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Russian Academy of Sciences

Ural Branch
INSTITUTE of GEOLOGY and GEOCHEMISTRY

Common
Use
Сеnter
е nter
GEOANALYST

Yekaterinburg
2018
Common Use Center “Geoanalyst”

General Information

The Common Use Center “Geoanalyst” was established in 2006 on the


basis of the institute analitycal laboratory.
“Geoanalyst” is an interdisciplinary research center outfitted with up-to-
date analytical equipment and a variety of techniques. The equipment can
provide quantitative information about the chemical (elemental and isotope)
and phase composition, the crystal and electronic structure parameters, the
lattice defect type, and the optical properties of minerals, rocks, soils,
sediments, ores, products of their enrichment, as well as synthetic
compounds, technogenic and biogenic objects.
The center equipment is located in specialized facilities with systems of
inflowing and outflowing ventilation, climate control, etc. Their total area is
about 1000 sq.m. The equipment for chemical decomposition,
chromatographic separation and subsequent study of trace-element and
isotope composition of samples is located in the cleanrooms of purity class 10
000 and 1 000 (ISO 7 and 6); their total area is about 600 sq.m.

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.

620016, Yekaterinburg, Academician Vonsovsky Street, 15


Phone: 8-343-2879013, 8-343-2879027
E-mail: Votyakov@igg.uran.ru, Shchapova@igg.uran.ru
Website: www.geoanalyst.igg.uran.ru

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Common Use Center “Geoanalyst”

Electron Probe Microanalysis


Microanalyzer Cameca SX100 with five wavelength spectrometers and
Bruker Xflash6 energy dispersive spectrometer; devices for carbon and
metal coating Q150TES (Quorum Technologies).
The equipment provides quantitative analysis of elements from light ones
Be, O, F to U in samples with a content of 0.01 to 100 wt.% and with lateral
(depth) resolution down to 1 μm; elemental mapping, SE, BSE and CL
imaging of grains; analysis of its internal texture, revealing of domains and
mineral inclusions using the JPD (Joint Probability Distribution) method
[Votyakov, et al., 2014, Zamyatin et al., 2017]; chemical U-Th-total Pb
dating of U-Th minerals [Votyakov et al., 2011].

Cameca SX 100 electron


probe microanalyzer

X-ray emission spectra in the region of the O Ka line in V, Fe2O3, rhodonite,


zircon and TiO2 (from top to bottom) obtained using LPCO crystal-
analyzer. Variation of measured oxygen content (O) and that estimated
from the matrix stoichiometry condition (Ost) in zones I-II of zircon
metamorphites (b).

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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]

Si Kβ-spectra (a, top) of well ordered (1) and radiation-damaged


unhydrated zircons (3-6); deviation of spectra 3-6 from the spectrum 1
(a, bottom); α-irradiation dose vs. Si Kβ line position (initial moment)
in zircons 1-6 (H2O<0.5 wt%) and in hydrated zone of zircons (4', 6', 6”)
formed by local alteration (b) [Zamyatin, Shchapova, Votyakov, et al.,
Min. Petr. 2017]

www.geoanalyst.igg.uran.ru E-mail: Votyakov@igg.uran.ru 4


Common Use Center “Geoanalyst”

JPD Analysis of BSE


and CL Images of Mineral Grains

A generalized diagram of BSE vs. CL intensities in zircons

JPD analysis of BSE and


CL images as the base for
investigation of zircon
texture, structural state
and chemical composition

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]

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Common Use Center “Geoanalyst”

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.

Interior region of high-U


zircon of the Aduisky massif:
BSE (a) and CL images (b);
JPD map with If, IIf, and IId
zones (c); distribution
patterns of the concentrations
of U, Th, Pb, O, and Ca (d-h)
and distribution pattern of the
age calculated from EPMA
results (i).
Histograms showing the variations of U(a), Th, Pb, and Ca
concentration (b), and calculated U–Th–total Pb age (c) within and
among zones Ie, IIa, and IIb in zircon from the Aduisky massif. Dash-
dot lines visualize the calculated weighted mean age in each of the
zones, and light grey rectangles visualize its 2σ uncertainty. [Zamyatin,
Shchapova, Votyakov, et al., Min. Petrol. 2017].

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.

JSM-6390LV scanning electron microscope

а б в

BES- and BEC-images of platinum and chromite crystals (a, b) and


zircon grains (c)

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Common Use Center “Geoanalyst”

Kikuchi diffraction patterns, orientation maps and orientation on


reverse pole figures of zircon and its quartz inclusions from
Mugodzhar metamorphic rocks [Zamyatin, Shchapova, Votyakov.
Yearbook of IGG, 2014, 2015].

BSE image of forsterite inclusions in the host clinopyroxene matrix


(a), the map of relative orientations of an individual olivine inclusion
(b), inverse pole figures from electron backscatter diffraction data

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.

EDX-800HS, XRF-1800 and VRA-30


X-ray fluorescence spectrometers

SRM-25 and SRM-35 X-ray fluorescence spectrometers

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Common Use Center “Geoanalyst”

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.

XRD-7000 Diffractometer and Diamond TG-DTA Thermal Analyzer

11 8 (343)287-90-37
Intensity, a.u.

299

298

3
V, A
297

296

295

0 200 400 600 800 1000


T, C

2O, degree

Powder diffractogram of monazite from the Aduisky massif (the Urals).


The sidebar shows a decrease in volume of monazite unit cell during
annealing from 100 to 1000°C, caused by radiation damage healing.

Intensity, a.u.

To C

Differential thermogravimetric, thermal and thermogravimetric curves


(red, black, blue) of a polymineral sample. Arrows – thermal effects; 1, 2
– pyrite decomposition; 3 – quartz α-β transition; 4-5 – clay minerals
dehydration and calcite dissociation; 6 - crystallization of amorphous
products of kaolinite decomposition.

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Common Use Center “Geoanalyst”

Cleanroom Facilities for


Microelement and Isotope Analysis
Cooling
systems

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

Scheme of rooms with mass spectrometry equipment on the first floor

1 2 Mass-spectrometer (class 10 000) and data processing


rooms
Laboratory table, table sink
Laminar flow box
Storage cabinet
Sample elevator
Pass-through window

The equipment in the mass-spectrometer room (first floor): Triton Plus


and Neptune Plus (multicollector), ELAN9000 and NexION 300S
(quadrupole) mass-spectrometers with NWR 213 and UP 266 Macro laser
ablation systems, Optima 8000 AES spectrometer

13 8 (343)287-90-37
2 3

4 5 6

Scheme of rooms with equipment for sample preparation for


microelement and isotope analyses on the second and third floors

2 Laboratory rooms for sample Laboratory table, table sink


preparation for microelement
and isotope analysis (class Fume hood
1 000) Storage cabinet
3 Data processing room Laminar flow box
4 Weighing room Sample elevator
Sample chemical decomposition Pass-through window
5
and chromatographic separation
rooms (systems of microwave
and high-pressure digestion)
6 Sample storage room

The equipment for


sample preparation

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Common Use Center “Geoanalyst”

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.

The equipment for sample preparation

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.

The equipment for sample preparation

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Common Use Center “Geoanalyst”

Atomic Emission and


Atomic Absorption Analysis
Perkin Elmer Optima 8000 inductively coupled plasma atomic emission
spectrometer and Analityk Jena ContrAA 700 high-resolution continuum
source atomic absorption spectrometer both with flame and electrothermal
atomization in graphite furnace.
The spectrometers provide high-precision high-throughput analysis of trace
(Li, Be, Sc, Ti, Cr, Ni, V, Co, Cu, Zn, Ga, Rb, Sr, Y, Zr, Nb, Mo, Sb, Cs, Ba, Hf, Ta,
Pb, Th , U) and rare earth elements at ppm levels in rock and mineral solu-
tions.

Optima 8000 ICP-


AES spectrometer

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

REE distribution in the Upper Devonian conodonts of the Southern Urals

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Common Use Center “Geoanalyst”

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.

NexION 300S ICP-MS


and NWR 213 LA
system

Neptune Plus
MC-ICP-MS

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Common Use Center “Geoanalyst”

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)

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Common Use Center “Geoanalyst”

Mass-Spectrometry Analysis of Rb, Sr,


Sm, Nd, and Pb Isotope Composition
Thermo Fisher Scientific Triton Plus thermal ionization and Neptune Plus
inductively coupled plasma multicollector mass-spectrometers.
The equipment provides the analysis of Sm-Nd and Rb-Sr isotope
composition of rocks and minerals using the isotopic dilution (ID) method by
Triton Plus; the analysis of the Sm-Nd (ID), Sr (SSB, standard-sample-
bracketing) and Pb (Tl-normalization method) isotope composition of rocks
and minerals by Neptune Plus.

Triton
Plus
TIMS

The laminar flow box with Re-filament


loading system and filament degassing unit

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

Sm, Nd, 147


Sm/ ±2s 143
Nd/ ±2s (143Nd/ T-DM
Sample
Проба ppm ppm 144
Nd 144
Nd 144Nd)i εNd Gol
74/240 3.63 20.74 0.10598 0.00011 0.512429 0.000013 0.512186 0.0 1021
74/280 3.49 20.30 0.10402 0.00008 0.512434 0.000009 0.512195 0.2 996
63/187 4.97 24.88 0.12069 0.00013 0.512543 0.000009 0.512266 1.5 996
56/150 3.74 21.24 0.10642 0.00021 0.512546 0.000018 0.512302 2.2 860

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

0,0 0,4 0,8 1,2 1,6 2,0 2,4 2,8


87
Sr/86Sr vs. 87Rb/86Sr for gneisses containing granites in the Kochkarsky
anticlinorium (the Southern Urals)

εSr(t) vs. εNd(t) for granitoids


(1-7) and gneisses (the Southern
Urals, 8).
I – the Main Ural fault zone;
II – the northwestern and
southeastern island-arc
continental megablocks;
III - the Ural Platinum belt.

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Common Use Center “Geoanalyst”

15.9 42

Pb/ Pb
а б

. лет
HIMU
Pb/204Pb

204
HIMU

лрд
15.8 Geochron 4.55 Ga
41

208
а 4.5
RL RL
207

15.7 GLOSS EМ2 NH EМ2 NH


40
рон

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

Isotopic composition of Pb in gabbro (D9-4) and tonalite (D6-4) of


the Revdinsky massif (the Urals) [Berzin, Streletskaya, 2014]. DM,
EM1, EM2, HIMU according to Zindler, Hart [1986], NHRL -
Northern Hemisphere Reference Line, MORB of the Pacific Ocean
according to Plank, Langmuir [1998], GLOSS - global subducted
sediments - according to White et al. [1987], island-arc volcanic
rocks of Kamchatka according to Sahaa et al. [2005].

(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

The content and isotope composition of Nd and Sr in the bone


remains of Paleolithic Ust-Ishim and medieval Tobol-Irtysh
ancient men; in the bone detritus of the mammoth, red and
northern deers, bison, brown bear, woolly rhinoceros (the
Western Siberia and Pechora Cis-Urals locations) and in host soil
washes from the mammoth fauna bones [Streletskaya et al.
Metallogeny of ancient and modern oceans. 2017].

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.

Horiba LabRam HR800 Raman spectrometer

Express identification of phases for applied mineralogy and gemmology

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.

www.geoanalyst.igg.uran.ru E-mail: Votyakov@igg.uran.ru 26


Common Use Center “Geoanalyst”

Express identification of radiation-damaged state of zircon

Raman spectra of zircon grains 1-6


with different degree of
metamictization (a): the map of
v3(SiO4) band width in zircon of the
Mugodzhar metamorphic rocks (b).

Express identification of polymorphic modification of minerals

Raman spectrum in the "water" region and its decomposition into


components for lizardite from ultrabasic rock (the Urals). Excitation by
the 514 nm wavelength laser. Identification of lizardite based on the lines
correspondence to the intrinsic stretching vibrations of inner (3703)
and outer (3643 и 3684 см-1) OH-groups in the mineral structure.

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

Optical images of typical liquid inclusions in quartz (the Krasnoe deposit,


Bodaibinsky region, the Eastern Siberia) (a, b) and fragments of their
Raman spectra (c, d). Laser power of 3.3 and 14 mV (c, d). [Pankrushina,
Votyakov, Ankusheva, et al. 2018].

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Common Use Center “Geoanalyst”

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.

Luminescence data as the base for


investigation of radiation-damaged state
of zircon: photoluminescence spectra of
Dy3+ in zircons with different degree of
metamictization (a): the map of Dy3+ (I)
band width in zircon of the Mugodzhar
metamorphic rocks (b).

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.

www.geoanalyst.igg.uran.ru E-mail: Votyakov@igg.uran.ru 30


Common Use Center “Geoanalyst”

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,

Fragments of IR absorption spectra in the "water" region of


clinopyroxene, orthopyroxene and olivine from ultramafic rock (the
Urals) and their decomposition into individual absorption lines

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

www.geoanalyst.igg.uran.ru E-mail: Votyakov@igg.uran.ru 32


Common Use Center “Geoanalyst”

Algorithm for Studying Zircon Grains


by Local Methods

BSE image of internal region (a),


histogram showing the
variations of oxygen
concentration within, and
among, zones If, IIf, IId, and Ic
(b) in high-U zircon from the
Aduisky massif. Ost -
stoichiometric oxygen calculated
based on concentrations and
valences of cations; O - oxygen
concentration measured by
EPMA using the O Kα X-ray line.

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.

Average cation-oxygen distances in (Zr1-х,Uх)SiO4 solid solution (a) and


standard deviation of Si-O distances from additive value (Sx) as a
measure of structural disorder (b) [Zamyatin et al., Glass Physics and
Chemistry, 2013]

Calculated solvus line on a phase diagram


for (Zr1-х,Uх)SiO4 solid solution

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The Common Use Center “Geoanalyst” is
willing to collaborate with geological,
environmental and any other interested
organizations in providing analyses of
samples, and organizing training courses,
workshops, seminars and exhibitions.

Common User Center “Geoanalyst”

620016 Yekaterinburg
Academician Vonsovsky Street, 15
+7 (343) 287-90-13, +7 (343) 2879027
Votyakov@igg.uran.ru
www.geoanalyst.igg.uran.ru

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