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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 UVVISNIR techniques and installing instrument accessories

selecting adapting and modifying standard test methods for unknown samples

preparing samples and standards and 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 UVVISNIR technique eg cell accessory is best suited to which type of sample eg gas liquid bulk solid fibre film and small quantity

sample preparation procedures including specialised techniques such as

handling unstablehazardous chemicals and samples fragilelabile biological material

dilution without causing chromaphoric shifts

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 cells and flow cells

cleaning of reflectance standards and liquid standards

alignment techniques for source mirrors and accessories

UVVISNIR spectroscopic terms and concepts such as

excitation absorption absorbance transmittance reflectance and fluorescence

electronic transitions during absorptionfluorescence and relationship to chemical properties interference and quenching

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

deviations from Beers Law polychromatic radiation and chemical reactions

chromaphores and auxochhromes

conjugation effects in organic molecules

pH effects in ionised samples

solvent effects

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

concentration and dilution

spectral matching

first and higher derivatives of spectra

multicomponent quantitation

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

sources such as deuterium and tungsten filament

monochromators such as prisms gratings and filters

sample holders such as quartz glass and plastic cuvettes cells and fibre optic dip probes

detectors such as photomultipliers photodiode diode arrays charge coupled devices and semiconductor devices for NIR eg PbS and InGaAs

accessories that extend capabilities such as autosamplers thermostat controlled cell holders multicell transports and diffuse and specular reflectance units

calibration procedures for

accuracy of wavelength and absorbance using hydrogendeuterium holmium oxide glass filters and holmium perchlorate solution

stray radiation using recommended liquids for each spectral range

photometric accuracy using potassium dichromate solution

zero absorbance baseline flatness

sources of spectral interferences such as

particulates

fluorescence from heavy metals

interfering chromaphores

masking by chelating agents

computer control software for operating and optimising instrument

procedures for optimising instrument performance such as

alignment of subsystems eg source mirror and accessories

adjustment of slit and signalnoise ratio to obtain satisfactory spectral resolution

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

external calibration with or without internal standardisation

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 UVVISNIR instrument consumables such as lamps and purge gases

install UVVISNIRaccessories such as optical fibre probes microscopes 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 UVVISNIR instruments to measure analytes

feedback from clients peers and supervisors

oral or written questioning of relevant UVVISNIR 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 workplacesetting

Forensic science

A forensic science team is examining some fibre samples taken from a crime scene and a suspect After a careful microscopic examination of the two sets of samples one technician determines that both contain blue polyester fibres Because of the problems associated with extracting dyes from fibres the team decides to first use a nondestructive analytical technique This involves obtaining the UVVIS absorption spectra of single fibres using microspectrophotometry Each fibre is mounted between a quartz slide and cover slip and examined in transmission The laboratorys instrument enables the technician to obtain a several spectra from a x spot for a wavelength range of nm to nm The repeat spectra for each fibre are first compared for internal consistency by overlaying the spectra in pairs The spectra for each fibre are then compared with those obtained for the other fibres and with the reference spectra for a large number of known blue polyester fibres in an international spectral library To provide enhanced discrimination derivative spectra are used to reveal subtle inflections and changes of gradient in the broad convoluted absorption peaks However because of the spatial variations in dye uptake within any one fibre these derivative spectra could not be relied on to provide conclusive identification The team then attempted to measure each fibres birefringence using a polarising microscope and employed a variety of FTIR transmission and reflectance techniques to shed more light on the chemical properties of the two sets of fibres

Food processing

A laboratory technicians manager asks himher to determine the concentration of Vitamin C in a sample of clear apple juice The technician is very familiar with the analytical methods used for determining Vitamin C in bulk pharmaceutical preparations but soon realises that these methods do not give a reliable result in this case Heshe considers alternative spectroscopic methods The technician is aware that the laboratory has a modern UVVIS spectrometer with an advanced spectrum calculator capable of producing up to th order derivative spectra After finding a suitable method the technician determines the Vitamin C content by using the instruments derivative capability to produce sharp peaks and overcome the broad UV absorption bands usually obtained with this kind of sample


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

AS3753-2001 Recommended practice for chemical analysis by ultraviolet/visible spectrophotometry

ISO 22891:2007 Paper - Determination of transmittance by diffuse reflectance measurement

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 (MSDS)

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

UV/VIS/NIR instruments and techniques

UV/VIS/NIR instruments and techniques may include:

peristaltic sample pumps for flow injection analysis and sipper cells

single/double beam instruments and single/double/triple monochromators

discrete analysers for specific analytes

gas, liquid and thermally jacketed cells

fibre optic probes to measure fluorescence from rocks, gems and minerals

diffuse reflectance, (variable angle) specular reflectance accessories

double aperture accessories

rear beam attenuators

tablet dissolution accessories

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

Testing that uses UV/VIS/NIR spectroscopy

Testing that uses UV/VIS/NIR spectroscopy may include:

medical (pathology) testing of whole blood and urine (e.g. phosphates, nitrates and creatine)

forensic testing to establish analyte 'fingerprint' and possible source of scene of crime samples (e.g. paint by specular reflectance)

environmental monitoring of pollution in air, water or soil (e.g. colour and oxidisable organics)

control of starting materials, in-process materials and final products in a wide range of industry sectors (e.g. paper)

food and beverage (e.g. colour and organic compounds), tri-stimulus analysis(determination of food components such as moisture and protein)

pharmaceuticals (e.g. limit tests for active ingredients)

geological testing (e.g. characterisation of rocks, gems and minerals by fluorescence)

Presumptive tests

Presumptive tests may include:

source of sample

type and quantity of sample

assessing suitability of sample and specified preparation for spectroscopic technique

presence of interfering substances

stability of chromophore

Sample and standard preparation

Sample and standard preparation may include:

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

grinding, dissolving, extraction, filtration, refluxing, 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

cell positioning

cell matching

checking integrity and alignment of accessories

wavelength accuracy

detector signal to noise ratio

stray light levels

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. absorption and emission)

wavelength range and start/finish

spectral bandwidth (slit width and signal to noise ratio)

scan speed/fixed wavelength

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

poor selectivity

alignment of external attachments

photo-degeneration and sample instability

Common equipment problems

Common equipment problems may include:

adjustment of optical elements such as mirrors and lamps

alignment of external accessories

cleanliness/optical matching of cells

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, 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