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. 2022 Jun;414(15):4379-4389.
doi: 10.1007/s00216-021-03821-7. Epub 2022 Jan 14.

Development of a sample preparation procedure for Sr isotope analysis of Portland cements

Anera Kazlagić  1 , Francesco F Russo  2 , Jochen Vogl  2 , Patrick Sturm  3 , Dietmar Stephan  4 , Gregor J G Gluth  3
Affiliations

Development of a sample preparation procedure for Sr isotope analysis of Portland cements

Anera Kazlagić et al. Anal Bioanal Chem. 2022 Jun.

Abstract

The 87Sr/86Sr isotope ratio can, in principle, be used for provenancing of cement. However, while commercial cements consist of multiple components, no detailed investigation into their individual 87Sr/86Sr isotope ratios or their influence on the integral 87Sr/86Sr isotope ratio of the resulting cement was conducted previously. Therefore, the present study aimed at determining and comparing the conventional 87Sr/86Sr isotope ratios of a diverse set of Portland cements and their corresponding Portland clinkers, the major component of these cements. Two approaches to remove the additives from the cements, i.e. to measure the conventional 87Sr/86Sr isotopic fingerprint of the clinker only, were tested, namely, treatment with a potassium hydroxide/sucrose solution and sieving on a 11-µm sieve. Dissolution in concentrated hydrochloric acid/nitric acid and in diluted nitric acid was employed to determine the 87Sr/86Sr isotope ratios of the cements and the individual clinkers. The aim was to find the most appropriate sample preparation procedure for cement provenancing, and the selection was realised by comparing the 87Sr/86Sr isotope ratios of differently treated cements with those of the corresponding clinkers. None of the methods to separate the clinkers from the cements proved to be satisfactory. However, it was found that the 87Sr/86Sr isotope ratios of clinker and cement generally corresponded, meaning that the latter can be used as a proxy for the clinker 87Sr/86Sr isotope ratio. Finally, the concentrated hydrochloric acid/nitric acid dissolution method was found to be the most suitable sample preparation method for the cements; it is thus recommended for 87Sr/86Sr isotope analyses for cement provenancing.

Keywords: Cement; Clinker; Provenancing; Sample preparation; Strontium isotopes.

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Conflict of interest statement

The authors declare no competing interests.

Figures

Fig. 1
Fig. 1
Schematic representation of the four sample preparation procedures for cement samples. Conc. acid refers to dissolution in concentrated hydrochloric acid/nitric acid, KOSH refers to selective dissolution of clinker phases, dil. acid refers to dissolution in dilute nitric acid, and sieving is dry sieving performed on a 11-µm sieve. XRD refers to X-ray diffraction and TIMS refers to thermal ionisation mass spectrometry
Fig. 2
Fig. 2
X-ray diffractograms of the cement samples 3022, 3028, 3050, 3063, and 3078 after KOSH treatment: (a) alite, (b) belite, (d) aluminate, (c) calcite, (q) quartz, (K) KOH
Fig. 3
Fig. 3
X-ray diffractograms of the cement samples 3022, 3028, 3050, 3063, and 3078 after conc. acid treatment: (A) anhydrite, (c) calcite, (q) quartz, (z1) zeolite-type phase
Fig. 4
Fig. 4
X-ray diffractograms of the cement samples 3022, 3028, 3050, 3063 and 3078 after dil. acid treatment: (G) gypsum, (m) monocarboaluminate, (c) calcite, (q) quartz
Fig.  5
Fig.  5
87Sr/86Sr isotope ratios of fifteen cement samples after conc. acid treatement (orange) and after the sieving method (purple); error bars represent expanded uncertainty (U, k = 2).
Fig. 6
Fig. 6
Comparison of 87Sr/86Sr isotope ratios from fifteen cement samples after KOSH treatment (red) and fifteen corresponding clinker samples after conc. acid treatment (blue-green)
Fig. 7
Fig. 7
Comparison of 87Sr/86Sr isotope ratios from fifteen cement samples after conc. acid treatment (orange) and fifteen corresponding clinker samples after conc. acid treatment (blue-green)
Fig. 8
Fig. 8
Comparison of 87Sr/86Sr isotope ratios from fifteen cement samples after dil. acid treatment (fluorescent green) and fifteen corresponding clinker samples after conc. acid treatment (blue-green)
Fig. 9
Fig. 9
Comparison of all four methods on fifteen processed cement samples presented as the absolute difference between the 87Sr/86Sr isotope ratio of the processed cement and the 87Sr/86Sr isotope ratio of the corresponding clinker
Fig. 10
Fig. 10
Comparison of all methods: average absolute difference of the 87Sr/86Sr isotope ratios of the processed cements and the corresponding clinkers
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