• No results found

groups are of equal reactivity regardless of the size of the polyion to which they are attached,

3. The activity of a component in the slag may be

defined in terms of Temkin ionic fractions, i,e. ^ 0 = Nm2+ x N 2-M 0

A model was formulated for linear chains only, in which Masson considered polycondensatioii reactions where S i O ^ could dimerise and then react with higher members of the silicate species. For a binary basic oxide-silica melt, the following expression was obtaineds-

2

which gives the activity of MO as a function of composition if is known (Figure 17) • The model gave some agreement with experimentally obtained activities of MO and enabled values of

to be designated to some binary MO-SiO^ systems.

An expression was also derived to define the ionic fraction of a silicate species;

N =n

r

1

<n"1f

1

1 + ®M0 j k h + 1

I

K11 “ ^0 ^ 1*140 1

"

^ 0 ^

2.9

2 (n + 1)- where N is the ionic fraction of Si 0 ' '

n n 3n + 1

and a^Q is given by equation 2,8.

Figure 18 shows the variation of the calculated ionic fraction of linear silicate anions of chain length n = 1 to n = 6 with mole fraction of SiOg for FeO - SiO^ melts at 1257-1307°C.

Models hased on polymer theory that pertain to "branched 92

chain configurations have "been developed • The three fundamental assumptions used previously were retained. The activity of MO was obtained from the following expressions

2.10 K11

the resultant variation of a^Q with x„.SiOg being presented

graphically in Figure 19#

The branched chain model gave good agreement with

experimental data for the systems SnO-SiO^# FeO-SiO^, PbO-SiO^ and MnO-SiOg with recent work further confirming agreement with

93

the MnO-SiOg system . Figure 20 shows a comparison between experimental data for the CaO-SiO^ system at 1600°C with the theoretical prediction for K equal to 0.0016. Table 1* records

for various systems.

For branched chains the ionic fraction of a silicate species was given as:-

TCT 3nl n = (2n + 1) In! r 'I 1 n - 1 r 1 + 3aM0 L 1 2n+1 3aM0 2.11

SiOj^ anion is the most abundant species at all compositions up to * S1O2 = 0.£. For the CaO-SiC) system the monomer is the2

sole species present below equal to 0*3, but in the FeO-SiO^ system longer chains exist at silica compositions below the orthosilicate composition*

Masson has suggested that the magnitude of the

equilibrium constants etc. provide a quantitative measure of polymerisation in binary silicate melts and that the

tendency towards polymerisation is determined by the nature of the cation. The average chain length of a melt would, therefore, be governed by the'difference in magnitude between cation-

silicate and cation-oxygen ion attractions. Consequently, the extent of cation-oxygen attraction influences the degree of ionic bonding in silicon-oxygen linkages so that changes in bond strength can be reflected in standard free energies of formation of the various silicates from their constituent oxides. Masson showed that for the reaction

MCL. + M_liq 3 2 7 Sio0 = 2M 2 4 liqSiO. ...

that,

BT In K. . = 2 AG° , 11 ortho - A G°pyro

This equation indicates that a tendency for polymerisation always exists in silicate melts because K.^ may be small but can never be zero, unless the rigfct hand side of the equation takes a value of minus infinity. Application of the equation is

limited as available thermodynamic data pertains to simple molecules thus restricting determination of

Criticisms of the Masson Models include doubts about the use of Temkin ionic fractions for a situation where different

size silicate anions are present. Also, the linear chain model predicts zero MO activity at the metasilicate composition which

go

is not observed experimentally • Since the development of the models, experimental evidence has indicated the existence of silicate rings in binary silicate melts and no provision has

73

been made for this situation .

Application of polymer theory to ternary silicate melts incurs difficulties due to the competitive interactions between the anions and various cations. An attempt has been made to develop a model for a ternary silicate melt where a common

9U

cation exists, e.g. MO-MF^-SiO^ This work retained the

assumptions of the previous models and although a new treatment was given to this type of melt, it served mainly to demonstrate

the complexities of dealing with ternary systems.

2.3*3 Constitution of Silicate Melts

(a) Practical Attempts to Determine Silicate Melt Structures At present, no technique has been found to directly observe and quantify the amounts of different silicate species in a melt. Workers have depended upon measurements of physical properties to provide structural interpretation of melts but the presence of immiscibility gaps in some systems can limit the

information obtainable.

Density measurements of CaO-PeO-SiO^ melts have confirmed 73

predictions that greater polymerisation occurs in iron

silicate melts compared with calcium silicate melts and relates 2+

to the preferred association of Ca cations with silicate

2+ 2— 95

anions thus releasing Pe cations to associate with 0 anions , 96 a phenomenon which increases the PeO activity in such melts ,

High temperature x-ray diffraction techniques, Raman spectroscopy and Mossbauer spectroscopy have all been used to examine silicate melts but no quantitative assessments of ionic distributions have been achieved Mossbauer spectroscopy examinations of basic electric arc slags sampled

2+

during the oxygen blow has shown that Pe cations can be present in a silicate phase or a 1mixed oxide1 phase, the proportion taken up in the latter phase increasing with

101

basicity , This tends to concur with Gaskell’s comments on the preferred association of cations with silicate or oxygen

96

anions ,

The distribution of silicate ions in a melt has been

80

inferred from studies of phosphate glasses dissolved in water , The dissolution technique cannot be applied to silicates as

hydrolysis readily occurs in aqueous media producing indefinite polymers related to silica gel

A technique has been developed \diere the blocking of O" sites of the parent silicate structure of a mineral by

trimethylsilyl (IMS) groups, (CH^)^Si- , has been used to retain some of the original structure. Gas Liquid Chromato­ graphy (GLC) and Mass Spectrometry (MS) were used for

respective separation and identification of the silicate derivatives

The trimethylsilylation of silicates is not always amenable to quantitative interpretation and attempts to improve this method by the formation of methyl and ethyl

102

silicates has been unsuccessful , The trimethylsilylation of silicates has been developed by a number of workers and will be discussed in more detail,

(b) The Trimeihylsilylation of Silicates

Trimethylsilylation is a pretreatment commonly applied to 10li organic materials to improve their suitability for GLC analysis Inorganic anions other than silicates have been trimethylsilylated

105,

106

Lentz trimethylsilylated various silicate minerals using a reaction mixture of crushed ice, propan-2-ol, hexamethyldisiloxane

103

and concentrated hydrochloric acid , The process was completed by use of an ion exchange resin, Amberlyst 15, A proposed reaction scheme commenced with leaching of the metal cation portions of the mineral to produce metal chloride and silicic acid:-

MoSi0. + I4HGL = H, SiO. + 2MGL

trimethylchlorosilane (TMCS) and trimethylsilanolj

[(CH^)^Si ] 2 0 + HC1 = (GH^)^SiCl + (CH ) SiOH

Either of the above products could be capable of reacting with silicic acid but Lentz considered

trimethylchlorosilane and the trimethysilylation reaction:- HjSiO, + U(CHJjS-CCl = [(CH ) Si]^ SiO^ + UHC1

where [(CH.) Sil SiO. is Hie IMS derivative of ihe 3 3 1 + 4

SiO. ^ anion,

4

Unfortunately, side reactions can occur and have been attributed to polymerisation and depolymerisation reactions taking place during trimethylsilylation and by hydrolysis of the

107

derivative itself , Success of trimethylsilylation is related 108

to both the type of metal cations and silicate anions 109

present . Leaching of the metal cation is undoubtedly 110 111

influenced by the cation type present 9 but the subject of acid attack on silicate minerals is still not fully understood 112• The presence of certain cations such as iron was

112

believed to aid leaching but increasing leachability by virtue of decreasing cation-oxygen bond strengih for a given

111

silicate group does not strictly confirm this . Complex silicate structures may render cations inaccessible to acids and so retard leaching For chain structures this appears

111