STSD-5 Certificate of Analysis

Certified Reference Material for a Stream Sediment

Printable version of the certificate (PDF, 414 kb)

First issued: February 2026
Version: February 2026

Note:

The certified, provisional and indicative values herein pertain to the material on an as-received basis. Values for the elements were generally derived from a variety of digestions with mixtures of acids and/or fusions, followed by instrumental analysis. The footnotes indicate the details of the analytical methods used to determine the values. For more detailed information, please refer to the certification report.

Table 1 – STSD-5 Certified Values
Analyte (see footnotes) Units Mean Within-laboratory Standard Deviation Between-laboratories Standard Deviation 95% Confidence Interval of Mean
Aga AD2 + ICP µg/g 0.241 0.010 0.010 0.006
Agb AD4 + ICP µg/g 0.270 0.019 0.019 0.010
Ala AD2 + ICP % 1.253 0.030 0.030 0.021
Al2O3c AD4 / FUS + ICP % 11.83 0.16 0.31 0.13
Al2O3d FUS + XRF % 12.05 0.07 0.20 0.13
Ase AD2 / AD4 + ICP µg/g 11.9 0.6 1.4 0.5
Baa AD2 + ICP µg/g 311 11 21 13
Baf AD4 / FUS + ICP / XRF µg/g 1030 25 40 14
Beb AD4 + ICP µg/g 1.407 0.043 0.093 0.050
Bie AD2 / AD4 + ICP µg/g 0.252 0.030 0.030 0.012
Cg COMB + IR % 3.71 0.05 0.19 0.10
Caa AD2 + ICP % 2.21 0.04 0.18 0.11
CaOc AD4 / FUS + ICP % 5.10 0.07 0.12 0.05
CaOd FUS + XRF % 5.153 0.016 0.047 0.034
Cde AD2 / AD4 + ICP µg/g 0.829 0.036 0.036 0.015
Cec AD4 / FUS + ICP µg/g 60.3 2.4 3.7 1.6
Coa AD2 + ICP µg/g 11.12 0.26 0.29 0.19
Coc AD4 / FUS + ICP µg/g 14.30 0.41 0.52 0.23
Cra AD2 + ICP µg/g 40.0 0.9 2.7 1.6
Crb AD4 + ICP µg/g 95.3 2.5 7.3 4.4
Crh FUS + ICP µg/g 114.0 5.4 5.4 2.8
Csc AD4 / FUS + ICP µg/g 3.14 0.10 0.12 0.06
Cui AD2 / AD4 / FUS + ICP µg/g 41.8 1.6 2.6 0.9
Dyh FUS + ICP µg/g 4.54 0.16 0.16 0.10
Erh FUS + ICP µg/g 2.67 0.16 0.16 0.08
Euc AD4 / FUS + ICP µg/g 1.220 0.055 0.055 0.023
Fea AD2 + ICP % 2.63 0.05 0.11 0.07
Fe2O3c AD4 / FUS + ICP % 5.22 0.07 0.16 0.07
Fe2O3d FUS + XRF % 5.374 0.028 0.053 0.039
Gaa AD2 + ICP µg/g 4.05 0.16 0.49 0.35
Gac AD4 / FUS + ICP µg/g 14.22 0.36 0.52 0.25
Gdc AD4 / FUS + ICP µg/g 4.91 0.21 0.21 0.06
Hfb AD4 + ICP µg/g 1.92 0.12 0.15 0.11
Hfh FUS + ICP µg/g 6.81 0.48 0.48 0.21
Hoh FUS + ICP µg/g 0.891 0.053 0.053 0.022
Inb AD4 + ICP µg/g 0.0817 0.0044 0.0044 0.0027
Ka AD2 + ICP % 0.108 0.005 0.010 0.007
K2Oc AD4 / FUS + ICP % 1.657 0.029 0.057 0.025
K2Od FUS + XRF % 1.680 0.016 0.025 0.018
Laa AD2 + ICP µg/g 14.17 0.53 0.53 0.41
Lac AD4 / FUS + ICP µg/g 31.2 1.2 1.7 0.7
Lic AD4 / FUS + ICP µg/g 24.3 0.7 1.6 0.9
Mga AD2 + ICP % 1.205 0.020 0.044 0.030
MgOc AD4 / FUS + ICP % 3.000 0.039 0.096 0.039
MgOd FUS + XRF % 3.080 0.013 0.052 0.037
Mna AD2 + ICP µg/g 591 9 13 9
MnOf AD4 / FUS + ICP / XRF % 0.1087 0.0018 0.0028 0.0011
Moa AD2 + ICP µg/g 3.33 0.10 0.17 0.11
Moc AD4 / FUS + ICP µg/g 3.80 0.11 0.19 0.11
Na2Oc AD4 / FUS + ICP % 2.055 0.039 0.046 0.022
Nbb AD4 + ICP µg/g 10.40 0.39 0.39 0.31
Nbh FUS + ICP µg/g 12.09 0.42 0.57 0.40
Ndc AD4 / FUS + ICP µg/g 28.4 1.0 1.1 0.6
Nia AD2 + ICP µg/g 29.83 0.81 0.88 0.55
Nic AD4 / FUS + ICP µg/g 37.9 1.0 1.7 0.7
Pa AD2 + ICP µg/g 890 23 30 20
P2O5f AD4 / FUS + ICP / XRF % 0.2256 0.0049 0.0056 0.0021
Pba AD2 + ICP µg/g 16.4 0.9 1.0 0.6
Pbc AD4 / FUS + ICP µg/g 20.2 0.9 1.7 0.8
Prc AD4 / FUS + ICP µg/g 7.44 0.29 0.29 0.15
Rbc AD4 / FUS + ICP µg/g 59.5 1.4 1.9 0.9
Sba AD2 + ICP µg/g 0.80 0.05 0.11 0.07
Sbc AD4 / FUS + ICP µg/g 1.356 0.097 0.097 0.036
Sca AD2 + ICP µg/g 4.38 0.14 0.40 0.27
Scc AD4 / FUS + ICP µg/g 13.8 0.5 1.2 0.5
SiO2h FUS + ICP % 57.53 0.56 0.56 0.34
SiO2d FUS + XRF % 57.71 0.18 0.59 0.43
Smc AD4 / FUS + ICP µg/g 5.52 0.23 0.23 0.09
Sra AD2 + ICP µg/g 61.5 1.4 3.1 1.9
Src AD4 / FUS + ICP µg/g 288 6 13 5
Tac AD4 / FUS + ICP µg/g 0.81 0.07 0.11 0.05
Tbc AD4 / FUS + ICP µg/g 0.714 0.032 0.044 0.024
Tha AD2 + ICP µg/g 3.41 0.30 0.30 0.23
Thc AD4 / FUS + ICP µg/g 8.28 0.47 0.47 0.17
Tia AD2 + ICP % 0.072 0.003 0.012 0.007
TiO2b AD4 + ICP % 0.707 0.015 0.060 0.038
TiO2h FUS + ICP % 0.793 0.015 0.044 0.023
TiO2d FUS + XRF % 0.8017 0.0059 0.0065 0.0050
Tlb AD4 + ICP µg/g 0.471 0.017 0.020 0.014
Ua AD2 + ICP µg/g 2.35 0.12 0.12 0.07
Ub AD4 + ICP µg/g 3.80 0.16 0.18 0.12
Uh FUS + ICP µg/g 4.19 0.15 0.20 0.14
Va AD2 + ICP µg/g 53.6 1.5 4.7 2.7
Vb AD4 + ICP µg/g 128.8 3.3 7.5 4.3
Vh FUS + ICP µg/g 141.8 2.9 7.4 4.2
Yb AD4 + ICP µg/g 21.3 0.7 2.3 1.4
Yh FUS + ICP µg/g 24.9 0.8 1.3 0.8
Ybh FUS + ICP µg/g 2.51 0.14 0.14 0.06
Zna AD2 + ICP µg/g 193.1 4.5 8.7 5.1
Znc AD4 / FUS + ICP µg/g 213 6 12 5
Zrb AD4 + ICP µg/g 67 3 10 6
Zrh FUS + ICP µg/g 262 11 15 10

a. AD2 + ICP: Mean based exclusively on results obtained from two-acid digestion (hydrochloric and nitric), followed by inductively coupled plasma – optical emission or mass spectrometry.

b. AD4 + ICP: Mean based predominantly on results obtained from four-acid digestion, followed by inductively coupled plasma – optical emission or mass spectrometry.

c. AD4 / FUS + ICP: Mean based on results obtained from four-acid digestions or fusions using various fluxes, followed by inductively coupled plasma – optical emission or mass spectrometry.

d. FUS + XRF: Mean based predominantly on results obtained from fusions using various fluxes, followed by X-ray fluorescence spectrometry.

e. AD2 / AD4 + ICP: Mean based predominantly on results obtained from two-acid or four-acid digestion, followed by inductively coupled plasma – optical emission or mass spectrometry.

f. AD4 / FUS + ICP / XRF: Mean based predominantly on results obtained from four-acid digestion or fusions using various fluxes, followed by X-ray fluorescence spectrometry or inductively coupled plasma – optical emission or mass spectrometry.

g. COMB + IR: Mean based exclusively on results obtained from combustion, followed by infrared spectrometry.

h. FUS + ICP: Mean based predominantly on results obtained from fusions using various fluxes, followed by inductively coupled plasma – optical emission or mass spectrometry.

i. AD2 / AD4 / FUS + ICP: Mean based predominantly on results obtained from two-acid or four-acid digestions, or fusions, followed by inductively coupled plasma – optical emission or mass spectrometry.

Table 2 – STSD-5 Provisional Values
Analyte (see footnotes) Units Mean Within-laboratory Standard Deviation Between-laboratories Standard Deviation 95% Confidence Interval of Mean
Bea AD2 + ICP µg/g 0.458 0.008 0.024 0.022
Cea AD2 + ICP µg/g 28.7 0.9 2.1 1.8
Csa AD2 + ICP µg/g 1.18 0.05 0.12 0.12
Ina AD2 + ICP µg/g 0.0571 0.0035 0.0046 0.0044
Lia AD2 + ICP µg/g 13.65 0.27 0.71 0.67
Lub AD4 / FUS + ICP µg/g 0.385 0.021 0.021 0.012
Na2Oc FUS + XRF % 2.076 0.014 0.066 0.048
Nba AD2 + ICP µg/g 1.19 0.05 0.18 0.16
Rba AD2 + ICP µg/g 10.54 0.32 0.88 0.74
Sd AD2 / AD4 + ICP, COMB + IR % 0.0861 0.0049 0.0049 0.0019
See AD2 / AD4 + ICP µg/g 0.91 0.11 0.11 0.07
Snf AD4 + ICP µg/g 1.79 0.11 0.18 0.14
Sng FUS + ICP µg/g 2.40 0.49 0.49 0.46
Tee AD2 / AD4 + ICP µg/g 0.072 0.014 0.014 0.006
Tla AD2 + ICP µg/g 0.140 0.009 0.011 0.009
Tmb AD4 / FUS + ICP µg/g 0.380 0.024 0.024 0.014
Wa AD2 + ICP µg/g 0.61 0.18 0.18 0.14
Wf AD4 + ICP µg/g 1.39 0.20 0.20 0.14
Ya AD2 + ICP µg/g 10.20 0.20 0.27 0.22
Ybf AD4 + ICP µg/g 1.97 0.08 0.22 0.21
Zra AD2 + ICP µg/g 1.95 0.15 0.35 0.30

a. AD2 + ICP: Mean based exclusively on results obtained from two-acid digestion (hydrochloric and nitric), followed by inductively coupled plasma – optical emission or mass spectrometry.

b. AD4 / FUS + ICP: Mean based on results obtained from four-acid digestions or fusions using various fluxes, followed by inductively coupled plasma – optical emission or mass spectrometry.

c. FUS + XRF: Mean based predominantly on results obtained from fusions using various fluxes, followed by X-ray fluorescence spectrometry.

d. AD2 / AD4 + ICP, COMB + IR: Mean based predominantly on results obtained from two-acid digestion or four-acid digestion, followed by inductively coupled plasma – optical emission or mass spectrometry, or combustion followed by infrared spectrometry.

e. AD2 / AD4 + ICP: Mean based predominantly on results obtained from two-acid or four-acid digestion, followed by inductively coupled plasma – optical emission or mass spectrometry.

f. AD4 + ICP: Mean based predominantly on results obtained from four-acid digestion, followed by inductively coupled plasma – optical emission or mass spectrometry.

g. FUS + ICP: Mean based predominantly on results obtained from fusions using various fluxes, followed by inductively coupled plasma – optical emission or mass spectrometry.

Table 3 – STSD-5 Indicative Values (semi-quantitative only)
Analyte (see footnotes) Units Mean Number of Accepted Laboratories / Values
Aua AD2 / FUS + ICP µg/g 0.005 5 / 25
Dyb AD2 + ICP µg/g 2 3 / 15
Dyc AD4 + ICP µg/g 4 5 / 25
Erb AD2 + ICP µg/g 1 3 / 15
Erc AD4 + ICP µg/g 2 5 / 25
Eub AD2 + ICP µg/g 0.6 3 / 15
Fd AD4 / FUS + ISE % 0.05 3 / 15
Gdb AD2 + ICP µg/g 3 3 / 15
Gec AD4 + ICP µg/g 0.1 4 / 20
Hfb AD2 + ICP µg/g 0.05 6 / 30
Hgb AD2 + ICP µg/g 0.1 7 / 35
Hoc AD4 + ICP µg/g 0.7 4 / 20
LOIe % 12 18 / 88
Lub AD2 + ICP µg/g 0.1 3 / 15
Luc AD4 + ICP µg/g 0.3 4 / 20
moisturef % 2 11 / 53
Nab AD2 + ICP µg/g 300 7 / 35
Ndb AD2 + ICP µg/g 15 3 / 15
Prb AD2 + ICP µg/g 4 3 / 15
Reg AD2 / AD4 + ICP µg/g 0.002 5 / 25
Smb AD2 + ICP µg/g 3 3 / 15
Snb AD2 + ICP µg/g 0.6 8 / 40
Tbb AD2 + ICP µg/g 0.4 4 / 20
Tmb AD2 + ICP µg/g 0.2 3 / 15
Wh FUS + ICP µg/g 2 5 / 25
Ybb AD2 + ICP µg/g 0.9 4 / 20

a. AD2 / FUS + ICP: Mean based on results obtained from two-acid digestion (hydrochloric and nitric) or fire assay, followed by inductively coupled plasma – optical emission or mass spectrometry, using sample weights of 0.5–1 g.

b. AD2 + ICP: Mean based exclusively on results obtained from two-acid digestion (hydrochloric and nitric), followed by inductively coupled plasma – optical emission or mass spectrometry.

c. AD4 + ICP: Mean based predominantly on results obtained from four-acid digestion, followed by inductively coupled plasma – optical emission or mass spectrometry.

d. AD4 / FUS + ISE: Mean based on results obtained from four-acid digestion or fusion, followed by ion-selective electrode.

e. Loss on ignition: Mean based on results obtained from as-received samples (1–3 g), ignited at 950–1,000 °C for varying durations; most samples dried to constant weight.

f. Moisture: Mean based on results obtained from as-received samples (1–3 g), dried at 100–110 °C for varying durations to constant weight.

g. AD2 / AD4 + ICP: Mean based predominantly on results obtained from two-acid or four-acid digestion, followed by inductively coupled plasma – optical emission or mass spectrometry.

h. FUS + ICP: Mean based predominantly on results obtained from fusions using various fluxes, followed by inductively coupled plasma – optical emission or mass spectrometry.

SOURCE

STSD-5 was prepared from a mixture of sediments obtained from various sites in Canada.

DESCRIPTION

The mineral species include: plagioclase (30.0%), quartz (8.1%), orthoclase/microcline (8.1%), clinochlore (5.3%), biotite (5.0%), dolomite (4.2%), amphibole/actinolite (2.0%),

epidote (1.4%), hematite/magnetite (1.2%), calcite (1.1%), amphibole (hornblende) (0.8%), cordierite (0.7%), enstatite (0.5%), kaolinite (0.4%), titanite (0.3%), olivine (0.3%), muscovite (0.2%), apatite (0.2%), ankerite (0.2%), ilmenite (0.1%), rutile (0.1%), and unclassified (9.3%).

INTENDED USE

STSD-5 is suitable for the analysis of elements in rocks at major, minor and trace levels of concentration. Examples of intended use include quality control and method development.

INSTRUCTIONS FOR USE

STSD-5 should be used “as is”, without drying. The contents of the bottle should be thoroughly mixed before taking samples. The values herein pertain to the material when produced. CanmetMINING is not responsible for changes occurring after shipment.

HANDLING INSTRUCTIONS

Normal safety precautions for handling fine particulate matter are suggested, such as the use of safety glasses, breathing protection, gloves and a laboratory coat.

METHOD OF PREPARATION

The raw material was crushed, milled and sieved. The recovery of the fraction less than 75 µm (minus 200 mesh) was 81%. The product was blended and bottled in 100-gram units. This is the only size that is available.

HOMOGENEITY

The homogeneity of the stock was investigated using fifteen bottles chosen according to a stratified random sampling scheme. Three subsamples were analyzed from each bottle. Subsamples of 0.05 grams were digested with a mixture of hydrochloric, nitric and perchloric acids using a microwave oven for the determination of cerium, strontium and vanadium. Concentrations were determined using inductively coupled plasma – mass spectrometry. Carbon was determined in samples of 0.1 grams using a combustion apparatus with infrared detection.

A one-way analysis of variance technique (ANOVA)Footnote 1 and statistical analyses were used to assess the homogeneity of these elements. No significant between-bottles variation was observed for all elements.

Use of a smaller subsample than specified above will invalidate the use of the certified values and associated parameters.

CERTIFIED VALUES

Twenty-one industrial, commercial and government laboratories participated in an interlaboratory measurement program using methods of their own choice.

Methods for the determination of the concentration of the elements included mainly preparation with various combinations of acids or various types of fusions followed by the determination with inductively coupled plasma optical emission spectroscopy and inductively coupled plasma mass spectrometry. Additionally, the concentration of some elements was determined by the preparation of a fused bead prepared with various fluxes followed by X-ray fluorescence.

The concentration of carbon was determined mainly using combustion followed by infrared spectrometry.

ANOVA was used to calculate the consensus values and other statistical parameters from the data from the interlaboratory measurement program. Values are deemed to be certified if derived from 10 or more sets of data that meet CCRMP’s statistical criterion regarding the agreement of the results. Ninety-two analytes were certified (see Table 1).

Full details of all work, including the statistical analyses, the methods and the names of the participating laboratories are contained in the Certification Report. For more details on how to use reference material data to assess laboratory results, users are directed to ISO Guide 33:2015, sections 8-9, and the publication, “Assessment of laboratory proficiency using CCRMP reference materials”, at www.ccrmp.ca.

UNCERTIFIED VALUES

Twenty-one provisional values (Table 2) were derived from 8 or 9 sets of data that fulfill the CCRMP statistical criterion regarding agreement; or 10 or more sets of data, that do not fulfill the CCRMP statistical criteria required for certification; or 7 sets of data for which the statistical analysis of the data warranted provisional status. Indicative values for twenty-six analytes, shown in Table 3, were derived from the means of a minimum of 3 sets of data.

TRACEABILITY

The values quoted herein are based on the consensus values derived from the statistical analysis of the data from the interlaboratory measurement program, and the standards used by the individual laboratories. The report for this material provides the available details.

CERTIFICATION HISTORY

STSD-5 was released as a new material in February 2026.

PERIOD OF VALIDITY

The certified values are valid until February 28, 2046.

LEGAL NOTICE

CanmetMINING has prepared this reference material and statistically evaluated the analytical data of the interlaboratory measurement program to the best of its ability. The purchaser, by receipt hereof, releases and indemnifies CanmetMINING from and against all liability and costs arising out of the use of this material and information.

CERTIFYING OFFICERS

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Jeffrey Scott – Project Lead and Data Processor

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________________________________
Maureen E. Leaver – CCRMP Manager

FOR FURTHER INFORMATION

STSD-5 was prepared in consideration of the principles in ISO 17034:2016 and ISO Guides 30, 31, 33 and 35. The Certification Report is available free of charge upon request to:

CCRMP
CanmetMINING (NRCan)
555 Booth Street, room 104
Ottawa, Ontario K1A 0G1
Canada

Telephone: (343) 543-6830
E-mail: ccrmp-pcmrc@nrcan-rncan.gc.ca

 
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