Chemically bound water as measure of degree of hydration: method and potential errors

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1 Chemially bound ater as measure of degree of hydration: method and potential errors Fagerlund, Göran Published: Link to publiation Citation for published version (APA): Fagerlund, G. (29). Chemially bound ater as measure of degree of hydration: method and potential errors. (Report TVBM; Vol. 315). Division of Building Materials, LTH, Lund University. General rights Copyright and moral rights for the publiations made aessible in the publi portal are retained by the authors and/or other opyright oers and it is a ondition of aessing publiations that users reognise and abide by the legal requirements assoiated ith these rights. Users may doload and print one opy of any publiation from the publi portal for the purpose of private study or researh. You may not further distribute the material or use it for any profit-making ativity or ommerial gain You may freely distribute the URL identifying the publiation in the publi portal L UNDUNI VERS I TY PO Box L und

2 LUND INSTITUTE OF TECHNOLOGY LUND UNIVERSITY Division of Building Materials CHEMICALLY BOUND WATER AS MEASURE OF DEGREE OF HYDRATION Method and potential errors Göran Fagerlund Report TVBM-315 Lund 29

3 ISRN LUTVDG/TVBM--9/315--SE(1-27) ISSN TVBM Lund Institute of Tehnology Telephone: Division of Building Materials Telefax: Box 118.byggnadsmaterial.lth.se SE-221 Lund, Seden

4 Content INTRODUCTION.. 1 I: CEMENT PASTE.. 2 I:1 Definition of degree of hydration of pure portland ement.. 2 I:2 Experimental determination of degree of hydration. 3 I:2.1 Without orretions. 3 I:2.2 Corretion for pre-hydrated ( moisture-damaged ) ement. 4 I:2.3 Corretion for limestone filler mixed in ement.. 6 I:2.4 Corretion for arbonation 9 II: CONCRETE. 14 REFERENCES. 17 APPENDIX 1: EFFECTS OF THE DRYING PROCEDURE. 18 Error ourring during preparation of the 18 Effets of the drying proedure before ignition. 19 Referenes. 24 APPENDIX 2: EFFECTS OF REACTIVE MINERAL ADMIXTURES.. 25

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6 1 INTRODUCTION Degree of hydration is defined as the fration of portland linker (inluding gypsum addition) that has fully reated ith ater. In this report, degree of hydration is assumed to be diretly proportional to the amount of hemially bound ater. Thus, it is assumed that a ertain quantity of portland linker binds exatly the same amount of ater, may it be at the beginning of the hydration proess, or at the end of this. All hemially bound ater is assumed to be lost at igniting the to 1 ºC. No hemially bound ater is assumed to be lost at heating to +15 ºC. The degree of hydration is therefore determined by eighing the after drying to +15 ºC and after ignition to 1 ºC. The eight differene orresponds to the hemially bound ater ontent. The ement may ontain omponents, other than ement linker, that loose eight at ignition, for example limestone filler that ontains bound CO 2 hih leaves the after +15 ºC, but before 1 ºC. The linker may be partly pre-hydrated (moisture damaged) hen the is manufatured. Water in pre-hydrated ement shall not be inluded in the determination of degree of hydration. The may be more or less arbonated. CO 2 from a arbonated ement is released at ignition and must be distinguished from hemially bound ater in ement. Aggregate in onrete may ontain rystal ater that is released at ignition. This ater shall not be inluded in the alulation of degree of hydration. Ways of making orretions for these potential soures of error are given in the report. The ay of defining the dryness of the before ignition has big influene on the measured amount of hemially bound ater. The more intense the drying, the loer is the measured amount of hemially bound ater. In this report, dryness is defined as the eight at equilibrium at drying at +15 ºC. Instead of drying at +15 ºC, drying an be made by exposing the to air of very lo relative humidity. The effet of the drying proedure is disussed in APPENDIX 1. For ement ontaining mineral admixtures like silia fume, hemially bound ater in reation produts from the mineral admixture might be dereased ith time, despite the fat that hydration proeeds. A method of ompensating for this effet hen alulating the degree of hydration of the portland omponent in the ement is disussed in APPENDIX 2.

7 2 I: CEMENT PASTE Only portland ement paste, ith or ithout mixed-in inert filler, is onsidered. When the ement ontains reative mineral admixtures, like silia fume, fly ash or blastfurnae slag, hemial reations ill our that atually ause a gradual redution in the loss on ignition ith inreased degree of hydration. In these ases, one annot use the amount of hemially bound ater as a measure of degree of hydration. The same restrition is valid if suh materials are mixed into onrete. The question is treated briefly in APPENDIX 2. I:1 Definition of degree of hydration of pure portland ement paste Degree of hydration is defined as the fration of ement that has fully reated ith ater relative to the total amount of ement in the. In the total ement ontent is not inluded the part of ement that as pre-hydrated hen the ement paste as mixed. In the laboratory the amount of non-evaporable ater ontent of the ement paste, n,, is determined by drying, folloed by ignition of the same. If the amount of ement in the is kno the relation alulated. This relation is a measure of the degree of hydration. / n, an be The ement ontent in a ontaining no air pores an be alulated from the ement ontent C (kg/m 3 ) and the speimen volume V (m 3 ) provided the ater ement ratio / is kno: C V 1 V.32 / (I.1) Where the oeffiient.32 is the speifi volume of ement (m 3 /g). The degree of hydration α of the is found by dividing n, ith the amount of nonevaporable ater in the same hen this is fully hydrated, ( ). n (I.2a) ( n, n ) A general expression for degree of hydration is:, (I.2b) here is the hemially bound ater at omplete hydration of the ement quantity. o n The quotient n / varies beteen about.18 and.26 depending on the omposition of the ement; [1]. Often the value.25 is used.

8 3 I:2 Experimental determination of degree of hydration I:2.1 Without orretions. A blok diagram over hydrated ement paste is sho in Fig.I.1. eight W d n, W i Figure I.1: Components in hydrated ement paste. The amount of hemially bound ater is obtained by drying effetive enough that all evaporable ater is released. Thereafter ignition at 1 ºC n W W here W d is the eight after drying, and W i is the eight after ignition (I.3) d i For pure ement paste the eight after ignition is the same as the ement ontent in the, : Wi (I.4) Thus, the degree of hydration is obtained by the folloing equation, see Eq. (I.2b): Wd (I.5) The assumptions behind this equation are; (1) the ement is not pre-hydrated at mixing, (2) the ement has no inlusion of limestone filler, (3) the is not arbonated. If these onditions are not valid, orretions aording to paragraphs I:2.2 to I:2.4 must be made. Gypsum added to the ement linker in onnetion ith grinding of this (about 5 eight-%) is inluded in the onept ement, i.e. it is inluded in the parameters and as they are used in the equations above. At alulation of the amount of hemially bound ater, the dry eight, W d, i.e. the eight before ignition, must be ell-defined. The dry eight depends on the method of drying the. Also the quotient n /, hih is used in the definition of degree of hydration depends on the drying method. The effet of drying method is disussed in APPENDIX 1.

9 4 Example The dry eight of a is 13 g. After ignition the eight is 83 g. The ratio atual ement is.24. n / of the The degree of hydration of the is: I:2.2 Corretion for pre-hydrated ( moisture-damaged ) ement The proedure desribed above requires that the loss on ignition of the ement before mixing is kno, sine this shall not be inluded in n. The loss on ignition of the ement before mixing is determined by drying and igniting a ement. The loss on ignition is found to be. n, / A blok diagram of a ement paste made ith moisture-damaged ement is sho in Figure I.2. eight W d W i n, (Δ n, /) Figure I.1: Components in a ement paste hen the ement as pre-hydrated before mixing. After orretion, n for a given is obtained by the folloing equation: n, n, Wd Wi (I.6) Insertion in Eq. (I.4) gives:,, Wd 1 (I.7) At alulation of the degree of hydration the part of the ement that as pre-hydrated at mixing must be exluded. The residual ( effetive ) ement ontent in the is: n, n,, efff 1 (I.8) n n

10 5 Aording to Eq. (I.2b) the degree of hydration is: n,, eff (I.9) Example The loss on ignition of a ertain ement is determined for a ement ith dry eight 5 g. After ignition the eight is 48 g. This is the effetive ement. The residual 2 g an be regarded as inert filler. The loss on ignition Δ n, / is (5-48)/5=.4 g/g ement. The on hih n, shall be determined has the dry eight 12 g. After ignition the eight is 12 g. Aording to Eq (I.7) n, beomes: 12 12(1.4) 13.9 g n, If no orretion as made the erroneous estimation of n ould be: g n, The ratio n / for the atual ement is assumed to be.23. Aording to Eq. (I.8) the effetive ement ontent is:.4, eff g.23 The true degree of hydration is, aording to Eq. (I.9): Was no orretion made, the folloing degree of hydration had been obtained: Therefore, the error in alulated degree of hydration is big also hen the ement has fairly limited pre-hydration.

11 6 I:2.3 Corretion for limestone filler mixed in ement Many ements ontain limestone filler. Examples from Seden are: CEM II/A-V (Sedish name Byggement ): about eight-% (Aording to the European ement standard, 25% is alloed) CEM I rapid hardening (Sedish name SH-ement ): about 4 eight-% CEM I moderate heat of hydration (Sedish name Anläggningsement : about 4 eight-% (% until April 29) CO 2 is leaving the limestone filler at ignition. 1 mole limestone, CaCO 3 (1 g) releases 1 mole CO 2 (44 g). Corretion for this must be made at alulation of n. In the further alulations it is assumed that the filler is inert and that it does not bind ater hemially. It is assumed that the ement is not pre-hydrated. A blok diagram over the omponents in a ement paste ontaining limestone filler is sho in Figure I.3. eight W d n, W i ΔCO 2 g C,eff Figure I.3: Components in ement paste ontaining limestone filler in the ement. The ement is assumed to ontain g eight-% limestone. The eight loss at ignition of the limestone in ement is: 44 CO g. g (I.1) The amount of ement in the (inluding limestone filler) is: W CO 44 i 2 Wi. g (I.11) Re-distribution of terms gives: Wi 1.44 g (I.12)

12 7 The amount of hemially bound ater is: W W (I.13) n, d i CO 2 Insertion of Eq. (I.1) gives: n, Wd Wi. 44 g (I.14) Insertion of Eq. (I.12) gives after simplifiation:.44 g, Wd Wi 1 (I.15) 1.44 g The effetive ement ontent in the used for alulation of the degree of hydration of the limestone-free ( pure ) ement is: Wi, eff 1 g 1 g (I.16) 1.44 g The degree of hydration of the limestone-free ement is obtained from:,, eff (I.17) Example. Cement ith 12 eight-% limestone filler A ement paste has the eight 12 g after drying and 97 g after ignition. The ratio n / for the linker (inl. gypsum) in the ement is.25. Aording to Eq. (I.15) the amount of hemially bound ater is: n, Aording to Eq. (I.16) the effetive ement ontent is: ( ) , eff 9. 1 g The degree of hydration of the linker part of the ement (inl. gypsum) is aording to Eq. (I.17): g

13 8 If the limestone filler as negleted, both hen it onerns ignition, as hen it onerns the effetive ement ontent, the degree of hydration had been alulated as: The error made hen the loss on ignition of the limestone is negleted is therefore very big. The same example, but loer filler ontent (4 eight-%) A ement paste has the eight 12 g after drying and 97 g after ignition. The ratio n / for the linker (inl. gypsum) in the ement is.25. Aording to Eq. (I.15) the amount of hemially bound ater is: n, Aording to Eq. (I.16) the effetive ement ontent is: , eff (1.4) g The degree of hydration of the linker part of the ement (inl. gypsum) is aording to Eq. (I.17): If the limestone filler as negleted, both hen it onerns ignition, as hen it onerns the effetive ement ontent, the degree of hydration had been alulated as: g The error made hen the loss on ignition of the limestone is negleted is therefore smaller at the loer limestone ontent.

14 9 I:2.4 Corretion for arbonation In the alulations belo it is assumed that pure portland ement is used. Thus, no orretion for loss on ignition of limestone filler is made. Furthermore, it is assumed that the ement is not pre-hydrated hen the paste is mixed. A blok diagram over arbonated ement paste is sho in Figure I.4. eight W d n, n,,unorr W i W CO2 Figur I.4: Components in arbonated ement paste. The density inreases hen ement paste arbonates. Carbon dioxide bound at arbonation is released at ignition of the paste. Thus, it ill be inluded in eight W d but not in W i hen Eq (I.3) is used for alulating the amount of hemially bound ater ontent, n,. Consequently, if arbonation is negleted, the degree of hydration alulated by Eq. (I.2b) ill be too high. The unorreted value of n, is: W W W (I.18) n,, unorr d i n CO2 here W CO2 is the eight of bound arbon dioxide in the. All alium ompounds in ement paste exept un-hydrated ement an arbonate. The amount of ement that is transformed to solid ement hydration produts during hydration is (hemially bound ater is exluded sine it does not ontain CaO): W aterfree solid (I.19) Inserting Eq. (I.2b) gives:,, Waterfree solid (I.2) here the parameter n / depends on the omposition of the portland linker

15 1 The eight fration CaO in un-hydrated ement, and therefore also in solid hydration produts (exept hydration ater), is assumed to be x. For ordinary Portland ements x is of the order.65 (65 eight-%). 1 mole CaO (56 g) reats ith 1 mole CO 2 (44g) to form 1 mole of CaCO 3 (1g). 1% arbonation Complete arbonation of all alium in the gel gives the folloing eight inrease of the ement paste: W 44, 2 x Waterfree solid x.79 Waterfree solid x. 79 (I.21) 56 CO Therefore, aording to Eq. (I.18) the orreted value of n, is:,,,,, unorr x.79 Wd Wi x. 79 (I.22) Re-distribution of terms gives the folloing expression for the amount of hemially bound ater: Wd Wi, (I.23) x The degree of hydration is: n, (I.2b) Inomplete arbonation The most rapidly arbonating mineral (exept for the small amount of Na 2 O and K 2 O also present in hydration produts) is Ca(OH) 2 (alium hydroxide) formed at ement reation. The amount of alium hydroxide in a normal portland ement is about 3 eight-% of the total solid hydration produts (hydration ater exluded). Besides alium hydroxide the solid hydration produts also ontain hydrates of the linker ompounds C 3 S, C 2 S, C 3 A, C 4 AF. These hydration produts an also arbonate hih is demonstrated by Figure I.5. At the surfae the quotient beteen CO 2 and CaO is about.6 to.7. Had only alium hydroxide arbonated, the expeted quotient should have been about.2 orresponding to a degree of hydration of about.7.

16 11 The fration of CaO in the solid reation produts that has arbonated is assumed to be y. Then, the eight inrease of the ement paste aused by arbonation is; f. Eq. (I.21): W, 2 x y. 79 (I.24) CO The true amount of hemially bound ater is; f. Eq. (I.23): Wd Wi, (I.25) x y The degree of hydration is given by Eq. (I.2b): Example: Completely arbonated ement paste A ement paste ontaining 2 g portland ement is fully arbonated. The CaO ontent in the atual ement is 65%. The dry eight of the is 31 g. The eight after ignition is the same as the ement ontent, 2 g. The parameter n / is supposed to be.25. The amount of hemially bound ater is; Eq. (I.23): 31 2 n 36.2 g The degree of hydration is; Eq. (I.2b): Had no orretion for arbonation been made, the alulated degree of hydration had been: This is an unreasonably high value, sine the degree of hydration annot transgress 1. Example: Partly arbonated ement paste A ement paste ith the ement ontent 3 g is arbonated to 2%. The CaO ontent in the ement is 65%.The dry eight of the is 39 g. The ignited eight is the same as the ement ontent, 3 g. The parameter n / is supposed to be.25.

17 12 The amount of hemially bound ater is; Eq. (I.23): 39 3 n 63.8 g The degree of hydration is: Had no orretion for arbonation been made, the alulated degree of hydration had been: This is also an unreasonably high value. Measurement of degree of arbonation The degree of arbonation expressed by the oeffiient y in the equations above must be kno. One method is to measure the gradual eight loss from a heated using TG. Within the temperature range 6-75ºC Ca(OH) 2 is deomposed and CO 2 released; [2]. The arbonated ement gel is deomposed already ithin the temperature range 38-6 ºC [2]. A problem is that also some hydrate ater is leaving ithin these temperature ranges. For TG to be used safely it is therefore important to develop a method by hih eight loss from release of CO 2 an be distinguished from eight loss due to release of hydrate ater. Consideration must also be taken to arbon bound in limestone filler in the ement. The safest method is to measure diretly the amount of arbon in the using a so-alled Leo-kiln. In Fig I.5 the result of suh measurements are sho.

18 13 Figure I.5: Binding of arbon dioxide in ement paste stored for 2 years in air of 8% RH. Variables: 1% portland ement, 15% fly ash, 3% fly ash; [3]. (upper) 28 days in ater before exposure. (loer) diret exposure to air.

19 14 II: CONCRETE The same equations, given about for ement paste, an also be used for alulation of the degree of hydration of onrete. Eq. (I.2b) an be used, provided the measured amount of hemially bound ater, and the (effetive) ement ontent in the are introdued in the equations. The aggregate might ontain a ertain amount of rystal ater hih leaves during ignition. This shall not be inluded in n. The loss on ignition of an aggregate ith the eight a is found to be n, a / a A blok diagram over a onrete ith rystal ater in aggregate and somehat prehydrated ement is sho in Fig.II.1. eight W d W i n, (Δ n, /) (Δ n,a /a)a a Figure II.1: Components in onrete. After orretion the hemially bound ater ontent in the is: n W d Wi n, a n, a a (II.1) here and a are the ement ontent and aggregate ontent in the. The relation beteen aggregate and ement in the onrete is K. a K (II.2)

20 15 Inserting K in Eq. (II.1) gives:,, a, Wd Wi K (II.3) a The effetive ement ontent is given by Eq. (I.8): The degree of hydration is given by Eq. (I.9). An approximate value of a an be alulated from the measured quantities W d oh W i ; see Fig. II.1 (the initial loss on ignition of ement and aggregate are negleted). It is assumed that the ement ontent is kno, either from the onrete reipe, or from a diret determination of the amount of CaO. W d d i a W W (II.4) The aggregate ontent beomes: a W 1 ) (II.5) i Alternative equations for alulation of the degree of hydration of onrete onsidering loss on ignition of ement and aggregate are given in referene [4]. 1 An exat value of the aggregate ontent is alulated by the folloing equations. The ement ontent is alulated from a determination of the ontent of CaO in the (provided the aggregate does not ontain alium). The aggregate ontent a is then obtained from the dry eight of the at hih onsideration is also taken to the loss on ignition of ement and aggregate at mixing. The dry eight is: W d n, n, a 1 Thus, the aggregate ontent in the is: n, n, a a W d 1 n, n, Thus, for an exat determination of the true aggregate ontent the amount of hemially bound ater in the must be estimated as orretly as possible.

21 16 Example The ement ontent in a onrete is 1 g. The aggregate ontent is 4 g, thus, K=4. Ignition of s of ement and aggregate gave the folloing values:,.5, a.5 a The dry eight and the eight after ignition of the onrete are: W d =52 g W i =498 g The amount of hemially bound ater is alulated by Eq. (II.3): (.5.54) 15 g n, The relation n / is supposed to be.25. The effetive ement ontent is alulated by Eq. (I.8):.5, eff 11 8 g.25 The degree of hydration is alulated by Eq. (I.9): If no orretions ere made for loss on ignition of ement and aggregate the folloing values should have been obtained: g n, Thus, the degree of hydration should have been heavily exaggerated. Example. The same as above, but rystal ater in aggregate is negleted, n, Wd Wi g The effetive ement ontent is unhanged, 8 g This is also a onsiderable overestimation of the degree of hydration.

22 17 REFERENCES [1] Poers, T.C, Broyard, T.L.: Studies of the physial properties of hardened portland ement paste. PCA Researh Laboratories, Bulletin 22, Chiago, Illinois [2] Helsing-Atlassi, E.: A quantitative thermogravimetri study on the nonevaporable ater in mature silia fume onrete. Chalmers Tehnial University, Div. of Building Materials, Publiation P-93:6, [3] Fagerlund, G.: Carbonation of onrete ith fly ash ement. In Durable Conrete ith Industrial By-produts. VTT Symposium 89, Esbo [4] Utgennant, P.: The influene of ageing on the salt frost resistane of onrete. Lund Institute of Tehnology, Div. of Building Materials, Report TVBM-121, Lund 24.

23 18 APPENDIX 1: EFFECTS OF THE DRYING PROCEDURE Error ourring during preparation of the During drying made before ignition, some ontinued hydration might our aused by ater left in the pores. This hydration is also stimulated by the elevated temperature hen drying at +15 ºC is used. This ill led to an error in the measured degree of hydration. Therefore, it is essential that the ongoing hydration in the an be stopped before drying. The folloing tehnique, used at the Sedish Cement and Conrete Researh Institute, has turned out to be appropriate. The method is as follos: 1. The is rushed and milled in pure ethyl alohol (96%). Milling goes on for about 3-5 minutes. 2. The produed poder is left in alohol for 2-4 hours. The time might be prolonged to 24 hours. 3. The poder-alohol slurry is entrifuged for 2 minutes in order to remove surplus alohol. 4. The remaining poder is dried in vauum for 1-4 hours. 5. Drying at +15 ºC ommenes and goes on until equilibrium is reahed. By milling in alohol muh of the pore ater is removed, hih makes hydration stop. The only unanted hydration ourring is restrited to a time less than ½ hour. Examples of the use of this method are sho in Figure A1.1. It has been possible to follo the hydration proess do to very lo values. Probably, tests ould also have been made at even loer onrete age. Figure A1.1: Chemially bound ater as funtion of onrete age. Curing temperature +5 ºC. Four different onrete types (A, B, C, D); [A1.1].

24 19 Effet of the drying proedure before ignition The alulated amount of hemially bound ater depends on the method used for drying the before ignition. Referene [A1.2] presents a thorough study on the effet of drying proedure on the dry eight; W d in equation (I.3). There are four main methods for determination of the dry eight. The first method is most ommonly used. 1. Drying at +15 ºC The vapour pressure in the oven varies sine it is the same as the vapour pressure in the laboratory. Thus, RH in the oven ill depend on the limate in the lab. Example: The room temperature is +2 ºC and RH of room air is 5%. Then, the vapour pressure in lab air is torr=8.75 torr. The saturation vapour pressure at +15 ºC is 96 torr. RH in the oven beomes (8.75/96) 1=.97%. If the room temperature is +25 ºC and RH of room air is 5%, the vapour pressure in the oven is =11.9 torr, and RH in the oven beomes (11.9/96) 1=1.31%. Suh fairly small variations in the vapour pressure of lab air affet the dryness and thus the amount of measured evaporable ater. A method that makes it possible to keep RH in the oven onstant, independently of variations in the outer vapour pressure has been developed; [A1.3]. 2. Drying over magnesium-perhlorate-hydrate (Mg(ClO 4 ) 2 2H 2 ), P-dying Vapour pressure torr. 3. Drying over dry ie, D-drying Vapour pressure torr. Drying temperature -79 ºC. 4. Freeze-drying, F-drying Drying temperature -1 ºC. The drying time is of big importane. In order to obtain the orret value of W d and thus the orret value of n,, drying must proeed until the rate of drying is virtually zero. In referene [A1.2] it is assumed that the orret dry eight is obtained hen the eight loss during 1 day does not exeed.1 gram per gram ement paste. Different drying methods give different results for W d. A less effiient drying method giving a high value of W d brings about a higher alulated value of n than a method that is more effiient. This is visualized by Fig. A1.2. A less effiient method leaves a higher amount of evaporable ater. This ill be ounted as hemially bound ater at alulation of the degree of hydration using Eq. (I.3). Measurements presented in [A1.2] of the effiieny of the four ommon drying methods are sho in Figure A.3. Furthermore, the effet of short drying time is sho for to methods; 12 hour D-drying and 3 hour +15 ºC drying.

25 2 eight W Evaporable ater W d,mild W d,hard Un-dried Evaporable ater Chemially bound ater n,,hard n,,mild W i Figure A1.2: Effet of the drying effiieny on the estimated amount of hemially bound ater. Figure A1.2: Drying effiieny of different methods of drying out evaporable ater; [A1.2]. The drying effiieny is alulated by Eq, (A1.1). To different drying times are tested for D- drying; 12 hours and drying to equilibrium. For +15 ºC drying values are given for 3 hours drying and 24 hours drying (equilibrium). In A1.2 the folloing expression is used for estimation of the effiieny of different drying methods. W W drying effiieny DE W W d (A1.1) i here W is the eight of the ement paste before drying. The higher the value of DE, the higher is the drying effiieny, and the loer is the hemially bound ater; see Fig. A1.2.

26 21 In all ases, fine-ground ater saturated ement paste ith the ater ement ratio.45 and 28 days of age, ere tested. All s had been pre-treated in exatly the same manner. Mixing as made in a glove-box in argon atmosphere and hydration ourred in air-tight ontainers in order to avoid arbonation. The folloing values of the drying effiieny DE ere observed. Type of drying Drying effiieny, DE D-drying.571 P-drying ºC drying 24 hours.637 F-drying.56 Drying at +15 ºC is the most severe drying method giving the loest amount of hemially bound ater, and the loest degree of hydration. Sine the s ere ater-stored until start of testing the three parameters in Eq. (A1.1) an be alulated using the folloing equations: W,. 25, (A1.2) here, is the ater ontent in the at mixing. The term.25 n, is ater taken up in the during uring. Water uptake is aused by hemial ontration of ater hen this is hemially bound to ement (the s ere stored in ater). W d, (A1.3) Wi (A1.4) Thus, equation (A1.1) an be quantified by:,.75, DE (A1.5).25, n, In the folloing disussion the ement is supposed to have no pre-hydration at mixing. Dividing all terms in Eq. A1.5 by the ement ontent in the gives:, /.75 DE (A1.6), /.25 here / is the ater-ement ratio (.45). Re-distribution of terms and exhange of for ement ontent in general,, gives: n / 1 DE (A1.7).25 DE.75

27 22 Data in Fig.A1.2 are valid for /=.45. Thus, equation (A1.7) is transformed into: n.45(1 DE) (A1.8).25 DE.75 NOTE If ater absorption during uring is negleted Eq. (A1.2) is hanged to: W, (A1.2b) Eq. (A1.7) is transformed to: n / (1 DE) (A1.7b) Eq. (A1.8) is transformed to: n.45 (1 DE) (A1.8b) The relation n / for the ement paste alulated by Eq. (A1.8) and Eq. (A1.8b) are given in the table belo. Drying method n / by Eq. (A1.8) n / by Eq. (A1.8b) D-drying P-drying ºC drying 24 hours F-drying The differene in measured amount of hemially bound ater, using different drying methods, is onsiderable. If the amount of hydrate ater at full hydration is kno ( n / ), the degree of hydration an be alulated by Eq. (I.2b), using the values in the table above. Often the parameter n / is onsidered a material onstant that is independent of the drying method. If it is assumed to be.25 for all drying methods the degree of hydration sho in the table belo are obtained. Drying method Degree of hydration, Eq. (I.2b) n / by Eq. (A1.8) n / by Eq. (A1.8b) D-drying P-drying ºC drying 24 hours F-drying

28 23 The relation in degree of hydration beteen the to most ommonly used drying methods, D-drying and drying at +15 ºC is: Eq. (A1.8): D drying D drying.772 Eq. (A1.8b): The differene is as high as about 2%. Comment on degree of hydration The amount of hemially bound ater, n, is depending on the drying method, as sho above. The degree of hydration is hoever not influene as muh as alulated above, depending on the fat that one shall not use the same value of the parameter n / for all drying methods. This value shall be inreased hen a less effetive drying method is used. The general value.25 used above is therefore not valid for all drying methods. Effet of the drying tehnique on alulated porosity A less effiient drying method ill make the alulated total porosity bigger. This ill be sho by the folloing equations. The total porosity of ement paste is: / P tot (A1.9).32 /.32 here.75 is the speifi volume of hydrate ater (m 3 /g),.32 is the speifi volume of ement (m 3 /g), and is the ater ontent in the fresh ement paste at mixing. The ement paste tested /=.45. Thus Eq. (A1.9) is hanged to: P tot (A1.9b).77 The observed value of n / for the different drying methods alulated by Eq. (A1.8) are inserted in this equation. The folloing porosities are obtained. Drying method Total porosity, % D-drying 37.4 P-drying ºC drying 24 hours 4.9 F-drying 36.8 Evidently, the differene beteen different drying methods is fairly big.

29 24 REFERENCES [A1.1] Fagerlund, G.: Influene of slag ements on the frost resistane of the green onrete. Sedish Cement and Conrete Researh Institute, Researh Fo 3.83, Stokholm [A1.2] Korpa, A., Trettin, R.: The influene of different drying methods on ement paste mirostruture as refleted by gas adsorption: Comparison beteen freeze-drying (F-drying), D-drying, P-drying and oven-drying methods. Cement and Conrete Researh 25. [A1.3] Danielsson,U.: An apparatus for easy determination of the amount of bound ater in ement pastes yielding highly reproduible results. Materials and Strutures, 7:4, 1974.

30 25 APPENDIX 2: EFFECTS OF REACTIVE MINERAL ADMIXTURES The basi idea behind the method for determination of degree of hydration desribed in this report is that there is a diret proportionality beteen the amount of hemially bound ater, as determined by ignition, and the amount of ement that has reated: onst n reated (A2.1) n total Therefore, the amount of hemially bound ater inreases gradually ith inreased hydration time. Examples of the time development of hemially bound ater are sho in Fig. A1.1. When reative mineral admixtures are added to ement or onrete the diret proportionality is no longer valid. One example is sho in Fig. A2.1 for ement paste ontaining silia fume. After about 9 days the amount of hemially bound ater gradually diminishes ith inreased hydration time. The mehanism behind this phenomenon is not totally larified. A hypothesis put forard is that a ertain poly-ondensation of the siliate hains ours, at hih previously bound ater is released. In [A2.2] the folloing expression for alulating the amount of hemially bound ater in onrete ontaining silia fume is suggested: n n n em Si Si em Si Si Si (A2.2) here em is the degree of hydration of the Portland ement, Si is the degree of reation of the silia fume, is the ement ontent, and Si is the silia fume ontent. The oeffiients.25 and.34 are the hemially bound ater at omplete hydration of ement and silia fume in relation to the total ement and silia fume ontents. Thus, it is assumed that the ement reats as if no silia fume is present, but that the reation of silia fume releases ater that as initially bound to ement hydration produts. Aording to Eq. (A2.2) the degree of hydration of the ement is: Si em Si (A2.3) Thus, in order to alulate the degree of hydration of the portland ement in the onrete or ement paste one has to determine the amount of bound ater by ignition of a in the normal ay. Thereafter, a orretion is made for the effet aused by the silia fume reation. Ho the amount of reated silia fume shall be determined is unlear. Possibly, it an be estimated from the amount of Ca(OH) 2 in the onrete, sine silia fume reation onsumes lime.

31 26 Example A ement paste ontaining silia fume that is 1 % of the ement eight is studied. The dry eight is 161 g. The ignited eight is 14 g. The amount of ement+silia fume is the same as the ignited eight, 14 g. The ement eight is 14/1.1=127 g. The amount of hemially bound ater is =21 g. The silia fume is assumed to be fully hydrated. Then, the degree of hydration of the Portland ement is: em If the effet of silia fume as not onsidered the alulated degree of hydration is: 21 em Thus, the effet of silia fume annot be negleted. Maybe, the effet of addition of other mineral admixtures, like fly ash or blast-furnae slag, an be treated in a similar ay, by adding orretions to the measured ratio beteen bound ater and ement ontent. Ho these orretions shall be made is, hoever, not kno. Suh materials are also used in muh bigger quantities than silia fume. Therefore, for onrete ontaining fly ah or slag, it seems reasonable not to use the amount of bound ater as a measure of degree of hydration. % 8% 16% Figure A2.1: Measurements of the amount of hemially bound ater in ement paste ontaining %, 8% or 16% silia fume (related to the ement eight); [A2.1] (Ålder=onrete age days)

32 27 REFERENCES A2.1 Zhang, M-H., Gjörv, O.E.: Effet of silia fume on ement hydration in lo porosity ement pastes. Cement and Conrete Researh. 1991(21): A2.2 Helsing Atlassi, E.: A quantitative thermogravimetri study on the non-evaporable ater in mature silia fume onrete. Chalmers University of Tehnology, Dept. of Building Materials, Publiation P-93:6, 1993.

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