Elements and Performance Criteria

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
AS 4873 Set: 2005 Recommended practice for inductively coupled plasma mass spectroscopy (ICP-MS)
ISO 22036: 2008 Soil quality - Determination of trace elements in extracts of soil by inductively coupled plasma atomic emission spectroscopy (ICP-AES)
ISO 11885: 2007 Water quality - Determination of selected elements by inductively methods coupled plasma optical emission spectroscopy (ICP-OES) methods
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
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
ICP instruments and techniques
Inductively coupled plasma instruments and techniques may include:
peristaltic sample pumps
nebulisers (e.g. cross-flow, V-groove, C spray, concentric, micro-concentric and ultrasonic)
spray chambers (temperature and pressure control)
alternative sample introduction systems such as:
laser ablation of solid samples
electrothermal vaporisation (ETV)
flow injection for samples high in total dissolved solids
chromatography (e.g. liquid and ion)
hydride generation
cold vapour mercury generation
plasma torch (RF generation and cooling), radial/axial alignment
plasma gas controls
interface (sample and skimmer cones) and ion lens
mass analysers such as:
quadrupole (peak jump mode, scan mode and single ion monitoring mode)
magnetic sector
time of flight
optical spectrum analysers (diffraction grating)
ion detectors (channeltron, electron multiplier tube and micro channel plate)
photon detectors (photomultiplier tubes and charge coupled devices)
replaceable items, such as valves, tubing and fittings, lamps, vacuum oil and argon gas
data systems, such as recorders, electronic integrators, and software packages for peak detection and integration
Testing that uses ICP spectroscopy
Testing that uses inductively coupled plasma spectroscopy may include:
medical (toxicology) testing of whole blood, urine, plasma, serum, packed red blood cells for:
exposure to heavy metals
metabolic function
forensic testing to establish elemental 'fingerprint' and possible source of scene of crime samples
environmental monitoring of pollution in air, water or soil
monitoring of waste water, sludges and trade effluents
control of starting materials, in-process materials and final products in a wide range of industry sectors (e.g. semi-conductor purity and ultra purity chemical reagents)
materials analysis (e.g. engine wear and oil analysis)
trace elements in food and wine
pharmaceuticals analysis (e.g. metal elements in drug products)
geological testing:
characterisation of rocks and minerals
analysis of mineral/ore samples during exploration, ore processing, final product quality
geochronology isotope ratio measurements
Presumptive tests
Presumptive tests may include:
pH
sample solubility in water and salinity
total dissolved solids
colour test
possible interferences and ion suppressants in sample matrix (e.g. presence of chlorides and chlorates)
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
digestion in nitric acid or aqua regia or hydrogen fluoride for geological samples
microwave digestion
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
preparation of internal standards, such as Indium and/or Gallium
Pre-use, calibration and safety checks
Pre-use, calibration and safety checks may include:
cleanliness of sample/skimmer cones, spray chamber and sample injection/nebuliser orifices
cleanliness of RF coils and quartz tubes
condition of sample and waste tubing on peristaltic pump lines
alignment of torch central tube with sample cone
initial mass calibrations (e.g. He isotopes in air, argon or other gases)
resolution checks
use of Rhodium levels, Cerium/oxide ratios and de-ionised water blanks to test sensitivity and alignment
Instrumental parameters
Instrumental parameters may include:
ICP parameters:
manual/auto sample, pump program, pre- and post-sample washes
sample introduction rate and sample uptake rate
nebuliser/water flow rates
torch gas flow rates
adjustment of plasma temperature to optimise ionisation and minimise interferences (e.g. oxide)
OES/AES detector/source control parameters:
wavelength choice for element sensitivity and/or interference
photomultiplier and charge coupled device
MS parameters:
vacuum pressures and gas flows
sample and skimmer cone alignment
sampling depth (distance between torch and sampling cone tip)
ion optics voltage
mass analyser control
detector settings, such as discriminator voltage, detector high voltage, dead time correction and dual mode/extended range detector calibration
scan, mass start/end, scan time and inter-scan delay
selective ion monitoring (SIM)
Common analytical procedure problems and remedies
Common analytical procedure problems and remedies may include:
lack of suitable reference standards
poor sensitivity
overlapping spectra
nebuliser interferences, such as changes in sample delivery rate, nebuliser efficiency and droplet size
MS polyatomic interferences, reduced by:
cooling the spray chamber to 2-50C
desolvating the aerosol using a condenser and/or semi-permeable membrane
using alternative sample introduction methods
reducing chlorides by using nitric acid digests
adding gases such as H2, N2 and CH4 to the inner, intermediate or outer gases
adding ethanol to the sample to reduce ArCl+
using spectral line fitting software
using cold plasma conditions
using correction equations
using a collision or reaction cell
MS non-spectral (matrix) interferences, reduced by:
matrix matching of calibration and sample solutions
equilibrating test sample solutions to room temperature
removal of dissolved gases from sample solutions
dilution of sample solution
using internal standards (i.e. reference elements)
analyte additions
isotope dilution
Common equipment problems
Common equipment problems may include:
system leaks
efficiency of rotary pump (oil and bearing wear) and turbo/molecular pumps
flat spots in sample/peristaltic pump tubing causing irregular sample or solvent delivery
contamination of sample, solvents, lines or other system elements
build up of salts/dissolved solids in sample valves, torch, MS spray chamber and/or cones
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
toxic fumes and ozone (plasma exhaust)
non-ionising radiation (UV and RF)
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

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 sample introduction and detector sub-systems
install ICP instrument sub-systems such as torch, nebuliser and spray chamber
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 ICP instruments to measure analytes
feedback from clients, peers and supervisors
oral or written questioning of relevant ICP 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 workplace setting.
Food processing
A technician is analysing trace metals in red wine. He/she knows from experience that the ethanol in the wine will extinguish the torch even under standard operating conditions. The technician has four possible remedies:
1. Dilute the sample solution
2. Boil the ethanol off
3. Adjust the torch operating conditions
4. Change the sample introduction equipment.
He/she considers factors such as the number of samples to be analysed and the likely analyte concentrations and searches the literature for recommended remedial actions. The technician decides to start by increasing the torch power from 1.0 to 1.3 KW and tuning the gas flow rates through the torch until the plasma is stable with normal sample introduction.
Environmental testing (1)
A technician receives a series of stream water samples from a client to test for elemental arsenic (As). The client advises the laboratory that they have acidified the samples as per the standard method to preserve the integrity of the sample during transit. Assuming that the client has used HNO3 to bring the pH of the samples down to 1, the technician proceeds with the ICP-MS analysis. However, the technician soon realises that the client has used HCl because there is overwhelming interference between 40Ar35Cl+ and 75As+. The clean up takes a considerable time and to prevent a recurrence of the problem, the laboratory now conducts rapid tests for chlorides in all water samples before ICP-MS analysis.
Environmental testing (2)
A technician receives a telephone call from a client requesting more information about the laboratory's ability to provide ICP-AES multi-element analysis of dry plant material as listed on the company website. The technician explains how the laboratory uses a dry ash method and requires about 500-1000 mg of sample. The technician briefly outlines how the samples are ashed in a silica crucible that is covered to prevent any contamination. The ash is then equilibrated with 5mL of 20% HCl at room temperature for 30 minutes before having 5mL of deionised water added, gently swirled and then allowed to settle for three hours. The solution is then decanted into 15mL plastic disposable tubes for direct determination by ICP-AES. The client mentions that they are particularly interested in the presence of Fe, Al and Cr and the technician notes that in this case, the laboratory usually refluxes the ash in 20% HCl to improve the recovery of these elements. The technician also advises the client that the laboratory reports elemental determinations as ppm on a weight element/dry sample weight basis and that ICP values are expressed on an atomic weight basis, not as any other molecular species.