hello my name is Greg Dunning and I'm a professor in the Department of

sciences at Memorial University my specialty is determining the age of

crystallization of rocks and today I'm going to take you through the labs
describe the procedures from start to finish and show you how we do this.
isotopes are separate atoms of the same element which differ in the
number of neutrons in a nucleus but have the same number of protons
which is what makes it a certain element certain isotopes of elements are
radioactive and decay at a set rate governed by what's called a decay
constant to a final stable isotope of another element so ones that are
used in geology include the rubidium 2 strontium. I stopped existing
potassium decaying to make the element argon samarium decaying to
produce the element neodymium, and uranium decaying to produce the
element lead there. the special case of uranium-lead dating of rocks
which is what we do in our lab is because there are two isotopes of
uranium with masses 238 and 235 and each of them is radioactive and
decays at a separate rate to a separate isotope of lead, uranium 238
decays to produce lead 206, and uranium 235 decays to produce lead
207. so this system is unique and that we have to chemically identical
isotopic systems which are totally separate and the uranium decays to
produce lead at different rates in each. so we can determine in two ages
for one mineral and compare them to each other and if the two ages are
the same that is a very good check that the age is correct and there's
been no disturbance of the system. the procedure to determine the age of
the rock actually should begin in the field where the student or the
mapping geologist figures out the relationships of the rocks and produces
a map of them and then selects the best sample to determine ages to
figure out the geological history of the área. so then when the mapping is
done they collect 20 kilogram rock sample or it's usually almost a meat
bucket full of rock, and bring it back to the lab we then start by washing it
and then we crush it through chips eyes and a crusher that's much like
those needs in a mine and then we pulverize it to a powder which is sort
of a consistency of baking flour. then we pan that powder on a panning
table to separate only certain minerals that we're going to want to look at
and analyze and wash away most of the sample office Pennington we
then have a concentrate of dense minerals which include those we can
date that are maybe a few hundred grams left of the 20 kilogram row now.
we have to separate each mineral from the other because we're going to
look for the mineral zircon which when it crystallizes takes uranium into its
structure and therefore is a mineral we can determine the age, and we do
this by separating them according to their density by passing them
through a very dense liquid and the dense mineral sink and the light
minerals float, and then we pass it through a magnetic field on a
separator that passes the minerals on a trough through dense magnetic
field and separates minerals according to their iron content their magnetic
susceptibility at the end, of this process we usually have a few milligrams
are 1020 milligrams in some rocks of the mineral zircon and have
removed essentially all other minerals from this concentrate that we got
from penny. we then take those minerals and select the very highest
quality ones that look the most like gems beautiful like not diamond shape
but prisms that are very high luster under a microscope we do this under
qahal so they don't blow away in the wind, and with using jewelers
tweezers to select individual crystals, and we picked a 40 or 50 of those
to process further we want to see the inside structure of the mineral to
see if there's any older nuclei on which the later zircon crystallized or is it
entirely a homogeneous single generation cristal, so we take some
crystals and we mount them in epoxy and we polish them down to the
center the crystals to examine them with a scanning electron microscope,
with the scanning electron microscope firing an electron beam at the
mineral and mapping it we can see the internal crystal structure and see if
it grew just as one layer on top of another on top of another to the current
size or whether there's internal disturbances was it partially corroded a
new material grow and then it was partially corroded and new material
grow so you can see that easily in images from the scanning electron
microscope, so we select the simplest crystals with the simplest
crystallization history and then we take them to a chemistry lab that when
all the air and all the water and acids are filtered and distilled so that it's
clean of lead the whole environment of the lab is clean al and. then we
wash the crystals and distilled acids and we place them in Teflon
capsules with hydrofluoric acid .And we put that in an oven at 200 REE
centigrade for three days and in the oven in this pressurized Teflon
capsule in hydrofluoric acid the entire crystal dissolves and when we take
it out and open the capsule we have a clear solution no crystals left that
clear solution contains all the elements that were in the mineral zircon
which are silicon zirconium rare earth elements and uranium and lid, we
spend a day usually doing six samples at a time passing them through a
procedure called ion exchange chemistry, it's a bit like the chemical filters
that you would get in a Brita Walter filter for example we passed this clear
solution through this ion exchange column filled with a resin and by
changing the composition of the water or the acid through that we pass
through the resin after we put the sample in we can wash certain
elements away out of the column while the resin chemically bonds to
other elements and holds them in the column. so by a simple design of
the chemical steps we remove silicon zirconium and the rare earth
elements and through all of that the lead and uranium are held on the ion
exchange column so everything else is washed away and the column is
only holding the uranium and lead. then at the last step we have a clean
sample beaker a small one and we wash water through the column and
water removes every element from this resin however the only elements
left to wash out our lead and uranium so in the beaker we're collecting
absolutely purified lead in uranium and all the other elements are
removed so we dry this down on a hot plate to a single drop and that
single drop now would contain ten to a hundred picograms of lead and a
picogram is ten to the minus twelve grams so this is a tiny tiny amount of
lead from that crystal of zircón. so now we have a beaker with all the lead
and uranium in it from 1 zircon crystal or sometimes 2 zircon crystals
dissolve together we have to measure this lead and uranium we have to
measure the ratio of the isotopes of the lead and the ratio of the isotopes
of the uranium to calculate an age we have to know how much light is
there and how much uranium is there. we add a special solution with a
purified non-natural lead isotope that we can add a known amount to the
sample before we measure it and that is our calibration, we don't know
how much of the lead of each isotope was present in the zircon but we do
know the exact amount of this unnatural light isotope which has the mass
205 that we've added to the simple. so we take this now to the analytical
instrument we're going to use to measure the ratios which is a mass
spectrometer because we're measuring masses different masses of the
element lead mass 204 206 207 and 208 and 206 and 207 remember are
the two masses of lead that were each produced by decay of uranium so
in the mass spectrometer we load the sample on a single ribbon of very
high temperature metal rhenium and we it's attached to electrical contacts
and we load that in a sample chamber and the electrical contacts are
made contact with others in the sample chamber which is pumped down
to very high vacuum so there's no oxygen no nitrogen no atmosphere in it
when you do that you can heat the ribbon of rhenium on which the
sample has been deposited up to 1,500 degrees centigrade without it
melting, and when you heat the ribbon up to that high temperature the
drop that we've placed on this filament it's evaporated of course but the
LED ionizes the LED loses an electron becomes a lead +1 ion and
suddenly now these are ions charged ions not atoms not neutral atoms
but we focus them with a set of electrical lenses so the series of lens is
much like the series of optical lenses in a camera that there's a series of
them with different spacings and different charges applied and as the ions
pass through them they're focused into a single beam of ions these are
accelerated down a flight tube by a very high voltage difference and this
that it's called a flight tube it's a it's a vacuum chamber but now it's a
narrow tube and this narrow tube enters a very powerful electromagnet
which is got a slot in the middle through which the tube passes and in a
magnetic field this very strong electromagnets magnetic field the charged
ions are bent through a curvature of 90 degrees as they fly down this tube
,so remember the lead atoms have different masses from mass 204 to
mass 208 they all have to turn 90 degrees while in this light tube while
passing through the magnetic field the lightest isotope LED 204 is turned
in the tightest radius and led 208 is in the most open radius it's like
turning a corner in a Maserati versus a Mack truck so when they come
out of the magnetic field and have turned 90 degrees they are now
separated into parallel ion beams according to their mass 2a4 the 205 we
added from the tracer solution the 206 207 and 208 so we now have five
parallel ion beams moving down the flight tuve, we want to count the
amount of each of these we want to measure each of these beams so we
have detectors at the end of the flight tube one in the position where it will
receive the beam from each of these each of these five beams 204 to 208
LED we measure them all simultaneously and the electrical current is
produced by measuring them is amplified through an amplifier and then
goes to a meter and is recorded and we count basically we are counting
the intensity of each ion beam which is proportional to the amount of each
isotope of LED that's present that's what we want to know the amount of
each isotope of LED that is present so we can work back to calculating an
age so a mass spectrometer produces the spectrum of the five masses of
lead and counts them all with five detectors and we can calculate the
number of atoms in each of those ion beams then we do the same for
uranium and we then know the number of atoms of uranium 238 and the
number of atoms of uranium 235 and their daughter elements lead
isotopes, and we used a decay equation of the age calculation equation
to calculate the time it took essentially for that amount of lead to
accumulate in that zircon crystal by decay of the uranium. so that's a fairly
simple calculation and it results in one data point one zircon crystal for
which we have the two ages the two the 238 to 206 radiometric age and
the 235 uranium to 207 lead age the two ages might not exactly agree
one might be 410 million years and the other one might be 400 9.8 million
years for example or 410 point 1 million years but they should usually
agree within hundreds of thousands of years at 400 million years and they
should always agree if it's a closed system they should agree within the
uncertainties on the two ages that we've calculated. this technique of
uranium-lead geochronology by thermal ionization mass spectrometry
involves chemical separation of the elements we analyze lead in uranium
and it's quick client time consuming and requires a very clean chemistry
lab and distill reagents it is the gold standard and uranium lead
geochronology gives the most accurate and precise results that are the
most trusted there are other techniques that are faster and more modern
and developed more recently one involves firing a laser beam at the
zircon in the mount like we saw and that laser beam atomized as the
sample right there all the elements are still present but then they are
filtered out in the process in the mass spectrometer and they separate the
peaks from lead and uranium from the other peaks from their errors and
Azarcon and zirconium and can still calculate an age, these are less
precise but they are good for as a rapid technique if you want to analyze
hundreds of zircon say as detritus from the Sam stone a third technique is
long standing and it's called ion probe analysis and instead of firing a
laser beam at the zircon mount you fire an oxygen ion beam and it
excavates a small pit in the sample in the zircon crystal and again
atomizes it and again you're measuring all the elements that are present
as aircon but separating in the mass spectrometer the lead and uranium
and calculating an age from them if two is less precise you're analyzing
only a tiny amount of the zircon on the surface instead of the whole
crystal like we do and that's the key reason it's less precise but it's also
commonly used they are both much faster techniques the beam analysis
techniques take minutes instead of weeks if you pay and precision for not
spending the time doing the chemical separation.