Rock samples are prepared for geochemical analysis by jaw crushing to 1.5 cm, sub-sampling and pulverizing in a Bico ceramic disc grinder followed by reduction to <100 mesh powder in a ceramic ball mill. Final product is a 20g vial of representative powdersuitable for acid dissolution or fusion. Approximately 5g total rock powder required for a standard whole-rock and trace-metal analysis.

1. Major elements (X-ray fluorescence) (METHOD XRF-100)

   Analysis is completed by fused disk wavelength dispersive X-ray Fluorescence. This method is not suitable for samples containing greater than 5% S or significant amounts of barite, percent levels of copper or lead or for samples for which insufficientquantities are available for producing a fused disk major elementdeterminations for these samples are completed using the ICPES-100package. When ICP-ES and ICP-MS are also requested, Ba, Nb, Rb, Sr andZr values may be obtained using these techniques.

   Analyte	Calibration range (%)	Limit of determination (%)
   SiO2	0 - 100	0.50
   TiO2	0 - 3	0.02
   Al2O3	0 - 60	0.40
   Cr2O3	0 - 4	0.02
   Fe2O3 total	0 - 90	0.10
   MnO	0 - 1	0.01
   MgO	0 - 50	0.10
   CaO	0 - 35	0.10
   Na2O	0 - 10	0.50
   K2O	0 - 15	0.05
   P2O5	0 - 1	0.02
   Ba	0 - 0.30	0.002
   Nb	0 - 0.04	0.003
   Rb	0 - 0.06	0.002
   Sr	0 - 0.20	0.002
   Zr	0 - 0.20	0.002

   Sample required: 1.0 g. If XRF-100 and L.O.I. are requested together (METHOD XRF-110), an additional 0.5 g sample is required.

2. Major elements (ICP-ES) (METHOD ICPES-100)

   Analysis is completed by fusing the sample with a mixed lithium metaborate - lithium tetraborate flux, dissolution of the fusion melt followed by analysis by ICP emission spectrometry. This method is suitable for samples containing greater than 5% S or significant amounts of barite, percent levels of copper or lead or samples forwhich sufficient quantities are not available for the determination ofmajor elements by XRF. If required, the determination of Rb, Sr, Nb andZr by ICP spectrometry is available on request. This method can also beapplied to samples smaller than 0.5 g when necessary.

   Analyte	Limit of determination (%)	Analyte	Limit of determination (%)
   SiO2	0.5	CaO	0.01
   TiO2	0.02	Na2O	0.03
   Al2O3	0.2	K2O	0.05
   Cr2O3	0.02	P2O5	0.01
   Fe2O3	0.06	Ba	0.003
   MnO	0.01	Loss on Ignition	0.1
   MgO	0.04

   Sample required: 0.5 g

3. Supplementary whole rock determinations (volatiles)

   Ferrous Iron is determined using the Wilson Method (titrimetric). H₂O (total), CO₂ (total) and S are determinedusing combustion followed by infra-red spectrometry, CO₂ (carbonate carbon)is determined by acid evolution followed by infrared spectrometry and C(total non-carbonate carbon) is calculated. Loss on ignition is determinedby gravimetry at 900 C.

   Parameter	Sample required	Limit of determination (%)	Method
   FeO	0.2g	0.2	CHEM-100
   H2Ototal	0.5g	0.1	CHEM-110
   CO2total	0.5g	0.1	CHEM-120
   CO2	0.5g	0.1	CHEM-130
   Stotal	0.5g	0.02	CHEM-140

4. Trace elements

   Determinations are based on the total dissolution of the sample using nitric, perchloric and hydrofluoric acids followed by a lithium metaborate fusion of any residual material. For ICPES-110 package analysis is done using ICP emission spectrometry. ForICPMS-100 and ICPMS-110 packages, analysis is done using ICP mass spectrometry.Elements listed in ICPES-110 may be determined by ICPMS-100 or ICPMS-110 at our discretion when analyte concentrations are too low for determinationby ICP-ES.

   Trace elements 1
   (ICP emission spectrometry)
   METHOD ICPES-110

   Element	Limit of determination (ppm)	Element	Limit of determination (ppm)
   Ag	5	Pb	10
   Ba	10	Sc	0.5
   Be	0.5	Sr	5
   Co	5	V	5
   Cr	10	Y	5
   Cu	10	Yb	0.5
   La	10	Zn	5
   Ni	10	Zr	10
   Mo	5

   Sample required: 1.0 g

   Trace elements 2
   (ICP mass spectrometry):
   Rare-earth elements + Y
   METHOD ICPMS-100

   Element	Limit of determination (ppm)	Element	Limit of determination (ppm)
   Ce	0.1	Nd	0.1
   Dy	0.02	Pr	0.02
   Er	0.02	Sm	0.02
   Eu	0.02	Tb	0.02
   Gd	0.02	Tm	0.02
   Ho	0.02	Y	0.02
   La	0.1	Yb	0.05
   Lu	0.02

   Trace elements 2
   (ICP mass spectrometry):
   Other trace elements
   METHOD ICPMS-110

   Element	Limit of determination (ppm)	Element	Limit of determination (ppm)
   Ag	0.1	Pb	2
   Bi	0.5	Rb	0.05
   Cd	0.2	Sn*	0.5
   Cs	0.02	Ta	0.2
   Ga	0.1	Th	0.02
   Hf	0.05	Tl	0.02
   In	0.05	U	0.02
   Mo	0.2	Zr	0.5
   Nb	0.05

   ^*on demand

   Sample required: 1.0 g

   Note: detection limits below those quoted are available on special request. Other elements on request.

5. Fluorine, chlorine, and sulphur (METHOD IC-100)

   Fluorine, chlorine and sulphur in rocks are determined using a pyrohydrolysis method followed by ion chromatography.For this method, the upper limit of determination is 1%.

   Element	Limit of detection (ppm)
   F	50
   Cl	100
   S	50

   Sample required: 0.2 gPlatinum group elements (METHOD PGE-100)

   The PGEs are determined using a mixed-acid dissolution, sodium peroxide fusion followed by telluriumco-precipitation to separate PGEs from matrix elements. Pt, Pd, Ru andIr are determined by isotope dilution ICP mass spectrometry and Rh is determinedusing external calibration ICP mass spectrometry.

   Element	Limit of detection (ppb)
   Pt	0.10
   Pd	0.10
   Ru	0.05
   Ir	0.05
   Rh	0.02

   Analyses of geological materials by this method is by special arrangement only. Please contact us for details.

   Sample required: 5.0 g

The analysis of waters is done using both ICP emission and mass spectrometry. Limits of detectionare given for fresh waters only. Limits of detection will be increasedfor saline waters, pore waters and brines and will vary according to thedilution factor used prior to analysis. Analysis of saline watersprocessed using chelation ion chromatography can give limits of detection(for selected elements) equivalent to or better than those given below.Analysis using this technique available on special request only. Otherelements than those listed may be available on request.

1. ICP emission spectrometry (METHOD ICPES-120)

   Element	Limit of determination (ppb)	Element	Limit of determination (ppb)
   Al	5.5	Mg	1.1
   As	12.0	Mn	0.2
   B	9.5	Na	12.1
   Ba	0.6	Ni	1.6
   Be	0.1	Pb	9.4
   Ca	2.8	Sc	0.3
   Cd	0.3	Se	23.8
   Co	3.1	Si	3.3
   Cr	29.0	Sr	0.2
   Cu	0.4	Ti	0.4
   Fe	1.9	V	1.0
   K	12.0	Zn	0.32
   Li	0.6

   ICP mass spectrometry (METHOD ICPMS-120)

   Element	Limit of determination (ppb)	Element	Limit of determination (ppb)
   Ag	0.2	In	0.2
   Al	0.5	Mn	0.2
   As	1.0	Mo	0.5
   Ba	0.5	Ni	1.0
   Be	1.0	Pb	0.2
   Bi	0.2	Rb	0.2
   Cd	0.5	Sb	0.2
   Co	0.2	Se	2.0
   Cr	2.0	Tl	0.2
   Cs	0.2	U	0.2
   Cu	0.5	V	0.2
   Ga	0.2	Zn	2.0
   Hg	0.2

   Anions in waters (METHOD IC-110)

   Anions are determined directly in waters by ion chromatography.

   Anions	Limit of detection (ppb)
   Nitrate	50
   Nitrite	50
   Fluoride	50
   Phosphate	50
   Sulphate	50
   Chloride	50
   Bromide	50

   Sample required: 15 mL

The Analytical Chemistry Laboratoriesis staffed by 12 scientists and technologists capable of meeting most analyticalneeds. Established and literature methods will be modified to accommodatenew elements, lower detection limits and new or difficult matrices. Contact usconcerning your enquiries or analytical needs.

Research staff of the Analytical Chemistry Laboratories have a long history of collaboration with geoscientists inresearch projects and programs requiring expert support in analytical chemistry.The Laboratories are equipped with state-of-the-art analytical instrumentationincluding leading-edge inductively coupled plasma mass spectrometry, laserablation and electrothermal vaporization sample introduction for ICP-MS.These techniques can quantitatively determine most elements of the periodictable as well as determine isotope ratios of these elements with absolutelimits of detection in the femtogram (10^-15 g) range. Sample sizes downto milligrams can be handled. Below are some examples of research gradeanalytical chemistry techniques developed in collaboration with geoscientists:

• Determination of boron isotope ratios in geological materials
• Determination of lithium isotope ratios in geological materials
• Determination of femtogram quantities of trace metals in environmental samples
• Determination of platinum group elements at the ppt concentration level
• Re/Os dating of sulphide and chromite bearing samples
• Determination of As, U and other elements in difficult matrices such as mineral phase selective reagent extracts

The Analytical Chemistry Section maintains standing offer agreements with commercial analytical chemistry laboratories. Laboratory staff will ship your samples and arrange for the analysis of your samples. Significant discounts compared to published prices have been negotiated and are available to those using this service. For large accounts, we will negotiate standing offer agreements to suit your particular needs. We can also assist you with quality control of services obtained from private analytical chemistry laboratories.

For more information, please contact Dr. D. Conrad Grégoire, Head, Analytical Chemistry Laboratories