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{{Short description|Calcium chloroaluminate formed by reaction of AFm hydrates with chloride ions}}
{{more footnotes|date=November 2012}}
<!-- To add extra fields, see Template:Chembox new --> <!-- To add extra fields, see Template:Chembox new -->
{{chembox {{chembox
| verifiedrevid = 403090628 | verifiedrevid = 441837457
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Calcium aluminium chlorohydroxide <br /> Calcium aluminium chlorohydroxide <br />
Calcium aluminium oxychloride Calcium aluminium oxychloride
| Section1 = {{Chembox Identifiers |Section1={{Chembox Identifiers
| CASNo = | CASNo =
| PubChem = | PubChem =
| SMILES = }} | SMILES = }}
| Section2 = {{Chembox Properties |Section2={{Chembox Properties
| Formula = Ca<sub>2</sub>Al(OH)<sub>6</sub>(Cl,&nbsp;OH)&nbsp;·&nbsp;2&nbsp;H<sub>2</sub>O | Formula = {{chem2|Ca2Al(OH)6(Cl, OH) * 2 H2O}}
| MolarMass = | MolarMass =
| Appearance = White solid | Appearance = White solid
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| Solubility = }} | Solubility = }}
| Section3 = {{Chembox Hazards |Section3={{Chembox Hazards
| MainHazards = | MainHazards =
| FlashPt = | FlashPt =
| Autoignition = }} | AutoignitionPt = }}
}} }}


'''Friedel's salt''' is an ] mineral belonging to the family of the ] (LDHs). It has affinity for anions as chloride and iodide and is capable to retain them to a certain extent in its crystallographical structure. '''Friedel's salt''' is an ] mineral belonging to the family of the ] (LDHs). It has affinity for anions as chloride and iodide and is capable of retaining them to a certain extent in its crystallographical structure.


==Composition== == Composition ==
Friedel's salt is a ] (LDH) of general formula:


:{{chem2|Ca2Al(OH)6(Cl, OH) * 2 H2O}}
Friedel's salt general formula is:


or more explicitly for a positively-charged LDH mineral:
:Ca<sub>2</sub>Al(OH)<sub>6</sub>(Cl,&nbsp;OH)&nbsp;·&nbsp;2&nbsp;H<sub>2</sub>O.


:{{nowrap|<sup>+</sup>&nbsp;&nbsp;(Cl<sup>–</sup>,&nbsp;OH<sup>–</sup>)&nbsp;·&nbsp;2&nbsp;H<sub>2</sub>O}}
In the ], considering that


or by directly incorporating water molecules into the Ca,Al hydroxide layer:
:2&nbsp;OH<sup>–</sup>&nbsp;↔&nbsp;O<sup>2–</sup>&nbsp;+&nbsp;H<sub>2</sub>O,


:{{nowrap|<sup>+</sup>&nbsp;&nbsp;(Cl<sup>–</sup>,&nbsp;OH<sup>–</sup>)}}
and doubling all the stoichiometry, it can also be written as follows:


where ] and ] anions occupy the interlayer to compensate the excess of positive charges.
:3CaO·Al<sub>2</sub>O<sub>3</sub>·CaCl<sub>2</sub>&nbsp;·&nbsp;10&nbsp;H<sub>2</sub>O


In the ] (CCN), considering that
Friedel's salt can also be considered as an ] in which chloride ions have replaced sulfate ions and is formed in cements initially rich in ] (C<sub>3</sub>A).


:2 Cl<sup>-</sup> + 3CaO·Al<sub>2</sub>O<sub>3</sub>·CaSO<sub>4</sub>&nbsp;·&nbsp;10&nbsp;H<sub>2</sub>O &nbsp;&nbsp;→&nbsp;&nbsp; 3CaO·Al<sub>2</sub>O<sub>3</sub>·CaCl<sub>2</sub>&nbsp;·&nbsp;10&nbsp;H<sub>2</sub>O + SO<sub>4</sub><sup>2-</sup> :{{nowrap|2&nbsp;OH<sup>−</sup>&nbsp;{{eqm}}&nbsp;O<sup>2−</sup>&nbsp;+&nbsp;H<sub>2</sub>O,}}


and doubling all the stoichiometry, it could also be written in CCN as follows:
It plays a main role in the retention of chloride anions in cement and concrete. However, Friedel's salt remains a poorly understood phase in the CaO-Al<sub>2</sub>O<sub>3</sub>-CaCl<sub>2</sub>-H<sub>2</sub>O system, and is critical for the stability of salt-saturated Portland cement-based grouts.


:{{chem2|3CaO*Al2O3*Ca(O,Cl2) * 11 H2O}}
==Discovery==


A simplified chemical composition with only Cl<sup>–</sup> in the interlayer, and without OH<sup>–</sup>, as:
Nowadays, Friedel's salt discovery is relatively difficult to trace back from the recent literature, simply because it is an ancient finding of a poorly known and non-natural product. It has been synthesised and identified in 1897 by ], mineralogist and crystallographer, son of the famous French chemist ].<ref name="Friedel1897">{{cite journal | url = http://www.archive.org/stream/bulletindelasoc16mingoog/bulletindelasoc16mingoog_djvu.txt | first = Georges | last = Friedel | title = Sur un chloro-aluminate de calcium hydrate´ se maclant par compression | journal = Bulletin de la Société française de minéralogie et de cristallographie | volume = 19 | year = 1897 | pages = 122&ndash;136}}</ref> Georges Friedel also synthesised ] (1903) in the framework of his work on the ]s theory (twin crystals). This point requires further verification.{{Citation needed|date=October 2008}}<ref name="Ref_"></ref>
:{{nowrap|Ca<sub>2</sub>Al(OH)<sub>6</sub>(Cl)&nbsp;·&nbsp;2&nbsp;H<sub>2</sub>O}}
can be also written in cement chemist notation as:<ref name="mindata">{{Cite web |title=Friedel's Salt |author= |work=mindat.org |date= |access-date=24 February 2021 |url= https://www.mindat.org/min-43838.html}}</ref>
:{{chem2|3CaO*Al2O3*CaCl2 * 10 H2O}}


Friedel's salt is formed in cements initially rich in ] (C<sub>3</sub>A). Free-chloride ions directly bind with the AFm hydrates (C<sub>4</sub>AH<sub>13</sub> and its derivatives) to form Friedel's salt.
==Formation==


== Importance of chloride binding in AFm phases ==
* Relation with ].
{{See also|AFm phases|Layered double hydroxides}}
* Incorporation of chloride.
Friedel's salt plays a main role in the binding and retention of chloride anions in cement and concrete. However, Friedel's salt remains a poorly understood phase in the CaO–Al<sub>2</sub>O<sub>3</sub>–CaCl<sub>2</sub>–H<sub>2</sub>O system. A sufficient understanding of the Friedel's salt system is essential to correctly model the reactive transport of chloride ions in reinforced concrete structures affected by chloride attack and steel reinforcement corrosion. It is also important to assess the long-term stability of salt-saturated Portland cement-based grouts to be used in engineering structures exposed to seawater or concentrated brine as it is the case for radioactive waste disposal in deep salt formations.
* Solid solutions.


Another reason to study ] and the Friedel's salt system is their tendency to bind, trap and to immobilise toxic anions, such as {{chem2|B(OH)4-}}, {{chem|SeO|3|2−}}, and {{chem|SeO|4|2−}}, or the long-lived radionuclide <sup>129</sup>I<sup>−</sup>, in cementitious materials. Their characterization is important to conceive anion getters and to assess the retention capacity of cementitious buffer and concrete barriers used for radioactive waste disposal.
==Role in cement==


== Chloride sorption and anion exchange in AFm phases ==
* Importance for the reactive transport of chloride in cement in relation with corrosion of steel reinforcement.
{{See also|AFm phases|Layered double hydroxides}}
Friedel's salt could be first tentatively represented as an ] in which two chloride ions would have simply replaced one sulfate ion. This conceptual representation based on the intuition of a simple stoichiometric exchange is very convenient to remind but such a simple mechanism likely does not directly occur and must be considered with caution:


:{{nowrap|2 Cl<sup>−</sup> + 3CaO·Al<sub>2</sub>O<sub>3</sub>·CaSO<sub>4</sub>&nbsp;·&nbsp;11&nbsp;H<sub>2</sub>O &nbsp;&nbsp;→&nbsp;&nbsp; 3CaO·Al<sub>2</sub>O<sub>3</sub>·CaCl<sub>2</sub>&nbsp;·&nbsp;11&nbsp;H<sub>2</sub>O + {{chem|SO|4|2−}}}}
==Anion getter==


Indeed, the reality appears to be more complex than such a simple stoichiometric exchange between chloride and sulfate ions in the AFm crystal structure. In fact, it seems that chloride ions are electrostatically sorbed onto the positively charged <sup>+</sup> layer of AFm hydrate, or could also exchange with hydroxide ions (OH<sup>–</sup>) also present in the interlayer. So, the simple and "apparent" exchange reaction first presented here above for the sake of ease does not correspond to the reality and is an oversimplified representation.<ref name="Suryavanshi1996">{{cite journal|last1=Suryavanshi|first1=A.K.|last2=Scantlebury|first2=J.D.|last3=Lyon|first3=S.B.|title=Mechanism of Friedel's salt formation in cements rich in tri-calcium aluminate|journal=Cement and Concrete Research|volume=26|issue=5|year=1996|pages=717–727|issn=0008-8846|doi=10.1016/S0008-8846(96)85009-5}}</ref>
* Trap toxic anions in cement such as, ''e.g.'', <sup>129</sup>I<sup>-</sup>, SeO<sub>3</sub><sup>2-</sup>, SeO<sub>4</sub><sup>2-</sup>


Similarly, Kuzel’s salt could seem to be formed when only 1 Cl<sup>–</sup> ion exchanges with {{sfrac|1|2}} {{chem|SO|4|2−}} in AFm (half substitution of sulfate ions):<ref name="Mesbah2011">{{cite journal|last1=Mesbah|first1=Adel|last2=François|first2=Michel|last3=Cau-dit-Coumes|first3=Céline|last4=Frizon|first4=Fabien|last5=Filinchuk|first5=Yaroslav|last6=Leroux|first6=Fabrice|last7=Ravaux|first7=Johann|last8=Renaudin|first8=Guillaume|title=Crystal structure of Kuzel's salt 3CaO·Al<sub>2</sub>O<sub>3</sub>·½CaSO<sub>4</sub>·½CaCl<sub>2</sub>·11H<sub>2</sub>O determined by synchrotron powder diffraction|journal=Cement and Concrete Research|volume=41|issue=5|year=2011|pages=504–509|issn=0008-8846|doi=10.1016/j.cemconres.2011.01.015}}</ref>
==See also==


:{{nowrap|1 Cl<sup>−</sup> + 3CaO·Al<sub>2</sub>O<sub>3</sub>·CaSO<sub>4</sub> · 11 H<sub>2</sub>O &nbsp;&nbsp;→&nbsp;&nbsp; 3CaO·Al<sub>2</sub>O<sub>3</sub>·{{sfrac|1|2}}CaSO<sub>4</sub>·{{sfrac|1|2}}CaCl<sub>2</sub> · 11 H<sub>2</sub>O + {{sfrac|1|2}} {{chem|SO|4|2−}}}}

Glasser ''et al.'' (1999) proposed to name this half-substituted salt in honor of his discoverer: ].<ref name="Glasser1999">{{cite journal | last1 = Glasser | first1 = F.P. | last2 = Kindness | first2 = A. | last3 = Stronach | first3 = S.A. | date = June 1999 | title = Stability and solubility relationships in AFm phases | journal = Cement and Concrete Research | volume = 29 | issue = 6 | pages = 861–866 | issn = 0008-8846 | doi = 10.1016/S0008-8846(99)00055-1 | pmid = | url = https://www.sciencedirect.com/science/article/abs/pii/S0008884699000551}}</ref>

However, Mesbah et al. (2011) have identified two different types of interlayers in the crystallographic structure they have determined and it precludes the common anion exchange reaction presented here above as stated by the authors themselves in their conclusions:<ref name="Mesbah2011" />

<blockquote>Kuzel's salt is a two-stage layered compound with two distinct interlayers, which are alternatively filled by chloride anions only (for one kind of interlayer) and by sulfate anions and water molecules (for the other kind of interlayer). Kuzel's salt structure is composed of the perfect intercalation of the Friedel's salt structure and the monosulfoaluminate structure (the two end-members of the studied bi-anionic AFm compound). The structural properties of Kuzel's salt explain the absence of extended chloride to sulfate or sulfate to chloride substitution.<br />
The staging feature of Kuzel's salt certainly explains the difficulties to substitute chloride and sulfate: the modification in one kind of interlayer involves a modification in the other kind of interlayer in order to preserve the electroneutrality of the compound. The two-stage feature of Kuzel's salt implies that each interlayer should be mono-anionic. </blockquote>

So, if the global chemical composition of Friedel's salt and Kuzel's salt corresponds well respectively with the stoichiometry of a complete substitution, or a half substitution, of sulfate ions by chloride ions in the crystal structure of AFm, it does not tell directly anything on the exact mechanism of anion substitution in this complicated system. Only detailed and well controlled chloride sorption, or anion exchange, experiments with a complete analysis of all the dissolved species present in aqueous solution (also including OH<sup>–</sup>, Na<sup>+</sup> and Ca<sup>2+</sup> ions) can decipher the system.

== Discovery ==
Friedel's salt discovery is relatively difficult to trace back from the recent literature, simply because it is an ancient finding of a poorly known and non-natural product. It has been synthesised and identified in 1897 by ], mineralogist and crystallographer, son of the famous French chemist ].<ref name="Friedel1897">{{cite journal | last1 = Friedel | first1 = Georges | date = 1897 | title = Sur un chloro-aluminate de calcium hydraté se maclant par compression | journal = Bulletin de la Société Française de Minéralogie et de Cristallographie | volume = 19 | pages = 122–136 | url = https://archive.org/stream/bulletindelasoc16mingoog/bulletindelasoc16mingoog_djvu.txt}}</ref> Georges Friedel also synthesised calcium aluminate (1903) in the framework of his work on the ]s theory (twin crystals). This point requires further verification.{{Citation needed|date=October 2008}}<ref name="Ref_"></ref>

== Formation ==
* Relation with ].
* Incorporation of chloride.
* Solid solutions.

== See also ==
* ]
* ] * ]
* ] * ]
** ], a mixture of general formula: Mg<sub>4</sub>Cl<sub>2</sub>(OH)<sub>6</sub> ** ], a mixture of general formula: Mg<sub>4</sub>Cl<sub>2</sub>(OH)<sub>6</sub>
** ], a french engineer who made a new form of cement from a combination of ] and ] ** ], a French engineer who made a new form of cement from a combination of ] and ]
* ] * ]
** ], also known as ''salzbeton'' ** ], also known as ''salzbeton''
Line 79: Line 109:
* ] * ]
* ] * ]
* ], a rich lineage of French scientists:

<br />
* ], a rich lineage of French scientists:
** ] (1832–1899), French chemist known for the ] ** ] (1832–1899), French chemist known for the ]
** ] (1865–1933), here above mentioned, French crystallographer and mineralogist; son of Charles ** ] (1865–1933), here above mentioned, French crystallographer and mineralogist; son of Charles
** (1895–1972), French Polytechnician and mining engineer, founder of ], the French geological survey; son of Georges ** (1895–1972), French Polytechnician and mining engineer, founder of ], the French geological survey; son of Georges
** ], (1921-), French physicist; son of Edmond, see the French site for ] ** ], (1921-2014), French physicist; son of Edmond, see the French site for ]


==References== == References ==
{{Reflist}}


== Further reading ==
<references/>
{{Refbegin}}
* {{Cite journal * {{Cite journal
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| title = Chloride ingress and strength loss in concrete with different PC–PFA–MK binder compositions exposed to synthetic seawater | title = Chloride ingress and strength loss in concrete with different PC–PFA–MK binder compositions exposed to synthetic seawater
| journal = Cement and Concrete Research | journal = Cement and Concrete Research
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| last = Barberon | last = Barberon
| first = F. | first = F.
| coauthors = V. Baroghel-Bouny, H. Zanni, B. Bresson, J. B. d'Espinose de la Caillerie, L. Malosse, Z. Gan | author2 = V. Baroghel-Bouny |author3=H. Zanni |author4=B. Bresson |author5=J. B. d'Espinose de la Caillerie |author6=L. Malosse |author7=Z. Gan
| year = 2005 | date = 2005
| title = Interactions between chloride and cement-paste materials | title = Interactions between chloride and cement-paste materials
| journal = Magnetic Resonance Imaging | journal = Magnetic Resonance Imaging
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| doi = 10.1016/j.mri.2004.11.021 | doi = 10.1016/j.mri.2004.11.021
| pmid = 15833625 | pmid = 15833625
| url = https://hal.archives-ouvertes.fr/hal-02362421/file/FC2.pdf
}} }}


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| last = Birnin-Yauri | last = Birnin-Yauri
| first = U. A. | first = U. A.
| coauthors = F. P. Glasser | author2=F. P. Glasser
| year = 1998 | date = 1998
| title = Friedel's salt, Ca<sub>2</sub> Al(OH)<sub>6</sub> (Cl, OH) · 2H<sub>2</sub>O: its solid solutions and their role in chloride binding | title = Friedel's salt, Ca<sub>2</sub> Al(OH)<sub>6</sub> (Cl, OH) · 2H<sub>2</sub>O: its solid solutions and their role in chloride binding
| journal = Cement and Concrete Research | journal = Cement and Concrete Research
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| last = Bothe | last = Bothe
| first = James V. | first = James V.
| coauthors = Paul W. Brown | author2=Paul W. Brown
| date = 2004-06 | date = June 2004
| title = PhreeqC modeling of Friedel's salt equilibria at 23 ± 1 °C | title = PhreeqC modeling of Friedel's salt equilibria at 23 ± 1 °C
| journal = Cement and Concrete Research | journal = Cement and Concrete Research
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| issue = 6 | issue = 6
| pages = 1057–1063 | pages = 1057–1063
| accessdate = 2008-10-04
| url = http://www.sciencedirect.com/science/article/B6TWG-4B94K0R-1/2/2182af1335b6bdcd0a4cecc34f70d7f7
}} }}


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* {{Cite journal
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* {{Cite journal| last1 = Mesbah| first1 = Adel| last2 = Cau-dit-Coumes| first2 = Céline| last3 = Frizon| first3 = Fabien| last4 = Leroux| first4 = Fabrice| last5 = Ravaux| first5 = Johann| last6 = Renaudin| first6 = Guillaume| date = 2011| title = A new investigation of the Cl<sup>−</sup>–CO<sub>3</sub><sup>2−</sup> substitution in AFm phases| journal = Journal of the American Ceramic Society| volume = 94| issue = 6| pages = 1901–1910| doi = 10.1111/j.1551-2916.2010.04305.x| issn = 1551-2916| url = https://onlinelibrary.wiley.com/doi/abs/10.1111/j.1551-2916.2010.04305.x}}

* {{Cite journal| last1 = Mesbah| first1 = Adel| last2 = Cau-dit-Coumes| first2 = Céline| last3 = Renaudin| first3 = Guillaume| last4 = Frizon| first4 = Fabien| last5 = Leroux| first5 = Fabrice| date = 2012-08-01| title = Uptake of chloride and carbonate ions by calcium monosulfoaluminate hydrate| journal = Cement and Concrete Research| volume = 42| issue = 8| pages = 1157–1165| doi = 10.1016/j.cemconres.2012.05.012| issn = 0008-8846| url = https://www.sciencedirect.com/science/article/pii/S0008884612001299}}

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{{Refend}}


==External links== == External links ==
* *
* *


{{DEFAULTSORT:Friedel's Salt}} {{DEFAULTSORT:Friedel's Salt}}
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Friedel's salt: Difference between revisions Add topic