Standard reference materials for cements

Sieber, John R.; Broton, D.; Fales, C.; Leigh, Stefan D.; MacDonald, Bruce S.; Marlow, Anthony F.; Nettles, Scott H.; Yen, James H.

doi:10.1016/s0008-8846(02)00896-7

Cited by 11 publications

(7 citation statements)

References 4 publications

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“…If the set of calibration standards is carefully designed to closely bracket the composition of the fused unknown for all constituents, the calibration function can be simplified to a line plus corrections for spectral line overlaps. The utility of this approach for high-accuracy determinations has been demonstrated for zeolite materials [13], portland cement [13,14], low alloy steel [15], and a Ti-Al aerospace alloy [15]. In these examples, the material was fused and measured to determine the nominal composition of the borate beads.…”

Section: All Copyrights For the Document Are Retained By Icddmentioning

confidence: 99%

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F08 Validation of an alkali reaction, borate fusion X-ray fluorescence method for silicon metal

et al. 2006

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The value assignment of candidate Standard Reference Material (SRM ®) 57b Silicon Metal provided an opportunity to develop an alkali reaction procedure as a precursor to borate fusion for the preparation of test specimens from the metal powder for X-ray fluorescence spectrometry (XRF). Suggested for this purpose by Blanchette (Adv. X-Ray Anal., 45, 415, 2002), the alkali reaction uses LiOH•H 2 O to convert Si to Li 2 SiO 3. Lithium silicate is fused with lithium borate flux without damage to platinum ware. Once specimens are fused and cast as beads, calibration standards are prepared to closely match the compositions of the specimens allowing a linear calibration for each analyte. The XRF method yields results that are directly traceable to the mole through NIST SRM spectrometric solutions. The method was validated in two ways. First, the reaction was used on older SRMs for Si metal: SRM 57 and SRM 57a. Second, XRF results for candidate SRM 57b were compared to results obtained using prompt gamma-ray activation analysis (PGAA) and inductively coupled plasma optical emission spectrometry (ICPOES). Bias tests show the XRF results are accurate for the elements Al, S, Ca, Ti, Cr, Mn, Ni, Cu, and Zr. Levels of S, Ca, Cr, and Cu in candidate SRM 57b are near the limits of quantification of the borate fusion method. Iron results may be subject to a low bias. Phosphorus is not quantitatively retained during the alkali reaction and borate fusion. These elements, plus B which cannot be determined after borate fusion, are listed in manufacturing specifications for Si metal.

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Section: All Copyrights For the Document Are Retained By Icddmentioning

confidence: 99%

“…The calibration approach for this method is the preparation of synthetic calibration standards to bracket the fused samples [13,14,15]. In this work, the primary reference materials used to prepare the synthetic calibrants are NIST single-element spectrometric solution SRMs.…”

Section: Quantitative Approachmentioning

confidence: 99%

F08 Validation of an alkali reaction, borate fusion X-ray fluorescence method for silicon metal

et al. 2006

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“…In addition, the RM needs to be stable only for the duration of the PT scheme, and not for the years required of a CRM [22]. The particular steps required to produce a CRM vary somewhat among the institutions engaged in developing CRMs, but all of the institutions share several important steps [20][21][22][25][26][27][28]. Statistical protocols for the certification of RMs in interlaboratory studies have been published [29].…”

Section: Introductionmentioning

confidence: 99%

“…The first is to minimize metal contamination, given that as gross contamination can occur during grinding, from any deposits remaining from previously processed samples, and also from contact with the grinding surfaces of the device(s) used [28,36]. Another consideration is to maximize the amount of material that can be processed at one time.…”

Section: Introductionmentioning

confidence: 99%

Development of candidate reference materials for the measurement of lead in bone

et al. 2008

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The production of modest quantities of candidate bone lead (Pb) reference materials is described, and an optimized production procedure is presented. The reference materials were developed to enable an assessment of the interlaboratory agreement of laboratories measuring Pb in bone; method validation; and for calibration of solid sampling techniques such as laser ablation ICP-MS. Long bones obtained from Pb-dosed and undosed animals were selected to produce four different pools of a candidate powdered bone reference material. The Pb concentrations of these pools reflect both environmental and occupational exposure levels in humans. The animal bones were harvested post mortem, cleaned, defatted, and broken into pieces using the brittle fracture technique at liquid nitrogen temperature. The bone pieces were then ground in a knife mill to produce fragments of 2-mm size. These were further ground in an ultra-centrifugal mill, resulting in finely powdered bone material that was homogenized and then sampled-scooped into vials. Testing for contamination and homogeneity was performed via instrumental methods of analysis.

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“…If the set of calibration standards is carefully designed to closely bracket the composition of the fused unknown for all constituents, the calibration function can be simplified to a line plus corrections for spectral line overlaps. The utility of this approach for high-accuracy determinations has been demonstrated for zeolite materials (Sieber, 2002), portland cement (Sieber, 2002; Sieber et al , 2002), low alloy steel (Sieber et al , 2005), and a Ti-Al aerospace alloy (Sieber et al , 2005). In these examples, the material was fused and measured to determine the nominal composition of the borate beads.…”

Section: Introductionmentioning

confidence: 99%

Validation of an alkali reaction, borate fusion, X-ray fluorescence method for silicon metal

et al. 2007

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The value assignment of candidate Standard Reference Material ͑SRM®͒ 57b Silicon Metal provided an opportunity to develop an alkali reaction procedure as a precursor to borate fusion for the preparation of test specimens from the metal powder for X-ray fluorescence spectrometry ͑XRF͒. Suggested for this purpose by Blanchette in a 2002 Advances in X-ray Analysis article ͓ 45, 415-420 ͑2002͒ ͔, the alkali reaction uses LiOH · H 2 O to convert Si to Li 2 SiO 3 . Lithium silicate is fused with lithium borate flux without damage to platinum ware. Once specimens are fused and cast as beads, calibration standards are prepared to closely match the compositions of the specimens, allowing a linear calibration for each analyte. The XRF method yields results that are directly traceable to the mole through NIST SRM spectrometric solutions. The method was validated in two ways. First, the reaction was used on older SRMs for Si metal: SRM 57 and SRM 57a. Second, XRF results for candidate SRM 57b were compared to results obtained using prompt gamma-ray activation analysis ͑PGAA͒ and inductively coupled plasma optical emission spectrometry ͑ICPOES͒. Bias tests show the XRF results are accurate for the elements Al, S, Ca, Ti, Cr, Mn, Ni, Cu, and Zr. Levels of S, Ca, Cr, and Cu in candidate SRM 57b are near the limits of quantification of the borate fusion method. Iron results may be subject to a low bias. Phosphorus is not quantitatively retained during the alkali reaction and borate fusion. These elements, plus B, which cannot be determined after borate fusion, are listed in manufacturing specifications for Si metal.

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Standard reference materials for cements

Cited by 11 publications

References 4 publications

F08 Validation of an alkali reaction, borate fusion X-ray fluorescence method for silicon metal

F08 Validation of an alkali reaction, borate fusion X-ray fluorescence method for silicon metal

Development of candidate reference materials for the measurement of lead in bone

Validation of an alkali reaction, borate fusion, X-ray fluorescence method for silicon metal

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