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Elements and Performance Criteria

  1. Determine sample characteristics and appropriate analytical methods
  2. Prepare samples and standards
  3. Set up instrument and perform trial analysis
  4. Optimise instrument performance
  5. Perform analysis
  6. Perform routine maintenance and troubleshoot instruments
  7. Maintain a safe work environment
  8. Maintain laboratory records

Required Skills

Required skills

Required skills include

establishing client needs for routine and nonroutine samples

interpreting client requests test methods and procedures accurately

selecting appropriate IR techniques and installing instrument accessories

selecting adapting and modifying standard test methods for unknown samples

preparing samples and standards optimising procedures and equipment to suit sampletest requirements

setting up starting up and shutting down equipment

checking the calibrationqualification status of equipment

selecting configuring checking and optimising instrument subsystems

performing routine instrument maintenance and replacement of consumables

obtaining valid and reliable data

calculating analyte concentrations with appropriate accuracy precision uncertainty and units

recognising atypical dataresults and troubleshooting common analytical procedure and equipment problems

recording and reporting dataresults using enterprise procedures

maintaining security integrity and traceability of samples and documentation

assessing risks applying specified control measures and working safely

minimising waste ensuring safe collection and disposal

applying relevant principles of good laboratory practice GLP procedures

maintaining technical knowledge by accessing journals technical updates suppliers product notes and test methods

Required knowledge

Required knowledge includes

criteria for determining which IR technique eg cell and accessory is best suited to which type of sample eg gas liquid bulk solid fibre film small quantity

sample preparation procedures including specialised techniques such as

handling unstablehazardous chemicals and samples fragilelabile biological material and hygroscopic samples

filtration or centrifugation to remove particulates

prevention of personal contamination of samples by exposure to analyst

cleaning andor handling of optical elements

cleaning techniques and handling of transmission cells and flow cells

cleaning of reflectance crystals and solidliquid standards

alignment techniques for source mirrors and accessories

IR spectroscopic terms and concepts such as

absorption absorbance transmittance diffuse and specular reflectance and attenuated total reflectance

fourier transform of interferograms to produce spectra

fast fourier transform FFT

Fourier Transform advantages Jacquinot Felgett Connes

electronic vibronic vibrational and rotational transitions during absorption and relationship to chemical properties

concepts such as Beers Law Bouguer or Lamberts Law and molar absorptivity

deviations from Beers Law polychromatic radiation and chemical reactions

spectral resolution spectral bandwidth and linear dispersion

limit of detection limit of quantitation and their application to quality control procedures

derivative spectra

multicomponent analysis

analysis of reaction kinetics

calculations and data processing involving

baseline correction and spectral smoothing

KubelkaMunk conversion to linearise diffuse reflectance data

KramerKronig transformation to remove refraction effects

Concentration and dilution

spectral matching

spectral subtraction and spectral deconvolution

first and higher derivatives of spectra

multicomponent quantitation techniques such as Classic Least Squares CLS Inverse Least Squares ILS Partial Least Squares PLS Principal Component Regression PCR

operation construction selectivity typical applications troubleshooting and routine maintenance of IR systems including details such as

scan settings sourcedetectorbeamsplitter combination number of scans scan range scan mode aperture resolution apodisation zero filling optical alignment sensitivity threshold optical path difference and velocity

sources egtungstenhalogen ceramic mercury arc glow bars and Nernst glowers

interferometer components eg beam splitters KBr CsI Mylar and metal mesh and mirrors

sample transmittance KBr ZnSe and CsI cells sample reflectance mounts and troughs fibre optic probes and microscope attachments

mid IR detectors eg HgCdTe or MCT DLaTGS far IR detectors eg DLaTGS liquid helium cooled Si bolometers

IR sensitive charge coupled array devices and focal plane array detectors for imaging

operation construction typical applications troubleshooting and routine maintenance of IR accessories such as

attenuated total reflectance single and multireflection unit and grazing angle

specular and diffuse reflectance units

single point microscope and spectrochemical imaging microscope

photoacoustic spectroscopy PAS

thermogravimetric analysers TGAIR

polariser

calibration procedures for

accuracy of wavelength using transmission and reflectance standards such as polystyrene germanium and rare earth oxide glasses such as holmium oxide

photometric accuracy using for example polystyrene or polyethylene terephthalate and potassium dichromate

zero absorbance baseline flatness

sources of spectral interferences such as

water and carbon dioxide

strongly absorbing matrix components

computer control software for operating and optimising instrument

procedures for optimising instrument performance such as

alignment of subsystems eg source mirror and beam splitter and accessories

adjustment signal to noise ratio to obtain satisfactory spectral resolution

use of manualcomputer calibration charts andor standards to identify and quantify analytes such as

external calibration

multicomponent analysis

semiquantitative analysis

library searching for spectral matching

derivative spectrum analysis

calculation steps to give results in appropriate units and precision

troubleshooting and maintenance procedures recommended by instrument manufacturer

enterprise andor legal traceability requirements

relevant health safety and environment requirements

Evidence Required

The Evidence Guide provides advice on assessment and must be read in conjunction with the performance criteria required skills and knowledge range statement and the Assessment Guidelines for the Training Package

Overview of assessment

Critical aspects for assessment and evidence required to demonstrate competency in this unit

Assessors should ensure that candidates can

interpret client requests test methods and procedures accurately

replace standard IRFTIR instrument consumables such as lamps desiccants and purge gases

install IRFTIR accessories such as sample cellsprobes microscope and reflectance units

safely set up start up and shut down instrument using enterprise procedures

prepare samples and calibration standards in accordance with test method

check calibrationqualification status of equipment

optimise instrument subsystems and procedures and equipment to suit sampletest requirements

operate equipment to obtain valid and reliable data

use software to identify analytes and calculate concentrations with appropriate accuracy precision and units

recognise atypical dataresults

troubleshoot common analytical procedure and equipment problems

record and report dataresults using enterprise procedures

maintain security integrity and traceability of samples and documentation

follow OHS procedures and principles of GLP

Context of and specific resources for assessment

This unit of competency is to be assessed in the workplace or simulated workplace environment

This unit of competency may be assessed with

MSLA Evaluate and select appropriate test methods and procedures

MSL976003A Evaluate and select appropriate test methods and procedures

MSLA Contribute to the validation of test methods

MSL977003A Contribute to the validation of test methods

MSLA Develop or adapt analyses and procedures

MSL977004A Develop or adapt analyses and procedures.

Resources may include

laboratory with specialised analytical instruments

laboratory reagents and equipment

SOPs and test methods

Method of assessment

The following assessment methods are suggested

review of test dataresultscalibration graphs obtained by the candidate over time to ensure accuracy validity precision and timeliness of results

inspection of results and technical records eg maintenance schedules and quality control logbooks completed by the candidate

observation of candidate using IRFTIR instruments to measure analytes

feedback from clients peers and supervisors

oral or written questioning of relevant IRFTIR spectroscopy concepts chemical principles underpinning sample preparation and separation of species instrument design and optimisation analytical techniques and enterprise procedures

In all cases practical assessment should be supported by questions to assess underpinning knowledge and those aspects of competency which are difficult to assess directly

Where applicable reasonable adjustment must be made to work environments and training situations to accommodate ethnicity age gender demographics and disability

Access must be provided to appropriate learning andor assessment support when required

The language literacy and numeracy demands of assessment should not be greater than those required to undertake the unit of competency in a work like environment

This competency in practice

Industry representatives have provided the case studies below to illustrate the practical application of this unit of competency and to show its relevance in a workplace setting

Forensic science

A forensic science team is examining some motor vehicle paint samples taken from a crime scene After a careful microscopic examination of the topcoat and undercoat layers one technician narrows the samples origin down to a small range of possible vehicle makes models and years of manufacture To aid identification another technician prepares a small paint chip for examination in the laboratorys FTIR spectrometer After referring to the recommended analytical methods heshe decides to use a transmittance technique because all the sampling wavelengths are subjected to the same path lengths and most of the reference data for paints binders pigments and additives consist of transmittance spectra The technician cuts a crosssection sample with a microtome to expose an edge of the multilayered sample and then mounts it using the microscope accessory Heshe adjusts the microscope aperture to minimise stray light and diffraction effects before obtaining spectra for each layer After comparing hisher results with the spectral library data for binders pigments and additives used by the manufacturers of interest the origin of the paint is identified Some weeks later confirmation is obtained when samples taken from a suspects vehicle match the physical and chemical features and spectra determined from the crime scene samples and diffuse reflectance measurements on the two sets of samples show identical weathering and surface contamination


Range Statement

The range statement relates to the unit of competency as a whole. It allows for different work environments and situations that may affect performance. Bold italicised wording, if used in the performance criteria, is detailed below. Essential operating conditions that may be present with training and assessment (depending on the work situation, needs of the candidate, accessibility of the item, and local industry and regional contexts) may also be included.

Codes of practice

Where reference is made to industry codes of practice, and/or Australian/international standards, it is expected the latest version will be used

Standards, codes, procedures and/or enterprise requirements

Standards, codes, procedures and/or enterprise requirements may include:

Australian and international standards, such as:

AS ISO 17025-2005 General requirements for the competence of testing and calibration laboratories

AS/NZS 2243 Set:2006 Safety in laboratories set

AS/NZS ISO 9000 Set:2008 Quality management systems set

AS 2830.1 Good laboratory practice - Chemical analysis

ASTM E168 - 06 Standard practices for general techniques of infra red quantitative analysis

ASTM E334 - 01(2007) Standard practice for general techniques of infra red microanalysis

ASTM E573 - 01(2007) Standard practices for internal reflection spectroscopy

ASTM E2224 - 02 Standard guide for forensic analysis of fibers by infra red spectroscopy

ISO/IEC Guide 98-3:2008 Uncertainty of measurement - Part 3 Guide to the expression of uncertainty in measurement (GUM)

Eurachem/CITAC Guide CG4 Quantifying uncertainty in analytical measurement

National Association of Testing Authorities (NATA) supplementary requirements for the field of testing

Australian code of good manufacturing practice (GMP)

principles of good laboratory practice (GLP)

material safety data sheets (MSDSs)

national measurement regulations and guidelines

enterprise procedures, standard operating procedures (SOPs) and operating manuals

quality manuals, equipment and procedure manuals

equipment startup, operation and shutdown procedures

calibration and maintenance schedules

cleaning, hygiene and personal hygiene requirements

data quality procedures

enterprise recording and reporting procedures

material, production and product specifications

production and laboratory schedules

quality system and continued improvement processes

safety requirements for equipment, materials or products

sampling procedures (labelling, preparation, storage, transport and disposal)

schematics, work flows and laboratory layouts

statutory and enterprise occupational health and safety (OHS) requirements

stock records and inventory

test procedures (validated and authorised)

waste minimisation, containment, processing and disposal procedures

IR/FTIR instruments and techniques

IR/FTIR instruments and techniques may include:

grating or interferometer as the dispersive element

gas sampling cells

liquid autosamplers and flow cells

beam condensers for micro-samples

reflection/transmission holders for FTIR microscopes

specialised infra red windows for FTIR microscopes

attenuated total reflectance ATR units (e.g. variable pressure, horizontal HATR trough plates, multiple internal reflectance MIR, single reflection ATR units and universal UATR units)

fixed/variable angle specular reflectance units

polarisers

single point microscopes and array-based imagers

discrete analysers (e.g. oil and SO2)

data systems such as recorders, electronic integrators, and software packages for peak detection and spectra manipulation

spectral library matching

Testing that uses IR/FTIR spectroscopy

Testing that uses IR/FTIR spectroscopy may include:

medical (pathology) testing (e.g. bacterial screening)

forensic testing to establish analyte 'fingerprint' and possible source of scene of crime samples (e.g. paint layers by specular reflectance, fingermark residues by ATR and fibres by polarisable ATR)

environmental monitoring of pollution in air, water or soil (e.g. multi-organic components in industrial emissions)

control of starting materials, in-process materials and final products in a wide range of industry sectors (e.g. surface defects in polymers, semiconductor contamination and quantitation of biodiesel components)

materials testing (e.g. lubricant condition)

food testing (e.g. moisture and protein determination in grain)

pharmaceuticals (e.g. drug testing of athletes)

geological testing (e.g. oil inclusions in rocks by grazing angle ATR)

Presumptive tests

Presumptive tests may include:

source of sample

type and quantity of sample

assessing suitability of sample and specified preparation for spectroscopic technique (e.g. pH and aqueous content)

Sample and standard preparation

Sample and standard preparation may include:

identification of any hazards associated with the samples and/or analytical chemicals

grinding, mulling and preparation of disks

dissolving, extraction, centrifuging, evaporation, washing and drying

determination of, and if appropriate, removal of any contaminants or impurities or interfering substances

Pre-use, calibration and safety checks

Pre-use, calibration and safety checks may include:

cleanliness of cells and dip/or probes

condition of desiccant packs and purge gas flows

detector coolant

optical alignment (e.g. beam splitter alignment, mirrors and accessories)

cell positioning and cell matching

checking integrity and alignment of accessories

wavelength accuracy using polystyrene

amplifier gain adjustment, signal to noise ratio

stray light levels

100% transmittance baseline flatness

spectral bandwidth (sharpness of peak, peak intensity and resolution of adjacent peaks)

Instrumental parameters

Instrumental parameters may include:

spectral lamp selection

measurement mode (i.e. transmittance, reflectance)

wavelength range, start/finish

spectral bandwidth (slit width and signal to noise ratio)

scan speed/fixed wavelength

number of scans

temperature control for kinetic studies

Common analytical procedure problems and remedies

Common analytical procedure problems and remedies may include:

cell cleanliness

mismatched optical cell pairs and incorrect cell path length

alignment of external attachments

full scale absorption and too much sample

non-homogeneity of samples

air gap between solid sample and reflectance crystal

Common equipment problems

Common equipment problems may include:

system leaks

adjustment of optical elements such as mirrors and lamps

alignment of external accessories

cleanliness/optical matching of cells and cell window degradation

cell blockages

contamination of reflectance crystal

Hazards

Hazards may include:

electric shock

biohazards, such as microbiological organisms and agents associated with soil, air, water, blood and blood products, and human or animal tissue and fluids

corrosive chemicals

sharps and broken glassware

flammable liquids and gases

fluids under pressure and sources of ignition

disturbance or interruption of services

Addressing hazards

Addressing hazards may include:

use of MSDS

accurate labelling of samples, reagents, aliquoted samples and hazardous materials

personal protective equipment such as gloves, safety glasses and coveralls

use of fumehoods, direct extraction of vapours and gases

use of appropriate equipment such as biohazard containers, laminar flow cabinets, Class I, II and III biohazard cabinets

handling and storage of all hazardous materials and equipment in accordance with labelling, MSDS and manufacturer's instructions

Occupational health and safety (OHS) and environmental management requirements

OHS and environmental management requirements:

all operations must comply with enterprise OHS and environmental management requirements, which may be imposed through state/territory or federal legislation - these requirements must not be compromised at any time

all operations assume the potentially hazardous nature of samples and require standard precautions to be applied

where relevant, users should access and apply current industry understanding of infection control issued by the National Health and Medical Research Council (NHMRC) and State and Territory Departments of Health