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Evidence Guide: MSL977009A - Apply advanced ultraviolet, visible and near infra red spectroscopic techniques to analysis

Student: __________________________________________________

Signature: _________________________________________________

Tips for gathering evidence to demonstrate your skills

The important thing to remember when gathering evidence is that the more evidence the better - that is, the more evidence you gather to demonstrate your skills, the more confident an assessor can be that you have learned the skills not just at one point in time, but are continuing to apply and develop those skills (as opposed to just learning for the test!). Furthermore, one piece of evidence that you collect will not usualy demonstrate all the required criteria for a unit of competency, whereas multiple overlapping pieces of evidence will usually do the trick!

From the Wiki University

 

MSL977009A - Apply advanced ultraviolet, visible and near infra red spectroscopic techniques to analysis

What evidence can you provide to prove your understanding of each of the following citeria?

Determine sample characteristics and appropriate analytical methods

  1. Interpret client request and/or perform presumptive tests to identify sample characteristics and determine the most appropriate UV/VIS/NIR spectroscopic technique
  2. Liaise with client or sample provider to review client needs, testing requirements and sample history, if necessary
  3. Identify analytical standards, reference materials, test methods and enterprise procedures that may be applicable
  4. Select the most appropriate standard test method that is consistent with testing requirements and instrument availability
  5. If no standard method exists, adapt or modify a test method to suit the sample characteristics
  6. If necessary, seek advice from supervisor about any proposed variations and document all approved changes to test methods
  7. Schedule analysis using enterprise procedures
Interpret client request and/or perform presumptive tests to identify sample characteristics and determine the most appropriate UV/VIS/NIR spectroscopic technique

Completed
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Liaise with client or sample provider to review client needs, testing requirements and sample history, if necessary

Completed
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Identify analytical standards, reference materials, test methods and enterprise procedures that may be applicable

Completed
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Select the most appropriate standard test method that is consistent with testing requirements and instrument availability

Completed
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If no standard method exists, adapt or modify a test method to suit the sample characteristics

Completed
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If necessary, seek advice from supervisor about any proposed variations and document all approved changes to test methods

Completed
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Schedule analysis using enterprise procedures

Completed
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Prepare samples and standards

  1. Log sample into instrument software
  2. Obtain a representative analytical portion of the laboratory sample
  3. Prepare sample in accordance with selected test method
  4. Prepare validation checks and/or calibration standards for analytical portions
Log sample into instrument software

Completed
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Obtain a representative analytical portion of the laboratory sample

Completed
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Prepare sample in accordance with selected test method

Completed
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Prepare validation checks and/or calibration standards for analytical portions

Completed
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Set up instrument and perform trial analysis

  1. Configure the appropriate instrument accessories to perform the selected test method
  2. Perform other pre-use, calibration and safety checks using enterprise procedures
  3. Set instrumental parameters in accordance with those specified in selected test method
  4. Check and optimise each instrument sub-system
  5. Measure analyte response for standards, validation checks and samples
  6. Assess instrument performance in terms of response and resolution
Configure the appropriate instrument accessories to perform the selected test method

Completed
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Perform other pre-use, calibration and safety checks using enterprise procedures

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Set instrumental parameters in accordance with those specified in selected test method

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Check and optimise each instrument sub-system

Completed
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Measure analyte response for standards, validation checks and samples

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Assess instrument performance in terms of response and resolution

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Optimise instrument performance

  1. Adjust instrumental parameters in a logical and efficient sequence to optimise performance
  2. When optimisation is achieved, check that the detector and system software can correctly identify and quantify the required species
Adjust instrumental parameters in a logical and efficient sequence to optimise performance

Completed
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When optimisation is achieved, check that the detector and system software can correctly identify and quantify the required species

Completed
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Perform analysis

  1. Measure analyte response for standards, validation checks and samples using optimised instrument settings
  2. Conduct sufficient measurements to obtain reliable data
  3. Use system software to produce calibration graphs, spectra, confirm data quality and calculate uncertainties
  4. Check that results are consistent with estimations and expectations
  5. Analyse trends in data and/or results and report out of specification or atypical results promptly to appropriate personnel
  6. Return instrument to standby or shutdown condition in accordance with enterprise procedures
  7. Report results with the appropriate accuracy, precision, uncertainty and units
Measure analyte response for standards, validation checks and samples using optimised instrument settings

Completed
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Conduct sufficient measurements to obtain reliable data

Completed
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Use system software to produce calibration graphs, spectra, confirm data quality and calculate uncertainties

Completed
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Check that results are consistent with estimations and expectations

Completed
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Analyse trends in data and/or results and report out of specification or atypical results promptly to appropriate personnel

Completed
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Return instrument to standby or shutdown condition in accordance with enterprise procedures

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Report results with the appropriate accuracy, precision, uncertainty and units

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Perform routine maintenance and troubleshoot instruments

  1. Regularly check the spectral and photometric performance of the instrument
  2. Regularly check and replace sample/waste tubing on peristaltic pump lines as appropriate
  3. Replace lamps and confirm optical matching for cell pairs as necessary
  4. Identify the need for repairs or servicing and determine whether local repair/maintenance is technically possible and economic
  5. Arrange for repair or servicing from an accredited agent or other appropriate personnel in accordance with enterprise procedures
Regularly check the spectral and photometric performance of the instrument

Completed
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Regularly check and replace sample/waste tubing on peristaltic pump lines as appropriate

Completed
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Replace lamps and confirm optical matching for cell pairs as necessary

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Identify the need for repairs or servicing and determine whether local repair/maintenance is technically possible and economic

Completed
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Arrange for repair or servicing from an accredited agent or other appropriate personnel in accordance with enterprise procedures

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Maintain a safe work environment

  1. Identify risks, hazards, safety equipment and control measures associated with sample handling/preparation and test method
  2. Use personal protective equipment and safety procedures specified for test method and materials to be tested
  3. Minimise the generation of wastes and environmental impacts
  4. Ensure the safe collection/disposal of laboratory wastes
  5. Clean, care for and store equipment and consumables in accordance with enterprise procedures
Identify risks, hazards, safety equipment and control measures associated with sample handling/preparation and test method

Completed
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Use personal protective equipment and safety procedures specified for test method and materials to be tested

Completed
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Minimise the generation of wastes and environmental impacts

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Ensure the safe collection/disposal of laboratory wastes

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Clean, care for and store equipment and consumables in accordance with enterprise procedures

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Maintain laboratory records

  1. Enter approved data and results into laboratory information management system (LIMS)
  2. Maintain logs of instrument calibration checks, use and maintenance in accordance with enterprise procedures
  3. Maintain security, integrity and traceability of samples, results and documentation
  4. Communicate results to appropriate personnel in accordance with enterprise procedures
Enter approved data and results into laboratory information management system (LIMS)

Completed
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Maintain logs of instrument calibration checks, use and maintenance in accordance with enterprise procedures

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Maintain security, integrity and traceability of samples, results and documentation

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Communicate results to appropriate personnel in accordance with enterprise procedures

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Assessed

Teacher: ___________________________________ Date: _________

Signature: ________________________________________________

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Instructions to Assessors

Evidence Guide

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 UV/VIS/NIR instrument consumables, such as lamps and purge gases

install UV/VIS/NIRaccessories 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 calibration/qualification status of equipment

optimise instrument sub-systems and procedures and equipment to suit sample/test 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 data/results

troubleshoot common analytical procedure and equipment problems

record and report data/results 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:

MSL976003A Evaluate and select appropriate test methods and procedures

MSL977003A Contribute to the validation of test methods

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 data/results/calibration graphs obtained by the candidate over time to ensure accuracy, validity, precision and timeliness of results

inspection of results and technical records (e.g. maintenance schedules and quality control logbooks) completed by the candidate

observation of candidate using UV/VIS/NIR instruments to measure analytes

feedback from clients, peers and supervisors

oral or written questioning of relevant UV/VIS/NIR 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 and/or 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 non-destructive analytical technique. This involves obtaining the UV/VIS absorption spectra of single fibres using micro-spectrophotometry. Each fibre is mounted between a quartz slide and cover slip and examined in transmission. The laboratory's instrument enables the technician to obtain a several spectra from a 2µ x 2µ spot for a wavelength range of 190 nm to 900 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 fibre's 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 technician's manager asks him/her 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. He/she considers alternative spectroscopic methods. The technician is aware that the laboratory has a modern UV-VIS spectrometer with an advanced spectrum calculator capable of producing up to 4th order derivative spectra. After finding a suitable method, the technician determines the Vitamin C content by using the instrument's derivative capability to produce sharp peaks and overcome the broad UV absorption bands usually obtained with this kind of sample.

Required Skills and Knowledge

Required skills

Required skills include:

establishing client needs for routine and non-routine samples

interpreting client requests, test methods and procedures accurately

selecting appropriate UV/VIS/NIR 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 sample/test requirements

setting up, starting up and shutting down equipment

checking the calibration/qualification status of equipment

selecting, configuring, checking and optimising instrument sub-systems

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 data/results and troubleshooting common analytical procedure and equipment problems

recording and reporting data/results 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 UV/VIS/NIR technique (e.g. cell, accessory) is best suited to which type of sample (e.g. gas, liquid, bulk solid, fibre, film and small quantity)

sample preparation procedures including specialised techniques such as:

handling unstable/hazardous chemicals and samples, fragile/labile biological material

dilution without causing chromaphoric shifts

filtration or centrifugation to remove particulates

prevention of personal contamination of samples by exposure to analyst

cleaning and/or 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

UV/VIS/NIR spectroscopic terms and concepts such as:

excitation, absorption, absorbance, transmittance, reflectance and fluorescence

electronic transitions during absorption/fluorescence and relationship to chemical properties, interference and quenching

concepts such as Beer's Law, Bouguer or Lambert's 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

multi-component analysis

analysis of reaction kinetics

calculations and data processing involving:

concentration and dilution

spectral matching

first and higher derivatives of spectra

multi-component quantitation

operation, construction, selectivity, typical applications, troubleshooting and routine maintenance of UV/VIS/NIR 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 (e.g. PbS and InGaAs)

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

calibration procedures for:

accuracy of wavelength and absorbance using hydrogen/deuterium, 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 sub-systems (e.g. source mirror) and accessories

adjustment of slit and signal-noise ratio to obtain satisfactory spectral resolution

use of manual/computer calibration charts and/or standards to identify and quantify analytes such as:

external calibration with or without internal standardisation

multi-component analysis

semi-quantitative 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 and/or legal traceability requirements

relevant health, safety and environment requirements

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