Sample Analysis Design. Solution Mode
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1 Sample Analysis Design Solution Mode
2 Step I Sample preparation The quality of your data will only be as good as the quality of your sample i.e. did you adequately prepare your sample in the clean lab? With respect to the destruction of matrices for samples requiring digestion Did you adequately spike samples with the correct internal standard? Sample handling protocol is extremely important, e.g. weighing
3 Solid Samples Analyze in solid state via LA-ICP-MS? Analyze in solid state via SIMS secondary ion mass spectrometry? Convert into a glass bead and analyze via XRF x-ray fluoresence? Take powder and digest into solution with acids?
4 Sample Analysis Design- Liquid (aqueous) samples run as-is? filter then run? dilute then run? acidify, dilute, then run?
5 Sample Analysis Design Method of sample preparation also depends upon the elements of interest e.g. don t analyze your samples in a hydrofluoric acid medium if you wish to measure Si abundances why? Elemental concentration determinations at ultra-trace level (ppb, ppt) are very susceptible to contamination during sample preparation and therefore should be conducted in clean laboratory environments
6 Clean room environment Laboratory clean room is a facility in which the concentration of airborne particles is controlled to specified limits. Eliminating sub-micron airborne contamination is a control-driven process since contaminants are generated by people, process, facilities and equipment. Hence, sub-micron particles must be continually removed from the air.
7 Clean room environment Typical office building air contains from 500,000 to 1,000,000 particles (0.5 microns or larger) per cubic foot of air. A Class 100 cleanroom is designed to never allow more than 100 particles (0.5 microns or larger) per cubic foot of air. Class 1000 and Class 10,000 cleanrooms are designed to limit particles to 1000 and 10,000, respectively
8 Clean room environment A human hair is about microns in diameter. A particle 200 times smaller (0.5 micron) than the human hair can cause major disaster in a clean room. Human hair typically concentrates elements/contaminants such as Pb!
9 Facilities: Sample Analysis Design - Sources of contamination Walls, floors and ceilings Paint and coatings Construction material (sheet rock, saw dust etc.) Air conditioning debris Room air and vapors Spills and leaks
10 People: Sample Analysis Design - Sources of contamination Skin flakes and oil Cosmetics and perfume Spittle Clothing debris (lint, fibers etc.) Hair
11 Sample Analysis Design - Contamination Control HEPA (High Efficiency Particulate Air Filter) - Extremely important for reducing contamination - filter particles as small as 0.3 microns with a 99.97% minimum particle-collective efficiency. Clean room design requires air flow dynamics to be the least disruptive as possible laminar flow Cleaning!
12 Sample Analysis Design - Contamination Control Purity of reagents, acids, cleanliness of digestion vessels, sample bottles, etc can dramatically effect background levels and data quality If possible, use highest purity commercial acids At the minimum - sometimes need to further process reagents e.g. acid distillation in our laboratory Digestion vessels made of disposable fluorinated polymers (teflon, PFTE, PFA, etc) Solutions stored in polypropylene or equivalent
13 Concentration terminology Concentrations are typically expressed as either µg/g, or µg/ml (1 µg - microgram = 1 x 10-6 grams), or ppm, ppb, ppt ppm = parts per million = 1 x 10-6 g/g = 1 µg/g (µg = microgram) ppb = parts per billion = 1 x 10-9 g/g = 1 ng/g (ng = nanogram) ppt = parts per trillion = 1 x g/g = 1 pg/g (pg = picogram)
14 Concentration terminology E.g. Zircon ZrSiO 4 ZrO 2 = 67.2 wt% SiO 2 = 32.8 wt% Atomic mass of Zr= Atomic mass of Si= Atomic mass of O= % Zr in ZrO 2 = /( ( *2)) = 74 % Si in SiO 2 = /( ( *2)) = 46.7
15 Concentration terminology If 100% = 1,000,000 ppm, then 74% Zr (out of 67.2 wt%) = 49.73% or 497,300 ppm (or µg/g) 46.7% Si (out of 32.8 wt%) = 15.32% or 153,200 ppm (or µg/g) If you are asked to weigh out g of zircon, then the amounts of total Zr and Si you would have are: Zr = 497,300 µg/g x g = 4.97 µg Si = 153,200 µg/g x g = 1.53 µg
16 Concentration terminology However, you are asked to prepare a solution of this zircon sample for ICP-MS analysis in solution mode; then what would be the minimum dilution factor required given that the maximal amount of ion signal intensity allowed is 50 x 10 6 cps and the yield for both elements in medium resolution mode is ~60,000 cps/ppb?
17 Concentration terminology Maximum allowable concentration is = Max. count rate/ yield = 50 x 10 6 cps/ 60,000 cps/ppb = 833 ppb (ng/g) 4.97 µg of Zr needs to be diluted into? ml of 5% HNO µg = 4970 ng/833 ng/g = ~5.97 g (ml) of 5% HNO 3
18 Matrix Requires a medium (i.e. acid) that Provides efficient ion transmission (HNO 3 > HCl > H 2 O) Won t dissolve the glassware of your introduction system for example, hydrofluoric acid (HF) would! Is relatively cheap and not deemed extremely hazardous to use Thus, dilute (1 to 5% volumetric) nitric acid (HNO 3 ) is the acid medium of choice for most ICP-MS analyses
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