ASTM C1605-04(2009)
(Test Method)Standard Test Methods for Chemical Analysis of Ceramic Whiteware Materials Using Wavelength Dispersive X-Ray Fluorescence Spectrometry
Standard Test Methods for Chemical Analysis of Ceramic Whiteware Materials Using Wavelength Dispersive X-Ray Fluorescence Spectrometry
ABSTRACT
These test methods details the standard procedures for the determination of ten major elements (SiO2, Al2O3, Fe2O3, MgO, CaO, Na2O, K2O, TiO2, P2O5, MnO), and LOI in ceramic whitewares clays and minerals using wavelength dispersive X-ray fluorescence spectrometry (WDXRF). Besides the simultaneous X-ray spectrometer, this test procedure shall also need Pt-Au alloy crucibles and molds, fluxers, muffle furnaces with rocker attachments, and hot plate and muffle furnaces. The sample is first ignited, then fused with lithium tetraborate and the resultant glass disc is introduced into a wavelength dispersive X-ray spectrometer. The disc is irradiated with X-rays from an X-ray tube. X-ray photons emitted by the elements in the samples are counted and concentrations determined using previously prepared calibration standards. In addition to the 10 major elements, the method provides a gravimetric loss-on-ignition.
SCOPE
1.1 These test methods cover the determination of ten major elements (SiO2, Al2O3, Fe2O3, MgO, CaO, Na2O, K2O, TiO2, P2O5, MnO, and LOI in ceramic whitewares clays and minerals using wavelength dispersive X-ray fluorescence spectrometry (WDXRF). The sample is first ignited, then fused with lithium tetraborate and the resultant glass disc is introduced into a wavelength dispersive X-ray spectrometer. The disc is irradiated with X-rays from an X-ray tube. X-ray photons emitted by the elements in the samples are counted and concentrations determined using previously prepared calibration standards. (1) In addition to 10 major elements, the method provides a gravimetric loss-on-ignition.
Note 1—Much of the text of this test method is derived directly from Major element analysis by wavelength dispersive X-ray fluorescence spectrometry, included in Ref (1).
1.2 Interferences, with analysis by WDXRF, may result from mineralogical or other structural effects, line overlaps, and matrix effects. The structure of the sample, mineralogical or otherwise, is eliminated through fusion with a suitable flux. Fusion of the sample diminishes matrix effects and produces a stable, flat, homogeneous sample for presentation to the spectrometer. Selecting certain types of crystal monochromators eliminates many of the line overlaps and multiorder line interferences. A mathematical correction procedure (2) is used to correct for the absorption and enhancement matrix effects.
1.3 Concentrations of the elements in clays and minerals are determined independent of the oxidation state and are reported in the oxidation state in which they most commonly occur in the earth’s crust.
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Standards Content (Sample)
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Designation: C1605 − 04(Reapproved 2009)
Standard Test Methods for
Chemical Analysis of Ceramic Whiteware Materials Using
Wavelength Dispersive X-Ray Fluorescence Spectrometry
This standard is issued under the fixed designation C1605; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
Concentration range
Element
(percent)
1.1 These test methods cover the determination of ten major
Al O 0.10 58.0
2 3
elements (SiO ,Al O,Fe O , MgO, CaO, Na O, K O, TiO , Fe O 0.04 28.0
2 3
2 2 3 2 3 2 2 2
MgO 0.10 60.0
P O ,MnO,andLOIinceramicwhitewaresclaysandminerals
2 5
CaO 0.02 60.0
using wavelength dispersive X-ray fluorescence spectrometry
Na O 0.15 30.0
(WDXRF). The sample is first ignited, then fused with lithium K O 0.02 30.0
TiO 0.02 10.0
tetraborate and the resultant glass disc is introduced into a
P O 0.05 50.0
2 5
wavelength dispersive X-ray spectrometer. The disc is irradi-
MnO 0.01 15.0
LOI (925°C) 0.01 100.0
atedwithX-raysfromanX-raytube.X-rayphotonsemittedby
the elements in the samples are counted and concentrations
1.5 This standard does not purport to address all of the
determined using previously prepared calibration standards.
safety concerns, if any, associated with its use. It is the
(1) In addition to 10 major elements, the method provides a
responsibility of the user of this standard to establish appro-
gravimetric loss-on-ignition.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
NOTE 1—Much of the text of this test method is derived directly from
Major element analysis by wavelength dispersive X-ray fluorescence
spectrometry , included in Ref (1).
2. Referenced Documents
1.2 Interferences, with analysis by WDXRF, may result
2.1 ASTM Standards:
from mineralogical or other structural effects, line overlaps,
C242 Terminology of Ceramic Whitewares and Related
and matrix effects. The structure of the sample, mineralogical
Products
or otherwise, is eliminated through fusion with a suitable flux.
C322 Practice for Sampling Ceramic Whiteware Clays
Fusion of the sample diminishes matrix effects and produces a
C323 Test Methods for Chemical Analysis of Ceramic
stable, flat, homogeneous sample for presentation to the
Whiteware Clays
spectrometer. Selecting certain types of crystal monochroma-
tors eliminates many of the line overlaps and multiorder line
3. Apparatus
interferences.Amathematical correction procedure (2) is used
3.1 Simultaneous X-ray Spectrometer, for example, Philips
to correct for the absorption and enhancement matrix effects.
PW1606 or equivalent.
1.3 Concentrationsoftheelementsinclaysandmineralsare
3.2 Pt-Au Alloy Crucibles and Molds, (3).
determined independent of the oxidation state and are reported
in the oxidation state in which they most commonly occur in
3.3 Fluxer, ((4) or equivalent).
the earth’s crust.
3.4 Two Muffle Furnaces with Rocker Attachments—A
1.4 Concentration ranges:
muffle furnace is not required if the fluxer has automatic
Concentration range
operation with its own heat source.
Element
(percent)
SiO 0.10 99.0
2 3.5 Hot Plate and Muffle Furnace.
4. Reagents
These test methods are under the jurisdiction of ASTM Committee C21 on
Ceramic Whitewares and Related Productsand are the direct responsibility of
Subcommittee C21.03 on Methods for Whitewares and Environmental Concerns.
Current edition approved Oct. 1, 2009. Published February 2010. DOI: 10.1520/ For referenced ASTM standards, visit the ASTM website, www.astm.org, or
C1605-04R09. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
The boldface numbers in parentheses refer to the list of references at the end of Standards volume information, refer to the standard’s Document Summary page on
this standard. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C1605 − 04 (2009)
TABLE 1 Operating Conditions for Determination of Elements by
4.1 DigestthesamplesinJohnsonMattheySpectroflux100
WDXRF
or equivalent brand (lithium tetraborate). A blend of lithium
Element Line Crystal Detector Gas Window
tetraborate (Spectroflux 100 ) and lithium metaborate (Spec-
Na Kα PX-1 Flow, P-10 2 µm, polypropylene
troflux 100A ) can be used if a lower fusion point is desired.
Mg Kα TLAP Flow, P-10 2 µm, polypropylene
The flux is ordered in powdered form, lot size as appropriate,
Al Kα PET Sealed neon 25 µm, beryllium
and identified by number and date.
Si Kα InSb Sealed neon 25 µm, beryllium
PKα Ge Sealed neon 50 µm, beryllium
4.2 Dry the minus 60-mesh material for the lot 2 days at
KKα LiF 200 Sealed krypton 100 µm, beryllium
Ca Kα LiF 200 Sealed krypton 100 µm, beryllium
300°C and keep in sealed Mason jars.
Ti Kα LiF 200 Sealed krypton 100 µm, beryllium
4.3 After drying, perform a loss-on-fusion for each lot of
Mn Kα LiF 200 Sealed krypton 100 µm, beryllium
Fe Kα LiF 200 Sealed krypton 100 µm, beryllium
flux from the manufacturer so that an appropriate amount of
fluxcanbeweighedouttoyield8.0000goflithiumtetraborate
PX-1 = Tungsten carbide layered; TLAP = thallium hydrogen phthalate; PET =
after fusion.
pentaerythritol tetrakis (hydroxymethyl) methane; InSb = indium antimonide; GE =
Germanium 111; LiF 200 = lithium fluoride (200 lattice orientation); P-10 gas = 90
4.4 Weigh the charges of flux using a Zymark robot to
percent argon + 10 percent methane.
60.0035 g (60.04 % precision). If the Zymark robot is not
available the samples can be weighed by hand.
6.3 The combined weights of the sample and the flux will
4.5 Clean the platinum ware in 50 percent reagent grade
result in an “infinitely thick” sample disc to the instrument.
HCl, rinse in deionized water and dry at 140°C. Other acids
maybeusedinsteadofHCl,dependingonthepreferenceofthe 6.4 Adda0.250mLaliquotofthe1:1LiBrsolution,serving
laboratory. as a nonwetting agent, to the sample.
4.6 Prepare the LiBr used as a nonwetting agent by neutral- 6.5 Load whatever number of crucibles (with samples) and
izing reagent grade concentrated HBr (48 %) with LiCO . molds the fluxer is equipped to hold and the same number of
empty molds onto the fluxer.
4.7 Filter the LiBr solution and dilute 1:1 with deionized
water. 6.6 Following the instructions of the fluxer, allow it to reach
a temperature of 1120°C for ten minutes, and then rock for 5
minutes to stir and homogenize the samples. If sulfur is to be
5. Safety Precautions
determined, fusion temperature must be 1050°C or less and the
5.1 Fusions and ignitions of samples in a muffle furnace
blend of lithium tetraborate/lithium metaborate must be used.
must be performed under a high velocity canopy hood. Boiling
of the HCl cleaning solution is performed in a chemical fume 6.7 Remove the fluxer from the furnace, pour the molten
mixtures into their respective molds, and cool to near room
hood with a safety sash. Safety glasses and special nonflam-
mable, nonasbestos, heat resistant gloves must be worn when temperature. An essential feature of this mold is the mold
design (3).
removing the fluxer from the muffle furnace. Glass discs are
sharp on the rear edge and should be handled with care. Dust
6.8 Samples with high concentrations of Cu, Cr, Ni, Fe, Mn
from the flux must not be inhaled, so pouring of the powdered
and high organic content require various special sample prepa-
flux must be done in a chemical hood. Preparation of the LiBr
rationtechniques,and,insomecases,cannotbepreparedatall.
solution must be done by slowly adding LiCO to the HBr so
6.9 Samples with arsenic or lead with concentrations in
the generation of CO does not cause the acid to spill over the
excess of 2000 ppm, or with combinedAs/Pb concentration in
edge of the beaker.The specific Chemical Hygiene Plan (CHP)
excess of 3000 ppm cannot be prepared because of risk of
for the laboratory, or laboratories if the corporation has more
damage of the Pt/Au crucibles.
than one, gives the first-aid treatment and disposal procedures
for chemical products used in this method. 6.10 Using the wavelength dispersive X-ray spectrometer,
themajorelementconcentrationsaredeterminedbycomparing
6. Procedure the intensities obtained from standards with those obtained
fromthesample (5,6).Forexample,thefollowinginstrumental
6.1 Ignite a 0.8000 g portion of minus 80-mesh sample in a
conditions are for the Phillips PW1606 spectrometer. These
tared 95 percent Pt/5 percent Au crucible at 925°C for 40
conditions will be different for other models of x-ray spectro-
minutes. Report the weight loss as percent loss on ignition
photometers:
(LOI).
Tube Rhodium, end window
6.2 Add a charge of lithium tetraborate (or a blend of
Power 35 Kv and 60 ma
lithium tetraborate/lithium metaborate) that will contribute Time 100 s
Atmosphere Vacuum
8.0000 g after fusion to the sample and thoroughly mix the
powders.
7. Operating Conditions for Determination of Elements
by WDXRF
7.1 Recalibrate the spectrophotometer every two weeks or
Spectroflux is a registered trad
...
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