CCU-1c is a copper flotation concentrate prepared from ore from the Ruttan mine, Lynn Lake, Manitoba, and donated by Hudson Bay Mining and Smelting, Flin Flon, Manitoba, Canada.
Copper concentrates generally contain chalcopyrite, pyrite, sphalerite, pyrrhotite and gangue minerals. CCU-1c is the fourth in a series, all from the same source, with predecessors, CCU-1b, CCU-1a and CCU-1. The first three materials in the series are no longer available.
CCU-1c is suitable for the analysis of copper, and other elements at major, minor and trace levels in materials with a similar matrix. Examples of intended use are for quality control, method development, arbitration and the calibration of equipment.
INSTRUCTIONS FOR USE
The assigned values pertain to the date when issued. CANMET is not responsible for changes occurring after receipt by the user. CCU-1c should be analyzed “as is”, without drying. The contents of the bottle should be thoroughly mixed before taking samples. The contents of the bottle should be exposed to air for the shortest time possible. Unused material should be stored under an inert gas in a desiccator, or in a new, heat-sealed laminated foil pouch.
Normal safety precautions, such as the use of safety glasses, breathing protection for fine particulate matter, gloves and a laboratory coat are suggested.
METHOD FOR PREPARATION
The raw material was dried at 66°C, sieved and blended to obtain a sub-74 micron (-200 mesh) product, which was bottled in 200-gram units. This is the only size available. Each bottle was sealed under nitrogen in a laminated aluminum foil-mylar pouch to prevent oxidation.
LEVEL OF HOMOGENEITY
The homogeneity of the stock with respect to its antimony, copper, gold, selenium, silver and zinc was investigated using twenty-two bottles chosen according to a stratified random sampling scheme. Two splits were analyzed from each bottle. The analyses for copper were performed by CANMET on 0.5 g samples using a multi-acid digestion followed by a titration with thiosulphate. Instrumental neutron activation was used on 0.5 g sample for antimony, selenium, silver and zinc and on a 5 g sample for gold. A one–way analysis of variance technique (ANOVA) was used to assess the homogeneity of these elements. 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 all six elements. Use of a smaller sub-sample will invalidate the use of the certified value and associated parameters.
Further details are available in the certification report.
Twenty-eight industrial, commercial and government laboratories participated in an interlaboratory certification program. Various elements were analyzed by methods of each laboratory's choice. Depending on the element, the separation step was performed using multi-acid digestion, microwave digestion, fusions, and solvent extraction. Determinations were performed using colourimetric analysis, cold vapour atomic absorption spectroscopy for mercury, direct current arc, direct current plasma, electrogravimetry, electrolysis, atomic absorption, graphite furnace atomic absorption spectroscopy, gravimetry, hydride generation atomic absorption spectroscopy, high pressure liquid chromatography, inductively coupled plasma – atomic emission spectroscopy, inductively coupled plasma – mass spectroscopy, ion specific electrode, combustion, titrimetry and x-ray fluorescence.
A one-way analysis of variance technique was used to estimate the consensus value and other statistical parameters. Fifteen elements were assigned certified values based on statistical criteria. These are indicated in Table 1.
Seven elements were assigned provisional values based on statistical criteria. These are indicated in Table 2. Informational values for fourteen elements were derived from the mean of fifteen to forty-seven results from a varying number of laboratories.
The certified values quoted herein are based on the consensus values derived from the statistical analysis of the data from the interlaboratory measurement program.
DATE OF CERTIFICATION
CCU-1c was originally released in November 2000. The second version of the certificate was issued in January 2004 due to the addition of an informational value for titanium, and the removal of an informational value for thallium. This version of the certificate, which was issued due the expiration of the second version, contains no changes in the values. Additional information in the text is included in conformance with ISO Guide 31:2000.
PERIOD OF VALIDITY
These certified values are valid until 2011. The stability of the material will be monitored every two years. Updates will be published on the CCRMP web site.