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Evidence Guide: MSL977006A - Apply specialised knowledge of gas chromatography 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

 

MSL977006A - Apply specialised knowledge of gas chromatography 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 identify sample characteristics that may affect sample preparation and/or analysis
  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 identify sample characteristics that may affect sample preparation and/or analysis

Completed
Date:

Teacher:		 Evidence:

 

 

 

 

 

 

 

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

Completed
Date:

Teacher:		 Evidence:

 

 

 

 

 

 

 

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

Completed
Date:

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

Completed
Date:

Teacher:		 Evidence:

 

 

 

 

 

 

 

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

Completed
Date:

Teacher:		 Evidence:

 

 

 

 

 

 

 

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

Completed
Date:

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Schedule analysis using enterprise procedures

Completed
Date:

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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
  5. Use specialised procedures for ultra trace sample and standard preparation as required
Log sample into instrument software

Completed
Date:

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Obtain a representative analytical portion of the laboratory sample

Completed
Date:

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Prepare sample in accordance with selected test method

Completed
Date:

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Prepare validation checks and/or calibration standards for analytical portions

Completed
Date:

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Use specialised procedures for ultra trace sample and standard preparation as required

Completed
Date:

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Set up instrument and perform trial analysis

  1. Configure the gas flow, injector, column, oven and detector sub-systems according to the selected test method
  2. Perform 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. Select an appropriate internal standard, if required
  6. Conduct performance tests using (internal standards), standards and samples
  7. Assess instrument performance in terms of response, resolution and run-time
Configure the gas flow, injector, column, oven and detector sub-systems according to the selected test method

Completed
Date:

Teacher:		 Evidence:

 

 

 

 

 

 

 

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

Completed
Date:

Teacher:		 Evidence:

 

 

 

 

 

 

 

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

Completed
Date:

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Check and optimise each instrument sub-system

Completed
Date:

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Select an appropriate internal standard, if required

Completed
Date:

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Conduct performance tests using (internal standards), standards and samples

Completed
Date:

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Assess instrument performance in terms of response, resolution and run-time

Completed
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Optimise instrument performance

  1. Apply an understanding of analyte and column chemistry, temperature control and gas flow rate to determine strategies for enhancing separation and detection of required species
  2. Adjust instrumental parameters in a logical and efficient sequence to optimise performance
  3. When optimum separation is achieved, check that the detector and system software can correctly identify and quantify the required species
Apply an understanding of analyte and column chemistry, temperature control and gas flow rate to determine strategies for enhancing separation and detection of required species

Completed
Date:

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Adjust instrumental parameters in a logical and efficient sequence to optimise performance

Completed
Date:

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

Completed
Date:

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Perform analysis

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

Completed
Date:

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Conduct sufficient measurements to obtain reliable data

Completed
Date:

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Regularly check for calibration drift and take appropriate action as necessary

Completed
Date:

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Use system software to produce calibration graphs, chromatographs and/or mass spectra, confirm data quality and calculate uncertainties

Completed
Date:

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Check that results are consistent with estimations and expectations

Completed
Date:

Teacher:		 Evidence:

 

 

 

 

 

 

 

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

Completed
Date:

Teacher:		 Evidence:

 

 

 

 

 

 

 

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

Completed
Date:

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

Completed
Date:

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Perform routine maintenance and troubleshoot instruments

  1. Regularly check the condition of gas cylinders, filters and traps and replace as necessary
  2. Regularly check that the injector, column and detector sub-systems are clean/undamaged and replace consumable items as necessary
  3. Change columns in accordance with manufacturer's instructions and ensure that the system is free of leaks and properly conditioned before re-use
  4. Investigate possible causes for the absence of peaks and presence of ghost peaks, split peaks or distorted peak shapes and apply recommended remedial actions
  5. Investigate possible causes for baseline instability and non-reproducible retention times and apply recommended remedial actions
  6. Identify the need for repairs or servicing and determine whether local repair/maintenance is technically possible and economic
  7. Arrange for repair or servicing from an accredited agent or other appropriate personnel in accordance with enterprise procedures
Regularly check the condition of gas cylinders, filters and traps and replace as necessary

Completed
Date:

Teacher:		 Evidence:

 

 

 

 

 

 

 

Regularly check that the injector, column and detector sub-systems are clean/undamaged and replace consumable items as necessary

Completed
Date:

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Change columns in accordance with manufacturer's instructions and ensure that the system is free of leaks and properly conditioned before re-use

Completed
Date:

Teacher:		 Evidence:

 

 

 

 

 

 

 

Investigate possible causes for the absence of peaks and presence of ghost peaks, split peaks or distorted peak shapes and apply recommended remedial actions

Completed
Date:

Teacher:		 Evidence:

 

 

 

 

 

 

 

Investigate possible causes for baseline instability and non-reproducible retention times and apply recommended remedial actions

Completed
Date:

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

Completed
Date:

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

Completed
Date:

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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
Date:

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

Completed
Date:

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Minimise the generation of wastes and environmental impacts

Completed
Date:

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Ensure the safe collection/disposal of laboratory wastes

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

Completed
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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
Date:

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

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

Completed
Date:

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Communicate results to appropriate personnel in accordance with enterprise procedures

Completed
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Assessed

Teacher: ___________________________________ Date: _________

Signature: ________________________________________________

Comments:

 

 

 

 

 

 

 

 

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

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 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 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 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 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 GC-MS instrument that is capable of quantifying low level pesticides using the SIM mode while simultaneously performing quantification of higher concentrations using full-scan (SIFI single ion and full ion) acquisition. The technician sets up for a typical run of samples. He/she uses the programmable split/splitless injector to provide 1µL samples. The injection port temperature is set at 275°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 30 cm/s. The oven temperature program is initially set to 80°C with no hold and ramped to 290°C at 20°C/min with a hold of 4.5 min. The total oven program is 15 min, with an injection to injection time of less than 20 min. The MS method contains multiple SIM functions overlapped by a m/z 40 to m/z 450 full scan function and the mass spectrometer transfer line and ion source are heated to 275°C.

Pharmaceutical testing

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

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

liquid-liquid extraction, solid-phase micro-extraction, derivatisation and diluting/concentrating

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 (plates/m), 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 pre-treatment of gases, such as drying, use of oxygen/moisture/hydrocarbon traps and filters

operation, construction, typical applications, troubleshooting and routine maintenance of injectorssuch as:

head space sampling

hot direct

split/splitless

solid phase micro-extraction (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 (GC-MS) (GC-MS-MS) using full scan or selective ion monitoring (SIM)

routine quality control procedures such as use of manual/computer calibration charts and/or standards

computer control software for operating and optimising instrument (peak detection and integration, drift parameters, baseline correction and instrument/integrator 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 (e.g. dilution 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

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