TLS-1 Certificate of Analysis
TLS-1 is discontinued and no longer available for purchase.
Certified Reference Material: Unoxidized Tailings
Printable version of the certificate (PDF, 135.84 kb)
First Issued : September 2004
Version: January 2009
|Element||Unit||Mean||Within-lab Standard Deviation||Between-labs Standard Deviation||95% Confidence Limit|
|Constituent||Unit||Mean||Within-Lab Standard Deviation||Between-labs Standard Deviation||95% Confidence Limit|
TLS-1 is a tailings material from the Clarabell Mill originally prepared as a custom certified reference material for Inco Limited, Copper Cliff, Ontario, Canada in 1998. The material is the waste product from the production of a copper-nickel sulphide concentrate in the form of a fine powder. Inco Limited agreed to donate some of the custom certified reference material to CANMET, Natural Resources Canada.
The raw material was dried at 93°C for five hours and allowed to return to ambient temperatures overnight. It was then crushed, sieved and blended to obtain a minus and plus 150 µm (100 mesh) fraction. The plus material was ground, sieved and blended to obtain second minus 150 µm fraction. These two minus fractions were then combined. The yield was 80%. The material comes in glass bottles containing 100 g each. This is the only size available.
TLS-1 is suitable for the analysis of various elements in tailings at major and minor levels. Examples of intended use are for quality control in the analysis of samples of a similar type, method development and arbitration.
Instructions for use
The assigned values pertain to the date when issued. TLS-1 should be used “as is”, without drying. The contents of the bottle should be thoroughly mixed before taking samples.
Normal safety precautions such as the use of safety glasses, breathing protection for fine particulate matter, gloves and a laboratory coat are suggested.
Level of homogeneity
The homogeneity of the final product was investigated using twenty-two bottles of TLS-1 chosen according to a stratified random sampling scheme. Two samples were analyzed from each bottle in a randomized order. Samples of 0.5 g were digested in nitric, hydrochloric, perchloric and hydrofluoric acids and the determination of copper and nickel was performed using atomic absorption spectroscopy.
Samples of 0.5 g were analyzed for sulphur by combustion using a LECO apparatus with infrared detection.
A one–way analysis of variance technique (ANOVA) was used to assess the homogeneity of these elementsFootnote 1. The ratio of the between-bottles to within-bottle mean squares is compared to the F statistic at the 95% level of probability. No evidence of inhomogeneity was observed for copper, nickel and sulphur. Use of a smaller mass will invalidate the use of the certified values and associated statistical parameters.
Eighteen industrial, commercial, and government laboratories participated in an interlaboratory measurement program. Various elements were analyzed by methods selected by the individual laboratories. These methods were to be selected so as to yield highly accurate and precise values. A one-way analysis of variance technique was used to estimate the consensus value and other statistical parametersFootnote 1. Methods included multi-acid digestions, fusion, electroplating, atomic absorption spectroscopy, combustion, titration, gravimetric methods, x-ray fluorescence and inductively coupled plasma - atomic emission spectroscopy. A one-way analysis of variance technique (ANOVA) was used to estimate the consensus value and other statistical parametersFootnote 1 Table 1 contains the means and associated statistical parameters for the six certified elements.
Table 2 contains the provisional elements which did not meet either one or both of the two criteria for certification. Table 3 contains the informational values derived from semi-quantitative analysis.
The certified values quoted herein are based on the consensus value derived from the statistical analysis of the data from the interlaboratory measurement program.
Date of certification
TLS-1 was prepared in 1998 for Inco Limited. In 2004 Inco donated some of the material to Natural Resources Canada to sell.
Period of validity
These certified values are valid until December 31, 2030. Updates will be published on the CCRMP web site.
CanmetMINING has prepared this reference material and statistically evaluated the analytical data of the interlaboratory certification 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.
Maureen E. Leaver – CCRMP Coordinator
Joseph Salley – Data Processor
For Further Information
555 Booth Street
Ottawa, ON K1A 0G1
E-mail: Contact CCRMP
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