Search

In this work, a complete beneficiation technical route combining physical and chemical methods, namely a roasting-flotation-leaching scheme, is proposed to produce a qualified grade Ti-concentrate from altered Vanadium titanomagnetite (VTM) ore. Based on the character of the ore sample, it is recommended to recover the Ti-bearing minerals, ilmenite and anatase, as composite mineral. Pretreatment experiments indicate that the oxidation roasting (800 °C) and acid washing methods increase the flotation indexes significantly. Flotation condition tests show that the optimal conditions are a grinding fineness of −0.045 mm 83%, sulfuric acid dosage of 2000 g/t, water glass dosage of 1500 g/t, oxalic acid dosage of 200 g/t, and EM328 dosage of 1500 g/t. An open flotation circuit test obtains a flotation concentrate with a TiO2 grade and recovery of 38.30% and 25.99%, respectively. A leaching exploration test shows that the TiO2 grade of the flotation concentrate can be improved to 53.90%. XRD analyses reveal that the ilmenite in the VTM ore is converted into anatase and rutile during the roasting process at 600–800 °C, but pseudobrookite begins to form at 900 °C. Compared to the flotation concentrate, it is confirmed that the content of Ti-bearing minerals is increased significantly in the leaching residue. [ABSTRACT FROM AUTHOR]

• Flotation separation of bastnaesite from fluorite and calcite is achieved. • Citric acid (H 3 Cit) is used as a selective depressant for fluorite and calcite. • H 3 Cit adsorbs spontaneously on the Ca–containing minerals surfaces. • Depression mechanism of H 3 Cit on the fluorite and calcite surfaces is investigated. Bastnaesite is a chief natural source of light rare earth elements (LREEs). The effective depression of Ca-containing minerals such as fluorite and calcite in bastnaesite flotation system is normally difficult, and it is imperative to exploit more environmentally-friendly depressants which can inhibit these gangue minerals simultaneously. Hence, we employ citric acid (H 3 Cit), a green, cheap and commonly available organic acid, to selectively depress the flotation of fluorite and calcite, and use octanohydroxamic acid (OHA) and sodium oleate (NaOL) with a molar ratio of 2:1 as mixed collectors. Micro-flotation results show that H 3 Cit decreases the recoveries of fluorite, calcite, and bastnaesite by 84.73%, 62.96%, and 9.23%, respectively at pH 8–9. The depression mechanism of H 3 Cit was investigated through zeta potential measurements, microcalorimetry measurements, solution chemistry and reaction thermodynamic analyses, and X-ray photoelectron spectroscopy (XPS) analyses. These further analyses at the minerals/water interfaces indicate that H 3 Cit preferentially adsorbs on the gangue mineral surfaces due to the positively charged fluorite and calcite surfaces which interact more easily with citrate ions (Cit3-), and the spontaneous interaction between Cit3- and Ca2+ on the surfaces. Accordingly, H 3 Cit is supposed to be a potential depressant for Ca-containing minerals in the flotation separation of bastnaesite. [ABSTRACT FROM AUTHOR]

Octanohydroxamic acid (OHA) and sodium oleate (NaOL) were employed as mixed collectors to reduce the cost, increase the recovery, and retain the selectivity for the flotation of bastnaesite. Flotation experiments, zeta potential measurements, Fourier transform infrared (FTIR) spectroscopy, pyrene fluorescence measurements and X-ray photoelectron spectroscopy (XPS) were used to investigate the flotation and possible adsorption mechanism of mixed OHA/NaOL collectors on bastnaesite. The flotation experiments show that a lower dosage of mixed OHA/NaOL collectors (total concentration 1 × 10−4 mol/L, OHA:NaOL = 2:1 at pH 7) can achieve a recovery of 94.02%, which is 33% higher than that using single OHA at the same condition. Zeta potential measurements and FTIR analyses indicate that OHA/NaOL chemisorb more strongly on bastnaesite surface than each of its components. Pyrene fluorescence measurements illustrate that the critical micelle concentration (CMC) of the mixed OHA/NaOL is lower than that of either component alone, together with a higher adsorption density on bastnaesite. XPS measurements show a new peak at 288.4 eV and an increase in the C (1s) peak intensity at 284.8 eV from 15.87% to 37.85% when using the mixed OHA/NaOL. Therefore, the mixed collectors have a stronger flotation ability and produce a thicker adsorption layer. • Bastnaesite flotation recovery using OHA/NaOL is higher than that of single collector. • The optimal flotation condition of the mixed OHA/NaOL was confirmed. • OHA/NaOL chemisorb more strongly on bastnaesite surface than single ones. • The adsorption mechanism of the mixed OHA/NaOL was investigated. [ABSTRACT FROM AUTHOR]

• The effect of fluorite and barite species on bastnaesite flotation was investigated. • Gangue supernatants appreciably reduced bastnaesite floatability with sodium oleate. • At pH 3, S O 4 2 - and F− hindered the chemisorption of oleate species on bastnaesite. • At pH 11, carbonate/hydroxy compounds concealed active sites on the mineral surface. The flotation of rare earth minerals, which is of current interest in the mineral processing field, is challenging owing to the dissolution of gangue minerals. In this study, dissolved fluorite and barite species were found to significantly affect the flotation behavior of bastnaesite. The mechanism was investigated using microflotation tests, zeta potential measurements, Fourier transform infrared (FTIR) spectroscopy, X-ray photoelectron spectroscopy (XPS), and solution chemistry analysis. The microflotation results confirmed that the presence of gangue supernatants significantly reduces the recovery of bastnaesite during flotation with sodium oleate as a collector. The zeta potential and solution chemistry analyses showed that the supernatant species can adsorb onto the bastnaesite surface by forming hydroxy and carbonate compounds, thus affecting the zeta potential value and reducing the adsorption of oleate species. The FTIR analysis suggested that treatment with supernatants weakens the adsorption of oleate species, and that Ca/Ba-oleate complexes are adsorbed on the bastnaesite surface. The XPS analysis confirmed that lattice ions from the gangue minerals adsorb/precipitate on the bastnaesite surface, hindering the chemisorption of oleate species and thus decreasing the floatability of bastnaesite. [ABSTRACT FROM AUTHOR]

• Dissolved calcite inhibits bastnaesite flotation by NaOL at high pH. • Calcite supernatant has a stronger effect than calcium or carbonate alone. • Calcium forms hydroxy complex and precipitate to hinder adsorption of NaOL. • Some NaOL in the solution is also converted to calcium oleate precipitate. The flotation behavior of bastnaesite, a major mineral source of rare earth elements, is strongly affected by the dissolved species of gangue minerals that change the solution chemistry and mineral surface properties. In this work, the effect of dissolved calcite species on the flotation of bastnaesite was investigated by conducting micro-flotation experiments, zeta potential measurements, Fourier-transform infrared (FT-IR), and X-ray photoelectron spectroscopy (XPS) analysis. Micro-flotation experiments confirmed that calcium and carbonate ions in calcite supernatant significantly reduced the flotation of bastnaesite in strongly alkaline condition. Zeta potential measurements showed that the IEP of higher bastnaesite was obtained after the addition of calcite supernatant species. Species distribution diagram demonstrated that the adsorption of sodium oleate on the surface species of bastnaesite was inhibited by the generation of calcium-containing hydroxy complexes and precipitates. FT-IR analysis suggested that the decrease the sodium oleate concentration in solution and the generation of calcium oleate precipitate on the mineral surface are possible reasons for the reduced recovery. XPS analysis further revealed that the metal carbonates and hydroxy complexes of calcium adsorbed on the bastnaesite surface in the presence of calcite supernatant, which concealed the surface active sites, caused the decrease in bastnaesite flotation recovery. [ABSTRACT FROM AUTHOR]

Herein, a novel method of ultrasonic treatment for selectively recovering ilmenite from titanaugite was investigated via systematic mineral flotation tests along with dissolution texts, microcalorimetry, scanning electron microscope (SEM), and X-ray photoelectron spectroscopy (XPS) analyses. Flotation tests indicate that ultrasonic treatment promotes the ilmenite floatability but depresses titanaugite floatability. When ultrasonic time and power are 5 min and 500 W, selectivity of ilmenite from titanaugite can be enhanced. Dissolution tests show that ultrasound can strengthen the dissolution of Ca and Mg but has little effect on Fe species. Microcalorimetric measurements confirm that ultrasonic-treated ilmenite is more prone to release heat than titanaugite. SEM images reveal that the surface roughness of the titanaugite is greater than that of the ilmenite, indicating that the particle collision of titanaugite is greater than ilmenite. XPS indicates that NaOL adsorption on ultrasonic-treated ilmenite surfaces is greater than that for titanaugite. Unlabelled Image • Ultrasonic pre-treatment promotes/depresses ilmenite/titanaugite floatability. • Ultrasound causes greater surface roughness of titanaugite than ilmenite. • Ultrasound strengthens Ca and Mg dissolution; it has little effect on Fe species. • NaOL adsorption on ultrasonic-treated ilmenite surface exceeds that of titanaugite. [ABSTRACT FROM AUTHOR]

• Under optimum conditions, the effect of sonication on ilmenite is significant. • Maximum flotation is at pH 4–5 (43.17% & 89.54% for raw & ultrasonicated ilmenite) • Post-ultrasound, Zeta potential shifts toward negative values and IEP to lower pH. • Adsorption-driven heat release (−Q ads) is higher for ultrasonicated ilmenite. • Post-ultrasound, Fe2+ oxidizes to Fe3+, improving ilmenite flotation recovery. In this study, we used flotation tests, Fourier transform infrared spectroscopy (FTIR), zeta potential, X-ray photoelectron spectroscopy (XPS), and microcalorimetry measurements to investigate the flotation and possible adsorption mechanisms of the ilmenite surface before and after ultrasonic pre-treatment. Flotation results show that under optimum conditions, the promotion effect of sonication on ilmenite is remarkable. The maximum recovery is 89.54% for ultrasonicated ilmenite at a pH of 4–5. For pH of 8–9, recovery increased again to 66.34%. Microcalorimetry indicates that the adsorption-driven heat release (−Q ads) is higher for ultrasonicated ilmenite than for raw one. After pre-treatment, the iso-electric point (IEP) changed from pH 6.2 to pH 4.2. FTIR spectra and zeta potential measurements indicated that metal ions as active sites on the ilmenite surface are probably changed by the ultrasonic treatment. XPS analysis shows that ultrasonic treatment can promotes the oxidation of Fe2+ to Fe3+ and improves the solubilization of Ca2+ and Mg2+ in the pH range of 4–5. Under weakly alkaline condition, ultrasound also can make Ca2+ and Mg2+ re-absorb onto the ilmenite surface as main active sites. [ABSTRACT FROM AUTHOR]

• Sonication remarkably affects ilmenite flotation performance. • Sonication increased chemical adsorption of oleate ions on ilmenite surface. • Flotation recovery is improved via significant conversion of Fe2+ to Fe3+. • Possibility of improved selective flotation of ilmenite from gangue minerals. Herein we investigate the flotation and possible adsorption mechanism on the surface of ilmenite and the changes in the surface composition of ilmenite before and after ultrasonic pre-treatment through flotation tests, Fourier-transform infrared (FTIR) spectroscopy, zeta potential measurement, X-ray photoelectron spectroscopy (XPS), and microcalorimetry. The flotation results reveal that, under optimum conditions, sonication has a remarkable effect on the flotation of ilmenite. The maximum flotation recoveries of raw and ultrasonically treated ilmenite in the pH range 4–5 are 43.17 and 89.54%, respectively. The zeta potential of the pre-treated ilmenite shifted toward negative values, thus shifting the iso-electric point from pH 6.2 to pH ∼4.2. The FTIR spectra and zeta potential values indicate that the ultrasonic pre-treatment helped enhance the chemical adsorption of oleate ions on the surface of ilmenite. The results of microcalorimetry analysis suggest that the adsorption heat released (−Q ads) from ultrasonically treated ilmenite is more than that released from raw ilmenite. The XPS analysis confirmed that the relative content of Fe3+ increased from 36.87 to 61.84% following the ultrasonic pre-treatment for 5 min in the pH range 4–5. After the treatment, Fe2+ ions on the ilmenite surface are abundantly oxidised to Fe3+ ions. The significant conversion of Fe2+ to Fe3+ helped improve the flotation recovery of ilmenite over a wide pH range. [ABSTRACT FROM AUTHOR]

Abstract In this study, the flotation and adsorption of Pb(II)/benzohydroxamic acid (BHA) complexes on the surfaces of ilmenite and titanaugite were compared to achieve their separation flotation. Single and synthetic mixed mineral flotation tests, zeta potential measurements, Fourier-transform infrared (FTIR) spectroscopy, as well as microcalorimetry analyses were carried out. The results of the flotation tests indicated that the separation of the minerals is feasible by using complexes with the molar ratio of Pb(II):BHA = 1:3 at pH = 6.0. Moreover, the Pb/BHA complexes exhibited better performance than sequentially added Pb(II) and BHA species. The zeta potentials indicated that Pb/BHA complexes might selectively adsorb on the surface of ilmenite in the mixed system. The FTIR results demonstrated that the Pb/BHA complexes exhibited higher adsorption capacity on the surface of ilmenite than by sequential dosing of Pb(II) and BHA. In contrast, on the titanaugite surface the adsorption ability of Pb/BHA complexes was similar to that of BHA, indicating that titanaugite could not be activated by Pb(II) ions. The microcalorimetric results revealed that the adsorption heats on the surfaces of ilmenite and titanaugite were ranked as Pb/BHA > BHA > Pb(II) ions, indicating that Pb/BHA complexes interacted most strongly with the two mineral surfaces, and chemisorption occurred on both surfaces by using BHA and Pb/BHA collectors. Thermodynamic analysis revealed that complexes with BHA are easier to generate when using Pb(II) than Ca2+ and Fe2+ ions, and the Pb/BHA complexes preferred to adsorb on the active sites of ilmenite (e.g. Fe2+ or Fe3+) rather than titanaugite (e.g. Ca2+), indicating that selective separation is feasible. Graphical abstract Unlabelled Image Highlights • Pb(II)/BHA complex used as collector to separate ilmenite from titanaugite. • Adsorption of BHA & Pb/BHA on the two minerals was compared. • ζ-potential, FTIR, microcalorimetry data all showed Pb/BHA prefers ilmenite. • Pb/BHA complex in 1:3 ratio (pH = 6) can effectively separate ilmenite in floatation. • Sequentially added Pb and BHA showed less selectivity than the complex. [ABSTRACT FROM AUTHOR]

• A mixed collector BHA/DDA efficiently separates spodumene from feldspar. • BHA first forms a complex with DDA, which then adsorbs onto the mineral surfaces. • In-situ ATR-FTIR and 2D-COS reveal the adsorption mechanism of the mixed collector. • Microcalorimetry compares the separating ability of single and mixed collectors. • Different sorption configuration of BHA/DDA depends on pH. Herein, benzohydroxamic acid/dodecylamine (BHA/DDA, optimal molar ratio of 6:1) demonstrated the excellent separation in the flotation of spodumene (ca. 88% recovery) from feldspar (ca. 24% recovery) at pH 8–9. To detect the underlying mechanism, in-situ attenuated-total-reflectance Fourier-transform infrared (ATR-FTIR) spectroscopy with two-dimensional correlation spectroscopy (2D-COS), zeta potential measurements, in-situ microcalorimetry, and X-ray photoelectron spectroscopy (XPS) were performed. In-situ microcalorimetry results indicated that the mixed collector released more heat than the individual collectors for both minerals. Moreover, The order of the difference in the adsorption reaction heat between this two minerals is as follows: |ΔQ| BHA/DDA (13.948 J·g−1) ˃ |ΔQ| DDA (3.116 J·g−1) ˃ |ΔQ| BHA (1.110 J·g−1), confirming the excellent separating ability of mixed collector. In-situ attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy and two-dimensional correlation spectroscopy (2D-COS) sequences results showed that the sorption process and configuration of BHA/DDA (0.4 mM, molar ratio = 6:1) on spodumene and feldspar surfaces were different at pH of 4–5 and 8–9, mainly due to the different BHA structure and the formation of hydrogen bond between BHA and DDA at different pH range. Zeta-potential and X-ray photoelectron spectroscopy (XPS) also suggested that their prominent separation is not simply due to the higher adsorption density for a single collector in the presence of mixed collector. Lastly, recommended adsorption models for the adsorption of the complex on the surfaces of spodumene and feldspar were proposed. This work provided powerful in-situ detection technologies to reveal the reagent-solid interaction in selective separation processes. [ABSTRACT FROM AUTHOR]

• Spodumene and feldspar have similar surface sites, making separation difficult. • Addition of 30 mg/L SA before 0.2 mM DAA at pH 6 allowed minerals separation. • Spodumene has more Al sites than feldspar, and, thus, adsorbs more DAA. • Sodium alginate of selective depressant exhibited strong pH dependence. • DAA could form a reticular structure with SA on the spodumene surface. Sodium alginate (SA) was investigated for use as a depressant in the spodumene–feldspar system. In this flotation system, the SA is added before the cation collector, dodecylamine (DDA). The effects of SA on mineral floatability were systematically investigated by flotation experiments, X-ray photoelectron spectroscopy (XPS), Fourier transform IR spectroscopy (FTIR), zeta potential measurements, and speciation analysis. Single-mineral flotation results showed that using 30 mg/L SA allowed the separation of spodumene from feldspar at pH 6, although there was a strong pH dependence. Zeta potential measurements and FTIR analysis showed that SA and DDA can adsorb onto both minerals. XPS analysis revealed the adsorption mechanism: the strong affinity of SA for the mineral surface arose from the complexation of SA and Al sites. Analysis of the surface and solution chemistry revealed that SA chelated Al3+ or its hydroxides and hindered the subsequent adsorption of DDA, resulting in a hydrophilic feldspar surface. In addition, there were more aluminium hydroxides and unsaturated O atoms on the spodumene surface than on that of feldspar, and these provided available sites for the adsorption of DDA to form a stable reticular structure with SA, thus improving the floatability of the spodumene at certain pH values. Lastly, a model for SA and DDA adsorption at the water–solid interface is proposed. [ABSTRACT FROM AUTHOR]

• Ilmenite is an iron-titanium mineral but separation from titanaugite is difficult. • Microwave pre-treatment can selectively promote ilmenite flotation. • Microwave treatment resulted in loss of Mg2+ and Ca2+ ions from titanaugite. • Optimal microwave conditions were 800 W for 450 s at pH 6. • A sodium oleate concentration of 2 × 10−4 mol/L allowed selective separation. The selective separation of titanium-containing minerals is industrially important. Microwave irradiation pre-treatment can be used to modify the surface properties of minerals to promote selective flotation. However, the effects of MW treatment on titanium-containing minerals is not well understood. Therefore, in this study, we investigated the effects of microwave treatment on the flotation behaviour of ilmenite and titanaugite in a mixture of these minerals. The effects of this pre-treatment method were investigated by various techniques, including flotation tests, scanning electron microscopy (SEM), inductively coupled plasma-optical emission spectrometry (ICP-OES), zeta potential measurements, X-ray photoelectron spectroscopy (XPS), and Fourier-transform infrared (FTIR) spectroscopy. The flotation tests results reveal that, under the optimum microwave conditions (800 W, 450 s), microwave irradiation has a remarkable effect on the flotation of ilmenite but no significant effect on the floatability of titanaugite at pH 6.0. The results of the SEM and ICP-OES analyses indicate that microwave irradiation promotes the dissolution of Ca2+ and Mg2+ ions from the titanaugite surface, whereas the dissolution of these ions from ilmenite is limited. Further, the zeta potential of the microwave-irradiated ilmenite shifted toward negative values, and the isoelectric point shifted from pH 4.9 to pH ~1.9. In addition, the XPS results reveal that microwave irradiation facilitates the conversion of Fe2+ to Fe3+ on the mineral surfaces. The FTIR spectra and zeta potential values indicate that microwave irradiation can enhance the chemical adsorption of oleate ions on the surface of the ilmenite. After microwave irradiation, the effects of both the dissolution of Ca2+ and Mg2+ ions and the oxidation of Fe2+ to Fe3+, the floatability of ilmenite was significantly improved, whereas that of titanaugite was not changed significantly. [ABSTRACT FROM AUTHOR]

Focusing on salt-type and oxide minerals, this paper reviews the research on anisotropic surface chemistry properties, including broken bonds, surface energy, wettability, and surface charge. Moreover, based on the analysis of anisotropic surface properties, the anisotropic adsorption behaviour of reagents on mineral surfaces is also reviewed. The research on anisotropic surface chemistry is instructive to understand some of the properties of the minerals themselves and the reactions in which minerals participate. In addition, the investigation on the anisotropic adsorption behaviour of reagent molecules on mineral surfaces will definitely strengthen the understanding of the efficiency of the interactions. In general, with the knowledge of mineral anisotropy, the relationship between the selective pre-treatment of a mineral and the efficient adsorption of reagent molecules on mineral surfaces will be established. [ABSTRACT FROM AUTHOR]

• Selective flotation separation of bastnaesite (B) from calcite (C) was realized. • Xanthan gum (XG) was used as a depressant and sodium oleate as a collector. • XG interacted with Ca ions on C surface in preference to rare earth ions on B surface. • XG adsorption on the surface of C suppressed oleate ion adsorption thereon. The inability of rare earth and gangue minerals to be efficiently separated by flotation due to their similar physicochemical properties is a major challenge of the rare earth industry. Bastnaesite is one of the principal sources of light rare earth elements. The use of traditional flotation reagents often poses the problem of poisonous wastewater generation. Therefore, we use xanthan gum (XG) as a non-toxic, biodegradable, and cheap depressant to selectively separate bastnaesite from calcite by flotation and probe the corresponding mechanism. Microflotation experiments/zeta potential measurements conducted with/without XG using sodium oleate as a collector demonstrate that at pH 8, XG decreases the flotation recoveries of calcite and bastnaesite by 85.09 and 22.37%, respectively. Further analysis of adsorption behaviour on the mineral surface and possible reagent-mineral interactions shows that selective mineral separation is due to the preferential interaction of XG with Ca ions on the calcite surface and the suppression of oleate ion adsorption thereon due to the steric hindrance of polymeric XG. Hence with regard to the potential of XG in calcium-bearing mineral separation, XG could be as a new depressant for RE mineral flotation. [ABSTRACT FROM AUTHOR]

• Al-Na 2 SiO 3 exhibited excellent depression capacity compared to individual species. • Si(OH) 4 can interact with Al(OH) 2 + and Al3+ ions to inhibit olivine floatability. • Polymeric species can connect to the surface by links of Mg–O–Si or Fe–O–Si. • NaOL are much easier to react with Mg and Fe than Al species when pH greater than 9. In this work, the performance of the novel depressant aluminum–sodium silicate (Al–Na 2 SiO 3) was compared to that of Na 2 SiO 3 , and the flotation and adsorption on the olivine surface were investigated with single-mineral flotation tests, zeta potential measurements, microcalorimetry, Fourier-transform infrared (FTIR) spectroscopy, and thermodynamic analyses. From the mineral flotation test results, Al–Na 2 SiO 3 was found to exhibit an improved depression capacity as compared to the samples in the absence of Al3+, and the depression properties of Al–Na 2 SiO 3 were found to depend on the Al3+ concentration. Thus, when the Al3+ concentration was higher than or equal to 0.1 mM, a significant depression capacity for olivine could be realized. From the obtained zeta potentials, it was found that by introducing assistant Al(III) species, the zeta potential of olivine exhibited a more positive integral shift than that of pure olivine and NaOL + Na 2 SiO 3. In addition, according to the species distribution of Al 2 (SO 4) 3 and Na 2 SiO 3 , Si(OH) 4 could interact with Al(OH)2+, Al(OH) 2 +, and Al3+ ions to form some monomeric silicate species and/or a polysilicate–aluminum material to inhibit the floatability of olivine. Moreover, the results of microcalorimetric measurements revealed that the reaction heats of the utilized reagents could be in the order of Al3+ < Na 2 SiO 3 < NaOL and Al–Na 2 SiO 3 + NaOL < Na 2 SiO 3 + NaOL, suggesting that the NaOL species exhibited the highest affinities to the olivine surface and Al–Na 2 SiO 3 impeded the adsorption of NaOL on the olivine surface. Furthermore, the thermodynamic analyses revealed that in the pH range of 2–9, the standard Gibbs free energy of Al3+ reacting with NaOL was lower than those of Mg2+ and Fe2+ but similar when the pH was above 9. This indicates that NaOL is more likely to interact with the Al3+ species in the pH range of 2–9; however, above pH 9, there is no significant difference in adsorption with Mg2+ or Fe2+. Finally, the FTIR spectra revealed that the adsorption of Al–Na 2 SiO 3 + NaOL on the olivine surface was weaker than that of the sample without assistant Al ions. [ABSTRACT FROM AUTHOR]