czn-3-eng
Certificate of Analysis
First issued: November 1996
Last revision: August 1997
CZN-3
Zinc Concentrate Reference Material
Certified Values and 95% Confidence Intervals
Constituent
Certified Value
95% C.I. Ag 45 μg/g ± 2 μg/g As 0.039 % ± 0.003 % Ca 0.058 % ± 0.005 % Cd 0.248 % ± 0.003 % Co
0.009 %
± 0.001 % Cu 0.685 % ± 0.008 % Fe 9.97 % ± 0.08 % Mg 0.051 %
± 0.001 % Pb 0.113 % ± 0.003 % S 31.6 % ± 0.4 % Zn 50.92 % ± 0.08 %
Provisional Values and 95% Confidence Intervals
Constituent
Provisional Value
95% C.I. Al 0.10 % ± 0.01 % Hg 5 μg/g ± 1 μg/g Mn 0.0096 % ± 0.0006 % Ni 31 μg/g ± 10 μg/g Sb 10 μg/g ± 2 μg/g SiO 2 0.94 %
± 0.06 %
Source
The raw material for CZN-3 is a currently-traded concentrate donated by Kidd Creek Division of Falconbridge Limited, Timmins, Ontario.
Description
The product is a compositional reference mate-rial having primarily a sulphide matrix and a zinc concentration of 51 %.
Intended Use
CZN-3 is intended for analysis of zinc, other majors and minors, including penalty elements, and trace elements in a zinc sulphide concen-trate.
Instructions for Use
CZN-3 should be used “as is” without drying, to duplicate conditions in the interlaboratory certi-fication program.. Thermogravimetric analysis at CANMET showed a moisture content of 0.8%. The contents of the bottle should be thor-oughly mixed before taking samples. After opening the sealed pouch, the bottle should be kept in a dessicator, or preferably, resealed under nitrogen to prevent oxidation. Bottles that have been left unsealed are prone to oxidation, which would, in time, cause a lowering of the concen-tration of the constituents. If CZN-3 is used for major element analysis, such bottles should be discarded and replaced with fresh stock. Method of Preparation
The raw material, in the form of fine powder, was shipped in three 150-kg lots to CANMET for processing.
Each lot was dried in batches and passed through primary and secondary crushers to breakdown agglomerates. Batches were re-dried at 150 °C for 5 h. The material was screened to -200 mesh. The oversize fraction was milled, in 25-kg batches, in a vibration energy mill, and screened to -200 mesh. The final -200-mesh product weighed 390 kg. CZN-3 was blended in a single lot in a conical blender that had been flushed with nitrogen, and bottled in 200-g units. Each bottle was sealed, under nitrogen, in a my-lar-aluminum foil pouch to provide long-term protection against oxidation.
State of Homogeneity
The homogeneity of the stock with respect to its zinc, cadmium, and lead contents was tested and confirmed at CANMET and Kidd Creek using bottles chosen according to a stratified random sampling scheme. Kidd Creek also determined iron, silver, copper and magnesium. Kidd Creek used titrimetric techniques for the determination of zinc and iron on 0.3-g and 1.0-g samples, re-spectively. For the other elements, they used a multi-acid digestion of a 0.3-g sample followed by ICP finish (AAS for silver on a 1.0-g sam-ple). CANMET used 0.25-g samples for the titrimetric zinc determinations and a multi-acid digestion of 1-g samples for the ICP determina-tion of cadmium and lead.
Method of Certification
CZN-3 was certified by an interlaboratory analy-sis program. Forty-one industrial, commercial, and government laboratories participated in a free-choice of method interlaboratory certifica-tion program by providing analyses for zinc and many other elements. A statistical analysis of the data yielded a certified value for zinc and ten other major, minor and trace elements, including penalty elements. Provisional status was con-ferred on six other constituents and information ranges are reported for twelve more. Data for other elements are either inadequate or inconclu-sive, but are disclosed in the final report. Legal Notice
The Canadian Certified Reference Materials Pro-ject has prepared this reference material and sta-tistically evaluated the analytical data of the in-terlaboratory certification program to the best of its ability. The purchaser, by receipt hereof, releases and indemnifies the Canadian Certified Reference Materials Project from and against all
liability and costs arising out of the use of this material and information.
Reference
The preparation and certification procedures used for CZN-3, including values obtained by individual laboratories, are given in CANMET report CCRMP 96-1E. This report is available free of charge on application to:
Coordinator, CCRMP
CANMET (NRCan)
555 Booth Street
Ottawa, Ontario, Canada
K1A 0G1
Telephone: (613) 995-4738
Facsimile: (613) 943-0573
E-mail:
ccrmp@nrcan.gc.ca Certifying Officers
_____________________________________
William S. Bowman
_______________________________________
Maureen E. Leaver
Information Ranges
Constituent Information
Range Au 0.05 - 0.08 μg/g
Ba 6 -14 μg/g
C 0.09 - 0.12 %
Bi 7 - 20 μg/g
Cl 20 -70 μg/g
Cr 6 - 10 μg/g
F 0.001 - 0.008 %
In 0.018 - 0.024 %
La 2 - 7 μg/g
Mo 2 - 20 μg/g
Se 110 - 115 μg/g
Sn 0.04 - 0.05 %