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Research Article
Nassiba Baimatova
Al-Farabi Kazakh National University
Corresponding Author
ORCiD: https://orcid.org/0000-0002-0631-3425
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Quantification of unsymmetrical dimethylhydrazine (UDMH) transformation products (TPs) in solid samples is an important stage in monitoring of environmental pollution caused by heavy rockets launches. The new method for simultaneous quantification of UDMH TPs in sand samples using vacuum-assisted headspace solid-phase microextraction (Vac-HSSPME) followed by gas chromatography-mass spectrometry (GC-MS) is proposed. Compared to regular HSSPME, Vac-HSSPME yielded 1.3–4.8 times higher responses for NDMA, MTA and PAl. Increasing air-evacuation time from 20 to 120 s at 23 ºC resulted in decreased responses of analytes by 25–46%. Freezing of samples (-30 ºC) had negligible effect on responses of analytes at air-evacuation time 20 s. The best combination of responses of analytes and their RSDs was achieved after air-evacuation of a sample (m = 1.00 g) for 20 s at 23 ºC, incubation for 30 min and 30-min extraction at 40°C by Car/PDMS fiber. Vac-HSSPME provided linear calibration plots in studied ranges of concentrations with coefficients of determination ranging from 0.9912 to 0.9938. The limits of detection for spiked sand samples varied from 0.035 to 3.6 ng g− 1. Spike recoveries of target analytes from sand samples were 84–97% with RSDs 1–11%. The developed method was successfully tested in the experiment on studying losses of analytes from open vials with model sand spiked with UDMH TPs. The developed method can be recommended for analysis of trace concentrations of UDMH TPs when studying their transformation, migration and distribution in contaminated sand.
Keywords
Vacuum-assisted headspace solid-phase microextraction, GC-MS, soil analysis, transformation products, dimethylhydrazine, rocket fuel
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View the published article at Environmental Science and Pollution Research.
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Posted 22 Mar, 2021
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Received 19 Mar, 2021
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See the published version of this preprint at Environmental Science and Pollution Research.
This is a preprint, a preliminary version of a manuscript that has not completed peer review at a journal. Research Square does not conduct peer review prior to posting preprints. The posting of a preprint on this server should not be interpreted as an endorsement of its validity or suitability for dissemination as established information or for guiding clinical practice.
Learn more about In Review
Research Article
Nassiba Baimatova
Al-Farabi Kazakh National University
Corresponding Author
ORCiD: https://orcid.org/0000-0002-0631-3425
Badges
Prescreen
This manuscript passed our Prescreen assessment
Complete author information
Appropriate declaration statements
Potential risks to human health
Prescreen
Peer Review Timeline
CURRENT STATUS: Published
View the published article at Environmental Science and Pollution Research.
Version 1
Posted 22 Mar, 2021
No community comments so far
Reviewers invited
Invitations sent on 19 Mar, 2021
Reviews received
Received 19 Mar, 2021
Editor invited
On 16 Mar, 2021
First submitted
On 04 Mar, 2021
Metrics
Comments: 0
PDF Downloads: ...
HTML Views: ...
Subject Areas
Environmental Engineering
License:
This work is licensed under a CC BY 4.0 License. Read Full License
View the published article at Environmental Science and Pollution Research.
Quantification of unsymmetrical dimethylhydrazine (UDMH) transformation products (TPs) in solid samples is an important stage in monitoring of environmental pollution caused by heavy rockets launches. The new method for simultaneous quantification of UDMH TPs in sand samples using vacuum-assisted headspace solid-phase microextraction (Vac-HSSPME) followed by gas chromatography-mass spectrometry (GC-MS) is proposed. Compared to regular HSSPME, Vac-HSSPME yielded 1.3–4.8 times higher responses for NDMA, MTA and PAl. Increasing air-evacuation time from 20 to 120 s at 23 ºC resulted in decreased responses of analytes by 25–46%. Freezing of samples (-30 ºC) had negligible effect on responses of analytes at air-evacuation time 20 s. The best combination of responses of analytes and their RSDs was achieved after air-evacuation of a sample (m = 1.00 g) for 20 s at 23 ºC, incubation for 30 min and 30-min extraction at 40°C by Car/PDMS fiber. Vac-HSSPME provided linear calibration plots in studied ranges of concentrations with coefficients of determination ranging from 0.9912 to 0.9938. The limits of detection for spiked sand samples varied from 0.035 to 3.6 ng g− 1. Spike recoveries of target analytes from sand samples were 84–97% with RSDs 1–11%. The developed method was successfully tested in the experiment on studying losses of analytes from open vials with model sand spiked with UDMH TPs. The developed method can be recommended for analysis of trace concentrations of UDMH TPs when studying their transformation, migration and distribution in contaminated sand.
Figure 1
Figure 2
Figure 3
Figure 4
Figure 5
Figure 6
This is a list of supplementary files associated with this preprint. Click to download.
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