3/12/99


Hi,

A student in the lab is looking at museum samples of dinosaur bones and

teeth on the SEM. He could get access to more samples if he could restore

them to their original condition ( ie, remove the gold). Is there a good

nondestructive way to do this?



Kim DeRuyter

Histology and Electron Microscopy Labs

University of Alaska Fairbanks


A less destructive way to analyze these samples would be to coat them with

carbon instead of gold, and then ashing the carbon off with O2. Gold is tricky

to remove on most materials (I work mostly with semiconductors), but would be

very difficult to remove on dinosaur bones. (This is assuming your samples are

small enough to fit into an available asher or RIE tool). There are several

labs that could perform both the coating and ashing - let me know if you have

trouble locating one close to your area.

Lisa Montanaro

Consultant, MME

CMontana4@aol.com


A good way to handle specimens of this sort is to make casts of the

surface and examine the casts in the SEM. This way there is no damage to

the original artifact. I had an anthropology grad student do this with

human teeth for his thesis research. He worked out a very inexpensive, low

tech, but reliable method to do the casting. He can be reached at the

following for full details of his method:

Dr. Chris Schmidt

Indianapolis University

cschmidt@indy.edu



Debby Sherman, Manager Phone: 765-494-6666

Microscopy Center in Agriculture FAX: 765-494-5896

Dept. of Botany & Plant Pathology E-mail: sherman@btny.purdue.edu

Purdue University

1057 Whistler Building

West Lafayette, IN 47907-1057


I believe that the 1 N NaOH is unecessarily strong to accomplish the purpose

and would result in damage to some specimens. A very brief exposure to NaCN

with a stronger oxidant such as ammonium persulfate or hydrogen peroxide

would probably accomplish the result without prolonged exposure to the

reagents which would lead to their becoming more deeply absorbed into

capillaries that may exist.



John Twilley

Conservation Scientist

jtwilley@sprynet.com


Kim

I seem to remember a story - a long time ago - about about dipping the sample in

liquid mercury - the gold is taken into the liquid as an amalgam and leaves the

specimen clean. I have never tried it. I do not know what any Safety person would

say about that these days!







Keith Ryan

Marine Biological Association of the UK

Citadel Hill

Plymouth

Devon PL1 2PB

England



Tel. 0044 1752 633249 (International)

Tel. 01752 633294 (National)



Fax. 0044 1752 633102 (International)

Fax. 01752 633102 (National)



e-mail: k.ryan@pml.ac.uk


Kim,

One thing that no one has mentioned, yet, is low kV operation. If

your instrument will operate at 5kV or lower (perferably around 1kV) and

you limit your beam current, you should be able to view uncoated

specimens at at least a couple of kX. Some intruments will go much

higher at that voltage range. Grains of quartz may still present a

problem because SiO2 is such a good insulator, but many other minerals

will work fine under those conditions.



Ken Converse

owner

Quality Images

third party SEM service

Delta, PA

qualityimages@netrax.net


Dear Kim,

an old method which I used a long while ago and now and then recently

to remove gold from calcareous surfaces of REM-samples is to leave

the sample in a solution of NaCN and NaOH and let air bubble through

by means of a small glass pipette. The amount of NaCN is about 1-2%

and NaOH should be 1 N or more. You may try it on a fresh part of

bone perhaps it works.

Dietmar Keyser

PLEASE NOTE THE CHANGE IN TELEFON AND FAX

Dr.Dietmar Keyser

Zoologisches Institut und Museum

Martin-Luther-King Platz 3

D-20146 Hamburg

Germany

Tel. +49 40/428 38 4232

Fax: +49 40/428 38 3937

E-mail: Keyser@zoologie.uni-hamburg.de


Of all the suggestions, I believe you'll want to develop the

casting procedure for your facility. I can give you the e-mail

address for Dr Robert Pastor who can let you know which resin

materials he used, but he used two ... one for the field while

casting the pliable negative mold of ancient Pakastani teeth,

and another casting resin for the durable positive mold in the

lab. You'd then be able to coat with gold and archive these

specimens for all types of future study ... and I was quite

impressed with the detail of the micr-wear and lack of artifacts.



cheerios, shAf



<>/\<\/>/\<\/>/\<\/>/\ cogito, ergo zZOooOM /\<\/>/\<\/>/\<\/>/\<>

Michael Shaffer, R.A. - ICQ 210524

Geological Science's Electron Probe Facility - University of Oregon

mshaf@darkwing.uoregon.edu - http://darkwing.uoregon.edu/~mshaf/




Getting gold off museum fossil pieces is nay impossible. Al

would be easier but basically its the same problem. C

coating is good enough for low powers, but again, Curators

do not like that dark coating,

To view these "hard, dry and non-conducting" specimens

uncoated, the best solution is a poor vacuum SEM; a fully

fledged Environmental SEM would also do well, but its a

more expensive instrument for that job. Poor vacuum SEM's

(I believe at least a couple of the major manufacturers

make instruments with that facility) use only mechanical

pump vacuum in the specimen chamber and because of a vacuum

limiting aperture retain high vacuum in the gun chamber.

Secondary mode is impossible, but a Robinson detector gives

excellent images for this type of work. Magnifications

under these conditions are limited to about 2000x, but

details in fossils do not warrant higher magnifications;

its the SEM's superior depths of field that wins out over

light microscopy.

Kim - all you require now is one of those scopes!

Years ago I modified an Etec Autoscan to function

reversibly as a poor vacuum instruments. It worked well but

it was a fair bit of trouble to accomplish the required

modifications.

Our online contain a link to an archive collated by Scott

Wight. This contains listserver contributions concerned

with Environmental and Poor Vacuum SEM.

Cheers

Jim Darley

ProSciTech Microscopy

PLUS

PO Box 111, Thuringowa QLD 4817 Australia

Phone +61 7 4774 0370 Fax: +61 7 4789 2313

Great microscopy catalogue, 500 Links, MSDS, User Notes

********************** www.proscitech.com.au *****


I agree with Jim that the best way to deal with gold on museum specimens, artwork,

taxonomic type specimens, fossils etc is to leave it off in the first place where

possible. The material can sometimes be viewed in a normal SEM by keeping kV

and probe current low, or generally more conveniently by using one of several types

of variable pressure SEM. Until recently the cheaper versions, working up to about

2 torr, were restricted to non-SE detection modes (BSE, CL, absorbed current etc)

but several SE detector systems working in this range have become commercially

available.

We have just installed a new Robinson detector which allows convenient BSE

and/or SE detection to low kV, in high vacuum or variable pressure conditions, on a

small Hitachi NSEM. (1992) and find the combination mode in particular gives very

good results for topographic imaging.

beats explaining a caustic cyanide stew to your friendly curator, I should think.



cheers



Sally

Dr Sally Stowe

Facility Coordinator

Australian National University EM Unit

Research School of Biological Sciences

Box 475,

ACT 2601, Canberra, Australia

FAX 06 (0)2 6279 8525


Hello Ricardo!

Especially for insects have a look at:



C. Arno': Removal of gold coatings from biological SEM specimens,

European Microscopy and Analysis, July 1998, p.13



In this suggestion bromine vapors are used. If you have problems to get

this article, let me know your fax number. I then will send a fax copy

--

Gerhard Frank

UNIVERSITAET ERLANGEN-NUERNBERG Phone: +49 9131 85

28606

Institut fuer Werkstoffwissenschaften VII Fax: +49 9131 85 28602

Cauerstr. 6, D-91058 Erlangen, Germany frank@ww.uni.erlangen.de




On the general subject of removing sputtered of evaporated metal from

SEM samples. I am told that removing silver can be a relatively

simple.

The following paper describes a method using "Farmer's"

reducer, a dilute aqueous solution of potassium ferricyanide and

sodium thiosulphate.



"Silver as a removable conductive coating for scanning electron

microscopy" by A.A. Mills Dept. Geology, University of Leicester. UK



Scanning Microscopy, Vol. 2, No. 3 1998 (pages 1265 - 1271)









Best regards

Mike Wombwell

Polaron range Business Manager

V G Microtech

The Birches Industrial Estate

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RH19 1UB

UK

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E&OE


I am wonder if Dietmar method could be used for beetles...

Regards



Ricardo

www.coleoptera.org


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