Documenti di Didattica
Documenti di Professioni
Documenti di Cultura
Ural Branch
INSTITUTE of GEOLOGY and GEOCHEMISTRY
Common
Use
Сеnter
е nter
GEOANALYST
Yekaterinburg
2018
Common Use Center “Geoanalyst”
General Information
Areas of Activity
џAnalytical support of fundamental and applied research in the Earth
sciences.
џImplementation of international, federal and regional initiative
projects and programs.
џDevelopment, improvement, approbation and presentation of
analytical techniques.
џHigher and postgraduate education, advanced training.
Head
Sergey L. Votyakov, Academician of the RAS
Tel. 8-343-2879013
E-mail: Votyakov@igg.uran.ru
Deputy Head
Yuliya V. Shchapova, Ph.D., Associate Professor
Tel. 8-343-2879027
E-mail: Shchapova@igg.uran.ru
Website: www.geoanalyst.igg.uran.ru
1 8 (343)287-90-37
Staff, Structure and Contacts
Twenty-three employees including 10 under the age of 35, one academician
of RAS, 5 candidates of science, 3 postgraduate students, 6 groups working
in the following areas:
џElectron probe microanalysis and scanning electron microscopy;
џX-ray fluorescence, atomic emission and atomic absorption analysis;
џX-ray diffraction and thermal analysis;
џMicroelement mass-spectrometry;
џIsotope mass-spectrometry and geochronology;
џPhysics and spectroscopy of minerals, computer simulation of the
mineral structure and properties.
3 8 (343)287-90-37
BSE image (a) and maps of Th, U, Pb, Ca, Ce, La, Y contents (b-h) in the
monazite grain from the Aduisky Massif (the Urals) [Zamyatin, et al.
Dokl. RAS. 2017]
BSE and CL images (a, b) of the zircon grain from the Mugodzhar
metamorphic rocks (the Urals), JPD map of zoning (c), JPD histogram
(e), images of zones Ia-c and II (d), highlighted on JPD histogram
[Votyakov, Zamyatin, Shchapova, et al.. Dokl. RAS. 2014]
5 8 (343)287-90-37
Chemical Microprobe Dating
of U, Th-minerals
Chemical U-Th-total Pb microprobe dating of U-Th minerals (monazite,
uraninite, zircon, etc.) is a low-cost express method with a high lateral (depth)
resolution down to 1 μm. It can be used on condition that the content of
nonradiogenic Pb in the mineral is negligible and its U-Th-Pb system is
closed. The method is based on an improved technique: patent No. 2457468
"Method of electron microprobe chemical U-Th-Pb-dating of U-Th minerals”,
[Votyakov, et al. Crystal chemistry and physics of radiation-thermal effects in
U-Th-containing minerals as a basis for their chemical microprobe dating.
Monograph. 2011].
BSE- and CL-images (a, b), mapping of U, Th, Pb, Ca, O-content and age
distribution (c-h) in zircon from the Shartashsky massif (the Urals). Cf
- coffinite inclusions; Ie, Id, IId zones are highlighted according to the
JPD analysis; the mapping area corresponds to the square shown on
BSE- and CL-images [Votyakov, Pribavkin, Zamyatin. Dokl. RAS. 2016]
JPD map of high-U zircon from the Shartashsky massif with highlighted
Ie, Id and IId zones (a); histogram showing the variations of age in the
zones (b); Pb vs. UO2* diagram (c). Ellipses indicate 2σ error.
7 8 (343)287-90-37
Scanning Electron Microscopy
Scanning electron microscope JSM-6390LV (Jeol) with an energy dispersing
attachment INCA Energy 450 X-Max 80 and EBSD attachment
(NordlysNano Oxford Instruments).
The equipment provides microobject imaging (maximum magnification up to
300 000; high- and low-vacuum operating modes; the latter one for
biological object analysis); pseudo-3D image analysis of the samples using
software package Mex 5.1; semiquantitative (qualitative) analysis of elements
from Na to U with a content of 0.1 to 100 wt%; obtaining diffraction patterns of
backscattered electrons.
а б в
Al Cr Fe
1 мм 1 мм 1 мм
Mg Si Ti
1 мм 1 мм 1 мм
Distribution patterns of Al, Cr, Fe, Mg, Si, Ti concentrations in
magnetite-ilmenite ores
9 8 (343)287-90-37
X-ray Fluorescence Analysis
X-ray fluorescence energy dispersive spectrometers EDX 90-HS and EDX-
8000 (Shimadzu, Japan), X-ray fluorescence multichannel spectrometers
SRM-25 (Burevestnik, Russia) and SRM-35 (Nauchpribor, Russia), XRF
1800 X-ray fluorescence spectrometers (Shimadzu, Japan ) and VRA-30 (Carl
Zeiss, Germany).
The equipment provides non-destructive, quantitative, semiquantitative and
operative qualitative analysis of solid-phase materials with the evaluation of
rock-forming and impurity elements from Na to U with a content of 0.1 to 100
wt.% and locality up to 1 mm.
X-ray Diffraction
and Thermal Analysis
XRD-7000 Diffractometer (Shimadzu, Japan) with polycapillary optics and
high temperature attachment NTK-1200N (Anton Paar) to operate in the
temperature range 25-1,500°C.
The equipment provides investigation of the structure of crystalline
materials; analysis of the sample perfection degree; evaluation of the phase
composition of polycomponent samples (quantitative, non-standard full-
profile analysis of diffractograms of powder samples using the software
complex SiroQuant with a built-in database and recalculation of the mineral
content in oxides with the X-ray fluorescence control); analysis of clay
minerals based on the study of oriented samples [Ryanskaya, Gulyaeva,
2017], etc.
Diamond TG-DTA
Thermal Analyzer
(Perkin Elmer).
The equipment provides
investigation of the
thermal characteristics
of rocks and minerals
(weighting more than 3-
10 mg) in the range of 25-
1,500°C; the study of
oxidation process,
degassing of OH-groups
and water separation,
etc.
11 8 (343)287-90-37
Intensity, a.u.
299
298
3
V, A
297
296
295
2O, degree
Intensity, a.u.
To C
Triton Plus
Filament
degassing unit 2
Neptune Plus
1
UP 266 Optima
NexIon 300S
8000
Cryogenic tank
for liquid argon
ELAN 9000 NWR 213
Liquid nitrogen
13 8 (343)287-90-37
2 3
4 5 6
Sample Preparation
for Microelement Analysis
The sample preparation is carried out in the Class 1 000 (ISO 6) cleanroom
equipped with high-pressure and microwave digestion systems for the
decomposition of rocks, minerals, ores, technogenic products, metals and
alloys: Ural-Gefest PLP-01 and Berghof Speedwave MWS-3 + and MWS-4+
systems of microwave digestion, Ankon AT MKP-05 and Berghof high-
pressure digestion (autoclave) systems, etc.
Ultra-pure reagents (acids purified by sub-boiling distillation, 18.2 MOm·cm
deionized water) and PTFE and polypropylene labware are used.
15 8 (343)287-90-37
Sample Preparation
for Isotopic Analysis
The sample preparation is carried out in the Class 1 000 (ISO 6) cleanroom
equipped with Ekros and TomAnalit heating plates, a programmable SNOL
heating and drying oven for sample decomposition, an antistatic kit for
Mettler Toledo analytical balance, etc.
Ultra-pure reagents (water and acids purified by double sub-boiling
distillation) and Nalgene and Savillex PTFE and PFA labware are used.
ContrAA 700
HR-CS-AAS
spectrometer
17 8-343-2879013
Microelement
Mass-Spectrometry Analysis
ELAN 9000 quadrupole mass-spectrometer with inductively coupled plasma
and UP266 Macro attachment for sample laser ablation.
The equipment provides high-precision simultaneous analysis of REE and
trace elements (Li, B, Be, Sc, Ti, Cr, Ni, V, Co, Cu, Zn, Ga, Rb, Sr, Y, Zr, Nb, Mo,
Sb, Cs, Ba, Hf, Ta, Pb, Th , U, etc) up to 0.n ppm in liquids and solid samples .
ELAN 9000 Q-
ICP-MS and UP
266 Macro LA
system
Sample/PAAS
500
TAZDol-1G
certified, ppm
1000000
100000 y = 1.1044x - 1E-11
R² = 1
10000
аттестовано, ppm
1000
100
10
1
0.1
0.01
0.01 1 100 10000 1000000
BBRZ-1G
measured, ppmppm
найдено, certified, ppm
1000000
100000 y = 1.1151x - 226.42
10000 R² = 0.9992
аттестовано, ppm
1000
100
10
1
0.1
0.01
0.01 1 100 10000 1000000
REE/chondrite measured, ppm
найдено, ppm
1000
аттестовано
certified
100 найдено
measured
аттестовано
РЗЭ/хондрит
certified BBRZ-1G
measured
найдено
10 TAZDol-1G
1
La Ce Pr Nd Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
The microelement composition of reference materials by laser ablation
mass-spectrometry analysis. TAZDol-1G dolerite (University of
Tasmania), BBRZ-1G basalt (University of Campanias, Brazil). 70 μm
laser spot, BBM-1 (basalt, USGS) is used for calibration.
19 8-343-2879013
Zircon U-Pb-Dating
and Lu-Hf Isotope Composition
NexION 300S inductively coupled plasma mass-spectrometer and Thermo
Fisher Scientific Neptune Plus multicollector inductively coupled plasma
mass-spectrometer with New Wave Research NWR213 laser ablation system.
Zircon U-Pb dating by NexION 300S and the analysis of Lu-Hf isotope system
by Neptune Plus is carried out by LA-ICP-MS with a crater diameter of at least
25 μm.
Neptune Plus
MC-ICP-MS
А Б
B C D
Typical craters in the 91500 and GJ-1 reference zircons (A, B and C, D,
respectively) after laser ablation with different laser beam parameters: A,
B – P=11 J/cm2, v=10 Hz, d=50 μm; C,D – 21 J/cm2, 20 Hz, 50 μm
0.125 1300
0.22
A B
0.115 0.20
U
U
238
238
650 1100
0.105 0.18
Pb/
Pb/
0.095 0.16
206
206
550 900
0.085 0.14
Age = 601.1 ± 1.4 Ma (1σ) Age = 1061.7 ± 3.1 Ma (1σ)
MSWD = 0.40 MSWD = 1.3
0.12
0.075
0.1 0.5 0.9 1.3 0 1 2 3 4
207 235 207 235
Pb/ U Pb/ U
206
Pb/238U vs. 207Pb/235U for the GJ-1 (A) and 91500 (B) reference zircons.
An unshaded ellipse represents a single measurement of the crater; blue is
weighted mean; solid line represents concordia; the error is 1σ; data
processing was with GLITTER V.4.4 and Isoplot 4.15 software.
0.2850 50 μm 25 μm 0.2830
А B 50 μm 25 μm
0.2845
Hf
Hf
0.2828
177
176 177
0.2840
Hf/
Hf/
0.2826
0.2835
176
0.2830 0.2824
0.2825
0.2822
2 4 6 8 10 12 14 2 4 6 8 10 12 14 16 18
N N
Variations of 176Hf/177Hf isotopic ratios in the GJ-1 (A) and 91500 (B)
reference zircons with the crater diameter of 50 μm and 25 μm. The dotted
line indicates 176Hf/177Hf (GeoREM database); N is crater number; Lu-Hf
data processing was by Hf-INATOR Excel macros.
21 8-343-2879013
4
a b a b a b
2
3
1
a b a b a b
CL and BSE images (a, b) of NP-47 zircon grains from granite of the
Nepluyevsky pluton (the Southern Urals) after LA-ICP-MS: 1– U-Pb dating,
2, 3 – Lu-Hf isotopic analysis (50 μm and 25 μm crater) [Osipova,
Zaitceva, Votyakov. Dokl. RAN. 2018]
0,072
0,068 a 0,061
b 380
0,064
U
0,059
U
238
380
238
0,060
Pb/
360
Pb/
0,057
206
0,056
206
0,052
0,055
300 340
0,048 Age = 360,4 ± 2,0 Ma (1σ)
Age = 368,0 ± 5,9 Ma (1σ)
MSWD = 0,041
0,044
MSWD = 0,0003 0,053
0,0 0,2 0,4 0,6 0,8 0,32 0,36 0,40 0,44 0,48 0,52 0,56
207 235 207 235
Pb/ U Pb/ U
206
Pb/238U vs. 207Pb/235U for the Np-47 zircon from the Nepluyevsky pluton:
a - LA-ISP-MS, b - SHRIMP (A.P. Karpinsky Russian Geological Research
Institute, VSEGEI)
εHf(t) vs. εNd(t) for the NP-47 granite from the Nepluyevsky pluton: 1, 2
– LA-ICP-MS and SHRIMP (VSEGEI)
Triton
Plus
TIMS
23 8 (343)287-90-37
The concentrations and isotope characteristics of Rb, Sr, Sm and Nd of the
Kochkarsky anticlinorium gneisses (the Southern Urals) [Fershtater, Borodina,
Soloshenko, Streletskaya. Lithosphere. 2015]
Sample
Проба Rb,ppm Sr,ppm 87
Rb/86Sr ±2s 87
Sr/86Sr ±2s (87Sr/86Sr)i εSr
56/150 127 256.27 0.636 0.010 0.706495 0.000030 0.703324 -10.9
61/36 62.37 434.87 0.415 0.006 0.707067 0.000033 0.705000 12.9
63/187 74 705.90 0.319 0.005 0.705960 0.000033 0.704367 3.9
74/240 136.46 160.16 2.467 0.037 0.716866 0.000008 0.704573 6.9
74/280 161.06 201.03 2.319 0.035 0.716096 0.000057 0.704537 6.4
87 86
Sr/ Sr
0,718
74/240
74/280
0,714
0,710
Age=354.9+/-4.5
61/36 ISr=0.704388+/-0.000049
0,706 56/150 MSWD=0.040 (n=3)
63/187
87 86
0,702 Rb/ Sr
15.9 42
Pb/ Pb
а б
. лет
HIMU
Pb/204Pb
204
HIMU
лрд
15.8 Geochron 4.55 Ga
41
5М
208
а 4.5
RL RL
207
Д6-4
Геох
15.6 GLOSS
Д9-4 39
EМ1
15.5 Д6-4
MORBMORB
Pacific Ocean
Тихий океан EМ1 Д9-4 MORBMORB
Pacific Ocean
38 Тихий океан
15.4 Island-arc volcanic rocks of Kamchatka
Островодужные
DM вулканиты Island-arc volcanic rocks of Kamchatka
Островодужные
15.3 Камчатки 37 вулканиты
Камчатки 206
206
Pb/204Pb DM Pb/204Pb
15.2
16 17 18 19 20 21 16 17 18 19 20 21
(0)
εNd 87
Sr/86Sr
0
0.710300 Brown bear
-2
Animal bone Ust-Ishim Man
-4
0.709800
-6 Host soil Host soil
-8 Tobol-Irtysh
Mammoth 0.709300
Turk
-10 Ust-Ishim Man
Mammoth
-12 0.708800
-14
-16 Tobol-Irtysh Turk 0.708300
-18
-20 0.707800
0 10 20 30 40 50 0 1000 2000 3000 4000
Nd, ppm
Sr, ppm
25 8 (343)287-90-37
Raman Spectroscopy
of Minerals
Horiba LabRam HR800 Evolution spectrometer (1800 and 600 pcs/mm
gratings) with the Olympus BX-FM microscope, Linkam THMS 600 thermo-
stat and He-Ne and Ar lasers (633, 514 and 488 nm lines).
The equipment provides analysis of Raman spectra of minerals and other
materials and fluid inclusions with spatial resolution up to 1 μm and spectral
resolution of 0.8-1 cm in the temperature range of 78-873 K; identification of
phases; grain mapping based on the Raman spectra parameters distribution;
the study of local features of mineral structure and composition (deforma-
tions and strains, solid solutions, structural imperfection, radiation damage,
etc.); the investigation of the thermal structural transformations and phase
transitions, etc.
Raman spectra of
diamond (1) and its
imitations, i.e. moissanite
SiC (2) and cubic ZrO2:Y
(3). Excitation by the 633
nm wavelength laser.
27 8-343-2879013
Raman spectra of
titanite from the
Shabrovsky deposit (the
Urals) at different
temperatures: 25, 125,
205, 305, 405, 505 and
585°C (1-7), illustrating
the phase transition in
the mineral
Luminescence of Minerals
CLAVI pulsed cathodoluminescence analyzer with temporal resolution
and Horiba LabRam HR800 spectrometer.
The equipment provides the study of the luminescence spectra of the
minerals at 78-873 K under excitation by Ar and He-Ne lasers; the grain
mapping with respect to spectral parameters; the analysis of pulsed
cathodoluminescence of the minerals.
Intensity, a.u.
Интенсивность, отн.ед.
Dy3+
Tb3+
1,0
0,8
0,6 B
Dy3+
0,4 Fe3+? B1
0,2
C A1
0,0
2 3 4 5 6
Энергия,
E, eV эВ
CLAVI pulsed analyzer and luminescence spectrum of zircon with
decomposition into components associated with REE ions and intrinsic A-
B-C defects
29 8-343-2879013
Raman spectra (a-e, 633 nm excitation) and superposition Raman and
luminescence spectra (h-k, 514 nm excitation; f, 488 nm) of zircon (a, f), titanite
(b, h), apatite (c, i), scheelite (d, j), and calcite (e, l).
The numbers (a-f) and the asterisks (f-l) show Raman lines; the arrows (f-l)
indicate luminescence lines.
Mapping of the Raman line position and width distribution of Ti-O vibration mode
(a, b) and the luminescence line of the impurity Nd3+ ion (e, f) in titanite. Dotted line
– zoning; solid line – zircon inclusions.
Infrared Spectroscopy
of Minerals
Spectrum One infrared Fourier spectrometer with Multiscope microscope
(PerkinElmer).
The equipment provides analysis of the IR spectra of minerals; qualitative
identification of phases; the study of local features of mineral structure and
composition; estimation of OH-groups concentration in the grains of nomi-
nally anhydrous silicates (olivine, pyroxenes) with a spatial resolution of 50
μm and above.
Spectrum One
spectrometer and
infrared FT-IR
microscope
3569
3670
3395
3672
3570 3513
3419
3460
3670
3410 3206
3570
2950 3220
2916
2600 2800 3000 3200 3400 3600 3800 2600 2800 3000 3200 3400 3600 3800 2600 2800 3000 3200 3400 3600 3800
Волновое
Wavenumber, см-1-1
число,cm Волновое см-1 -1
число,cm
Wavenumber, Волновое см-1-1
число,cm
Wavenumber,
31 8-343-2879013
Electron Spin Resonance
Spectroscopy of Minerals
ESR-70-03 DX/2 electron spin resonance spectrometer with the attachment
to operate in the temperature range 77-400 K.
The equipment provides analysis of electron spin resonance spectra of
minerals in the initial state and after various types of irradiation and anneal-
ing; investigation their micro- and nanostructure, type, local structure and
concentration of paramagnetic defects; estimation of the distribution of
paramagnetic ions in solid solutions of minerals; analysis of radiation
phenomena; paleodosimetric reconstructions, etc.
g1
DH1
g4
g6
g g 1
2 3
g0
g4
g5
g6
ESR-70-03 DX/2 2
spectrometer g
7 g4
g6 3
Electron spin resonance spectra of
electron-beam irradiated bone
fossils of small mammals from
different locations of the Urals (1-4)
[Votyakov, Smirnov, et al., I1
Physicochemical characteristics of
fossilized bone remains of 4
mammals and the problem of I4
estimating their relative age. I2
I3
Monograph. 2009]
3290 3300 3310 3320 3330 3340 3350 3360
Magnetic field, E
33 8-343-2879013
Common Use Center “Geoanalyst”
Computer Simulation
of Mineral Structure and Properties
Software products - ab initio cluster Xα-DVM discrete variation method
[Averill, Ellis, 1977], GULP semi-empirical method of atomistic structure
simulation [Gale, 2010], DL-POLY method of molecular dynamics [Todorov,
Smith, 2010] and Monte -Carlo SRIM [Zeigler, 2008].
Software products provide simulation of atomic and electronic structure of
minerals, chemical bonding, structure and spectroscopic properties of the
defects, calculation of thermodynamic properties and structure of solid
solutions, simulation of radiation and matter interaction.
620016 Yekaterinburg
Academician Vonsovsky Street, 15
+7 (343) 287-90-13, +7 (343) 2879027
Votyakov@igg.uran.ru
www.geoanalyst.igg.uran.ru