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Elemental Analysis Matrix CRMs

Elemental analysis matrix CRMs are most valuable in the validation of analytical methods. Here their primary role is to calibrate the mass-transfer process. However they are also important as:

  • quality control tools for assuring the ongoing performance of test methods and the validity of associated test results
  • a benchmark for comparing measurements made between different laboratories

Certified values are metrologically traceable to SI units. They have been determined with high accuracy measurement techniques (including isotope dilution and ICP-SF-MS) and formal assessment of method precision, method trueness, homogeneity and stability. Measurement uncertainty has been estimated in accordance with ISO-GUM and is reported with a 95% level of confidence.

Information values are derived from our interlaboratory proficiency tests. Using the results obtained, the best estimate of the reference values for the individual trace metal content of each material was assigned. Where possible, high resolution ICPMS was used to confirm reference values of trace metals prone to matrix interference in conventional quadrupole ICPMS. Measurement uncertainty is reported with a 95% level of confidence.

For further information contact chemref@measurement.gov.au, +61 2 9449 0191 or use our on-line form

MX014 Trace Elements in Sea Water — Certified Values for As, Cd, Co, Cr, Cu, Fe, Hg, Mn, Ni, Pb, Se, V

MX014 - an acidified coastal sea water CRM bottled in units of approximately 120 mLMX014 is an acidified coastal sea water CRM bottled in units of approximately 120 mL.

Cost

Australia $264 excl GST (rest of the world $370) plus delivery and handling.

Intended Use

To verify and/or validate analytical methods for elemental analysis in sea waters or similar sample matrices.

Certified Values

Element Mass fraction (μg/kg) Mass concentration (μg/L)
As 2.96 ± 0.26 3.06 ± 0.26
Cd 1.318 ± 0.034 1.363 ± 0.036
Co 2.864 ± 0.068 2.961 ± 0.070
Cr 2.613 ± 0.075 2.701 ± 0.077
Cu 2.90 ± 0.25 2.99 ± 0.27
Fe 21.70 ± 0.32 22.43 ± 0.34
Hg 0.433 ± 0.010 0.448 ± 0.010
Mn 1.48 ± 0.16 1.53 ± 0.16
Ni 3.66 ± 0.10 3.78 ± 0.12
Pb 2.467 ± 0.065 2.550 ± 0.067
Se 3.06 ± 0.26 3.17 ± 0.28
V 4.67 ± 0.12 4.93 ± 0.14

Details of Production

human hand scooping seawaterMX014 is a natural coastal sea water sample collected from the shore of Curl Curl beach in Sydney, Australia. The bulk sea water was filtered through 0.45 μm and 0.20 μm filters then acidified with high purity HNO3 to a final acid concentration of 0.3 M HNO3. All the analytes for which certified values are provided were fortified using Australian marine environment regulatory limits as a guide. The bulk sea water was mixed thoroughly by end-over-end tumbling for several hours. The CRM was then subsampled into 125 mL acid-cleaned LDPE bottles (360 units) in a trace metals clean laboratory using a pre-cleaned volumetric dispensing apparatus. Each bottle was labelled with a unique bottle number and sealed in an aluminised polyethylene terephthalate bag to prevent solvent transpiration from the CRM.

Analytical Methods

Certified values for:

  • Cd, Cr, Cu, Fe, Hg, Ni, Pb and Se were determined by isotope dilution ICP‑MS quantification
  • As, Co, Mn and V were determined by standard addition ICP‑MS quantification

Mass concentration reference values were calculated from the mass fraction and the density of MX014 (1.0339 ± 0.0016 kg/L applicable for 20 °C ± 5 °C).

Expiry of Certification

Valid until 30 October 2017 (may be reassessed prior to the certificate expiration date to investigate an extension of the certification period). After opening the original packaging has a shelf life of 12 month.

Case Study

Click here for a case study on improving the reliability of sea water testing.

MX009 Trace Elements in Prawn Tissue — Certified Values for Hg and Information Values for 15 other Elements

MX009 - a freeze-dried prawn tissue powder bottled in units of approximately 10 gMX009 is a freeze-dried prawn tissue powder bottled in units of approx 10 g.

Cost

Australia $231 excl GST (rest of the world $323) plus delivery and handling.

Intended Use

To verify and/or validate analytical methods for elemental analysis in prawn tissue, marine biota and similar sample types.

Certified Values

Element Mass fraction (dry mass basis) (μg/kg) Mass fraction (undried basis) (μg/kg)
Hg 148.3 ± 5.1 134.5 ± 9.0

Information Values

Element Mass fraction (dry mass basis) (mg/kg) Mass fraction (undried mass basis) (mg/kg) Number of results from which value is derived
As 4.2 ± 0.4 3.8 ± 0.4 22
Ba 1.40 ± 0.22 1.27 ± 0.21 15
Ca 5 800 ± 300 5 300 ± 400 23
Cd 0.143 ± 0.009 0.130 ± 0.010 35
Co 0.107 ± 0.016 0.097 ± 0.015 13
Cu 16.5 ± 0.7 15.0 ± 1.0 31
Fe 115 ± 10 104 ± 11 24
K 1 610 ± 60 1 460 ± 90 20
Mg 1 950 ± 90 1 770 ± 120 24
Mn 5.6 ± 0.3 5.1 ± 0.4 25
Na 14 200 ± 500 12 900 ± 800 23
P 7 100 ± 400 6 400 ± 500 22
Pb 0.39 ± 0.04 0.35 ± 0.04 36
Se 2.85 ± 0.19 2.59 ± 0.21 24
Zn 76 ± 3 69 ± 4 30

Details of Production

fresh prawnsMX009 was prepared from fresh prawns (approximately 300 kg) collected from the Central Coast, Queensland, Australia. The prawns were cooked and shelled then freeze-dried. The prawn tissue was then ground in an industrial blender fitted with stainless steel blades and passed through a 212 μm sieve. The sieved powder was thoroughly homogenised in a drum-hoop mixer and then bottled into 10 g portions using a rotary sample divider. The entire production batch was gamma irradiated to prevent microbial activity.

Analytical Methods

Certified mass fraction of Hg was measured by double isotope dilution ICP-MS using a sample size of 0.5 g. The sample was digested using nitric acid and hydrogen peroxide (1:1) with microwave heating in sealed high-pressure vessels.

Expiration of Certification

Valid until 31 December 2016 (may be reassessed prior to the expiration date to investigate extension of the certification period).

MX008 Trace Elements in Nutritional Supplement — Certified Values for Cr and Information Values for 14 other Elements

MX008 - a nutritional supplement powder bottled in units of approximately 25 gMX008 is a nutritional supplement powder bottled in units of approximately 25 g. The material consists of a typical pharmaceutical excipient containing dietary nutrients and essential elements.

Cost

Australia $462 excl GST (rest of the world $647) plus delivery and handling.

Intended Use

To verify and/or validate analytical methods for elemental analysis in nutritional supplements, pharmaceutical products or similar sample types.

Certified Values

Element Mass fraction
(dry mass basis) (mg/kg)
Mass fraction
(undried basis) (mg/kg)
Cr 14.3 ± 0.8 13.3 ± 1.0

Information Values

Element Mass fraction (dry mass basis) (mg/kg) Mass fraction (undried basis) (mg/kg)  Number of results from which value is derived
Al 36 ± 5 33 ± 5 19
B 85 ± 7 79 ± 8 21
Ba 4.5 ± 0.3 4.2 ± 0.4 20
Ca 42 000 ± 3 000 39 000 ± 3 000 21
Cu 94 ± 6 87 ± 7 22
Fe 1 040 ± 60 960 ± 70 21
K 8 200 ± 600 7 600 ± 600 13
Mg 13 000 ± 500 12 000 ± 700 20
Mn 556 ± 21 516 ± 31 21
Mo 6.2 ± 0.5 5.7 ± 0.5 21
Na 3 800 ± 400 3 600 ± 400 14
P 30 000 ± 120 0 27 800 ± 1 700 20
Sr 20.6 ± 0.8 19.2 ± 1.2 19
Zn 3 300 ± 120 3 060 ± 180 21

Details of Production

bottle and pillsMX008 is a composite of commercial dietary supplement products, pharmaceutical formulations and pharmaceutical placebo material. The major excipient component is calcium phosphate. The excipient contributes percent quantities of Ca, P, Mg, K and also contains silicates. Starting materials were crushed to a powder before combining. The bulk powder was blended thoroughly then passed through a coarse sieve (1000 μm) and a fine sieve (150 μm). The sieved powder was homogenised by tumbling in a drum-hoop mixer for several hours then bottled into 25 g units using a rotary sample divider. The entire production batch was gamma-irradiated to prevent microbial activity.

Analytical Methods

Certified mass fraction of Cr was measured by double isotope dilution ICP-MS using a sample size of 0.5 g. The sample was digested with nitric acid and microwave heating in sealed high-pressure vessels.

Expiration of Certification

Valid until 31 December 2016 (may be reassessed prior to the expiration date to investigate extension of the certification period).

Non-certified Reference Materials

We maintain a limited collection of non-certified reference materials from NMI’s interlaboratory proficiency tests.

NMI reference Unit of issue (mg) Cost Australia
($ excl GST)
Cost rest of the world ($)
River sediment X235 50 179 N/A
Biosoil (sewage sludge and soil) X285 50 179 N/A
Bovine liver X286 30 179 N/A
Cabbage leaves X287 25 179 N/A