebd5816785161582a60889fe1d1196700591755c38fcc&X-Amz-SignedHeaders=host&x-amz-checksum-mode=ENABLED&x-id=GetObject)
Figure 3
Figure 4
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 | ||||
|---|---|---|---|---|
| Stage | Time (s) | Intensity (μA) | Comp (10 mV) | Conductometric detector |
| 1 | 50 | 80 | 0 | |
| 2 | 70 | 120 | 50 | |
| 3 | 20 | 90 | 0 | X |
| 4 | 250 | 50 | 50 | |
| 5 | 325 | 120 | 0 | X |
Characteristic of the applied analytical method
| Analyte | Linearity determination coefficient above 0.9987 |
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 |
Limit of quantification LOQ = 3.3 x LOD |
Recovery the sample was enriched with 4 ml of a solution containing 2 μg fil-1 of the examined ion, n = 6 |
|---|---|---|---|---|---|
| ( |
3.1–50.4 | 3.0–4.2 | 2.2 | 7.3 | 91 ± 5 |
| ( |
2.8–49.6 | 3.2–4.5 | 2.1 | 6.9 | 92 ± 3 |
| ( |
2.9–51.3 | 2.8–4.1 | 2.3 | 7.6 | 92 ± 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 column | Mean recovery values and SD (%) | ||
|---|---|---|---|
| (72) | (73) | (79) | |
| RP Si–C18 | 85.3 ± 4.2 | 84.7 ± 3.9 | 85.1 ± 3.5 |
| RP Si–C8 | 82.2 ± 4.3 | 82.9 ± 4.9 | 83.7 ± 4.6 |
| RP Si–FP | 89.3 ± 3.9 | 91.3 ± 3.6 | 93.9 ± 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 |