Hi Matthew,

Welcome to the wonderful world of clay mineralogy !

Separating the clay (typically <2 um) by gravity settling is actually 
preferable to centrifuging, as you can more easily check for flocculation. [If 
this is a problem add some drops of sodium hexametaphosphate (‘Calgon’) 
solution.]  At BGS, we dry our isolated <2 um fractions right down in a 
moisture extraction oven (set at 55degC), homogenise and then resuspend a known 
amount (¬80 mg) to produce a consistently thick oriented mount.

If you are not aware of it – Moore & Reynolds (1997) is the bible for clay 
preparation and analysis – very easy to follow.

Moore, D.M. and Reynolds, R.C. 1997.  X-Ray Diffraction and the Identification 
and Analysis of Clay Minerals, Second Edition. Oxford University Press, New 

Best regards, Simon

Simon Kemp
Senior Mineralogist

p       +44 (0)115 936 3448
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British Geological Survey | Nicker Hill | Keyworth | Nottingham NG12 5GG | UK


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From: rietveld_l-requ...@ill.fr <rietveld_l-requ...@ill.fr> On Behalf Of 
Matthew Rowles
Sent: 01 July 2021 05:26
To: RIETVELD_L Distribution List <rietveld_l@ill.fr>
Subject: Clay sample preparation

Hi all

I’m gingerly venturing into clay analysis.

I’ve done previous analyses on pre-separated clay fractions by resuspending the 
clay in a little ethanol and dripping onto a Si wafter to make an oriented 
mount (which is then also successively glycolated and heat treated).

I have some upcoming work which will necessitate creating the clay fraction.

I don’t have a centrifuge, so I have to separate the clay fraction by settling. 
The USGS methodology looks like a good method to follow: 

After I’ve suctioned off the clay suspension, what is the best way to get at 
the clay? Leave it settle more? Evaporate the water?

(I’m also in the middle of commissioning a spray-drier, so that will help with 
the random mounts.)


Matthew Rowles
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