Skip to main content
SpringerLink
Log in

Critical evaluation of quantitative determination of minerals in slags by a new MCQMA and QXRD methods

  • Original Article
  • Published:
Materials and Structures Aims and scope Submit manuscript

Abstract

A new modified chemical quantitative mineral analysis (MCQMA) method was developed and used for quantitative calculation of crystalline and amorphous phases in ladle and blast furnace slags and their slag blends with 20–100 wt% of the amorphous phase. MCQMA calculation was created by combination of the original chemical quantitative mineral analysis (CQMA) with bulk chemical analysis (XRF) and QXRD–Rietveld method with an internal standard (QXRD*). These X-ray diffraction data were used for a) identification of crystalline minerals and for the support of calculation of average oxide formula of amorphous phase for MCQMA calculation and b) for independent separated quantitative determination of crystalline (C12A7, C3A, C2S, C3S, MgO) and amorphous minerals and their comparison with data calculated by MCQMA. The advantage of the MCQMA consists also in the possibility to test separately the quality of determined phase percentages provided by MCQMA and QXRD* methods using their feedback conversion on recalculated chemical analysis and compared them with bulk chemical analysis. For the tested data, the comparison showed that both methods provided comparable results.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7

Similar content being viewed by others

Notes

  1. For CQMA calculation, crystallochemical and/or their related oxide formula coefficients of a given mineral phase are interchangeable.

  2. Regardless the value of the constant (const) in Eq. (7), the calculated OFCCaO from equation (Eq. (8)) equals to const too. For example: a) for const = 10.0 and 10CaO 4SiO2 2Al2O3, i.e., Ca10Si4Al4O24 then OFCCaO = 10.0 or b) for const = 1.00 and 1.00CaO 0.40SiO2 0.20Al2O3 i.e. Ca1.00Si0.40Al0.40O2.40 then OFCCaO = 1.00). The calculated OFCCaO = const. indicates that the different value selected for const (Eq. (7)) does not influence the ratio among the i-th oxides in OFCi and therefore the value of const in Eq. (7) does not influence the calculated wt% of phases calculated by MCQMA. This conclusion was numerically verified.

Abbreviations

CQMA:

Chemical quantitative mineral analysis

MCQMA:

Modified Chemical quantitative mineral analysis

WA:

Weighted averages

OFC:

Oxide formula coefficient

COFC:

Compiled oxide formulas coefficients

CHA:

Chemical analysis

m:

Mass of sample [g]

i:

Index indicating the i-th oxide of element

j:

Index indicating the j-th phase

k:

Index indicating the k-th phase for MCQMA or QXRD method

A, B, AB:

Labels for the sample A (laddle slag), B (blast furnace slag) or their blend AB

cr:

Crystalline phase

References

  1. Yildirim IZ, Prezzi M (2011) Chemical, mineralogical, and morphological properties of steel slag. Adv Civ Eng. https://doi.org/10.1155/2011/463638

    Article  Google Scholar 

  2. Dippenaar R (2005) Industrial uses of slag (the use and re-use of iron and steelmaking slags). Ironmak Steelmak 32:35–46. https://doi.org/10.1179/174328105X15805

    Article  Google Scholar 

  3. Kostura B, Kulveitová H, Leško J (2005) Blast furnace slags as sorbents of phosphate from water solutions. Wat Res 39:1795–1802. https://doi.org/10.1016/j.watres.2005.03.010

    Article  Google Scholar 

  4. Woolley GR, Goumans JJJM, Wainwright PJ (2000) Waste materials in construction: science and engineering of recycling for environmental protection. Elsevier Science. eBook ISBN: 9780080543659

  5. Tossavainen M, Engstrom F, Yang Q, Menad N, Lidstrom LM, Bjorkman B (2007) Characteristics of steel slag under different cooling conditions. Waste Manage 27:1335–1344. https://doi.org/10.1016/j.wasman.2006.08.002

    Article  Google Scholar 

  6. Shi C (2002) Characteristics and cementitious properties of ladle slag fines from steel production. Cem Concr Res 32:459–462. https://doi.org/10.1016/S0008-8846(01)00707-4

    Article  Google Scholar 

  7. Vlcek J, Tomkova V, Ovcacikova H, Ovcacik F, Topinkova M, Matejka V (2013) Slags from steel production: properties and their utilization. Metalurgija 52:329–333

    Google Scholar 

  8. Shi C (2004) Steel slag-Its production, processing, characteristics, and cementitious properties. J Mater Civ Eng 16:230–236. https://doi.org/10.1061/(ASCE)0899-1561(2004)16:3(230)

    Article  Google Scholar 

  9. Shi C, Krivenko DR (2003) Alkali-activated cements and concretes, 1st edn. Taylor & Francis, London

    Book  Google Scholar 

  10. Kutchko BG, Kim AG (2006) Fly ash characterization by SEM-EDS. Fuel 85:2537–2544. https://doi.org/10.1016/j.fuel.2006.05.016

    Article  Google Scholar 

  11. Wang T, Ishida T, Gu R (2020) A study of the influence of crystal component on the reactivity of low-calcium fly ash in alkaline conditions based on SEM-EDS. Constr Build Mater 243:118227. https://doi.org/10.1016/j.conbuildmat.2020.118227

    Article  Google Scholar 

  12. Valášková M (2016) Structural characteristics of cordierites based on commercial vermiculites in relation to the natural and synthetic cordierites. Ceram Silic 60:308–316. https://doi.org/10.13168/cs.2016.0046

    Article  Google Scholar 

  13. Trumbulović L, Aćimović Z, Panić S, Andrić L (2003) Synthesis and characterization of cordierite from kaolin and talc for casting application. FME Trans 31:43–47

    Google Scholar 

  14. Guo X, Shi H (2013) Modification of steel slag powder by mineral admixture and chemical activators to utilize in cement based materials. Mater Struct 46:1265–1273. https://doi.org/10.1617/s11527-012-9970-7

    Article  Google Scholar 

  15. Dinnebier RE, Billinge SJL, Garnier E (2009) Powder diffraction theory and practice. RSC Publishing, Cambridge

    Google Scholar 

  16. Rietveld HM (1967) Line profiles of neutron powder-diffraction peaks for structure refinement. Acta Crystallogr. https://doi.org/10.1107/S0365110X67000234

    Article  Google Scholar 

  17. Bish L, Post JE (1989) Modern powder diffraction. Mineralogical Society of America, Washington, DC

    Book  Google Scholar 

  18. Young RA (1995) The rietveld method. Oxford University Press, Oxford

    Google Scholar 

  19. Zhao P, Lu L, Liu X, De la Torre AG, Cheng X (2018) Error analysis and correction for quantitative phase analysis based on rietveld-internal standard method: Whether the minor phases can be ignored? Crystals 8:110. https://doi.org/10.3390/cryst8030110

    Article  Google Scholar 

  20. Chancey RT, Stutzman P, Juenger M, Fowler D (2010) Comprehensive phase characterization of crystalline and amorphous phases of a Class F fly ash. Cem Concr Res 40:146–156. https://doi.org/10.1016/j.cemconres.2009.08.029

    Article  Google Scholar 

  21. Madsen I, Scarlett N, Kern A (2011) Description and survey of methodologies for the determination of amorphous content via X-ray powder diffraction. Z. Kristallographie 226:944–955. https://doi.org/10.1524/zkri.2011.1437

    Article  Google Scholar 

  22. García-Maté M, Santacruz I, Cuesta A, León-Reina L, Aranda MAG, Baco I, Morin V, Walenta G, Gartner E, De la Torre AG (2015) Amorphous determination in calcium sulfoaluminate materials by external and internal method. Adv Cem Res 27:417–423. https://doi.org/10.1680/adcr.14.00026

    Article  Google Scholar 

  23. Leng Y (2008) Material characterization: introduction to microscopic and spectroscopic methods, 2nd edn. Wiley, Hoboken

    Book  Google Scholar 

  24. Gottlieb P, Wilkie G, Sutherland D, Ho-Tun E, Suthers S, Perera K, Jenkins B, Spencer S, Butcher JR (2000) Using quantitative electron microscopy for process mineralogy applications. JOM 52:24–25. https://doi.org/10.1007/s11837-000-0126-9

    Article  Google Scholar 

  25. Ziel R, Haus A, Tulke A (2008) Quantification of the pore size distribution (porosity profiles) in microfiltration membranes by SEM, TEM and computer image analysis. J Membr Sci 323:241–246. https://doi.org/10.1016/j.memsci.2008.05.057

    Article  Google Scholar 

  26. Hodoroaba VD, Rades S, Unger WES (2014) Inspection of morphology and elemental imaging of single nanoparticles by high resolution SEM/EDX in transmission mode. Surf Intersurf Anal 46:945–948. https://doi.org/10.1002/sia.5426

    Article  Google Scholar 

  27. Shindo D, Oikawa T (2002) Energy dispersive X-ray spectroscopy. In: Analytical electron microscopy for materials science. Springer: Tokyo, Japan.

  28. Braun GE (1986) Quantitative analysis of mineral mixtures using linear programming. Clays Clay Miner 34:330–337. https://doi.org/10.1346/CCMN.1986.0340314

    Article  Google Scholar 

  29. Hodgson M, Dudeney AWL (1984) Estimation of clay proportions in mixtures by X-Ray diffraction and computerized chemical mass balance. Clays Clay Miner 32:19–28. https://doi.org/10.1346/CCMN.1984.0320103

    Article  Google Scholar 

  30. Johnson LJ, Chu CH, Hussey GA (1985) Quantitative clay mineral analysis using simultaneous linear equations. Clays Clay Miner 33:107–117. https://doi.org/10.1346/CCMN.1985.0330204

    Article  Google Scholar 

  31. Whiten B (2007) Calculation of mineral composition from chemical assays. Miner Process Extr Metall Rev 29:83–97. https://doi.org/10.1080/08827500701257860

    Article  Google Scholar 

  32. Coelho C, Roqueiro D, Hotza D (2002) Rational mineralogical analysis of ceramics materials. Mater Lett 52:394–398. https://doi.org/10.1016/S0167-577X(01)00429-3

    Article  Google Scholar 

  33. Klika Z, Kolomazník I, Matýsek D, Kliková Ch (2016) Critical evaluation of a new method for quantitative determination of minerals in solid samples. Cryst Res Technol 51:249–264. https://doi.org/10.1002/crat.201500214

    Article  Google Scholar 

  34. Valášková M, Klika Z, Novosad B, Smetana B (2019) Crystallization and quantification of crystalline and non-crystalline phases in kaolin-based cordierites. Materials 12:3104. https://doi.org/10.3390/ma12193104

    Article  Google Scholar 

  35. Klika Z, Valášková M, Bartoňová L, Maierová P (2020) Quantitative evaluation of crystalline and amorphous phases in clay-based cordierite. Minerals 10:1122. https://doi.org/10.3390/min10121122

    Article  Google Scholar 

  36. Madsen IC, Scarlett NVY, Cranswick LMD, Lwin T (2001) Outcomes of the international union of crystallography commission on powder diffraction round robin on quantitative phase analysis: samples 1a to 1h. J Appl Crystallogr 34:409–426. https://doi.org/10.1107/S0021889801007476

    Article  Google Scholar 

  37. Scarlett NVY, Madsen IC, Cranswick LMD, Lwin T, Groleau E, Stephenson G, Aylmore M, Agron-Olshina N (2002) Outcomes of the international union of crystallography commission on powder diffraction round robin on quantitative phase analysis: samples 2, 3, 4, synthetic bauxite, natural granodiorite and pharmaceuticals. J Appl Crystallogr 35:383–400. https://doi.org/10.1107/S0021889802008798

    Article  Google Scholar 

Download references

Acknowledgements

This work was supported by the Ministry of Education, Youth and Sports of the Czech Republic under Project No. [CZ.02.1.01/0.0/0.0/17_049/0008426].

Author information

Authors and Affiliations

  1. Department of Chemistry and Physico-Chemical Processes, Faculty of Materials Science and Technology, VŠB-Technical University of Ostrava, 17. Listopadu 15, Ostrava-Poruba, 708 00, Czech Republic

    Zdeněk Klika, Lucie Bartoňová, Bruno Kostura & Jana Dobrovská

  2. Department of Thermal Engineering, Faculty of Materials Science and Technology, VŠB-Technical University of Ostrava, 17. Listopadu 15, Ostrava-Poruba, 708 00, Czech Republic

    Petra Maierová & Jozef Vlček

  3. Department of Geological Engineering, Faculty of Mining and Geology, VŠB-Technical University of Ostrava, 17. Listopadu 15, Ostrava-Poruba, 708 00, Czech Republic

    Dalibor Matýsek

  4. Liberty Ostrava a.s., Vratimovská 689/117, 719 00, Ostrava–Kunčice, Czech Republic

    Jiří Krčmář

Authors
  1. Zdeněk Klika
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Lucie Bartoňová
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Bruno Kostura
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Petra Maierová
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Jozef Vlček
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. Jana Dobrovská
    View author publications

    You can also search for this author in PubMed Google Scholar

  7. Dalibor Matýsek
    View author publications

    You can also search for this author in PubMed Google Scholar

  8. Jiří Krčmář
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Bruno Kostura.

Ethics declarations

Conflict of interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

Additional information

Publisher's Note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Klika, Z., Bartoňová, L., Kostura, B. et al. Critical evaluation of quantitative determination of minerals in slags by a new MCQMA and QXRD methods. Mater Struct 55, 246 (2022). https://doi.org/10.1617/s11527-022-02069-6

Download citation

  • Received:

  • Accepted:

  • Published:

  • DOI: https://doi.org/10.1617/s11527-022-02069-6

Keywords

Search

Navigation