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ARCH-METALS  October 2018

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Subject:

Re: ARCH-METALS Digest - 4 Oct 2018 to 5 Oct 2018 (#2018-44)

From:

Stanislav Strekopytov <[log in to unmask]>

Reply-To:

Arch-Metals Group <[log in to unmask]>

Date:

Mon, 8 Oct 2018 08:37:53 +0000

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Dear David, 
The loss of Sn (or any other element forming volatile chlorides) due to the volatility might be important if HCl is used on its own, but in aqua regia it should not be an issue because of the presence of less volatile nitric acid. 
 
As Duncan mentioned below, we used aqua regia for both copper and tin bronze: 
"The samples (10–20 mg for copper ingots and 4–7 mg for bronze artefacts) were weighed to±0.01 mg, digested in a mixture of 0.55 ml of concentrated HNO3 and 1.75 ml of concentrated HCl (both acids SpA™ grade, ROMIL Ltd) with careful heating for a few minutes to improve dissolution of sulphide inclusions, and made up to 25 ml with ultra-pure water" 
Quanyu Wang, Stanislav Strekopytov & Benjamin W. Roberts, September 2018, ‘Copper ingots from a probable Bronze Age shipwreck off the coast of Salcombe, Devon: Composition and microstructure’, Journal of Archaeological Science 97(9):102-117. 
 
However, for pure tin we used a slightly different method: 
"The samples (4-25 mg) were weighed to ±0.01 mg, digested in 1 ml of concentrated HCl (SpA™ grade, ROMIL Ltd) with the addition of several drops of HNO3 (SpA™ grade, ROMIL Ltd) and H2O2 (Merck, Suprapur®), and made up to 25 ml with ultra-pure water." 
Wang, Q., Strekopytov, S., Roberts, B.W., Wilkin, N., 2016a. Tin ingots from a probable Bronze Age shipwreck off the coast of Salcombe, Devon: composition and microstructure. J. Archaeol. Sci. 67, 80–92. 
 
Both papers show the level of Quality Control that is expected for this type of analyses.  
My advice would be to test any lab you want to use for analysing bronzes with a set of bronze matrix reference materials, plenty of which are commercially available. 
 
Kind regards, 
Stas 
 
Stanislav Strekopytov, PhD, MRSC 
Senior Analytical Chemist 
Imaging and Analysis Centre 
Natural History Museum 
Cromwell Road 
London 
SW7 8QA 
 
Tel: +44 207 942 5498 
[log in to unmask] 
https://twitter.com/s_strekopytov 
http://www.nhm.ac.uk/our-science/departments-and-staff/staff-directory/stanislav-strekopytov.html 
 
 
 
 
----------------- 
 
Date:    Fri, 5 Oct 2018 10:35:57 +0000 
From:    Duncan Hook <[log in to unmask]> 
Subject: Re: Loss of tin from bronze in solution ICP analysis 
 
Dear David, 
For ICP-AES at the BM we used the method previously used for AAS (gentle warming of 2 mils of aqua regia diluted to 20 mils): 
 
M.J. Hughes, M.R. Cowell, P.T. Craddock 1976. ‘Atomic Absorption Techniques in Archaeology’, Archaeometry, 19-37. 
 
e.g. 
Hook, D.R., 1998. 'Inductively-coupled plasma atomic emission spectrometry and its role in numismatic studies', eds. W.A.Oddy and M.R. Cowell, Metallurgy in Numismatics, Royal Numismatic Society, (London) 4, pp. 237-252. 
 
I believe Nigel Blades used reverse aqua regia for copper alloys, which would keep the chloride down but I’m not sure whether it would work for high tin bronzes: 
Blades, N., 1995 ‘Copper alloys from English Archaeological Sites 400-1600 AD: An analytical study using ICP-AES’, PhD thesis, Royal Holloway & Bedford New College. 
 
Recently, Stas Strekopytov at the Natural History Museum in London has developed a method for analysing copper ingots and bronzes using both ICP-AES and ICP-MS: 
 
Quanyu Wang, Stanislav Strekopytov & Benjamin W. Roberts, September 2018, ‘Copper ingots from a probable Bronze Age shipwreck off the coast of Salcombe, Devon: Composition and microstructure’, Journal of Archaeological Science 97(9):102-117. 
 
 
I‘d prefer not to use HF if I could avoid it! 
Best wishes, 
Duncan 
 
Duncan Hook 
Department of Scientific Research 
The British Museum 
London 
WC1B 3DG 
 
The security classification of the email is OFFICIAL 
 
 
From: Arch-Metals Group [mailto:[log in to unmask]] On Behalf Of Strahan, Donna 
Sent: 04 October 2018 14:46 
To: [log in to unmask] 
Subject: Re: Loss of tin from bronze in solution ICP analysis 
 
David, 
 
The lab we worked with used nitric acid, which can have a similar problem in terms of tin. 
 
Matt Clarke, Scientist in Freer/Sackler, suggested another research paper used a small amount of HF to stabilize the Sn. 
Young, S. M. M., P. Budd, R. Haggerty, and A. M. Pollard. "Inductively Coupled Plasma‐Mass Spectometry for the Analysis of Ancient Metals." Archaeometry 39, no. 2 (1997): 379-392. 
 
Donna 
 
Donna Strahan 
Head, Department of Conservation and Scientific Research 
Freer Gallery of Art and Arthur M. Sackler Gallery 
 
From: Arch-Metals Group <[log in to unmask]<mailto:[log in to unmask]>> On Behalf Of Killick, David J - (killick) 
Sent: Wednesday, October 3, 2018 4:05 PM 
To: [log in to unmask]<mailto:[log in to unmask]> 
Subject: Loss of tin from bronze in solution ICP analysis 
 
We are using a new ICP lab that is more used to analyzing soils than metals, and are getting back numbers that suggest substantial loss of tin (compared to microprobe analyses of the same objects).  Can any of you provide a tested protocol for ICP analysis of tin-bearing copper alloys?  I’ve tried searching the Agilent and Perkin Elmer application notes but haven’t yet come up with anything useful. 
 
 
 
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