MISCELLANEOUS ANALYSIS

Samples 1g in size are encapsulated in a polyethylene vial and placed in a thermalized beam of neutrons produced from a nuclear reactor. Samples are measured for the doppler broadened prompt gamma ray at 478 KeV using a high purity GE detector. Samples are compared to certified reference materials used to calibrate the system. A minimum of four standards are analyzed with every work order. Duplicates are analyzed when samples are provided. The detection limit reported is a function of the counting times required for each.

AnalysisMethodDetection LimitUpper Limit
BPGNAA0.5 ppm10,000 ppm
BPGNAA2 ppm10,000 ppm

Samples 1 g in size are encapsulated in a polyethylene vial and placed in a thermalized beam of neutrons produced from a nuclear reactor. Samples are measured for the doppler broadened prompt gamma ray at 478 KeV using a high purity GE detector. Samples are compared to certified reference materials used to calibrate the system. A minimum of four standards are analyzed with every work order. Duplicates are analyzed when samples are provided. The detection limit reported is a function of the counting times required for each.

AnalysisMethodDetection Limit
ClINAA0.01%

Samples 0.2 g in size are fused with a combination of lithium metaborate and lithium tetraborate in an induction furnace to release the chloride ions from the sample matrix. The fuseate is dissolved in dilute nitric acid, prior to analysis the ion strength of the solution is adjusted. The chloride ion electrode is immersed in this solution to measure the fluoride-ion activity directly.

AnalysisMethodDetection Limit
Cl (ISE)FUS-ISE0.01%

Samples 0.2 g in size are fused with a combination of lithium metaborate and lithium tetraborate in an induction furnace to release the fluoride ions from the sample matrix. The fuseate is dissolved in dilute nitric acid, prior to analysis the solution is complexed and the ionic strength adjusted with an ammonium citrate buffer. The fluoride ion electrode is immersed in this solution to measure the fluoride-ion activity directly. An automated fluoride analyzer from Mandel Scientific is used for the analysis.

AnalysisMethodDetection Limit
FFUS-ISE0.01%

FeO is determined through titration, using a cold acid digestion of ammonium metavanadate, and hydrofluoric acid in an open system. Ferrous ammonium sulphate is added after digestion and potassium dichromate is the titrating agent.

This cold digestion will dissolve silicates and some sulphides. Pyrite may not be totally dissolved. The extent of dissolution is affected by the ferric iron content higher Fe(3+) concentration increases the solubility of pyrite. Concentrations of S(II) has a tendency to reduce Fe(3+) to Fe(2+). This is minimized in an open system. If the S concentration is greater than 10% an alternative hot digestion method is used for FeO. 

When titrating, the endpoint is determined by colour.  Certain solutions high in MnO2 or certain matrices make the endpoint determination difficult or impossible.

AnalysisMethodDetection Limit
FeOTitration0.1%

Modified method from Wilson (1955. Bull Geol. Sur. Gt. Britain , volume 9, pp. 56-68)

H2O-(moisture) is determined gravimetrically using a 2 g sample heated in an oven at 105°C (Other temperatures may be used at special request).  0.3 g of the dried sample(from H2O-) is thermally decomposed in a resistance furnace in a pure nitrogen environment at 1000 °C (interstitial water, H2O+), using an ELTRA CW-800, directly releasing H2O. H2O absorbs IR energy at a precise wavelength within the IR spectrum. Energy from the IR source is absorbed as the gas passes through the cell, preventing it from reaching the IR detector. All other IR energy is prevented from reaching the IR detector by a narrow bandpass filter. Because of the filter, the absorption of IR energy can be attributed only to water (H2O). The concentration of H2O is detected as a reduction in the level of energy at the detector.

AnalysisMethodDetection Limit
H2O +/-Infrared0.1%

A 0.2g sample is combusted in a resistance furnace at 1350 °C, using a LECO CNS-2000. Combustion gases are collected in a 4.5-liter ballast tank and then flow to the detectors. Nitrogen in the form of N2 is detected by thermal conductivity detection. A Leco CNS-2000 is used for the analysis

AnalysisMethodDetection Limit
Total NThermal Conductivity0.01%

A 0.5 g sample is digested with aqua regia at 90ºC. The Hg in the resulting solution is oxidized to the stable divalent form. Since the concentration of Hg is determined via the absorption of light at 253.7 nm by Hg vapour, Hg (II) is reduced to the volatile free atomic state using stannous chloride. Argon is bubbled through the mixture of sample and reductant solutions to liberate and to transport the Hg atoms into an absorption cell. The cell is placed in the light path of an Atomic Absorption Spectrophotometer. The maximum amount absorbed (peak height) is directly proportional to the concentration of mercury atoms in the light path. Measurement can be performed manually or automatically using a flow injection technique (FIMS).Hg analysis is performed on a Perkin Elmer FIMS 100 cold vapour Hg analyzer.

Code 1G (Hg-CV Add-On) Detection Limit (ppb)

ElementDetection LimitUpper Limit
Hg5100,000

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