Estimation of unfrozen water content of saturated sandstones using nuclear magnetic resonance, mercury intrusion porosimetry, and ultrasonic tests

The unfrozenwater content(UWC)is a crucial parameter that affects the strength and thermal properties of rocks in relation to engineering construction and geological disasters in cold regions.In this study,three different methods were employed to test and estimate the UWC of saturated sandstones,including nuclear magnetic resonance(NMR),mercury intrusion porosimetry(MIP),and ultrasonic methods.The NMR method enabled the direct measurement of the UWC of sandstones using the free induction decay(FID).The MIP method was used to analyze the pore structures of sandstones,with the UWC subsequently calculated based on pore ice crystallization.Therefore,the MIP test constituted an indirect measurement method.Furthermore,a correlation was established between the P-wave velocity and the UWC of these sandstones based on the mixture theory,which could be employed to estimate the UWC as an empirical method.All methods demonstrated that the UWC initially exhibited a rapid decrease from 0C to5C and then generally became constant beyond20C.However,these test methods had different characteristics.The NMR method was used to directly and accurately calculate the UWC in the laboratory.However,the cost and complexity of NMR equipment have precluded its use in the field.The UWC can be effectively estimated by the MIP test,but the estimation accuracy is influenced by the ice crystallization process and the pore size distribution.The P-wave velocity has been demonstrated to be a straightforward and practical empirical parameter and was utilized to estimate the UWC based on the mixture theory.This method may be more suitable in the field.All methods confirmed the existence of a hysteresis phenomenon in the freezing-thawing process.The average hysteresis coefficient was approximately 0.538,thus validating the GibbseThomson equation.This study not only presents alternative methodologies for estimating the UWC of saturated sandstones but also contribute to our understanding of the freezing-thawing process of pore water.

Estimation of the unfrozen water content of saturated sandstones by ultrasonic velocity

The unfrozen water content(UWC)of rocks at low temperature is an important index for evaluating the stability of the rock engineering in cold regions and artificial freezing engineering.This study addresses a new method to estimate the UWC of saturated sandstones at low temperature by using the ultrasonic velocity.Ultrasonic velocity variations can be divided into the normal temperature stage(20 to 0℃),quick phase transition stage(0 to-5℃)and slow phase transition stage(-5 to-25℃).Most increment of ultrasonic velocity is completed in the quick phase transition stage and then turns to be almost a constant in the slow phase transition stage.In addition,the UWC is also measured by using nuclear magnetic resonance(NMR)technology.It is validated that the ultrasonic velocity and UWC have a similar change law against freezing and thawing temperatures.The WE(weighted equation)model is appropriate to estimate the UWC of saturated sandstones,in which the parameters have been accurately determined rather than by data fitting.In addition,a linear relationship between UWC and ultrasonic velocity is built based on pore ice crystallization theory.It is evidenced that this linear function can be adopted to estimate the UWC at any freezing temperature by using P-wave velocity,which is simple,practical,and accurate enough compared with the WE model.

A model of unfrozen water content in rock during freezing and thawing with experimental validation by nuclear magnetic resonance

The unfrozen water content of rock during freezing and thawing has an important influence on its physical and mechanical properties.This study presented a model for calculating the unfrozen water content of rock during freezing and thawing process,considering the influence of unfrozen water film and rock pore structure,which can reflect the hysteresis and super-cooling effects.The pore size distribution cu rves of red sandsto ne and its unfrozen water conte nt under different temperatures during the freezing and thawing process were measured using nuclear magnetic resonance(NMR) to validate the proposed model.Comparison between the experimental and calculated results indicated that the theoretical model accu rately reflected the water content change law of red sandstone during the freezing and thawing process.Furthermore,the influences of Hamaker constant and surface relaxation parameter on the model results were examined.The results showed that the appropriate magnitude order of Hamaker constant for the red sandstone was 10J to 10J;and when the relaxation parameter of the rock surface was within 25-30 μm/ms,the calculated unfrozen water content using the proposed model was consistent with the experimental value.

Hysteresis in the ultrasonic parameters of saturated sandstone during freezing and thawing and correlations with unfrozen water content

Determining the mechanical properties of frozen rock is highly important in cold-area engineering.These properties are essentially correlated with the content of liquid water remaining in frozen rock.Therefore,accurate determination of unfrozen water content could allow rapid evaluation of mechanical properties of frozen rock.This paper investigates the hysteresis characteristics of ultrasonic waves applied to sandstone(in terms of the parameters of P-wave velocity,amplitude,dominant frequency and quality factor Q)and their relationships with unfrozen water content during the freeze-thaw process.Their correlations are analysed in terms of their potential for use as indicators of freezing state and unfrozen water content.The results show that:(1)During a freeze-thaw cycle,the ultrasonic parameters and unfrozen water content of sandstone have significant hysteresis with changes in temperature.(2)There are three clear stages of change during freezing:supercooled stage(0℃to-2℃),rapid freezing stage(-2℃to-3℃),and stable freezing stage(-3℃to-20℃).The changes in unfrozen water content and ultrasonic parameters with freezing temperature are inverse.(3)During a single freeze-thaw cycle,the ultrasonic parameters of sandstone are significantly correlated with its unfrozen water content,and this correlation is affected by the pore structure.For sandstones with mesopores greater than 50%,there are inflection points in the curves of ultrasonic parameters vs.unfrozen water content at-3℃during freezing and at-1℃during thawing.It was found that thermal deformation of the mineral-grain skeleton and variations in the phase composition of pore water change the propagation path of ultrasonic waves.The inflection point in the curve of dominant frequency vs.temperature clearly marks the end of the rapid freezing stage of pore water,in which more than 70%of the pore water freezes.Consequently,the dominant frequency can be used as an index to conveniently estimate the unfrozen water content of frozen rock and,hence,its mechanical properties.

Effectiveness of gelatin solidification for unfrozen preservation and transportation of astrocytes

We herein studied a non-cryogenic cell preservation and transportation method. We found that astrocytes can be preserved in an unfrozen state at 4℃ (without medium exchange), while maintaining good condition in comparison with cryopreservation for the periods of 5 - 7 days. The gelatin solidification method can also prevent decreases in survival rate by preventing damage to astrocytes during transportation. Therefore, the gelatin solidification method at 4℃ may be a useful choice for short-term preservation and transportation.

Effects of thawing-induced softening on fracture behaviors of frozen rock

Due to the presence of ice and unfrozen water in pores of frozen rock,the rock fracture behaviors are susceptible to temperature.In this study,the potential thawing-induced softening effects on the fracture behaviors of frozen rock is evaluated by testing the tension fracture toughness(KIC)of frozen rock at different temperatures(i.e.-20℃,-15℃,-12℃,-10℃,-8℃,-6℃,-4℃,-2℃,and 0℃).Acoustic emission(AE)and digital image correlation(DIC)methods are utilized to analyze the microcrack propagation during fracturing.The melting of pore ice is measured using nuclear magnetic resonance(NMR)method.The results indicate that:(1)The KIC of frozen rock decreases moderately between-20℃ and-4℃,and rapidly between-4℃ and 0℃.(2)At-20℃ to-4℃,the fracturing process,deduced from the DIC results at the notch tip,exhibits three stages:elastic deformation,microcrack propagation and microcrack coalescence.However,at-4℃e0℃,only the latter two stages are observed.(3)At-4℃e0℃,the AE activities during fracturing are less than that at-20℃ to-4℃,while more small events are reported.(4)The NMR results demonstrate a reverse variation trend in pore ice content with increasing temperature,that is,a moderate decrease is followed by a sharp decrease and-4℃ is exactly the critical temperature.Next,we interpret the thawing-induced softening effect by linking the evolution in microscopic structure of frozen rock with its macroscopic fracture behaviors as follow:from-20℃ to-4℃,the thickening of the unfrozen water film diminishes the cementation strength between ice and rock skeleton,leading to the decrease in fracture parameters.From-4℃ to 0℃,the cementation effect of ice almost vanishes,and the filling effect of pore ice is reduced significantly,which facilitates microcrack propagation and thus the easier fracture of frozen rocks.

冰水赋存演化下冻结土石混合体-结构界面强度劣化机制及模型

温升下冻结土石混合体-结构界面层孔隙内冰水赋存改变极易诱发强度劣化,而目前界面强度劣化机制及劣化规律定量表征的相关研究存在空白。制备0%,15%,30%,45%等4种含石率组合体试样,通过核磁共振、直剪试验研究了正融过程冰水赋存演化下界面强度劣化特性,结合莫尔-库仑准则首次提出以薄膜水及毛细水含量变化率为参变量的强度劣化模型。得到结论:含石改变界面孔隙结构分布使毛细水占比升高;温升下界面抗剪强度劣化程度随含石率增加而降低;正融后不同含石率界面黏聚力衰减程度均大于内摩擦角衰减程度;黏聚力、内摩擦角与未冻水含量关系曲线分别呈阶段非线性特点及两阶段线性特点,其实质在于薄膜水及毛细水发育使得界面黏聚力和内摩擦角产生不同程度及形式的劣化。模型分析表明:随含石率升高,薄膜水及毛细水劣化系数具有“此消彼长”的特性,颗粒间及颗粒与结构接触面滑动摩擦强度和咬合摩擦强度劣化比例系数分别呈现下降、上升趋势。

基于土−水特征曲线的非饱和冻土未冻水含量预测

对非饱和土体在冻结温度以下土中未冻水含量进行了理论分析,给出了一种简便的预测方法及其数学模型。基于非饱和土孔隙中气液两相的化学平衡和力学平衡关系,结合土−水特征曲线,给出了以Van Genuchten土−水特征曲线模型参数表示的土体孔隙体积分布密度函数,且水分冻结与土体孔径分布密切相关。根据初始有效饱和度对应的液态水填充的最大孔径和一定冻结温度对应的起始结晶孔径之间的关系,分析了土体孔隙中冰水相变的特征及其临界有效饱和度。当初始有效饱和度超过临界结晶饱和度后,冻结现象才会发生。给出了非饱和土体在冻结温度以下土中未冻水饱和度的预测公式,并通过已有的试验结果对其有效性进行了验证。

Experimental study on the movement of oil spill under freeze-thaw action

Oil leakages cause environmental pollution,economic losses,and even engineering safety accidents.In cold regions,researchers urgently investigate the movement of oil spill in soils exposed to freeze-thaw cycles.In this study,a series of laboratory model experiments were carried out on the migration of oil leakage under freeze-thaw action,and the distributions of the soil temperature,unfrozen water content,and displacement were analyzed.The results showed that under freeze-thaw action,liquid water in soils migrated to the freezing front and accumulated.After the pipe cracked,oil pollutants first gathered at one side of the leak hole,and then moved around.The pipe wall temperature affected the soil temperature field,and the thermal influence range below and transverse the pipe wall(35–40 cm)was larger than that above the pipe wall(8 cm)owing to the soil surface temperature.The leaked oil's temperature would make the temperature of the surrounding soil rise.Oil would inhibit the cooling of the soils.Besides,oil migration was significantly affected by the gravity and water flow patterns.The freeze-thaw action would affect the migration of the oil,which was mainly manifested as inhibiting the diffusion and movement of oil when soils were frozen.Unfrozen water transport caused by freeze-thaw cycles would also inhibit oil migration.The research results would provide a scientific reference for understanding the relationship between the movement of oil pollutants,water,and soil temperature,and for establishing a waterheat-mass transport model in frozen soils.

基于核磁共振技术的土体冻结特征曲线试验研究

冻结特征曲线描述了土中未冻水含量随温度变化的规律,给出适用不同土质的冻结特征曲线计算模型具有重要的工程价值。利用核磁共振技术对6种土体的冻结特征曲线进行了测试,给出了描述土体冻结特征曲线的Michalowski模型参数的确定方法,分析了初始含水率和土体性质对冻结特征曲线的影响,利用Michalowski模型参数的特征对模型进行了改进。研究表明,冻结特征曲线与初始含水率无关,冻结过程中不同初始含水率土体的冻结特征曲线相同。在不考虑温度影响时,模型参数wa近似等于土中最大结合水含量,可以作为分析和评价黏性土特性的重要指标参数。改进后的单参数Michalowski模型可实现对未冻水含量的良好预测,降低了模型的复杂性,提升了模型的实用价值,但模型的适用范围,有待验证。

易溶盐含量对伊犁黄土未冻水含量影响研究

处于常年季冻区的伊犁河谷自然灾害频发主要与伊犁黄土的未冻水含量有关,土体中分布不均匀的盐分影响着未冻水含量的变化趋势。采用低频核磁共振技术分析了不同Na_(2)SO_(4)含量下未冻水含量随温度的变化关系,并提出了与易溶盐含量有关的未冻水数学模型。研究表明,Na_(2)SO_(4)含量主要在正温降温阶段以及冻结温度附近自由水冻结阶段对伊犁黄土未冻水含量产生影响;在冻结温度附近易溶盐分别对未冻水含量减小起抑制和促进作用,未析出含盐量越高,抑制作用越明显;温度越低,初始含盐量对未冻水含量的影响越小。

粉煤灰对膨胀土未冻水含量的影响——基于低场核磁共振技术检测

为探究冻融循环条件下粉煤灰对膨胀土未冻水含量的影响,利用低场核磁共振(nuclear magnetic resonance,NMR)技术对不同粉煤灰掺量(3%、6%、9%、12%和15%)的改性膨胀土进行T2谱测定,分析不同温度下改性膨胀土的孔隙结构变化特征,并得出不同粉煤灰掺量的改性膨胀土未冻水含量的变化规律。试验结果表明:改性膨胀土相较于原状土,微、小孔隙的孔径分布在掺灰比为9%的试样出现降低,其余掺灰比的试样出现增长,掺灰比为6%的试样最显著;中孔隙增幅最显著的是掺灰比为12%的试样,大孔隙增幅最显著的是掺灰比为3%的试样;在冻结过程中,掺灰比为9%的试样未冻水含量在下降阶段变化最快,在融化阶段变化速率最慢;掺入粉煤灰降低了土壤的相变温度,且抑制土体冻结过程中的未冻水含量。

冻融循环作用下土石混合体水-热-变形相互作用过程研究

冻融循环作用显著影响土石混合体的水-热-变形相互作用过程及力学特性。基于此,本文开展了单向冻融循环作用下土石混合体水-热-变形相互作用及无侧限抗压强度试验。通过单向冻融循环装置对30%砾石含量的土石混合体进行了4次单向冻融循环试验,每次循环根据设定的温度变化曲线持续168小时,模拟实际自然环境中冻结和融化的周期。同时,利用微机控制电液伺服万能试验机开展了未冻融和冻融循环后试样的力学特性测试,并探讨了冻融循环对土石混合体微观结构劣化机理的影响。研究结果表明:单向冻融循环对试样内温度、水分和变形有显著影响。冻融循环过程中土石混合体的融化速率大于冻结速率,试样在冻融循环过程中存在着体积未冻水的迁移和重分布。第一次冻融循环对土石混合体变形影响最为显著,试样的净变形随着冻融循环次数的增加先增大后趋于稳定。此外,反复的单向冻融循环改变了试样的孔隙结构。冻融循环后试样的抗压强度和变形模量分别减小了45.31%和60.92%,其衰减幅值随着冻融循环次数的增加而降低。

细粒含量对冻结粉质黏土力学特性的影响

季节冻土力学性能对工程影响显著,季节冻土中细粒含量是其力学性质的重要参数。为研究细粒含量对季节冻土强度的影响,通过冻土三轴试验,研究了不同细粒含量(40%、45%、50%、60%、70%)、不同冻结温度(-5℃、-10℃、-15℃)、不同围压(50 kPa、80 kPa、120 kPa)下冻结粉质黏土的力学性质。结果表明:试样的三轴应力-应变曲线均为软化型。同一细粒含量下,随着冻结负温的降低,土样峰值强度逐渐增大,其中-10~-5℃增长比-15~-10℃更加剧烈。随细粒含量的增加,土体脆性指数分布呈现抛物线形,土样黏聚力呈现上升趋势,而土样内摩擦角减小。同时,采用测温法得出了各细粒含量下未冻水含量分布,建立了冻土黏聚力在不同负温下随细粒含量变化的计算模型,能较好地预估任意冻结负温及任意细粒含量下冻土黏聚力。

考虑孔隙比的冻胀弱敏感性土修正PCHeave模型研究

针对我国严寒地区高速铁路路基填料和机场填方等工程具有严格的压实度要求,而考虑孔隙比的冻胀弱敏感性土冻胀影响研究尚未有系统性的理论分析,采用理论与经验分析相结合的方法,基于冻胀弱敏感性土的孔隙比与渗透系数和未冻水含量之间的关系,建立考虑孔隙比的修正PCHeave模型。基于该模型分析孔隙比与冻胀量、冻结深度和冻胀率之间的关系,并进行试验对比验证。研究结果表明:孔隙比与冻胀弱敏感性土的未冻水含量之间存在很好的线性关系;冻胀弱敏感性土的冻胀量和冻胀率均随孔隙比先增大再减小,即存在一个最不利孔隙比使得冻胀量和冻胀率均达到最大值;冻胀弱敏感性土的冻结深度随孔隙比增大而逐渐增大;若仅考虑孔隙比对饱和渗透系数的影响,冻胀量和冻胀率均随孔隙比显著增加,若仅考虑孔隙比对未冻水含量的影响,冻胀量和冻胀率均随孔隙比减小,但减小幅度很小。冻胀弱敏感性土通常被认为不能产生显著冻胀,在一定孔隙比下也能产生较大冻胀,同时考虑孔隙比对饱和渗透系数与未冻水含量的影响要更合理。冻胀弱敏感性土的冻胀不能忽略孔隙比的变化,与试验结果对比,该模型能够较好地描述孔隙比对冻胀弱敏感性土的冻胀影响。

冻土未冻水含量与其微结构相关试验分析研究

在既定负温下冻土中未冻水和固相冰的动态关系与其初始含水率密切相关,冻土中未冻水含量的改变直接影响了其微观结构的变化,加强不同初始含水率下冻土的未冻水含量与微观结构的定量关系研究对于揭示冻土特殊的物理力学性质具有重要的意义。本文利用新型冷冻扫描电镜对既定负温不同初始含水率(11.8%、23.1%、32.2%、42.2%、54.1%、64.2%、74.8%)下的冻结黏土进行微观结构测试,揭示了不同初始含水率下冻土微观结构的演化特征。同时,利用核磁共振技术测试不同初始含水率和不同温度下冻土的未冻水含量变化过程,探讨了既定负温下初始含水率对冻土未冻水含量与其微结构之间的定量关系。研究结果表明:冻结黏土含水率在液限范围内,随着初始含水率的增加,孔隙结构由集合物间孔隙向粒间孔隙发育,含水率超过液限后,随着初始含水率增加,超集合物间孔隙开始发育,并且在同一负温条件下,随着初始含水率的增加,孔隙分形维数和孔隙面积随之增大;对于高温冻土,随着初始含水率的增加,孔隙分形维数随未冻水含量的增加而增加,对于低温冻土,孔隙分形维数随未冻水含量的减少而增加;最后,建立了不同试验条件下冻土微观结构与其未冻水含量的经验方程,为揭示冻土特殊物理力学特性提供理论基础。

富水地层多圈水平杯型冻结温度场分布形式及变化机理研究

为了掌握富水地层多圈水平杯型冻结温度场的分布形式及发展规律,以昆明地铁城市轨道交通5号线冻结加固工程为背景,通过现场监测、数值计算、室内试验对冻结帷幕温度场变化规律及内在机理展开研究,分析冻结壁温度场在形成过程中的变化规律.试验结果表明:在外部降温计划的作用下,冻结壁温度场按照温度变化过程分为快速降温阶段、潜热释放阶段、稳定温度阶段及冻结维护阶段4个阶段.各阶段曲线变化速率与加固范围内试样未冻水含量变化具有一定的关联,未冻水往往通过影响比热容、导热系数与潜热等热参数对冻结壁温度场的变化规律从而影响到整体下的温度场分布规律.未冻水含量变化通过改变冻结冰体圆柱与土柱的几何位置关系从而影响试样冻结过程中的热传导形式,其中比热容在正温阶段时随温度降低逐渐增加.

正融过程中盐渍土路基抗剪强度影响因素分析

对冀北地区非饱和盐渍土进行了正融过程中三种压实度和10个温度节点的直剪试验,用土壤参数速测平台记录了正融过程中土体的温度发展及孔隙水相变过程,并分析了未冻水、压实度对其力学特性的影响关系。结论如下:在正融过程中,该盐渍土未冻水含量的变化呈现出“四阶段”,其中未冻水速增阶段相较于盐结晶失水阶段,增速较快。随着压实度的增大,土体温度变化速率、未冻水含量的增长以及试件强度下降速率都越快,黏聚力增加程度明显大于内摩擦角。当压实度较小、温度较低时,应力应变曲线则呈现脆性破坏特征。此外,土体黏聚力随温度的升高而显著降低,内摩擦角则出现很小幅度的增大,在-2℃到1℃之间,两者均出现短暂回滞现象。

单向冻结条件下非饱和土水分迁移规律研究

为了揭示路基冻结过程中地下水和土性对水分迁移规律的影响,针对开放体系和封闭体系的粉质黏土和砂土进行了单向冻结条件下的水分迁移试验。通过土柱上层位置设置碎石层,阻断液态水迁移路径,监测冻结过程中土柱的水热变化,结合土柱冻结深度、冻结速率曲线、含水率分布曲线和补水时程曲线,分析仅水汽补给时对土柱顶部水分聚集和冻结特征的影响。试验结果发现,无论是封闭体系还是开放体系,粉质黏土和砂土土柱都会在冻结区中形成两处水分聚集区:第一水分聚集区为控温板底部,以霜的形式聚集,主要是由土柱顶部土体的水汽迁移并凝华相变形成;第二水分聚集区为冻结区中液态水和气态水共同迁移形成,随着冻结锋面的向下推移,形成不连通孔隙的界面,液态水向0℃冰锋线迁移聚集并相变成冰,水汽迁移路径受阻而凝华成冰,致使该处含水率显著增加。相较于封闭体系,开放体系使两处水分聚集区产生更大的水分增量。相比于粉质黏土,砂土介质孔隙较大,在试验时间内水汽补给对水分聚集区的影响更明显,但由于砂土持水能力减弱,水汽补给速率随时间逐渐减小。

冻融作用下水泥改良土未冻水含量及孔隙特征试验研究

水泥基材料注浆是控制人工冻结地层冻融变形普遍有效的措施。基于核磁共振技术,对冻融作用下不同水泥掺量的粉质黏土未冻水含量及冻融前后孔隙特征进行测试,结合扫描电镜和压汞技术分析了冻融前后水泥改良土的孔隙特征变化规律及冻融损伤微观机理。结果表明:①含水量一定时,随着水泥掺量的增大,孔隙中水分子磁化程度对温度的敏感性先增大后减小;②当水泥掺量为0~10%时,正融过程同一温度下,随着水泥掺量的增加,冻结土体中未冻水含量先减小后增大;③相比于未掺水泥的粉质黏土,水泥改良粉质黏土冻融前后孔隙的变化程度较小,当水泥掺量为5%时,其孔隙特征及微观结构受冻融循环影响较小。研究结果可为改良土体抗冻融损伤研究及人工冻结工程地层冻胀融沉稳定性控制提供参考。