acid preparation of fossils using sulfamic a

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Acid preparation of fossils using sulfamic acid, a weak organic acid, and its advantages over acetic and formic acid preparation Carlos B. Padilla & Mary Luz Parra Fundación Colombiana de Geobiología

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Page 1: Acid preparation of fossils using sulfamic a

Acid preparation of fossils using sulfamic

acid, a  weak organic acid, and its advantages over acetic  and formic acid preparation

Carlos B. Padilla & Mary Luz Parra

Fundación

Colombiana

de Geobiología

Page 2: Acid preparation of fossils using sulfamic a

Fundacion

Colombiana

de Geobiologia

Page 3: Acid preparation of fossils using sulfamic a

Large Volume of Calcareous Matrix : we pursued less immersions

• Authors of Vertebrate Paleontological Techniques vol 1 encompass

acid preparation with 

formic and acetic acids and suggest that discussions with Daniel

Gouget

(Institut

de 

Paleontologie

du Museum, Paris) supported their use of formic acid.

• They felt the stronger formic acid was more stressful to the fossil material but would require 

many less immersions than necessary with acetic acid.

Vertebrate Paleontological Techniques vol.1, Cambridge University Press, Patrick Leiggi and Peter May , 1994

Page 4: Acid preparation of fossils using sulfamic a

Sulfamic

Acid (H2

NSO3

H)

• Also known as amidosulfonic

acid; amidosulfuric

acid, sulphamic

acid; 

aminosulfonic

acid; kyselina

aminosulfonova; suphamidic

acid; sulfamidsäure

in 

German; acido

sulfamidico

in Spanish; acide

sulfamidique

in French, is a weak 

organic acid with marked characteristics that set it apart from acetic and formic 

acids:

• It is a stronger weak acid than both acetic and formic.

• Solid, crystalline powder which dissolves easily in water.

• A powder with melting point of 205°C.

• Non hydroscopic.

• Very stable and easy to transport.

• Less toxic

• Good history of use, common in domestic and industrial cleaning products 

designed to remove scale deposits. 

Page 5: Acid preparation of fossils using sulfamic a

Logarithmic Dissociation Constants (pKa) at 25°C  and NFPA Hazard Ratings 

NFPA 

Rating

State  fumes pKa health Fire reactivity

Sulfamic

Acid

solid  no 1.18 2 0 0

Formic 

Acid

liquid yes 3.74 3 2 0

Acetic 

Acid

liquid yes 4.76 2 2 2

Page 6: Acid preparation of fossils using sulfamic a

Commercial Sulfamic

Acid with pH  indicator

Page 7: Acid preparation of fossils using sulfamic a

The Procedure

• Follows most traditional guidelines.

• Time frames and concentrations varied.

• Initially used all three acids 5% by weight by volume,  eventually reduced to 4% for rapid matrix removal 

where significant fossil is not exposed.

• Once significant fossil material is exposed, acid   reduced to 2% weight by volume for most work  providing balance between time, number of 

immersions and bone integrity. 

Page 8: Acid preparation of fossils using sulfamic a

Comparative TestingAcid bath : 100 ml 2% (wbv)

Sample Matrix size: 10 gram fragment

Cycle time:   2hrs.Sample CBP‐17 CBP‐4 CBP‐21

Formic

Acid:

Cycles 4 4 7

Start

pH 2 2 2

End

pH 3 4 2

Residual matrix 0 gms 0 gms 7 gms

Acetic

Acid

Cycles 7 6 7

Start

pH 2 2 2

End

pH 4 3 2

Residual matrix 0 gms 0 gms 7 gms

Sulfamic

Acid

Cycles 4 4 7

Start

pH 1 1 1

End

pH 1 1 1

Residual matrix 0 gms 0 gms 6 gms

Page 9: Acid preparation of fossils using sulfamic a

Protection with Paraloid B-72

Preliminary cleaning

NO OK

CONTROL(porosity, etc)

Acid Inmersion

Neutralization

Mechanical preparation of soft parts

SUFAMIC ACID ACID(WASH

AND DRY)PARALOID B-72 inALCOHOL

SULFAMIC ACID(4-2%)

Ready More prep.needed

(RUNNING WATERAND DRY )

WASH

Page 10: Acid preparation of fossils using sulfamic a

Pliosaur

Specimen FCG‐CBP/004

Page 11: Acid preparation of fossils using sulfamic a

Chose the segments and tested

Page 12: Acid preparation of fossils using sulfamic a

Control of acid activity in fractures

Page 13: Acid preparation of fossils using sulfamic a

Repeat same procedure with more segments

12/16/02 Right lateral 01/09/03 Left lateral

01/14/03 Left lateral 01/30/03 Left lateral

Page 14: Acid preparation of fossils using sulfamic a

Ventral and Dorsal Views

Sutures and foramina well defined, excess B-72 removed

Page 15: Acid preparation of fossils using sulfamic a

Lateral right and left sides FCG‐CBP/004

Page 16: Acid preparation of fossils using sulfamic a

Delicate sclerotic rings

Page 17: Acid preparation of fossils using sulfamic a

Jan. 1999 Plesiosaur Specimen FCG‐CBP/003  

Page 18: Acid preparation of fossils using sulfamic a

CT Scan as a tool

to

preview

fossil material while

acid

cleaning

Page 19: Acid preparation of fossils using sulfamic a

Again well defined sutures and foramina

Page 20: Acid preparation of fossils using sulfamic a

Ventral view

Page 21: Acid preparation of fossils using sulfamic a

Vertebrae also enclosed in calcareous matrix

Page 22: Acid preparation of fossils using sulfamic a

Vertebrae ventral and lateral

Page 23: Acid preparation of fossils using sulfamic a

Articulated cranium

Page 24: Acid preparation of fossils using sulfamic a

Findings

• When all three acids are used for the same period of time per 

cycle, formic and sulfamic

will remove the same amount of 

matrix by weight, acetic at half the rate. This applies until the 

initial pH changes.

• Whereas the pH changes with formic and acetic acids after 2 

hrs of work, sulfamic

maintains the original pH up to 12 hrs 

later allowing for longer cycles without changing the acid 

bath.

Page 25: Acid preparation of fossils using sulfamic a

Mechanical and Acid vs

Acid preparation

FCG‐CBP/3 

Mechanical and Acid preparation

• Cycle time:

3‐5 hrs

• (7) seven cycles  with 4% 

acid.

• (3) three cycles with 2% 

acid.

FCG‐CBP/4

Only acid preparation

• Cycle time: 3‐5 hrs

• (15) fifteen cycles with 4% 

acid.

• (6) six cycles with 2% acid.

Page 26: Acid preparation of fossils using sulfamic a

Matrix thin sections and residue analysis

FCG-CBP-21

FCG-CBP-17

FCG-CBP-4

Grainstone (Durham 62)Haematite 8%Micro sparite 87%nummulites

Grainstone (Durham 62)Haematite 7%Micro sparite 86%

Gypsum 47%Haematite 47%

Clay 13%Quartz 4%Opaques 83%

Clay 88%Quartz 5%Opaques 2%

Clay 88%Quartz 2%Opaques 9%

Page 27: Acid preparation of fossils using sulfamic a

Conclusions

Page 28: Acid preparation of fossils using sulfamic a

Many Thanks to:• Mary Luz Parra, Fundacion

Colombiana

de Geobiologia.

• Jane Mason, Senior Museum Preparator, University of California Museum of Paleontology.

• Mark Norell,  Chairman and Curator Div. of Paleontology, American Museum of Natural 

History.

• Amy Rachel Davidson, Senior Principal Preparator, Dept. of Paleontology, American Museum 

of Natural History.

• Leslie Noè, Curator of Natural Science, Thinktank, Birmingham Science Museum.

• Carlos Jaramillo, Smithsonian Tropical Research Institute, Panama.

• Maria Paramo, Research Professor, Universidad Nacional

de Colombia.

• Eugene S. Gaffney, Curator, Dept. of Paleontology, American Museum of Natural History.

• John Maisey, Curator and Axelrod Research Chair, American Museum of Natural

History.

• Fernando Etayo, Researcher, INGEOMINAS.

• Diego Pol, M.E.F., Trelew, Patagonia Argentina.

• Marcela Gomez, CASP, University of Cambridge.

• Tatiana Gaona, INGEOMINAS ( Instituto

Colombiano

de Geologia

y Minas).

• Juan de Dios Parra, Fundacion

Colombiana

de Geobiologia.