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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 adapting and modifying standard test methods for unknown samples including consideration of suitable stationary phase support solvent temperature flow rate column type column length and detection

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 and ensuring safe collection and disposal of waste materials

applying relevantprinciples 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

scope of samples that can be tested using gas chromatography GC techniques

sample preparation procedures including specialised techniques such as

handling unstablehazardous chemicals and samples and fragilelabile biological material

liquidliquid extraction solidphase microextraction derivatisation and dilutingconcentrating

GC principles for separation of analytes such as

separation modes chemical structure of stationary phase and its interaction with the analyte

order of elution based on analyte volatility and polarity

predicting effect of condition changes

chromatography concepts and calculations involving

retention times peak widths peak asymmetry capacity factor k and resolution

column selectivity column efficiency platesm optimum flow rate minimum theoretical plate height Van Deemter and related equations

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

types of gases and requirements for purity and pretreatment of gases such as drying use of oxygenmoisturehydrocarbon traps and filters

operation construction typical applications troubleshooting and routine maintenance of injectorssuch as

head space sampling

hot direct

splitsplitless

solid phase microextraction SPME

program temperature vaporisation PTV

gas desorption

purge and trap

on column

choice use and maintenance of syringes

operation construction selectivity sensitivity linear range typical applications troubleshooting and routine maintenance of GC systems including details such as

packed columns

capillary columns including megabore

column conditioning and replacement

gas inlets septum septum purge injector insert heater block tubing materials column connection split valve and vent and compatibility of connectors

checking for leaks and system conditioning

operation construction selectivity sensitivity linear range typical applications troubleshooting and routine maintenance of GC detectors such as

thermal conductivity detectors TCD

flame ionisation detectors FID

electron capture detector ECD

flame photometric detector FPD

mass spectrometry GCMS GCMSMS using full scan or selective ion monitoring SIM

routine quality control procedures such as use of manualcomputer calibration charts andor standards

computer control software for operating and optimising instrument peak detection and integration drift parameters baseline correction and instrumentintegrator zero

procedures for optimising instrument performance such as

investigation of elution order

optimising separation by changing injection technique sample size and sample preparation

effects on instrumental outputs and analytical results by fine tuning injection temperature gas flow rate column pressures and changing column type and detector type

use of temperature flow gradient and pressure programming

steps in identifying and quantifying analytes including relative retention data peak area normalisation and response factors internal standards and spiking

calculation steps eg dilution 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

select operate and maintain a variety of GC injectors columns and detectors

install injectors and columns

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 controllogbooks completed by the candidate

observation of candidate using GC instruments to measure analytes

feedback from clients peers and supervisors

oral or written questioning of relevant gas chromatography concepts chemical principles underpinning sample preparation and separation of speciesinstrument 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

Environmental testing

A laboratory routinely analyses samples of foodstuffs for pesticide residues Traditionally they have used GC combined with ECD and FID detectors to quantify one or two classes at a time Recently the laboratory has commissioned a new GCMS instrument that is capable of quantifying low level pesticides using the SIM mode while simultaneously performing quantification of higher concentrations using fullscan SIFI single ion and full ion acquisition The technician sets up for a typical run of samples Heshe uses the programmable splitsplitless injector to provide L samples The injection port temperature is set at C isothermal and the capillary column uses a phase specifically designed for separation of pesticides The helium carrier gas is programmed with a constant velocity of cms The oven temperature program is initially set to C with no hold and ramped to C at Cmin with a hold of min The total oven program is min with an injection to injection time of less than min The MS method contains multiple SIM functions overlapped by a mz to mz full scan function and the mass spectrometer transfer line and ion source are heated to C

Pharmaceutical testing

A laboratory technician working for a major cosmetics company is given a retail sample of a competitors perfume and asked to determine its composition Heshe has to start somewhere and decides to use one of the laboratorys GCMS instruments to simplify the identification process and to avoid the need for multiple spikes The GCMS is already set up to measure the companys own perfume and so the technician uses standard instrumental parameters as a starting point However heshe finds that many peaks are not resolved and some take a long time to elute The technician realises that heshe should either modify the temperature andor pressure programming or change columns Sensibly the technician chooses to modify the easiest parameter ie temperature before changing the column This overcomes the problem of slow elution but does not resolve all peaks Heshe then varies the pressure programming which provides better resolution but does not completely separate all peaks The technician then uses the instruments spectral matching software to identify as many peaks as possible including the ones that overlap


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 E355 Standard practice for gas chromatography terms and relationships

ASTM E516 Standard practice for testing thermal conductivity detectors used in gas chromatography

ISO 6889 Natural gas rapid analysis by gas chromatography

BS 5443 Recommendations for standard layout for methods of chemical analysis by gas chromatography

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

GC instruments and techniques

GC instruments and techniques may include:

sample introduction, such as:

micro-syringe, split/splitless

head space analysis

thermal desorption

purge and trap

on column injection

packed columns, capillary columns, support coated open tubular (SCOT), wall coated (WCOT) and porous layer (PLOT) types

ovens including temperature stability and temperature programming capability

detectors, such as:

thermal conductivity (TCD)

flame ionisation (FID)

electron capture (ECD

atomic emission (AED)

flame photometric (FPD)

photo ionisation (PID)

fourier transform infra red (FTIR)

'hyphenated' mass spectrometry (GC-MS) (GC-MS-MS)

ionisation - chemical, plasma/glow discharge, electron impact, electro spray, electric field and laser ionisation

design layout - ion cyclotron resonance fourier transform, ion trap, magnetic-sector, quadrupole and time of flight

ion detectors - channeltron, Daly, electron multiplier tube and micro-channel plate

full scan or selective ion monitoring (SIM)

replaceable items, such as gas inlets, septum, septum purge, injector insert, heater block, tubing materials, column connectors, split valve and vent, and lamps

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

Testing that uses GC instruments

Testing that uses GC instruments may include:

forensic testing, such as toxicology of biological samples, identification of fire and explosive residues

medical testing, such as using isotopic labelling of metabolic compounds

testing of athletes for performance enhancing drugs

environmental cleanup and monitoring of pollution in air, water or soil (e.g. organochloride pesticides)

control of starting materials, in-process materials and final products in a wide range of industry sectors (pharmaceuticals, biotechnology, petroleum and manufacturing)

multi-analyte determination

testing for contaminants in food and beverages

analysis of flavour and fragrance

Sample characteristics that may affect analysis

Sample characteristics that may affect analysis may include:

presence of non-volatiles, such as carbohydrates

Sample preparation

Sample preparation may include:

conversion to small volumes (1µL)

derivatisation

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

grinding, dissolving, extraction, filtration, refluxing, centrifuging, evaporation, washing and drying

solid-phase micro-extraction

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

ultra-trace procedures requiring high purity solvents, clean rooms, ultra clean glassware and specialised glassware

Instrumental parameters

Instrumental parameters may include

GC parameters:

injection mode (direct, split/splitless, on column)

manual/auto sample (injector volume, speed and time)

pre- and post-sample washes

gas flow controls

isothermal versus temperature programming

isobaric versus pressure programming

detector/source parameters and single/split system

MS parameters:

vacuum pressures and gas flows

nebuliser gas flow

ionisation control

interface cone alignment

ion lens voltage

mass analyser control

solvent delay

scan, mass start/end, scan time and inter-scan delay

selective ion monitoring (SIM)

Common analytical procedure and equipment problems

Common analytical procedure and equipment problems may include:

system leaks

syringe blockage or incorrect type and inappropriate septum

column overloading

contamination of sample, gas or solvents, lines or other system elements and out gassing of traps

overcoming problems with interfering substances by using SIM

lack of suitable reference standards

poor separation due to inappropriate selection of column or operating parameters (temperature and flow)

poor sensitivity

absence of peaks and presence of ghost peaks, split peaks or distorted peak shapes and broad solvent peaks

baseline instability and non-reproducible retention times

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

hot surfaces

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