Investigation of reinforcement of the modified carbon black from wasted tires by nuclear magnetic resonance

Pyrolysis has the potential of transforming waste into recyclable products. Pyrolytic carbon black (PCB) is one of the most important products from the pyrolysis of used tires. Techniques for surface modifications of PCB have been developed. One of the most significant applications for modified PCB is to reinforce the rubber matrix to obtain high added values. The transverse relaxation and the chain dynamics of vulcanized rubber networks with PCB and modified PCB were studied and compared with those of the commercial carbon blacks using selective 1H transverse relaxation (T2) experiments and dipolar correlation effect (DCE) experiments on the stimulated echo. Demineralization and coupling agent modification not only intensified the interactions between the modified PCB and the neighboring polyisoprene chains, but also increased the chemical cross-link density of the vulcanized rubber with modified PCB. The mechanical testing of the rubbers with different kinds of carbon blacks showed that the maximum strain of the rubber with modified PCB was improved greatly. The mechanical testing results confirmed the conclusion obtained by nuclear magnetic resonance (NMR). PCB modified by the demineralization and NDZ-105 titanate coupling agent could be used to replace the commercial semi-reinforcing carbon black.

Characterization of Average Molecular Structure of Heavy Oil Fractions by ~1H Nuclear Magnetic Resonance and X-ray Diffraction

The chemical structure of heavy oil fractions obtained by liquid-solid adsorption chromatography was character-ized by 1 H nuclear magnetic resonance and X-ray diffraction.The molecular weight and molecular formula of asphaltene molecules were estimated by combining 1 H nuclear magnetic resonance and X-ray diffraction analyses,and were also ob-tained from vapor pressure osmometry and elemental analysis.Heteroatoms,such as S,N,and O atoms,were considered in the construction of average molecular structure of heavy oils.Two important structural parameters were proposed,including the number of alkyl chain substituents to aromatic rings and the number of total rings with heteroatoms.Ultimately,the av-erage molecular structures of polycyclic aromatics,heavy resins and asphaltene molecules were constructed.The number of α-,β-,γ-,and aromatic hydrogen atoms of the constructed average molecular structures fits well with the number of hydro-gen atoms derived from the experimental spectral data.

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.

Utilization of nuclear magnetic resonance (NMR) in the determination of water status on rice seeds

The relation between seed viability and waterstatus in seed was studied.The experimentwas carried out at Zhongshan University.Seeds of hybrid rice Shanyou 63 were collectedfrom Guangdong Academy of Agriculture Sci-ences in 1993 and then stored for one year inopen air or with silica gel.Before and afterstorage,the relative content of free water andbound water in seeds were measured with

A new permeability calculation method using nuclear magnetic resonance logging based on pore sizes: A case study of bioclastic limestone reservoirs in the A oilfield of the Mid-East

It is difficult to accurately obtain the permeability of complex lithologic reservoirs using conventional methods because they have diverse pore structures and complex seepage mechanisms.Based on in-depth analysis of the limitation of classical nuclear magnetic resonance(NMR)permeability calculation models,and the understanding that the pore structure and porosity are the main controlling factors of permeability,this study provides a new permeability calculation method involving classifying pore sizes by using NMR T_2 spectrum first and then calculating permeability of different sizes of pores.Based on this idea,taking the bioclastic limestone reservoir in the A oilfield of Mid-East as an example,the classification criterion of four kinds of pore sizes:coarse,medium,fine and micro throat,was established and transformed into NMR T_2 standard based on shapes and turning points of mercury intrusion capillary pressure curves.Then the proportions of the four kinds of pore sizes were obtained precisely based on the NMR logging data.A new NMR permeability calculation model of multicomponent pores combinations was established based on the contributions of pores in different sizes.The new method has been used in different blocks.The results show that the new method is more accurate than the traditional ones.

Application of nuclear magnetic resonance technology to carbon capture,utilization and storage:A review

Carbon capture,utilization and storage (CCUS) is considered as a very important technology for mitigating global climate change.Carbon dioxide (CO2) injected into an underground reservoir will induce changes in its physical properties and the migration of CO2 will be affected by many factors.Accurately understanding these changes and migration characteristics of CO2 is crucial for selecting a CCUS project site,estimating storage capacity and ensuring storage security.In this paper,the basic principles of nuclear magnetic resonance (NMR) and magnetic resonance imaging (MRI) technologies are briefly introduced in the context of laboratory experiments related to CCUS.The types of NMR apparatus,experimental samples and testing approaches applied worldwide are discussed and analyzed.Then two typical NMR core analysis systems used in CCUS field and a self-developed high-pressure,low-field NMR rock core flooding experimental system are compared.Finally,a summary of the current deficiencies related to NMR applied to CCUS field is given and future research plans are proposed.

Relaxation study of cement based grouting material using nuclear magnetic resonance

Aiming at actual condition of poor effect of hole sealing for the reason of poor cement paste fluidity in the process of coal mine gas drainage,by adding a water reducing agent,cement paste for hole sealing was produced.The changes of initial distribution,weighted average values and total relaxation signal intensity of transverse relaxation time(T 2) of water in pure cement paste and water reducing agent added cement paste were studied with low field proton nuclear magnetic resonance(NMR).The results show that there are four peaks in T2 distribution curves of cement paste:the first peak is related to the bound water in flocculation,the second and the third peaks are related to the water in flocculation,water reducing agent makes it extending towards the long relaxation time,increasing its liquidity,and the fourth peak is related to the free water.By using weighted average values of T2 and total relaxation signal intensity,hydration process of cement pastes could be roughly divided into four stages:the initial period,reaction period,accelerated period and steady period.By analyzing the periods,it makes sure that the grouting process should be completed in the reaction period in the site,and the drainage process should be started in the steady period.The results have great guiding significance to the hole sealing and methane drainage.

Review of nuclear magnetic resonance studies on iron-based superconductors

The newly discovered iron-based superconductors have triggered renewed enormous research interest in the condensed matter physics community. Nuclear magnetic resonance （NMR） is a low-energy local probe for studying strongly correlated electrons, and particularly important for high-Tc superconductors. In this paper, we review NMR studies on the structural transition, antiferromagnetic order, spin fluctuations, and superconducting properties of several iron-based high-Tc superconductors, including LaFeAsOl_xFx, LaFeAsOl_x, BaFe2As2, Bal_xKxFe2As2, Cao.23Nao.67Fe2As2, BaFe2（Asl_xPx）2, Ba（Fel_xRux）2As2, Ba（Fel_xCox）2As2, Lil＋xFeAs, LiFel_xCoxAs, NaFeAs, NaFel_xCoxAs, KyFe2_xSe2, and （T1,Rb）yFe2_xSe2.

Three dimensional structure prediction and proton nuclear magnetic resonance analysis of toxic pesticides in human blood plasma

The purpose of this study was to investigate the nuclear magnetic resonance （NMR） assignments of hydrolyzed products extracted from human blood plasma. The correlations between chemical, functional and structural prop- erties of highly toxic pesticides were investigated using the PreADME analysis. We observed that toxic pesticides possessed higher molecular weight and, more hydrogen bond donors and acceptors when compared with less toxic pesticides. The occurrence of functional groups and structural properties was analyzed using ~H-NMR. The ~H- NMR spectra of the phosphomethoxy class of pesticides were characterized by methyl resonances at 3.7-3.9 ppm （8） with the coupling constants of 11-16 Hz （Je-cns）. In phosphoethoxy pesticides, the methyl resonance was about 1.4 ppm （8） with the coupling constant of 10 Hz （Je-cH2） and the methylene resonances was 4.2-4.4 ppm （8） with the coupling constant of 0.8 Hz （Jp-cH3）, respectively. Our study shows that the values of four parameters such as chemical shift, coupling constant, integration and relaxation time correlated with the concentration of toxic pesticides, and can be used to characterise the proton groups in the molecular structures of toxic pesticides.

Nuclear magnetic resonance measurement station in SECUF using hybrid superconducting magnets

Nuclear magnetic resonance （NMR） is one of the most powerful tools to explore new quantum states of condensed matter induced by high magnetic fields at a microscopic level. High magnetic field enhances the intensity of the NMR signal, and more importantly, can induce novel phenomena. In this article, examples are given on the field-induced charge density wave （CDW） in high-To superconductors and on the studies of quantum spin liquids. We provide a brief introduction to the high magnetic field NMR platform, the station 4 of the Synergetic Extreme Condition User Facility （SECUF）, being built at Huairou, Beijing.

Nuclear magnetic resonance study of the formation and dissociation process of nature gas hydrate in sandstone

In this work,the authors monitored the formation and dissociation process of methane hydrate in four different rock core samples through nuclear magnetic resonance(NMR)relaxation time(T_(2))and 2D imaging measurement.The result shows that the intensity of T_(2) spectra and magnetic resonance imaging(MRI)signals gradually decreases in the hydrate formation process,and at the same time,the T_(2) spectra move toward the left domain as the growth of hydrate in the pores of the sample accelerates the decay rate.The hydrate grows and dissociates preferentially in the purer sandstone samples with larger pore size and higher porosity.Significantly,for the sample with lower porosity and higher argillaceous content,the intensity of the T_(2) spectra also shows a trend of a great decrease in the hydrate formation process,which means that high-saturation gas hydrate can also be formed in the sample with higher argillaceous content.The changes in MRI of the sample in the process show that the formation and dissociation of methane hydrate can reshape the distribution of water in the pores.

Analysis of Internal Moisture Change of Camphor Seeds during Drying by Low-Field NMR

In this study,low-field nuclear magnetic resonance(LF-NMR)was used to collect the transverse relaxation signals of camphor seeds that had been dried at different temperatures and for different durations.The transverse relaxation time of the hydrogen nucleus was obtained by SIRT(Simultaneous Iterative Reconstruction Technique)inversion,and the correlation between the moisture content on dry basis and the amplitude of NMR signal of camphor seeds sampled at different drying stages was analyzed.The results showed that water existed in three main forms strongly bound water,weakly bound water and free water in camphor seeds.During the drying process,the peak position of strongly bound water remained unchanged,but the peak positions of weakly bound water and free water fluctuated.Drying rate increased with drying temperature increasing.In addition,there was a very significant linear relationship between the total NMR signal amplitude and moisture content on dry basis,and the correlation coefficient reached 0.984 4.

NMR signal separation of ionic liquids by poly( sodium-p-styrenesulfonate)-assisted chromatographic NMR spectroscopy--Dedicated to Professor Xiuwen Han on the occasion of her 80th birthday

Diffusion-ordered nuclear magnetic resonance spectroscopy(DOSY),dubbed chromato-graphic NMR spectroscopy,can be used to simultaneously distinguish and identify the structures of components in a mixture according to their different diffusion coefficients.In order to improve the resolution of DOSY on the diffusion dimension,a lot of matrices have been developed to expand the application of this technique in mixture analysis.However,there is no matrix to detect the mixture of ionic liquids(ILs).Herein,we introduced a new matrix,poly(sodium-p-styrenesulfonate)(PSSNa),which can be used to fully separate the signals of a mixture of different ILs.The mixture of three imidazolium ILs of 1-butyl-3-methylimidazolium bromide,1-allyl-3-vinylimidazolium bromide and 1-arboxymethy-3-methylimidazolium chloride could be fully distinguished by virtue of their different interactions with PSSNa.We also investigated the influences of PSSNa amount,IL con-centration and solution pH value on the signal resolution of mixtures.This work provides a scientific reference for the analysis of the other IL analytes.

Conformational dynamics in GPCR signaling by NMR

G-protein-coupled receptors(GPCRs)mediate a wide range of cellular responses to various ligands or stimuli,and are the most important drug targets associated with human diseases.While major advances in GPCR structural biology have greatly deepened our understanding of its activation mechanism,the highly complex changes in the structural dynamics of GPCRs during activation remain underdetermined and their links to physiological functions largely unknown.Solution nuclear magnetic resonance(NMR)spectroscopy is an essential technique that allows the characterization of protein structural dynamics at atomic level,and has been applied in the studies of GPCR structural-function relationship in the past decade.Herein,we summarize a few specific studies in which solution NMR methods were employed and provided novel insights into questions difficult to be addressed by other methods.

Further discussion of CO_(2) huff-n-puff mechanisms in tight oil reservoirs based on NMR monitored fluids spatial distributions

Due to the poor physical properties of tight reservoirs,CO_(2) huff-n-puff(HNP)is considered a potential enhanced oil recovery(EOR)method after primary depletion.Optimization plays a critical role in the effective implementation of CO_(2) huff-n-puff.But the optimization requires a good understanding of the EOR mechanisms.In this work,the spatial distribution of oil saturation under different experimental conditions was analyzed by the NMR method to further discuss the HNP mechanisms.According to the variation of 1D frequency signal amplitude,we divided the core into the hardly movable area and movable area,the region with the obvious signal decline was defined as the movable area,and the hardly movable area was the region with limited signal decline.Based on that the recovery characteristics of different scenarios were evaluated.Firstly,the necessity of the soaking stage was studied,where three scenarios with different soaking times were carried out.Secondly,the injection pressure was adjusted to investigate the effect of the pressure gradient.The T_(2) spectra show that soaking has significantly improved the production of crude oil in small pores,and higher oil recovery in a single cycle is observed,but it is lower when the elapsed time(total operation time)is the same.31.03% of oil can be recovered after 3 cycles HNP,which increases to 33.8% and 37.06% for the 4 cycles and 6 cycles cases.As the pressure gradient increases,more oil is removed out of the matrix,and the oil in the deep part of the reservoir can be effectively recovered.During the CO_(2) huff-n-puff process,the oil distributions are similar to the solution gas drive,the residual oil is distributed at the close end of the core and the range that the oil can be efficiently recovered is limited.

Found Different Attitude Fracture Characteristics of the NMR Curve by Application of 3D Printing Samples

Nuclear magnetic resonance (NMR) has many advantages, such as little testing time, no harm to rock specimen, and is widely used in the measurement of reservoir pore structure. 3D printing also has many advantages, such as repeating the printing the same attributes samples, forming sample by known rock pore structure, adding different pores or fractures to sample. For the study of fractured reservoir provides a new train of thought by combining NMR and 3D printing. Nuclear magnetic core analysis is an important work in the study of core, using a T2 spectrum at a certain echo time can also be found in the core fractures. The study, by CT scans to establish reservoir pore structure, based on the basic of adding different attitude fracture forming four fracture characteristics of rock sample, using 3D printing for solid sample, through the analysis of the nuclear magnetic resonance (NMR) of these sample, get the response characteristics of fracture characteristics on the T2 curve, the quantitative calculation of fracture porosity of rock sample, the result accord with to establish the model of fracture porosity is very good. For the study of fractured oil and gas reservoir development the new field.

基于干燥动力学结合LF-NMR分析的不同干燥过程中天麻切片水分变化

为探究天麻(Gastrodia elata Blume)切片干燥过程中水分迁移变化规律,并建立其量化表征方法,本研究采用低场核磁共振(Low-Field Nuclear Magnetic Resonance, LF-NMR)技术分析热风干燥(Hot Air Drying, HAD)和微波干燥(Microwave Drying, MWD)过程中不同热风温度(60、70、80℃)和不同微波功率密度(2、3、4 W/g)条件下的天麻切片,结合干燥特性曲线建立基于LF-NMR参数的天麻切片含水量预测模型。结果表明,MWD速率远大于HAD,在热风温度(60-80℃)和微波功率密度(2-4 W/g)范围内,高温、高功率密度有利于提高干燥速率,缩短干燥时间。Logarithmic模型可以准确描述天麻切片HAD和MWD过程中含水量的变化。经LF-NMR技术分析,在HAD和MWD过程中,天麻切片的横向弛豫时间曲线整体上呈现左移的趋势,各状态水的弛豫峰信号强度不断降低;干燥结束时天麻切片中的自由水完全被脱去,仅存少量的不易流动水和结合水。无论是HAD还是MWD,弛豫峰总面积A_(2)和天麻片的干基含水量相关性均在0.99以上。研究结果可为阐明天麻切片干燥机制和干燥工艺参数的优选提供参考。

ASSURE-NMR-HSQC实验检测保健食品中西地那非类物质

本研究通过使用灵敏度增强的带梯度形状脉冲进行异核单量子相干(HSQC)实验检测保健食品中违法添加的西地那非类物质。待测样品以甲醇溶解超声辅助提取,减压浓缩后以氘代DMSO溶解上机测试;利用Assure-NMR软件将得到的未知样品异核单量子相干(Heteronculear Single Quantum Coherence)谱图与已知西地那非类物质谱图进行模拟匹配。本方法检出限可以达到200μg·kg-1,能快速有效的对保健食品中西地那非类物质的违法添加侦察识别。该方法简便快捷,可以为食品安全监管部门提供一种新颖便捷的那非类物质监管稽查参考办法。

Enhanced recovery of tight reservoirs after fracturing by natural gas huff-n-puff: Underlying mechanisms and influential factors

Tight oil resources are abundant in the world.It is very important to strengthen the research on the development theory and technology of tight oil reservoirs for ensuring national energy security.Natural gas huff-n-puff can effectively improve the oil recovery of tight oil reservoirs.However,the pore-scale oil production characteristics and the mechanisms of natural gas huff-n-puff in matrix-fracture cores are poorly understood.The influence degree of important factors on oil recovery is not clear and the interactions between factors are rarely considered.In this paper,the oil production characteristics and mechanisms of natural gas huff-n-puff in tight cores with different fracture lengths were quantitatively analyzed by combining nuclear magnetic resonance(NMR)with numerical simulation technology.The influencing factors and their interactions were evaluated by the response surface method(RSM).The results show that tight cores mainly consist of medium pores(0.1–1μm)and small pores(0.01–0.1μm).The fracture mainly increases the proportion of macro-pores(1–10μm)and medium pores.In the natural gas huff-n-puff process,crude oil from macro-pores(1–10μm)and medium pores is mainly developed,and the contribution percentage of crude oil in medium pores to oil recovery is the largest,up to 98.28%.The position of gas–oil contact(GOC)moves deeper as the number of huff-n-puff cycles increases.The contents of CH_(4) and CO_(2) in the oil phase remain at a high level within the GOC,while between the GOC and the component sweep front,the contents of CH_(4) and CO_(2) in the oil phase decrease with the increase in dimensionless distance.The gas component sweep volume is increasing with the increase in fracture length.Moreover,the injected natural gas mainly extracts C_(3)–C_(10) components from crude oil.The reduction law of crude oil viscosity is consistent with the migration laws of CH_(4) components along the path.Compared with soaking time and gas diffusion coefficient,the injection pressure is the most significant factor underlying the recovery of natural gas huff-n-puff in tight cores.Besides the influence of single-factor,the interaction effects of gas injection pressure and diffusion also should be considered to determine the huff-n-puff parameters in the field implementation of natural gas huff-n-puff in tight reservoirs after fracturing.

纳米氧化铝改性地面井固井水泥水化机制研究

随着地面井固井技术发展加快,工程现场对于地面井固井水泥浆的早期流动性及凝结性能有了更高的要求。为了提高固井工程注水泥作业的顶替效率,改善固井工程现场作业应用情况,提出了纳米氧化铝颗粒改性固井水泥的方法,利用核磁共振技术对质量分数为0、0.05%、0.10%、0.15%及0.20%的纳米氧化铝改性水泥浆(水灰比为0.44)在不同水化龄期的水化反应变化特征进行了研究,探究了纳米氧化铝改性水泥的水相分布、物理结合水总信号量变化、峰形指数及迁移速率。结果表明:纳米氧化铝改性水泥浆在水化阶段的T2图谱会出现3个弛豫峰,分别对应絮凝结构填充水(0.1~10 ms)、毛细水(10 ms)、自由水(800~1000 ms);其物理结合水总信号随纳米氧化铝质量分数增加而逐步减少,其中质量分数为0.20%的纳米氧化铝改性水泥浆信号量减少速率最快;峰形指数呈现先上升后下降的趋势,当水化反应进行至600 min时,质量分数为0.20%的改性水泥浆变化速率最快,弛豫峰向短弛豫方向移动速率加快;结合迁移速率将纳米氧化铝改性固井水泥水化反应阶段划分,其水化机制分别作用在4个水化时期:①初始水化期(5~60 min),水化速率未发生明显改变;②加速水化期(60~600 min),纳米氧化铝使水泥浆中物理结合水转化为化学结合水所经历时间变短,水化进程加快,达到促进水泥水化的效果;③稳定水化期(600~1200 min),水泥体系趋于稳定;④延缓水化期(1200~1800 min),物理结合水转化为化学结合水速率变慢,水泥水化进程减慢。研究结论得到,纳米氧化铝改性水泥浆水化时期可以划分为4个阶段,分别起到物理填充、加速、稳定、延缓的作用。在加速期,纳米氧化铝促进水泥的早期流动,有利于水泥浆的泵送及流动,在延缓期,纳米氧化铝延缓水泥的进一步水化进程,利于发展早期强度。其中,质量分数为0.20%的纳米氧化铝改性水泥浆对于水泥水化进程影响最大,促进填充水向结合水的转化,在加速水化期间对于水泥浆水化反应加速程度最大,以此作为依据对现场固井水泥的制备及应用提供指导。