Focused Interest Group on MicroAnalytical Standards ... › PDF ›...
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1) The problem 2) Earlier studies 3) Need for a community-wide group 4) Online database & publications 5) Schedule & expected member participations Olivine #1 Olivine #1 Mn Mn 80 μm Olivine #1 Rockport Fayalite Focused Interest Group on MicroAnalytical Standards (FIGMAS): Assessing the quality, availability & need for standards in the microanalytical community Julien M. Allaz, U. of Colorado-Boulder, Dept. of Geological Sciences, Boulder (CO) Owen K. Neill, Washington State U., School of the Environment, Pullman (WA) Anette von der Handt, U. of Minnesota Twin Cities, Dept. of Earth Sciences, Minneapolis (MN) 1) The problem Over the past years, different EMP & SEM laboratories have come to use different sets of standards and reference materials (SRM) for quantitative analysis. Unfortunately... ● Some SRM have become unavailable (e.g., USNM - Smithsonian Institution collection) or are only available to a restricted group of people (e.g., internal reference materials). ● Other SRM are also available commercially or provided by other institutions and research centers, but they sometimes lack either broad availability or acceptable characterization (e.g., NIST and Corning glasses, Drake & Weill REE-glasses [1,2]). ● A clear assessment of SRM quality is often missing (see for example terminology by Carpenter [3], Fig. 1). ● Individual lab managers do commonly examine their own SRM collections to re-evaluate compositional homogeneity and accuracy of published compositions. Therefore, multiple accepted compositions for individual standards may exist. However, such information is only rarely disseminated in any systematic way. 2) Earlier studies Information about which SRM are available, how to obtain new SRM, and which existing SRM are the “Good”, the “Bad”, or the “Ugly” (to use Carpenter’s [3] terminology, Fig. 1, 2) is incredibly valuable to the microprobe community, but such information is often unpublished or hard to find. In fact, the most complete published review of common microprobe standards is now 30 years old [4]. More recently, a limited set of natural and synthetic Smithsonian microbeam SRM was reviewed, including: ● A check for their homogeneity and the presence of mineral inclusions or impurities [5,6,7,8] (Fig. 2), ● An investigation on the presence of Pb in the synthetic REE-phosphates [9], ● An evaluation of the micro- to nano-scale impurities in Kakanui Hornblende [10], and ● A review of the quality of several pyroxene standards [11]. References: [1] P.K. Carpenter et al., J. Res. Natl. Inst. Stand. Technol. 107 (2002), 703–718. [2] M.J. Drake and D.F. Weill, Chemical Geology 10 (1972), 179-181. [3] P.K. Carpenter, Microscopy & Microanalysis meeting 14 (2008), 530-531. [4] J.S. Huebner and M.E. Woodruff, US Geological Survey Open File Report 85-718 (1985), 237 pp. [5] E. Jarosewich, J.A. Nelen and J.A. Norberg, Geostandard newsletter 4 (1980), 43-47. [6] E. Jarosewich, J. Res. Natl. Inst. Stand. Technol. 107 (2002), 681–685. [7] T.R. Rose, Microscopy & Microanalysis meeting 14 (2008), 528-529. [8] Smithsonian Microbeam Standards – http://mineralsciences.si.edu/facilities/standards.htm [9] J.J. Donovan et al., The Canadian Mineralogist 41 (2003), 221-232. [10] E.P. Vicenzi and T. Rose, Microscopy & Microanalysis meeting 14 (2008), 522-523. [11] J. Fournelle, AGU Fall meeting (2012), V23C-2827. [12] Geological & Environmental Reference Materials – http://georem.mpch-mainz.gwdg.de 3) Need for a community-wide group The microprobe community needs a better assessment of the availability and quality of SRM, as well as developing new SRM to fill gaps in existing SRM collections. To address these issues, the Focused Interest Group on MicroAnalytical Standards (FIGMAS) aims to promote and facilitate the creation of a community-wide SRM collection that supports consistency and inter-laboratory comparison. This effort will include: ● Creating an online database of the currently available SRM used in EMP and SEM laboratories. ● Preparing round robins of selected SRM for interlaboratory calibration and further evaluation (homogeneity, composition). ● Assessing the need of additional SRM for quantitative analysis by EDS, WDS, or other in situ techniques (LA-ICP-MS, SIMS, etc.). ● Collecting and publishing known procedures for synthesizing or sintering a homogeneous SRM (glass or mineral), and developing new procedures for synthesizing or sintering SRM. In the future, this database could be extended and cross-referenced to other reference material databases already available for other analytical techniques (e.g., GEOREM for LA-ICP-MS, SHRIMP or SIMS [12]). The FIGMAS seeks to determine the availability and quality of each SRM used and to define them as Standard Reference Material, Reference Material or Certified Reference Material following the definition from the National Institute of Standards and Technology (NIST; http://www.nist.gov/srm/definitions.cfm). Each SRM will also vreceive a “score” reflecting its quality. The group will particularly focus on criteria such as: ● Quantity available & average particle size, ● Compositional homogeneity, ● Pervasiveness of impurities or inclusions, ● Resistance to beam damage and to high vacuum, ● Relative solubility the material in eluents used for polishing and cleaning, ● Long term stability (potential for oxidation, hydration, changes in crystal structure, etc.), and ● Availability and quality of quantitative analyses for each of the material’s constituent elements, including the analytical method used and the availability of a certificate from a trusted source (e.g., NIST or a similar recognized institution). 4) Online database & publications The results of the FIGMAS will be made available on an online database that the microbeam community can use as reference (e.g., Fig. 3), supplemented by peer-reviewed publications. FIGMAS members will be given access to the database to facilitate the addition of new SRM data. The committee will be responsible for reviewing any entry to validate its provenance, delete inappropriate or spurious entries, consolidate duplicates, and ensure completeness of the record. Each SRM must ideally contain the following information to achieve the desired quality of the database: ● Name & Identification number, ● Natural or synthetic origin, ● Source and reference (NMNH, NIST, etc.), ● Availability and purchase cost, list of vendors, etc., ● General material classification group (e.g., glass, silicates, oxides, alloy); additional classification terms when applicable, ● A mineral formula for natural or synthetic minerals, ● Standard hazards (e.g., poisonous, radioactive) and physical properties (e.g., solubility in eluent, long-term stability), ● List of available chemical analyses. Several analyses might be associated with one single SRM, and recommendation will be made for the “best” one. Each analysis should include the analytical method, the name of the analyst or the laboratory, the complete list of analyzed elements and concentrations, the analysis date, references to any publication or trusted website (i.e., GEOREM, NIST), etc. Additional details on the database content and format will be defined by the committee members. WE NEED YOUR HELP, to... - Fill-in the standard database - Evaluate standards (round robin...) - Create new standards Poster #399 5) Schedule & expected member participations Visit our website: http://figmas.geoloweb.ch * M.J. Drake & D.F. Weill (University of Oregon) * J. Hanchar (Memorial University) * D. Harlov (GFZ Potsdam, Germany) * And many other SRM... FIGMAS does not endorse or recommend any commercial products from the company mentioned above. They are mentioned as being provider of standards. Other providers might exist, and we apologize if these are not represented here. Figure 3: Example of what the database could look like: a listing of available SRMs and details for each SRM. The database will be managed by FIGMAS members and supervised by the committee. Screenshot taken from Julien’s website (http://cub.geoloweb.ch). With YOUR help, this database will constantly evolve to widely distribute valuable information, enhance inter-laboratory comparability, and permit some “bad” standards to, one day, join the “good” standards realm. In subsequent years, FIGMAS will continue to pursue its initial aims with adding additional SRM evaluations, searching for new SRM & developing new SRM creation techniques, etc. Fall/Winter 2015-2016: - Building online database (J. Allaz & committee) - Compiling commercially available SRM data (e.g., Astimex, MAC standards), SRM developed by recognized institutions (NIST, Smithsonian…), shared “in-house” SRM, “out-of-print” standards still in use (e.g., Drake & Weil, C.M. Taylor), etc. GOOD BAD UGLY The Good The Bad The Ugly Winter – Summer 2016: Quality evaluation of SRM begins; each SRM to be reviewed by at least 2-3 FIGMAS members. Evaluation should include automatic scoring of to reflect SRM quality (scale/grading TBD). Three evaluation options: (a) Previous good quality evaluation of SRM exists, (b) FIGMAS members will review SRM already in their collections that have not been evaluated satisfactorily. (c) New SRM will be distributed in round robins to selected FIGMAS members for evaluation. Additional thoughts and rules will be developed following suggestions from FIGMAS members. Winter/Spring 2017: - Gathering information on SRM preparation (synthesis/sintering). - Assessing needs of new SRM preparation procedures. - Determination of a priority list of SRM to be prepared. August 2016 – M&M Columbus (OH): First official FIGMAS meeting Fall 2016: Preparation of round robins for further evaluation. Summer 2017: Seek private sponsors to donate money and/or existing SRM for evaluation and for creation of new SRM (support will be acknowledged on the website and through official meetings; sponsor must remain neutral regarding the evaluation of SRM they have donated or helped creating). June 2015: Request for FIGMAS submitted to MAS & MSA. August 2017 – M&M St. Louis (MO): Second official FIGMAS meeting August 2015 (today): First unofficial FIGMAS meeting MAS & MSA accept our request? Aug.-Sept. 2015: Survey to to determine work of each FIGMAS member YEAR 1 YEAR 2 YEAR 3 Figure 2: Examples of standards – (a) “good” standard of Pb-free PrPO4, (b-d) “bad” standards with inclusions and inhomogeneous domains (b) in Olivine #1 (C.M. Taylor), (c) in Rockport Fayalite (NMNH), (d,e) in glass standard USNM 113716 (plagioclase inclusion and devitrification; courtesy of P. Carpenter), and (f) “ugly” Mn standard with oxygen map revealing oxidation. Astimex Astimex Astimex Figure 1: Carpenter “Clint Eastwood” categories of standards and practices: - Heterogeneous, intra grain variability, non-BSE variation (garnets), - Poorly maintained metals standards with oxide layer. - Materials which can be redeemed, - Not homogeneous, separate contaminated, undocumented source, - Not characterized at all, or only by EPMA, - In-house single primary reference with no secondary standards. - Homogeneous, inclusion- & impurity-free, widely available, free, - Well characterized, EPMA & wet chemistry, other techniques, - Primary and secondary standard comparison in EPMA runs. PrPO 4 a b c d e Mn O Ka in Mn f USNM 113716 Glass Plag.
Transcript of Focused Interest Group on MicroAnalytical Standards ... › PDF ›...
1) The problem
2) Earlier studies
3) Need for a community-wide group 4) Online database & publications 5) Schedule & expected member participations
Olivine #1Olivine #1
MnMn
80 μmOlivine #1
RockportFayalite
Focused Interest Group on MicroAnalytical Standards (FIGMAS): Assessing the quality, availability & need for standards in the microanalytical communityJulien M. Allaz, U. of Colorado-Boulder, Dept. of Geological Sciences, Boulder (CO)Owen K. Neill, Washington State U., School of the Environment, Pullman (WA)Anette von der Handt, U. of Minnesota Twin Cities, Dept. of Earth Sciences, Minneapolis (MN)
1) The problemOver the past years, different EMP & SEM laboratories have come to use different sets of standards and reference materials (SRM) for quantitative analysis. Unfortunately...
● Some SRM have become unavailable (e.g., USNM - Smithsonian Institution collection) or are only available to a restricted group of people (e.g., internal reference materials).
● Other SRM are also available commercially or provided by other institutions and research centers, but they sometimes lack either broad availability or acceptable characterization (e.g., NIST and Corning glasses, Drake & Weill REE-glasses [1,2]).
● A clear assessment of SRM quality is often missing (see for example terminology by Carpenter [3], Fig. 1).
● Individual lab managers do commonly examine their own SRM collections to re-evaluate compositional homogeneity and accuracy of published compositions. Therefore, multiple accepted compositions for individual standards may exist. However, such information is only rarely disseminated in any systematic way.
2) Earlier studiesInformation about which SRM are available, how to obtain new SRM, and which existing SRM are the “Good”, the “Bad”, or the “Ugly” (to use Carpenter’s [3] terminology, Fig. 1, 2) is incredibly valuable to the microprobe community, but such information is often unpublished or hard to find. In fact, the most complete published review of common microprobe standards is now 30 years old [4]. More recently, a limited set of natural and synthetic Smithsonian microbeam SRM was reviewed, including:
● A check for their homogeneity and the presence of mineral inclusions or impurities [5,6,7,8] (Fig. 2),
● An investigation on the presence of Pb in the synthetic REE-phosphates [9],
● An evaluation of the micro- to nano-scale impurities in Kakanui Hornblende [10], and
● A review of the quality of several pyroxene standards [11].
References:[1] P.K. Carpenter et al., J. Res. Natl. Inst. Stand. Technol. 107 (2002), 703–718.[2] M.J. Drake and D.F. Weill, Chemical Geology 10 (1972), 179-181.[3] P.K. Carpenter, Microscopy & Microanalysis meeting 14 (2008), 530-531.[4] J.S. Huebner and M.E. Woodruff, US Geological Survey Open File Report 85-718 (1985), 237 pp.[5] E. Jarosewich, J.A. Nelen and J.A. Norberg, Geostandard newsletter 4 (1980), 43-47.[6] E. Jarosewich, J. Res. Natl. Inst. Stand. Technol. 107 (2002), 681–685.[7] T.R. Rose, Microscopy & Microanalysis meeting 14 (2008), 528-529.[8] Smithsonian Microbeam Standards – http://mineralsciences.si.edu/facilities/standards.htm[9] J.J. Donovan et al., The Canadian Mineralogist 41 (2003), 221-232.[10] E.P. Vicenzi and T. Rose, Microscopy & Microanalysis meeting 14 (2008), 522-523.[11] J. Fournelle, AGU Fall meeting (2012), V23C-2827.[12] Geological & Environmental Reference Materials – http://georem.mpch-mainz.gwdg.de
3) Need for a community-wide groupThe microprobe community needs a better assessment of the availability and quality of SRM, as well as developing new SRM to fill gaps in existing SRM collections. To address these issues, the Focused Interest Group on MicroAnalytical Standards (FIGMAS) aims to promote and facilitate the creation of a community-wide SRM collection that supports consistency and inter-laboratory comparison. This effort will include:
● Creating an online database of the currently available SRM used in EMP and SEM laboratories.
● Preparing round robins of selected SRM for interlaboratory calibration and further evaluation (homogeneity, composition).
● Assessing the need of additional SRM for quantitative analysis by EDS, WDS, or other in situ techniques (LA-ICP-MS, SIMS, etc.).
● Collecting and publishing known procedures for synthesizing or sintering a homogeneous SRM (glass or mineral), and developing new procedures for synthesizing or sintering SRM.
In the future, this database could be extended and cross-referenced to other reference material databases already available for other analytical techniques (e.g., GEOREM for LA-ICP-MS, SHRIMP or SIMS [12]).
The FIGMAS seeks to determine the availability and quality of each SRM used and to define them as Standard Reference Material, Reference Material or Certified Reference Material following the definition from the National Institute of Standards and Technology (NIST; http://www.nist.gov/srm/definitions.cfm). Each SRM will also vreceive a “score” reflecting its quality. The group will particularly focus on criteria such as:
● Quantity available & average particle size,● Compositional homogeneity,● Pervasiveness of impurities or inclusions,● Resistance to beam damage and to high vacuum,● Relative solubility the material in eluents used for polishing and cleaning,● Long term stability (potential for oxidation, hydration, changes in crystal structure,
etc.), and● Availability and quality of quantitative analyses for each of the material’s constituent
elements, including the analytical method used and the availability of a certificate from a trusted source (e.g., NIST or a similar recognized institution).
4) Online database & publicationsThe results of the FIGMAS will be made available on an online database that the microbeam community can use as reference (e.g., Fig. 3), supplemented by peer-reviewed publications. FIGMAS members will be given access to the database to facilitate the addition of new SRM data. The committee will be responsible for reviewing any entry to validate its provenance, delete inappropriate or spurious entries, consolidate duplicates, and ensure completeness of the record. Each SRM must ideally contain the following information to achieve the desired quality of the database:
● Name & Identification number,● Natural or synthetic origin,● Source and reference (NMNH, NIST, etc.),● Availability and purchase cost, list of vendors, etc.,● General material classification group (e.g., glass,
silicates, oxides, alloy); additional classification terms when applicable,
● A mineral formula for natural or synthetic minerals,● Standard hazards (e.g., poisonous, radioactive) and
physical properties (e.g., solubility in eluent, long-term stability),
● List of available chemical analyses. Several analyses might be associated with one single SRM, and recommendation will be made for the “best” one. Each analysis should include the analytical method, the name of the analyst or the laboratory, the complete list of analyzed elements and concentrations, the analysis date, references to any publication or trusted website (i.e., GEOREM, NIST), etc.
Additional details on the database content and format will be defined by the committee members.
WE NEED YOUR HELP, to...
- Fill-in the standard database
- Evaluate standards (round robin...)
- Create new standards
Poster #399
5) Schedule & expected member participations
Visit our website:http://figmas.geoloweb.ch
* M.J. Drake & D.F. Weill (University of Oregon)* J. Hanchar (Memorial University)* D. Harlov (GFZ Potsdam, Germany)* And many other SRM...
FIGMAS does not endorse or recommend any commercial products from the company mentioned above. They are mentioned as being provider of standards. Other providers might exist, and we apologize if these are not represented here.
Figure 3: Example of what the database could look like: a listing of available SRMs and details for each SRM. The database will be managed by FIGMAS members and supervised by the committee.
Screenshot taken from Julien’s website (http://cub.geoloweb.ch).
With YOUR help, this database will constantly evolveto widely distribute valuable information, enhance inter-laboratory comparability, and permit some “bad” standards to, one day, join the “good” standards realm.
In subsequent years, FIGMAS will continue to pursueits initial aims with adding additional SRM evaluations, searching for new SRM & developing new SRMcreation techniques, etc.
Fall/Winter 2015-2016:- Building online database (J. Allaz & committee)- Compiling commercially available SRM data (e.g., Astimex, MAC standards), SRM developed by recognized institutions (NIST, Smithsonian…), shared “in-house” SRM, “out-of-print” standards still in use (e.g., Drake & Weil, C.M. Taylor), etc.
GO
OD
BA
DU
GLY
The GoodThe Bad
The Ugly
Winter – Summer 2016:Quality evaluation of SRM begins; each SRM to be reviewed by at least 2-3 FIGMAS members. Evaluation should include automatic scoring of to reflect SRM quality (scale/grading TBD). Three evaluation options:
(a) Previous good quality evaluation of SRM exists,(b) FIGMAS members will review SRM already in their collections that
have not been evaluated satisfactorily.(c) New SRM will be distributed in round robins to selected FIGMAS
members for evaluation.Additional thoughts and rules will be developed following suggestions from FIGMAS members.
Winter/Spring 2017: - Gathering information on SRM preparation (synthesis/sintering).- Assessing needs of new SRM preparation procedures.- Determination of a priority list of SRM to be prepared.
August 2016 – M&M Columbus (OH): First official FIGMAS meeting
Fall 2016: Preparation of round robins for further evaluation.
Summer 2017: Seek private sponsors to donate money and/or existing SRM for evaluation and for creation of new SRM (support will be acknowledged on the website and through official meetings; sponsor must remain neutral regarding the evaluation of SRM they have donated or helped creating).
June 2015: Request for FIGMAS submitted to MAS & MSA.
August 2017 – M&M St. Louis (MO): Second official FIGMAS meeting
August 2015 (today): First unofficial FIGMAS meeting MAS & MSA accept our request?Aug.-Sept. 2015: Survey to to determine work of each FIGMAS member
YEA
R 1
YEA
R 2
YEA
R 3Figure 2: Examples of standards – (a) “good” standard of Pb-free PrPO4,
(b-d) “bad” standards with inclusions and inhomogeneous domains (b) in Olivine #1 (C.M. Taylor), (c) in Rockport Fayalite (NMNH), (d,e) in glass standard
USNM 113716 (plagioclase inclusion and devitrification; courtesy of P. Carpenter), and (f) “ugly” Mn standard with oxygen map revealing oxidation.
AstimexAstimexAstimex
Figure 1: Carpenter “Clint Eastwood” categories of standards and practices:
- Heterogeneous, intra grain variability, non-BSE variation (garnets),- Poorly maintained metals standards with oxide layer.
- Materials which can be redeemed,- Not homogeneous, separate contaminated, undocumented source,- Not characterized at all, or only by EPMA,- In-house single primary reference with no secondary standards.
- Homogeneous, inclusion- & impurity-free, widely available, free,- Well characterized, EPMA & wet chemistry, other techniques,- Primary and secondary standard comparison in EPMA runs.
PrPO4
a b c d e Mn
O Kain Mn
fUSNM113716Glass
Plag.
