| 2002 Analytical Chemistry Division Archive
News |
|
New
and Renewal SRMS Released
|
New
SRMs - SRMs 2721 and 2722 Crude Oil SRMs for Sulfur, Mercury, and
Water Analysis
W.Robert Kelly, Analytical
Chemistry Division
|
NIST
announces the release of two Standard Reference Materials (SRMs) -
2721 Crude Oil (Light-Sour) and 2722 Crude Oil (Heavy-Sweet) which
are certified for sulfur, mercury, and water. These two SRMs are commercial
crude oils from two different Texas fields. They will be useful for
evaluating current and new analytical techniques and calibrating instruments
for total sulfur, mercury, and water in crude oil and materials of
a similar matrix.
Each crude oil used was passed through a 10µm filter and blended
before being ampouled. A unit of each crude oil consists of five amber
ampoules, each containing approximately 10 mL of crude oil.
With recent increased global interest in sulfur and mercury contaminants
in fuels, these SRMs are expected to be valuable additions to petroleum
laboratories worldwide. |
|
|
New
SRMs - SRM 2241 Relative Intensity Correction Standard for Raman
Spectroscopy
Steven Choquette,
Analytical Chemistry Division
|
SRM
2241 Relative Intensity Correction Standard for Raman Spectroscopy
is a certified spectroscopic standard for the correction of the relative
intensity of Raman spectra obtained with instruments employing 785
nm laser excitation. SRM 2241 consists of an optical glass that emits
a broadband luminescence spectrum when excited with 785 nm laser radiation.
The relative spectral intensity of the glass luminescence has been
determined through the use of a white-light, uniform-source, integrating
sphere that has been calibrated for its irradiance at NIST.
The shape of the luminescence spectrum of this glass is described
by a polynomial expression that relates the relative spectral intensity
to the wavenumber (cm-1) expressed as the Raman shift from the excitation
wavelength of 785 nm. This polynomial, together with a measurement
of the luminescence spectrum of the standard, can be used to determine
the spectral intensity response corrction that is unique to each Raman
system. The resulting instrument-intensity response correction may
then be used to obtain Raman spectra that are instrument independent.
This SRM is intened for use in measurements over the range of 20 °C
to 25 °C and with Raman systems that employ laser excitation at
785 nm. It may also be used for Raman excitation with lasers that
range from 784nm to 786 nm in excitation wavelength. |
|
|
New
SRMs - SRM 2298 Sulfur in Gasoline (High Octance)
W.Robert Kelly, Analytical
Chemistry Division
|
Federal,
state, and foreign nations' guidelines and standards for the release
of sulfur from high-octane gasoline to the atmosphere are constantly
being tightened. Certain high-performance automobile engines, as well
as aircraft engines require high octane gasoline, but these engines
also must reduce their sulfur emissions to the atmosphere, to comply
with ever more stringent guidelines. To ensure that engine emissions
meet these guidelines, the manufacture of high octane gasoline with
sharply reduced sulfur content is required. Manufacturers must show
that the use of their products will ensure that engines meet emission
guidelines.
NIST announces the release of reference values for its SRM 2298 Sulfur
in Gasoline (High Octane), which will be applied to evaluating methods
and calibrating instruments used to determine total sulfur in gasoline
or materials of similar matrix. A unit of SRM 2298 consists of five
amber ampoules, each one of which contains about 20 mL of gasoline,
which was donated by ExxonMobil Company (Fairfax, VA).
The certified value is based on analyses by isotope dilution thermal
ionization mass spectrometry (ID-TIMS). Homogeneity testing was done
by X-ray fluorescence spectrometry. The uncertainty in the certified
value, expressed as an expanded uncertainty, is calculated according
to the method in the ISO Guide, and is based on a 95 % prediction
interval. The certification is valid until 31 December 2008 and is
considered to be stable during the period of certification, but it
is nullified if the SRM is damaged, contaminated, or otherwise modified.
Certified Value (mass fraction) Sulfur: 4.7 µg/g ± 1.3 µg/g. |
|
|
New
SRMs - SRM 2299 Sulfur in Gasoline (Reformulated)
W.Robert Kelly, Analytical
Chemistry Division
|
Federal,
state, and foreign nations' guidelines and standards for the release
of sulfur from reformulated gasoline to the atmosphere are constantly
being tightened. Gasoline had to be reformulated with certain oxygen-containing
compounds because of the ban on tetraethyl lead as an anti-knock compound
and also because of requirements for reformulation that would reduce
automotive emissions of ozone/smog precursors. In addition, automotive
emissions of sulfur to the atmosphere must be curtailed, to comply
with ever more stringent guidelines. To ensure that engine emissions
meet these guidelines, the manufacture of reformulated gasoline with
sharply reduced sulfur content is required. Manufacturers must show
that the use of their products will ensure that engines meet emission
guidelines.
NIST announces the release of reference values for its SRM 2299 Sulfur
in Gasoline (Reformulated), which will be applied to evaluating methods
and calibrating instruments used to determine total sulfur in gasoline
or materials of similar matrix. A unit of SRM 2299 consists of five
amber ampoules, each one of which contains about 20 mL of gasoline,
which was donated by ExxonMobil Company (Fairfax, VA).
The certified value is based on analyses by isotope dilution thermal
ionization mass spectrometry (ID-TIMS). Homogeneity testing was done
by X-ray fluorescence spectrometry. The uncertainty in the certified
value, expressed as an expanded uncertainty, is calculated according
to the method in the ISO Guide, and is based on a 95 % prediction
interval. The certification is valid until 31 December 2008 and is
considered to be stable during the period of certification, but it
is nullified if the SRM is damaged, contaminated, or otherwise modified.
Certified Value (mass fraction) Sulfur: 13.6 µg/g ± 1.3 µg/g |
|
|
New
SRMs - SRMs 3143 Rhenium. and 3144 Rhodium
Gregory Turk, Analytical
Chemistry Division
|
NIST
announces the availability of SRM 3143 Rhenium, and SRM 3144 Rhodium
Standard Solutions. These standards are much anticipated renewals
and part of the 3100 series of high purity, single element in solution
standards. The rhenium and rhodium standards have been a particular
challenge to produce. Because of newly developed certification measurement
methods at NIST, the standards should be in good supply for some time.
The method of certification is based on high performance inductively
coupled plasma optical emission spectrometry. (HP-ICP-OES). Rhodium
metal is very difficult to dissolve and NIST had to prepare a set
of primary standards from rhodium metal using a Carius tube digestion
in order to certify the SRM. Commercial standards laboratories also
experience the same problems in preparing rhodium standards from the
metal. With the release of the SRM 3144, these labs can use more soluble
rhodium salts and rely on the SRM 3144 to assure the accuracy of their
standards.
Rhenium and rhodium are both very expensive metals. Rhodium is most
often associated with use as an industrial catalyst and in automobile
catalytic converters.It can sell for over $500 per gram, and imprecise
measurements can cost commercial users tens of millions of dollars
annually. Rhenium is used for filaments for mass spectrographs and
ion gauges and as a catalyst in chemical manufacturing and refining.
Both SRMs have a five-year shelf life.
Each unit of SRM 3143 and SRM 3144 is packaged as a set of five, 10
mL sealed borosilicate ampoules of an acidified aqueous solution.
|
|
|
Renewal
SRMS - SRM 956a Electrolytes in Frozen Human Serum
Michael Welch, Analytical
Chemistry Division
|
|
Standards are
essential for promoting accuracy in measurements pertaining to human
health and nutrition.Electrolyte concentrations in the body affect
most intra- and inter-cellular processes. Abnormal levels of electrolytes
may cause or result from a variety of conditions. Thus, measurement
of serum levels of electrolytes is a vital part of health status
assessment
NIST announces the addition of reference values for ionized calcium
and chloride in its SRM 956a Electrolytes in Human Serum with the
revision of its certification of 13 November 1996.The values for
these new analytes complement the previously certified values for
total calcium, lithium, magnesium, potassium, and sodium in the
material, all of which were determined by primary clinical methods.
The new chloride values were determined by microcoulometry. The
new, ionized calcium values were determined by ion selective electrode
potentiometry, the candidate designated comparison method of the
NCCLS. The usefulness of SRM 956a as an ionized calcium reference
material was established by an interlaboratory study involving 19
industrial and clinical laboratories using various types of commercial
instrumentation.
This SRM can be used for standardizing direct-reading ion-selective
electrode analyzers and for validating working or secondary reference
materials for electrolytes in either diluted or undiluted human
serum or plasma.
A unit of SRM 956a consists of six flame-sealed ampoules of frozen
human serum: two ampoules each of three different concentration
levels. Each ampoule contains approximately 2.00 mL of human serum.
The development of this SRM is the result of a cooperative effort
between NIST and the NCCLS Subcommittee on Electrolytes.
|
|
|
|
|
| NIST
announces a new release of SRM 1575a Pine Needles, which is intended
primarily for use in the evaluation of inorganic analytical techniques
used to determine element content of botantical and agricultural materials.
The needles were collected in North Carolina from freshly felled loblolly
pine (Pinus taeda) trees of about the same age and origin.
One unit of SRM 1575a consists of approximately 50 g of dried, jet-milled,
and sterilized pine needles. Certified and reference concentrations
are provided for 23 elements. This material replaces the original
SRM 1575 Pine Needles. |
|
|
Renewal
SRMs - SRM 1941b Organics in Marine Sediment
Stephen Wise,
Analytical Chemistry Division
|
This
SRM is widely used by marine pollution monitoring programs for assessing
the condition of the marine environment. Most contaminants in aquatic
systems, including polycyclic aromatic hydrocarbons (PAHs), polychlorinated
biphenyls (PCBs), pesticides, and organo-tin compounds, are associated
with particulate matter and tend to accumulate in sediments. Resuspension
of sediment by dredging, storms, and currents often result in desorption
of the contaminants into the water column.
This is the third issue of SRM 1941b since 1989. The sediment used
for SRM 1941b was collected from the Chesapeake Bay at the mouth of
the Baltimore, MD harbor, very near the sites where SRM 1941 and SRM
1941a were collected. The sediment contains natural levels of contaminants
in this area (not spiked). SRM 1941b is intended for use in evaluating
analytical methods for the determination of PAHs, PCB congeners, and
chlorinated pesticides in sediment. The material is certified for
the concentrations of 24 PAHs, 29 PCB congeners, and 7 chlorinated
pesticides. There are also reference values for 43 additional PAHs;
13 additional PCB congeners; 2 additional pesticides; mono-, di-,
and tributyltin; total tin; and total organic carbon. SRM 1941b has
certified and reference values for approximately 50 more organic constituents
than in the previous issue for SRM 1941 and is the first SRM with
values assigned for the organotins. In addition, there are information
values for carbon, hydrogen, and nitrogen contents. SRM 1941b complements
SRM 1944 (New York/New Jersey Waterway Sediment) with concentrations
of the PAHs and PCB congeners approximately an order of magnitude
lower in SRM 1941b as compared to SRM 1944. The concentrations in
these two materials span the range found in most urban waterways around
the world. |
|
|
Renewal
SRMS - SRM 3190, 3198, & 3199 Aqueous Electrolytic Conductivity
Standard
Franklin Guenther,
Analytical Chemistry Division
Date:
September 2002
|
|
Specimens
Collected from Pilot Whale Stranding for NIST Specimen Bank
Rebecca
Pugh, Analytical Chemistry Division,
Hollings Marine Laboratory, Charleston, SC
Barbara
J. Porter, Analytical
Chemistry Division, Gaithersburg, MD
|
|
On
Monday, July 29, 2002 a mass stranding of 57 long-finned pilot whales
(Globicephala melas) occurred in Dennis, MA on Cape Cod. Strandings
of marine mammals occur regularly at Cape Cod; however, a stranding
of this magnitude creates considerable activity among the scientific
and volunteer personnel of the local stranding networks and aquariums,
as well as tourists and the press. Barbara Porter and Rebecca Pugh
of the Analytical Chemistry Division of CSTL participated at the
stranding site in the collection of tissue specimens from the whales
for archival in the NIST National Biomonitoring Specimen Bank (NBSB).
Since 1987, the NIST NBSB has participated in collecting and banking
of tissues from marine mammals from U.S. waters of the Atlantic,
Gulf of Mexico, and Pacific, including Alaska. The NBSB is designed
to cryogenically preserve environmental and biological specimens
over long periods of time (decades) for future retrospective analyses.
A major activity of the NBSB is the National Marine Mammal Tissue
Bank (NMMTB), established by Federal Legislation in 1992, and maintained
at the NBSB through partial support from the National Oceanic and
Atmospheric Administration (NOAA), National Marine Fisheries Service
(NMFS) and the U.S. Geological Survey, Biological Resources Division.
The CSTL scientists
worked with scientists and volunteers from the New England Aquarium,
the Northeast Stranding Network, the NMFS, and the Woods Hole Oceanographic
Institute to obtain samples for inclusion in the NMMTB. Tissue specimens
were collected from 11 animals that died on the first day of the
stranding. Three late stage pregnancies were found among the 11
whales, and tissue specimens were also removed from the 3 fetuses
for a total of 14 animals sampled. Tissue specimens for the NMMTB
are collected and processed following rigid standard operating procedures
designed to reduce any contamination to the tissue. After processing,
the tissue samples were immediately frozen and eventually stored
in liquid nitrogen vapor freezers at the NIST NBSB satellite facility
located at the Hollings Marine Laboratory in Charleston, SC. These
specimens, along with over 2,000 tissue specimens from over 715
other marine mammals already archived in the NBSB, will be used
to determine the levels of contaminants not only in marine mammals,
but the health of the marine environment as well, and they will
be available to scientists for evaluation for many years to come.
|
|
|
|
|
|
| Figure1.
Volunteers use buckets to keep the skin of the dying whales moist. |
Figure
2. Whales stranded on the beach with onlookers watching. |
Figure
3. Map of Cape Cod Bay; location of this stranding. |
Figure
4. Whale being helped off shore. |
Photos
courtesy of the Cape Cod Times.
Date: July 2002 |
|
NIST
Reaffirms Commitment to Cement Industry with Updated SRMs
John
R. Sieber, Analytical Chemistry Division, CSTL
|
|
The
entire suite of NIST cement and clinker Standard Reference Materials
(SRMs) have been updated. These SRMs have been essential to laboratories
which certify concrete products for performance and evaluate mechanisms
for concrete corrosion and failure.
For more information
on Cement SRMs, see the Standard Reference Material website: http://ts.nist.gov/ts/htdocs/230/232/232.htm
Date: September
2002
|
|
|
Photo
is Courtesy of Ash Grove Cement Company.
|
|
|
NIST
Chemists Define and Refine Properties of Plastic Microsystems
Laurie
Locascio, Analytical Chemistry Division, CSTL
David
Ross, Process Measurements Division, CSTL
Tim Johnson
There
may well be a plastic biochip in your future, thanks in part to
the National Institute of Standards and Technology (NIST).
Microfluidics
devices, also known as lab-on-a-chip systems, are miniaturized
chemical and biochemical analyzers that one day may be used for
quick, inexpensive tests in physicians offices. Most microfluidics
devices today are made of glass materials. Cheaper, disposable devices
could be made of plastics, but their properties are not yet well
understood.
NIST is contributing
to the development of these plastic microfluidics. One study looked
at how fluids flowed in plastic microchannels by tracking fluorescent
dye in the fluids. NIST researchers also developed an easy technique
for accurately
measuring fluid temperaturesan important parameter for chemical
reactions. A
third project spawned a method for concentrating and separating
an ionic (charged) substance in solution within microchannels. The
technique concentrates the substance as much as 10,000-fold or more,
making it easier to detect in ultrasmall quantities (nanolitersa
billionth of a literor less).
Finally, NIST
staff designed a novel system to overcome the difficult problem
of slow mixing in microfluidics devices. The mixer consists of a
T-shaped microchannel imprinted in plastic that is modified with
a laser to create a series of slanted wells.
The wells speed the mixing of two streams entering the passage.
Date:
August 2002
|
 |
 |
| 1.
Temperature Gradient Focusing.
Concentration and separation of a wide variety of analytes using temperature
gradient focusing in a microfluidic channel. |
2.
Microfluidic Mixers.
White-light and fluorescence microscopy images of passive mixing for
various ablated patterns under low and high EO flowrates. Note that
mixing is only achieved at low flowrates for the middle column, but
is achieved at high flowrates for the pattern shown in the right column.
At high flowrates (middle column) stream splitting is seen. |
|
|
NIST
Chocolate Standard Raises the 'Bar' on Accuracy
Katherine
S. Sharpless, Analytical Chemistry Division, CSTL
Chocoholics,
rejoice. Now theres a way to know more precisely than ever
how much fat (and other constituents) are in chocolate and similar
foods. The National Institute of Standards and Technology (NIST)
has issued Standard Reference Material (SRM) 2384, Baking Chocolate,
which has been characterized with state-of-the-art measurement methods
to show how much fat, protein, carbohydrates, individual fatty acids,
elements, vitamins and other components it contains. It is part
of a series of food-matrix SRMs that can be used by food processors
to validate analytical methods and for quality assurance when assigning
values to products with similar compositions. The baking chocolate
SRM is the first standard to contain a high proportion of fatmore
than 50 percent. A high-fat food standard has been identified as
a priority by manufacturers. Because of this high fat content, the
new SRM can be analyzed by manufacturers of chocolate and by quality
assurance labs of companies that produce other types of fatty products,
such as black olives and potato chips. This SRM also is the first
to have values assigned for catechins (which, as antioxidants, may
help protect the body against damage associated with age-related
diseases) and caffeine. NISTs food-matrix SRMs will help manufacturers
comply with the Food and Drug Administration labeling requirements.
Date: August
2002
|
|
|
Temperature
Gradient Focusing in Microfluidic Channels
David
Ross, Process Measurements Division, CSTL
Laurie Locascio, Analytical
Chemistry Division, CSTL
Scientists in
the Process Measurements and Analytical Chemistry Divisions of CSTL
have developed a new method to concentrate and separate chemical
species in microfluidic channels. Microfluidic, or "lab-on-a-chip,"
devices are miniaturized chemical and biochemical analysis systems
that one day may replace conventional bench top instruments.
The new technique, temperature gradient focusing, balances the electrophoretic
motion of analytes in a microchannel against the bulk flow of buffer
solution through the microchannel while applying both an electric
field and a temperature gradient along the length of the channel.
For buffer solutions having temperature-dependent ionic strength,
the applied temperature gradient results in a corresponding gradient
in the electrophoretic velocity of a charged analytes in the channel.
The bulk flow velocity can then be adjusted so that the total analyte
velocity (the sum of the bulk and electrophoretic velocities) is
zero at some point along the channel length, and all of the analyte
in the channel will be focused, or concentrated, at that point.
The technique gives simultaneous focusing and separation of differently
charged analytes in a manner analogous to isoelectric focusing of
proteins, but is much simpler to implement than isoelectric focusing
and has the additional advantage of working with any charged analyte,
rather than just proteins. Temperature gradient focusing has been
demonstrated for a variety of different analytes including fluorescent
dyes, amino acids, proteins, DNA, and colloidal particles. In addition,
it has been shown to be capable of greater than 10,000-fold concentration
of a dilute analyte. A description of the technique has been submitted
for publication in the journal Analytical Chemistry.
Date: May
2002
|
|
High
Accuracy Technique Revolutionizes Platinum Group Metals Assay
Marc
Salit, Analytical Chemistry Division, CSTL
CSTL
researchers Marc Salit and Greg Turk have developed a high performance
approach to the measurement of elemental composition using inductively
coupled plasma optical emission spectroscopy. This technique uses
an innovative experiment design coupled with a novel drift correction
approach to minimize and quantify the major sources of uncertainty
in this chemical analysis. A recent publication documents the
performance of the method, high performance inductively coupled
plasma optical emission spectrometry, for 64 elements where the
typical relative expanded uncertainty observed is 0.1 percent
(Analytical Chemistry 2001, 73, 4821-4829). This technique
utilizes unmodified, commercially available equipment, is well
suited to automation, and yields results comparable to the best
attainable by classical methods.
After we presented this technique and our results at an ASTM E01
committee meeting in May 2001, we established a collaboration to
implement it with Metalor Technologies USA, North Attleboro, Mass.,
a precious metals and advanced materials supplier. Together, we
developed methods for the determination of palladium and platinum
in metallic samples. NIST provided software tools to perform the
calculations. Less than one year later, this technique was in routine
use at Metalor, complementing the gravimetric wet chemical technique
used in their labs. According to Arnold Savolainen of Metalor, This
technique has revolutionized our Platinum Group Metals assay lab.
Assay completion times which ran 20 to 30 days, now average four
to six days. Assay precisions have improved by more than an order
of magnitude. Accuracy, as measured by the number of assays sent
for umpire laboratory analysis, has improved to the point that we
have not had to go to umpire in over three months. I am now setting
up the procedure for the determination of gold at major levels.
Date:
May 2002
|
|
Return to ACD Home
Return to Top of Document
Date
created: May 13, 2002
Last updated:
January 15, 2003
Contact: acd_webmaster@nist.gov
|
|