Kinetochemical and morphological differentiation of ettringites by the Le Chatelier-Anstett test

In this research, former XRD experiments have been verified by Le Chatelier-Ansttet (L-A) test. For this purpose, 28 cements consisting of 7 Portland cements and 21 blended cements containing 20%, 30% and 40% metakaolin have been submitted to the Le Chatelier-Anstett (L-A) test for 2 years. With all these cements, L-A specimens were manufactured and a direct parameter was measured for these specimens: increase in diameter, Δ∅, or diameter growth. Other complementary determinations were chemical analysis, XDA patterns and SEM of ettringites and specific properties of some cements tested. The experimental results have borne out that the formation rate of the ettringite formed from the reactive alumina, Al₂O₃^r−, present in pozzolans must be considerably higher than the formation rate of the ettringite from C₃A and much higher than the ettringite from C₄AF, both present in OPC. Owing to this, these ettringites were proposed being named “rapid formation” (ett-rf), “slow formation” (ett-lf) and “very slow formation” (ett-vlf) ettringites, respectively. On the other hand, these experimental results have also shown that the ett-rf has a much smaller size than the ett-lf (this is a direct consequence of the aforementioned conclusion); that almost all the alumina, Al₂O₃, present in M pozzolan must be regarded as being “reactive,” Al₂O₃^r−, or at least, the greatest part; that the detrimental effects derived from gypsum attack are shown much earlier in these POZC than in their plain OPC and, to such an extent, that this aggressive action can be described as rapid gypsum attack; and that none of the 21 POZC tested can be described as high nor moderate sulphate resistant cements according to L-A test.     

Internal deterioration of concrete by the oxidation of pyrrhotitic aggregates

This paper presents research results on the causes of a severe concrete deterioration, which occurred in many building foundations approximately 2 years after construction. Concrete samples were investigated with X-ray diffraction (XRD) analysis, a scanning electron microscope (SEM) and a petrographic examination performed with a stereomicroscope. It was found that the early cracking of concrete stemmed from the oxidation of the pyrrhotite found in the anorthosite aggregates used to produce the concrete. The oxidation process led to the precipitation of iron hydroxides having a higher volume than the original pyrrhotite does. The presence of micas (biotite) close to the pyrrhotite seemed to promote and accelerate the oxidation process.     

Groundnut Yield Response to Single Superphosphate, Calcitic Lime and Gypsum on Acid Granitic Sandy Soil

Phosphorus and calcium are the major nutrients limiting groundnut production. The objectives were to determine (a) optimum application levels of P and Ca, and (b) compare the effectiveness of calcitic lime (40% Ca, 4.5% Mg) and gypsum (22% Ca, 17% S) as sources of Ca for groundnut grown on sandy soils. Field experiments were established in smallholder farming areas using four levels of P (0, 8.5, 17 and 34 kg ha⁻¹) combined factorially with calcitic lime (0, 200, 400 and 800 kg ha⁻¹) to give 16 treatments. Similar levels of P were combined factorially with gypsum (0, 100, 200 and 400 kg ha⁻¹) to give sixteen treatments. Experiments were laid in a randomized complete block design with three replications. Phosphorus had a significant effect on groundnut yield at the majority of the experimental sites. Application of P at 8.5 kg ha⁻¹ gave the optimum groundnut yield response. The optimum application rates for calcitic lime and gypsum were 200 and 100 kg ha⁻¹. Gypsum and calcitic lime were not significantly different as sources of Ca for groundnut. Soil chemical properties were significantly improved following application of P and Ca sources.     

Evaluation of the wettability of spherical cement particle surfaces using penetration rate method

The wettability of cement particles is related to the fluidity of cement paste. This paper describes the mechanism of the higher fluidity imparted by the spherical cement particles in light of their wettability. In addition, the effects of gypsum on the wettability were also studied. This study has shown the following: (1) The weight of water and water-reducing agent solution penetrating the spherical cement powder bed is 24-150% higher than that for the ordinary Portland cement powder bed. This results in the improvement of the wettability of the particle surfaces of spherical cement. The high wettability of spherical cement contributes to its high fluidity. (2) The presence of many fine gypsum particles on the spherical cement particle surface reduces the wettability. (3) To prepare spherical cement, the optimum amount of gypsum added is determined by the acceleration of the formation of spherical particles and the wettability of particle surfaces.     

Impact of gypsum supersaturated process water on the interactions between silica and zinc sulphide minerals

Flotation recovery and selectivity problems have been reported in the flotation of fine sulphide minerals in gypsum supersaturated process water. In this study, the effect of gypsum supersaturated solution on the interactions between silica and sphalerite (ZnS) minerals was examined by observing deposition behaviour of silica nanoparticles on sphalerite surface using a quartz crystal microbalance with dissipation (QCM-D). Significant deposition of silica nanoparticles on ZnS coated sensor surface was observed in the gypsum supersaturated solution, indicating consequential slime coating of silica fines on sphalerite mineral surface. Substantial deposition of silica nanoparticles on SiO₂ coated surface was also observed suggesting strong homo-aggregation of silica fines in the gypsum supersaturated solution. The interaction behaviour between silica–sphalerite and silica–silica is mainly attributed to the high calcium concentration of the gypsum supersaturated solution. Similar deposition behaviour of silica nanoparticles onto ZnS or SiO₂ coated sensor surface was observed in 800 ppm calcium solution, which is similar to the calcium concentration of the gypsum supersaturated solution. Colloidal force measurement between a silica particle and a fractured sphalerite surface or a silica wafer surface by an atomic force microscopy (AFM) revealed attractive van der Waals force between the mineral particles in both gypsum supersaturated solution and 800 ppm calcium solution. The high calcium concentration of the gypsum supersaturated solution induced the hetero-aggregation between silica and sphalerite, accounting for the observed decrease in flotation selectivity.     

A hydration study of various calcium sulfoaluminate cements

The present work studies the hydration process and microstructural features of five calcium sulfoaluminate (CSA) cements and a ternary mixture including also ordinary Portland cement (OPC). The pastes were studied with simultaneous differential thermal-thermogravimetric (DTA-TG) analysis, mercury intrusion porosimetry (MIP), scanning electron microscopy (SEM), and expansion/shrinkage tests. The DTA-TG analysis confirmed the role of the hydration reactions involving the main CSA clinker constituent, tetracalcium trialuminate sulfate, which produced (i) ettringite when combined with lime and calcium sulfate, (ii) ettringite and aluminum hydroxide in the presence of calcium sulfate alone, and (iii) monosulfate and aluminum hydroxide in the absence of both lime and calcium sulfate. The MIP and SEM were able to discriminate between expansive (ternary mixture and CSA cement containing 50% gypsum) and non-expansive cements. Expansive cement pastes had (i) a nearly unimodal pore size distribution shifted toward higher radii and (ii) ettringite crystals smaller in size during the first day of curing. In a SEM image of a hardened paste of the CSA cement containing 50% gypsum, a stellate ettringite cluster was observed.     

Impact of gypsum supersaturated solution on surface properties of silica and sphalerite minerals

In some sulphide mineral flotation operations, the process water contains high concentrations of calcium and sulphate ions that exceed the solubility limit of gypsum. It has been speculated that the gypsum supersaturated process water would lead to precipitation of gypsum which could coat on mineral surfaces by either nucleation or coagulation, resulting in reduced flotation recovery and selectivity. In this study, a laboratory prepared gypsum supersaturated solution is used to represent the gypsum supersaturated process water, the effect of gypsum supersaturated solution on the surface properties of silica and sphalerite minerals was investigated using zeta potential distribution measurements, scanning electron microscope (SEM), X-ray photon spectroscopy (XPS), Auger electron spectroscopy (AES), and quartz crystal microbalance with dissipation (QCM-D). Our results show that silica and sphalerite minerals carry identical surface charge (−10 mV of zeta potential) in the gypsum supersaturated solution at pH 10 although they are charged differently in simple electrolyte solution at the same pH. Needle shape gypsum precipitates are found in both silica and sphalerite minerals systems conditioned with gypsum supersaturated solution. The gypsum precipitates do not grow on the minerals surfaces but form in the bulk gypsum supersaturated solution. The heterocoagulation between the examined minerals and gypsum particles is insignificant in the gypsum supersaturated solution. It is the high calcium concentration in the gypsum supersaturated solution that has significant effect on the surface properties of silica and sphalerite minerals. The zeta potentials of silica and sphalerite in a 800 ppm calcium solution (similar to the calcium concentration in the gypsum supersaturated solution) are similar to those measured in the gypsum supersaturated solutions. Both silica and sphalerite minerals surfaces are indiscriminately coated with calcium. The surface coating of calcium results in the identical surfaces between silica and sphalerite minerals, and ultimately causes problems for the flotation separation of silica and sphalerite.     

氨法生产硫酸钾的工艺研究

实验研究了氨作为硫酸钾结晶助剂,在常温常压下石膏和氯化钾在水盐相体系中有选择地结晶硫酸钾的原理及工艺流程。该流程具有节省热能,操作维护容易,效率高等优点。     

脱硫石膏制备粉刷石膏的试验研究

本文利用未煅烧的脱硫石膏制备高附加值的粉刷石膏,主要研究了外加剂和保水剂的种类、养护条件等对脱硫石膏基粉刷石膏制品性能的影响。结果表明:当脱硫石膏∶矿粉∶水泥∶硫铝酸盐水泥∶柠檬酸钾∶生石灰∶硫酸钾=365∶138∶48∶60∶0.5∶9.6∶0.5,水灰比为0.32时,获得了性能优异,满足国标JC/T517-2004要求的粉刷石膏。     

高温水泥浆体系研究与应用

针对土库曼斯坦南约洛坦气田膏盐层固井对高温抗盐水泥浆性能的要求,研究了高温缓凝剂GHN和高温抗盐降失水剂GFL.GHN由有机膦酸钠盐、有机酸组成,对水泥浆其它性能无不利影响,对水质和水泥品种适应性强,其加量与稠化时间具有良好的线性.GFL为单磺酸四元共聚物AA-AM-VP-AMPS,抗温达180℃,抗欠饱和盐水.为提高固井质量,在高温水泥浆中还使用了硅粉、稳定剂及微膨胀剂.该高温水泥浆性能优越,应用温度范围为100～180℃,失水量在100mL以内,在土库曼的7口井中进行了试验,现场施工顺利,固井质量合格率为100％,解决了该气田高温盐膏层固井技术难题及高压、多气层固井过程中井漏与气侵并存的问题.