Identification of magnetic minerals by scanning electron microscope and application of ferrofluid

Magnetic minerals are mostly identified by a combination of rock magnetic and microscopic techniques and the ferrofluid method in combination with an optical microscope was applied during the last decades. But today, scanning electron microscopy (SEM) is preferred for the observation of mineral phases because its depth of focus and resolving capability at the same magnification. In this study, we report on a method, which allows ferrofluid application under the SEM. We coated a polished basalt sample containing titanomagnetite grains with high demagnetizing fields, with a colloidal suspension containing magnetite particles (ferrofluid) ranging in size between 11 and 20 nm. Due to large gradients of multidomain grains the ferrofluid particles adhered to their surfaces. Other grains of similar composition present (ilmenohematite) but with low demagnetizing fields do not generate large magnetic gradients and therefore do not attract the colloidal particles. Upon evaporation of the ferrofluid and covering the sample with conducting material the magnetic grains with high demagnetizing field are easily identifiable under the scanning electron microscope. The different mineralogy observed by this method is confirmed by temperature dependent variation of magnetic susceptibility, revealing titanomagnetite and ilmenohematite as magnetic carriers in the basaltic samples.     

Variations in the Intensity of the Earth's Magnetic Field

The Earth's main magnetic field can be approximated by an axial, geocentric dipole. The remaining non-dipole field is much smaller and is a regional rather than a global feature – quite large changes can occur in a few ka. This review is concerned with changes in the dipole component of the geomagnetic field, and one of the problems is in separating the non-dipole from the dipole contributions to the field. Unlike the many determinations of the direction of the Earth's magnetic field in the past (which have led to fundamental contributions to our understanding of plate tectonics and shown that the field can on occasion reverse its polarity), estimates of the intensity of the field are comparatively few, especially before the Holocene. This is mainly the result of experimental difficulties in obtaining reliable measurements of the field. These problems are discussed in some detail and are followed by a short account of archaeomagnetic intensities and results from Hawaii where many of the first determinations were obtained. Measurements for the last 100 ka from both lavas and lacustrine and oceanic sediments are reviewed and results from different areas compared. An asymmetric saw-tooth pattern has been observed in some of the records over the last few Ma, and this rather controversial question is discussed. Finally an account is given of the far more limited data on palaeointensities in earlier times.A short discussion is given of the interpretation of coherent short wavelength variations which are observed in many marine magnetic profiles. Although short reversals of the field may be responsible for some of these tiny wiggles, it is more likely that in general they are the result of changes in the strength of the Earth's magnetic field.     

地球磁场相对强度研究现状与展望

对利用沉积物确定地球磁场相对强度的实验方法进行了综述评述，在些基础上本文总结了目前常用的恢复沉复沉积物记录古强度的方法，重点介绍了全新世、晚更新世和布容时地球磁场相对强度变化特征，评价了环境因素对沉积物记录地球磁场相对强度的影响。对未来有关地球磁场相对强度研究发展趋势提出了借鉴。     

Low-field variation of magnetic susceptibility measured by the KLY-4S Kappabridge and KLF-4A magnetic susceptibility meter: Accuracy and interpretational programme

The KLY-4S Kappabridge and KLF-4A Magnetic Susceptibility Meter enable automated measurement of susceptibility variation with field in the ranges of 2–450 A/m and 5–300 A/m (in effective values), respectively. Unfortunately, the measurement accuracy decreases with decreasing field and it is not easy to decide whether the susceptibility variation at the lowest fields is natural phenomenon or results from measuring errors. To overcome this problem, the accuracies of both the above instruments were investigated experimentally using artificial specimens (mixture of pure magnetite and plaster of Paris) with variable susceptibilities ranging from 1 × 10⁻⁵ to 5 × 10⁻². The complete curve of the field variation of susceptibility of each specimen was measured 10 times and the relative error was calculated for each field. In the KLY-4S Kappabridge, in specimens with susceptibilities higher than 100 × 10⁻⁶, the relative errors are lower than 3% in all fields and lower than 1% in the fields stronger than 10 A/m. In the KLF-4A Magnetic Susceptibility Meter, in relatively strongly magnetic specimens with susceptibilities 5 × 10⁻⁴ to 5 × 10⁻², the relative error is less than 1.5% in the entire field range. While the former instrument is convenient for investigating almost all rock types, the latter instrument is convenient for measuring moderately and strongly magnetic specimens. To facilitate work with field variation of susceptibility curves, showing variable accuracies with field, the programme FieldVar was written. One of its options is plotting the measured data with corresponding field-variable error bars. In this way, a tool is offered for interpreting such susceptibility changes that are sound and reasonable from the point of view of measuring accuracy.     

Indices for Numerical Characterization of the Alteration Processes of Magnetic Minerals Taking Place During Investigation of Temperature Variation of Magnetic Susceptibility

The alteration of magnetic minerals taking place during the investigation of the temperature variation of bulk magnetic susceptibility is obvious from different courses of heating and cooling susceptibility vs. temperature curves. A set of indices is introduced to characterize these changes numerically. The A ₄₀ alteration index characterizes the change in susceptibility after executing the whole cycle of heating and cooling. The maximum difference between the heating and cooling curves is characterized by the A _max alteration index. The mean or average difference between the heating and cooling curves is characterized by the A _m alteration index. The situation whether the heating and cooling curves cross, is characterized by the A _cr alteration index. The technique of progressive repeated heating is proposed, together with the above indices, to locate the temperature intervals with weak and strong magnetic mineral changes induced by heating.     

Magnetic Characteristics of Different Soil Types from Bulgaria

Magnetic studies of different soil types can provide valuable information about palaeoenvironmental conditions at the time they were formed. Results of investigations of rock-magnetism of genetically different soil types, which developed over varying time intervals (Meadow Chernozem - formed during the last 6000 years BP; Leached Cinnamonic soil - formed since the 3rd-2nd century BC and Pellic Vertisoil - the oldest, formed since the Late Pliocene) are presented. The soil profiles of the Leached Cinnamonic and Pellic Vertisoil are characterized by lower values of magnetic susceptibility, as compared to that of the parent materials. It is shown that using percentage frequency-dependent susceptibility (Xfd%) and viscous remanent magnetization (VRM), pedogenic alteration could be detected even in such circumstances. The variations of the parameters measured along the depth of the studied Meadow Chernozem soil profile are characterized by gradual smooth magnetic enhancement, pointing to the absence of secondary redistribution of pedogenic magnetites. In contrast to this case, the two other profiles (Leached Cinnamonic and Pellic Vertisoil) show magnetically enhanced lower (illuvial) horizons due to processes of acid destruction and re-precipitation of the original pedogenic ferromagnetic minerals down the profiles. These specific magnetic properties are of particular importance in using susceptibility variations as a palaeoclimatic proxy record.     

Low-Temperature Oxidation of Magnetite in Loess-Paleosol Sequences: a Correction of Rock Magnetic Parameters

Low-temperature oxidation under atmospheric conditions affects the magnetic properties of magnetite in natural rocks: the coercivities of magnetite grains increase and other parameters change accordingly. It was recently shown that heating to 150°C largely removes the effects of low-temperature oxidation (van Velzen and Zijderveld, 1995). Heating may therefore serve as a detection tool for the presence of the effect of low-temperature oxidation. In the present study, a collection of loess and paleosol samples from various loess regions of the world is examined for the influence of low-temperature oxidation. In all samples of the collection a decrease of coercivities was found after heating to 150°C. Generally loess samples were affected to a larger extent than paleosol samples. The original range of remanent coercivities(B _cr)of 21-58 mT changed to 20-42 mT after heating. The IRM capacity of the samples decreased from 0 up to 25%. ARM showed changes between a decrease of 10% and an increase of 15%. The grain-size indicative parameter IRM/ARM is considerably influenced by the heating and therefore by low-temperature oxidation. The changes in susceptibility are limited and will not influence the interpretation of large-scale features of the susceptibility record as a paleoclimate proxy. Small variations, however, may be obscured by the varying influence of oxidation in the outcrop, which can significantly modify the rock-magnetic record. Rock-magnetic parameters used to determine magnetic mineral content and grain sizes should be corrected for the effect of low-temperature oxidation. To this end heating to 150°C is recommended. The occurrence of the changes is in itself already an indication for the presence of magnetite. Low-temperature oxidation will not only be due to recent weathering in the outcrop, but also to earlier oxidation processes in the source area, during transport and deposition of the loess and during pedogenesis. Truly fresh sediment samples are only influenced by this earlier oxidation. In that case heating will reveal the degree of ancient low-temperature oxidation, which may be related to climate at the time of deposition and pedogenesis.     

Flow direction and magnetic mineralogy of lava flows from the central parts of the Peninsula of Baja California,Mexico

Magnetic properties of two apparently unrelated lava suites (one tholeiitic and the other alkalic) coexisting in the central parts of the Peninsula of Baja California, Mexico, were measured in this study. Macroscopic indicators and measurements of anisotropy of magnetic susceptibility (AMS) were combined to infer the flow direction on those lavas. These measurements were used to investigate the likelihood of the existence of an abnormally long tholeiitic lava flow in this part of the Peninsula. The obtained results indicate that the tholeiitic flows in the region constitute regular length flows, and are likely to have been issued through vents located within the area of study. Additionally, comparison of the magnetic signature of tholeiitic and alkalic lavas reveals a systematic difference in some of the magnetic parameters (bulk susceptibility and Curie temperatures). In particular, it is proposed that the narrow range of Curie temperatures characteristic of each lava type can be used as a reliable proxy for the identification of each lava type in the region. All of these findings show that the alkalic and tholeiitic lavas of the region are more closely related to each other than previously suspected.Editorial responsibility: R. Cioni     

Two pedogenic models for paleoclimatic records of magnetic susceptibility from Chinese and Siberian loess

The magnetic susceptibility (MS) of Chinese loess showing a general proportional relationship to pedogenic grade has been widely recognized and used for reconstruction of paleoclimate by Quaternary scientists. The in-situ pedogenic enhancement of ferrimagnetic content is normally believed to be the main reason for the increase of susceptibility in soil units. However, this pattern of high magnetic susceptibility in palaeosols, and low values in loess, are not replicated in some loess deposits. Siberian loess deposits display a completely opposite susceptibility behavior: high values in loess and low values in palaeosols. This inverse relationship has been explained by the idea that magnetic susceptibility is reflecting the magnitude of an aeolian ferrimagnetic component of consistent mineralogy, the grain size of which is related to average wind velocity. Our magnetic study of Siberian samples in this paper suggests that there are notable differences in magnetic properties between Siberian loess and developed palaeosols, not only in magnetic grain-size and concentration but also in magnetic mineralogy. This evidence is difficult to explain fully through variation in wind strength alone, but implies that the low magnetic susceptibility values in the Siberian paleosol units are a reflection, at least in part, of the alteration of the ferrimagnetic content by post-depositional processes. The Loess Plateau is a very arid area where potential evaporation is always higher than precipitation; pedogenesis occurs under dry oxidising conditions. The Siberian Kurtak region is located on the edge of the tundra where it is always wet and saturation during interglacials will lead to a reducing pedogenic environment. Ferrimagnetic minerals under this condition will be destroyed, resulting in lower magnetic susceptibility. Therefore, great care should be taken when using susceptibility values for paleoclimatic reconstruction.     

巴基斯坦Bahawalpur黄土岩石磁学特征及磁化率变化机制研究

风成黄土是陆地上分布最广泛的沉积物之一,记载了各种古气候演化信息.目前巴基斯坦的黄土研究甚少,磁化率与气候对应的变化机制研究尚未开展.本文对位于巴基斯坦印度河平原Bahawalpur地区新发现的黄土-古土壤剖面进行系统的岩石磁学研究,结合粒度和漫反射光谱(DRS)数据,讨论巴基斯坦黄土的磁化率变化机制.实验结果显示：Bahawalpur (BH)剖面黄土层主要的载磁矿物为磁铁矿,同时含有少量磁赤铁矿和针铁矿,磁性颗粒以原生的MD和PSD颗粒为主.相对于黄土层,古土壤层则是以针铁矿为主,含有顺磁性矿物和少量磁铁矿.BH剖面磁化率与成土作用关系和中国黄土高原典型剖面相反,磁化率的变化可能存在一个阈值12.8×10^-8m³·kg^-1,在阈值之上,强磁性矿物(磁铁矿、磁赤铁矿)占主导;阈值之下,以弱磁性矿物(主要是针铁矿)为主,这种磁性矿物的转变可能导致磁化率降低.本文可为今后利用磁化率解读该地区地层蕴含的古气候信息提供新线索.

     

The method of high harmonics for determining reheating palaeotemperatures

Summary When reheated to temperatures below the Curie temperature (T_c) and subsequently cooled in a constant magnetic field it has been shown that rocks which contain magnetic minerals will acquire an induced magnetic anisotropy (IMA). The IMA is capable of retaining information on the palaeointensity of the geomagnetic field and the palaeotemperature of this most recent heating. A novel technique for determining the palaeotemperature has been developed, employing the high-harmonics method.     

Changes in Magnetic Properties of Baked Archaeological Samples. Implications for Palaeointensity Determination

Rock magnetic investigations of archaeological materials of burnt clay from Eneolithic ovens (4500 years BC) showed particular changes with time in the magnetic mineralogy of samples, stored under normal conditions. Our results indicate that well-burnt clay from the archaeological materials contains a significant amount of very fine magnetic grains, which could notably influence the rock magnetic properties and behavior at room temperature. The main observations after 4 years of storage under laboratory conditions are as follows: 1) decrease in the final unblocking temperature of NRM from 600–620°C to 580°C and 2) increase in the capacity of laboratory TRM acquisition. The most probable mechanism responsible for the observed changes is supposed to be fast low-temperature oxidation of the finest (superparamagnetic) grains and the development of the maghemite shell in coarser single-domain grains. The Thellier palaeointensity experiments, carried out at the beginning of the study, showed very good results, which satisfy all acceptance criteria, applied to evaluation of the results, quite well. Palaeointensity determinations repeated 4 years later on samples from the same material showed the experimental results to be of significantly inferior quality. The main difference is the presence of the significant deviation (change in the slope) on the Arai diagram after T>350–400°C. The calculated palaeointensity is either higher than the one obtained before, or similar, but evaluated with large uncertainty. Therefore, we conclude that the possibility to obtain biased palaeointensity values increases during short-time storage (i.e. several years) due to the low-temperature changes of the material.     

磁组构的分离与岩石构造变形分析

目前实验条件下获得的AMS（磁化率各向异性）是岩石内所有磁性矿物磁化率各向异性叠加的综合响应,详细的岩石磁学和构造地质学的综合分析表明常规AMS测试结果通常无法揭示岩石复杂的构造变形过程.本文综述了运用非磁滞剩磁各向异性（AARM）、低温AMS（LT-AMS）和高场AMS（HF-AMS）等实验方法对岩石AMS组分进行分离,可以定量获取不同磁性矿物的磁组构贡献,进而解释其不同的变形特征.在此基础上阐述了近年来针对不同磁性矿物组合的AMS分离方法的理论技术创新和进展及其在岩石构造变形特征分析中的应用前景,讨论了常见磁性矿物单晶的岩石磁学性质及各向异性度（P_j）与形状因子（T）在揭示岩石变形特征中的复杂性与局限性,最后举例并分析了磁组构分离技术在造山带岩石构造变形分析中的应用.

     

Pressure Instability of Magnetic Susceptibility of Pyrrhotite Bearing Rocks from the KTB Borehole

Experimental results of pressure-induced changes in mean magnetic susceptibility of rock samples from the main KTB borehole are reported. It was found that susceptibility values of rocks from depths between 5200 and 7000 m show unstable behaviour upon application of pressure, showing an increase in susceptibility of between 20 and 120%. This unstable behaviour was only detected in samples from the above mentioned depth interval, which contain both ferrimagnetic and antiferromagnetic phases of pyrrhotite. On the basis of thermomagnetic analysis, magnetic field treatment, optical microscopy and domain observations of undeformed and deformed samples, reasons for this instability are discussed and interpreted in relation to redistribution of internal stresses within the ferrimagnetic phase, resulting in changes in domain wall mobility.     

Global and Local Multiscale Analysis of Magnetic Susceptibility Data

Geophysical well-logs often show a complex behavior which seems to suggest a multifractal nature. Multifractals are highly intermittent signals, with distinct active bursts and passive regions which cannot be satisfactorily characterized in terms of just second-order statistics. They need a higher-order statistical analysis. In contrast with monofractals which have a homogeneous scaling, multifractals may include singularities of many types. Here we describe how a multiscale analysis can be used to describe the magnetic susceptibility data scaling properties for a deep well (KTB, Germany), down to about 9000 m. A multiscale analysis describes the local and global singular behavior of measures or distributions in a statistical fashion. The global analysis allows the estimation of the global repartition of the various Holder exponents. As such, it leads to the definition of a spectrum, D(), called the singularity spectrum. The local analysis is related to the possibility of estimating the Lipschitz regularity locally, i.e., at each point of the support of a multifractal signal. The application of both approaches to the KTB magnetic susceptibility data shows a meaningful correlation between the sequence of Holder exponents vs. depth and the lithological units. The Holder exponents reach the highest values for gneiss units, intermediate ones for amphibolite units and the lowest values for variegated units. Faults are found to correspond to changes for H also when they are of intra-lithological type.     

苏北盆地兴化1#钻孔沉积物的岩石磁学特征

对苏北盆地兴化1#钻孔岩心沉积物进行了质量磁化率、频率磁化率、变化曲线、等温剩磁和磁滞回线等参数的测试分析,结果表明,粘土质沉积物中的主要载磁矿物为磁铁矿和赤铁矿;砂质沉积物中的磁性矿物除了磁铁矿和赤铁矿外,还含有少量的磁赤铁矿和针铁矿.针铁矿普遍存在于钻孔下部的样品中.整个钻孔沉积物中的磁性矿物颗粒都是介于单畴和多畴之间的准单畴颗粒,但粘土质沉积物中的磁性矿物颗粒更趋近于单畴颗粒,而砂质沉积物中的磁性矿物颗粒更趋近于多畴.根据不同的磁性矿物组合特征,选择合理的温度和磁场强度区间对古地磁退磁结果进行分析,得到沉积物可靠的特征剩磁方向,为古地磁年代学提供依据.     

Loess in the Czech Republic: Magnetic properties and paleoclimate

Summary We have studied 454 oriented samples from seven loess outcrops in the Czech Republic for comparison and correlation of the magnetic properties with those of the loess profiles in China and Central Asia. Three sections at Sedlec (Prague), Zeměchy and Dolní Věstonice cover the time span of the last glacial-interglacial cycle. Loess from the middle Pleistocene period including pedocomplexes V and VI was studied at Sedlešovice (Znojmo) and Karlštejn. Loess of uncertain — possibly lower to middle Pleistocene age — was sampled at Sedlec near Mikulov. At Červeny Kopec (Red Hill, Brno) we investigated the oldest loess near the Matuyama/Brunhes (M/B) boundary. The characteristic remanence (ChRM) determined after magnetic clearning is of normal polarity throughout all sections except at Červeny Kopec. There, two polarity changes from reversed to normal were found within two sections initially thought to represent two successive stratigraphic intervals. However, the marked similarities between lithological, susceptibility, declination and inclination profiles lead us to suggest that the two polarity changes are in fact one and the same. The two sections are therefore laterally equivalent and both have recorded the M/B field reversal. The susceptibility variations were used to mutually correlate the Czech sections and to construct a composite profile across the present day loess outcrops in the Czech Republic. They also serve as a paleoclimate proxy which can be compared and correlated with the paleoclimatic records observed in the Chinese and Central Asian loess. The origin of the low field susceptibility variations was studied by measuring the frequency dependence of susceptibility which revealed that the enhancement within the pedocomplexes is controlled by the amount of fine-grained ferromagnetic minerals present.     

Effect of Stress on the Magnetic Memory of Induced Magnetic Anisotropy of Rocks and Its Mathematical Model

When re-heated to temperatures below the Curie temperature and subsequently cooled in a constant magnetic field (H _T), rock samples which contain magnetic minerals can acquire an induced magnetic anisotropy (IMA). As the result of acquiring the IMA, a constriction develops in the hysteresis loop of the magnetization of these rocks at the values of the magnetizing field close or equal to the HT. Thus the IMA is capable of retaining the information on the palaeointensity of the geomagnetic field, i.e., if IMA was created in a rock in the geomagnetic field in a past geological epoch, it preserves the information on the intensity of that field. Investigations have shown, that when IMA is created in a rock under external stress, the stress has an impact on the magnetic memory. Here we also deal with the issue of how stress affects the magnetic memory of IMA. A mathematical model for the effect of stress on magnetic memory phenomena related to induced magnetic anisotropy in rocks containing multidomain magnetite and titanomagnetite grains is proposed herewith. The effect of temperature on the magnetic memory of rocks is discussed also.     

Magnetic properties of the Tertiary red clay from Gansu

The study on magnetic properties of the red clay indicates that the red clay and loesspaleosol sequence have a common magnetic mineralogy, with magnetite, maghemite, hematite (and possibly goethite) contributing to the magnetic behavior. The red clay magnetic susceptibility is also found to have a positive relation with extrafine superparamagnetic grains. This suggests that, like the Quaternary loess-paleosols, an ultrafine ferrimagnetic component produced during pedogenesis in the red clay under humid conditions also plays an important role in susceptibility enhancement in the soil units. This is supported by the correlation between Rb/Sr ratio and magnetic susceptibility. This signifies that, like the above loess-paleosol sequence, the magnetic susceptibility of the red clay can be used as a general proxy paleoclimatic indicator, although whether its susceptibility in the red clay is comparable to pedogenesis intensity and requires further investigation. Magnetic susceptibility variation in the red clay thus also provides an eolian/pedogenic record of paleoclimatic evolution. Study of the background susceptibility indicates that, on average, the absolute scale of the paleoclimatic shift from red clay development to Quaternary loess deposition is similar to the climatic shift from stage 5 (S1) to stage 2–4 (L1). This may suggest that during the Quaternary there is an evident strengthening of the absolute wind intensity to bring more (about double) coarser and less weathered (non-SP fraction) eolian magnetic input from the source regions to the Loess Plateau than during the Pliocene. The presence of eolian red clay since 7.5 Ma BP in central-northern China implies an important environmental change from the underlying Cretaceous red sandstone. The red clay development was closely related to global drying and climate cooling since the Cretaceous and closely associated with the abrupt uplift of the Qinghai-Xizang Plateau at about that time. This uplift of the plateau intensified the East Asia monsoon system and started red clay deposition.     

Magnetic fabric of bulgarian loess sediments derived by using various sampling techniques

Summary The anistropy of low field magnetic susceptibility has been studied for seven outcrops of loess sediments in North-Eastern Bulgaria. Different sampling methods were applied in order to choose the best technique for obtaining the primary magnetic fabric of such unconsolidated sediments. AMS results show significant changes in the petrofabric of samples collected by the first technique which disturbs the original sedimentary fabric. The second applied technique does not cause such a strong deformation but some disturbance of the magnetic fabric is probable. Typical sedimentary fabric is obtained from hand samples and it is therefore concluded that this represents the best method for obtaining reliable AMS results from soft sediments.