The Uptake and Distribution of Potassium in Roots of Duckweed (Lemna Minor L) As Measured using Low Temperature X-Ray Microanalysis

1982 ◽  
Vol 40 ◽  
pp. 408-411
Author(s):  
Patrick Echlin ◽  
Clifford Lai ◽  
Thomas L. Hayes
Keyword(s):  
Low Temperature ◽  
Background Subtraction ◽  
Cell Walls ◽  
Lemna Minor ◽  
Beam Current ◽  
X Ray ◽  
Dark Regime ◽  
Low Temperature Microscopy

Lemna minor L. plants were grown in a 14 H light and 10 H dark regime at 298 K in a medium containing 2 mM [K+]. Roots, 20 mm long and photosynthetically active, were removed and prepared for low temperature microscopy using methods described elsewhere. Fracture faces were made using the AMRAY Biochamber and the analysis carried out using an AMRAY 1000A SEM fitted with an LaB6 gun and a Kevex Si (Li) x-ray detector at 15-17 kV and a beam current of 1-2 nA. A reduced raster (1.0 μm2) was placed at the centre of the cell being analysed, care being taken to avoid any contact with the cell walls. Samples were maintained at 100-110 K throughout analysis and an LN2 cooled anti-contamination device was inserted close to the specimen. The spectra were analysed using the peak/background (P/B) ratio technique following use of background subtraction and peak de-convolution routines. Between eight and twelve fracture faces were analysed for each of the ten sites along the length of the root and the data pooled and presented in Table I.

Low temperature x-ray microanalysis of frozen-hydrated tobacco leaves

1984 ◽  
Vol 42 ◽  
pp. 284-285
Author(s):  
S. Edith Taylor ◽  
Patrick Echlin ◽  
May McKoon ◽  
Thomas L. Hayes
Keyword(s):  
Low Temperature ◽  
Lemna Minor ◽  
Root Tips ◽  
Tobacco Leaves ◽  
X Ray ◽  
Whole Cells ◽  
Carbon Coated ◽  
The Right ◽  
Beam Currents ◽  
The University

Low temperature x-ray microanalysis (LTXM) of solid biological materials has been documented for Lemna minor L. root tips. This discussion will be limited to a demonstration of LTXM for measuring relative elemental distributions of P,S,Cl and K species within whole cells of tobacco leaves.Mature Wisconsin-38 tobacco was grown in the greenhouse at the University of California, Berkeley and picked daily from the mid-stalk position (leaf #9). The tissue was excised from the right of the mid rib and rapidly frozen in liquid nitrogen slush. It was then placed into an Amray biochamber and maintained at 103K. Fracture faces of the tissue were prepared and carbon-coated in the biochamber. The prepared sample was transferred from the biochamber to the Amray 1000A SEM equipped with a cold stage to maintain low temperatures at 103K. Analyses were performed using a tungsten source with accelerating voltages of 17.5 to 20 KV and beam currents from 1-2nA.

A Practical Approach to Low Temperature Microscopy and X-Ray Microanalysis

2000 ◽  
Vol 6 (S2) ◽  
pp. 306-307
Author(s):  
Patrick Echlin
Keyword(s):  
Solid State ◽  
Low Temperature ◽  
Building Block ◽  
Solid Matrix ◽  
X Ray ◽  
State Water ◽  
The Subject ◽  
Living Material ◽  
Low Temperature Microscopy

Water is the most abundant and most important molecule in the hydrosphere, outer lithosphere and the biosphere of our planet. It is also the most abundant and energetically the least expensive building block of living material, forms an integral parts of natural inorganic matrices such as soil and is a constituent of many synthetic organic materials such as paints and polymers. Paradoxically, water does not exist naturally, in the pure state. Water, when converted to the solid state, can provide the perfect matrix in which we may observe the structure and study the in situ chemistry of hydrated samples. We will consider the nature of this solid matrix, and its constituent components in a range of sample, and show how it may be formed, manipulated, examined and analysed. In the short amount of time and space available, one can do little more than highlight the main features of the subject.

Bulk standards for low-temperature biological x-ray microanalysis

1984 ◽  
Vol 42 ◽  
pp. 282-283
Author(s):  
P. Echlin ◽  
M. McKoon ◽  
E.S. Taylor ◽  
C.E. Thomas ◽  
K.L. Maloney ◽  
...  
Keyword(s):  
Phase Separation ◽  
Low Temperature ◽  
Analytical Method ◽  
Salt Solutions ◽  
Absolute Concentration ◽  
Cooling Process ◽  
X Ray ◽  
The Absolute ◽  
Analytical Procedures ◽  
Electrical Conductors

Although sections of frozen salt solutions have been used as standards for x-ray microanalysis, such solutions are less useful when analysed in the bulk form. They are poor thermal and electrical conductors and severe phase separation occurs during the cooling process. Following a suggestion by Whitecross et al we have made up a series of salt solutions containing a small amount of graphite to improve the sample conductivity. In addition, we have incorporated a polymer to ensure the formation of microcrystalline ice and a consequent homogenity of salt dispersion within the frozen matrix. The mixtures have been used to standardize the analytical procedures applied to frozen hydrated bulk specimens based on the peak/background analytical method and to measure the absolute concentration of elements in developing roots.

The Microstructure of Steatite (Protoenstatite)

1985 ◽  
Vol 43 ◽  
pp. 236-237
Author(s):  
W. E. Lee ◽  
A. H. Heuer
Keyword(s):  
High Frequency ◽  
Glass Ceramics ◽  
Magnesium Silicate ◽  
Beam Current ◽  
Glassy Matrix ◽  
Angle Of Incidence ◽  
X Ray ◽  
Mechanical And Electrical Properties ◽  
Argon Ions ◽  
High Temperature Polymorph

IntroductionTraditional steatite ceramics, made by firing (vitrifying) hydrous magnesium silicate, have long been used as insulators for high frequency applications due to their excellent mechanical and electrical properties. Early x-ray and optical analysis of steatites showed that they were composed largely of protoenstatite (MgSiO3) in a glassy matrix. Recent studies of enstatite-containing glass ceramics have revived interest in the polymorphism of enstatite. Three polymorphs exist, two with orthorhombic and one with monoclinic symmetry (ortho, proto and clino enstatite, respectively). Steatite ceramics are of particular interest a they contain the normally unstable high-temperature polymorph, protoenstatite.Experimental3mm diameter discs cut from steatite rods (∼10” long and 0.5” dia.) were ground, polished, dimpled, and ion-thinned to electron transparency using 6KV Argon ions at a beam current of 1 x 10-3 A and a 12° angle of incidence. The discs were coated with carbon prior to TEM examination to minimize charging effects.

Practical Importance of Spatial Resolution and Analytical Sensitivity in AEM X-ray Microanalysis

1990 ◽  
Vol 48 (2) ◽  
pp. 432-433
Author(s):  
J. Zhang ◽  
D.B. Williams ◽  
J.I. Goldstein
Keyword(s):  
Spatial Resolution ◽  
Practical Importance ◽  
Beam Current ◽  
Specimen Thickness ◽  
Analytical Sensitivity ◽  
Related Factors ◽  
X Ray ◽  
Probe Size ◽  
Excitation Volume ◽  
Two Parameters

Analytical sensitivity and spatial resolution are important and closely related factors in x-ray microanalysis using the AEM. Analytical sensitivity is the ability to distinguish, for a given element under given conditions, between two concentrations that are nearly equal. The analytical sensitivity is directly related to the number of x-ray counts collected and, therefore, to the probe current, specimen thickness and counting time. The spatial resolution in AEM analysis is determined by the probe size and beam broadening in the specimen. A finer probe and a thinner specimen give a higher spatial resolution. However, the resulting lower beam current and smaller X-ray excitation volume degrade analytical sensitivity. A compromise must be made between high spatial resolution and an acceptable analytical sensitivity. In this paper, we show the necessity of evaluating these two parameters in order to determine the low temperature Fe-Ni phase diagram.A Phillips EM400T AEM with an EDAX/TN2000 EDS/MCA system and a VG HB501 FEG STEM with a LINK AN10 EDS/MCA system were used.

The promises and perfidy of cryomicroscopy and analysis

1994 ◽  
Vol 52 ◽  
pp. 382-383
Author(s):  
Patrick Echlin
Keyword(s):  
Low Temperature ◽  
High Energy ◽  
Short Paper ◽  
List Type ◽  
Time Resolved ◽  
Energy Beam ◽  
Cellular Analysis ◽  
Dissolved Ions ◽  
Embedding Medium ◽  
Low Temperature Microscopy

The unusual title of this short paper and its accompanying tutorial is deliberate, because the intent is to investigate the effectiveness of low temperature microscopy and analysis as one of the more significant elements of the less interventionist procedures we can use to prepare, examine and analyse hydrated and organic materials in high energy beam instruments. The promises offered by all these procedures are well rehearsed and the litany of petitions and responses may be enunciated in the following mantra.Vitrified water can form the perfect embedding medium for bio-organic samples.Frozen samples provide an important, but not exclusive, milieu for the in situ sub-cellular analysis of the dissolved ions and electrolytes whose activities are central to living processes.The rapid conversion of liquids to solids provides a means of arresting dynamic processes and permits resolution of the time resolved interactions between water and suspended and dissolved materials.The low temperature environment necessary for cryomicroscopy and analysis, diminish, but alas do not prevent, the deleterious side effects of ionizing radiation.Sample contamination is virtually eliminated.

Electron behavior in the gaseous environment of the ESEM chamber

1996 ◽  
Vol 54 ◽  
pp. 838-839 ◽  
Author(s):  
S.A. Wight
Keyword(s):  
Secondary Electron ◽  
High Vacuum ◽  
Beam Current ◽  
Chamber Pressure ◽  
Environmental Scanning ◽  
Carbon Block ◽  
Faraday Cup ◽  
X Ray ◽  
Gaseous Environment ◽  
Working Distance

Measurements of electrons striking the sample in the Environmental Scanning Electron Microscope (ESEM) are needed to begin to understand the effect of the presence of the gas on analytical measurements. Accurate beam current is important to x-ray microanalysis and it is typically measured with a faraday cup. A faraday cup (Figure 1) was constructed from a carbon block embedded in non-conductive epoxy with a 45 micrometer bore platinum aperture over the hole. Currents were measured with an electrometer and recorded as instrument parameters were varied.Instrument parameters investigated included working distance, chamber pressure, condenser percentage, and accelerating voltage. The conditions studied were low vacuum with gaseous secondary electron detector (GSED) voltage on; low vacuum with GSED voltage off; and high vacuum (GSED off). The base conditions were 30 kV, 667 Pa (5 Torr) water vapor, 100,000x magnification with the beam centered inside aperture, GSED voltage at 370 VDC, condenser at 50%, and working distance at 19.5 mm. All modifications of instrument parameters were made from these conditions.

Elemental mass loss in silicate minerals during x-ray analysis

1990 ◽  
Vol 48 (4) ◽  
pp. 804-805
Author(s):  
P.E. Champness ◽  
R.W. Devenish
Keyword(s):  
Mass Loss ◽  
Current Density ◽  
Damage Mechanism ◽  
Beam Current ◽  
Single Chain ◽  
Plagioclase Feldspar ◽  
X Ray ◽  
Alkali Ions ◽  
Structural Order ◽  
Sheet Silicate

It has long been recognised that silicates can suffer extensive beam damage in electron-beam instruments. The predominant damage mechanism is radiolysis. For instance, damage in quartz, SiO2, results in loss of structural order without mass loss whereas feldspars (framework silicates containing Ca, Na, K) suffer loss of structural order with accompanying mass loss. In the latter case, the alkali ions, particularly Na, are found to migrate away from the area of the beam. The aim of the present study was to investigate the loss of various elements from the common silicate structures during electron irradiation at 100 kV over a range of current densities of 104 - 109 A m−2. (The current density is defined in terms of 50% of total current in the FWHM probe). The silicates so far ivestigated are:- olivine [(Mg, Fe)SiO4], a structure that has isolated Si-O tetrahedra, garnet [(Mg, Ca, Fe)3Al2Si3AO12 another silicate with isolated tetrahedra, pyroxene [-Ca(Mg, Fe)Si2O6 a single-chain silicate; mica [margarite, -Ca2Al4Si4Al4O2O(OH)4], a sheet silicate, and plagioclase feldspar [-NaCaAl3Si5O16]. Ion- thinned samples of each mineral were examined in a VG Microscopes UHV HB501 field- emission STEM. The beam current used was typically - 0.5 nA and the current density was varied by defocussing the electron probe. Energy-dispersive X-ray spectra were collected every 10 seconds for a total of 200 seconds using a Link Systems windowless detector. The thickness of the samples in the area of analysis was normally 50-150 nm.

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