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Aquacheck PROFICIENCY SCHEME Scheme Description 2007- 2008 LGC Proficiency Testing Group Aquacheck Scheme Europa Business Park Barcroft Street Bury Lancashire BL9 5BT United Kingdom Telephone: +44 (0) 161 762 2500 Fax: +44 (0) 161 762 2501 Email: [email protected] Website: www.aquacheck.net

LGC, QM and Aquacheck – promoting excellence throug h proficiency testing

of 34 Aquacheck Issue 1 2007

1 Aims of scheme The Aquacheck scheme provides proficiency testing samples and services for the analysis of organic and inorganic chemicals in clean and wastewaters, sludges, sediments and soils. In this way, Aquacheck helps laboratories meet the requirements of accreditation organisations and assists laboratories to optimise their quality control and analytical performance for the benefit of their customers. Participation in Aquacheck provides independent evidence of laboratory performance for both laboratory management and customers. 1.1 Criteria for participation Aquacheck is a world-wide scheme with no restrictions on participation. 2. Scheme Organisation The Aquacheck scheme year operates from April to March. This document sets out the details of the Aquacheck scheme for the period April 2007 to March 2008. Participants can select to receive a set of samples called a ‘Group’. The Distribution Schedule for these Groups is prepared annually and the current Schedule is given in Appendix A. Descriptions of the Groups available on the Scheme for the current year is given in Appendix B. All aspects of the operation of the Aquacheck scheme are provided to participants in the form of a computer Help file which can be accessed from ADARS2 or used as a standalone utility. The Help file and the ADARS2 software are provided free to all participants. Participants are invited to attend the Aquacheck User Group Meetings which are held annually. Further details of these meetings will be sent to all participants in advance. 2.1 Scheme Coordination The scheme is coordinated internally by a team of customer service, technical and administrative personnel. Advice from independent experts is sought where appropriate and a panel of advisers is used for this purpose. 2.2 Timescales Samples are dispatched on the dates specified in the Schedule and laboratories then have approximately 3 weeks in which to analyse the samples and report their results before the specified reporting deadline. The reporting deadline is detailed in the Schedule. 2.3 Frequency of participation Laboratories can join at any time and can choose to participate in as many or as few distributions as they would like. For the purpose of laboratory accreditation and to gain the benefit of trend analysis of bias, participation in all distributions or a minimum of 5 per year is recommended. 3 Test materials In order to provide an accurate a picture as possible of normal laboratory performance, PT samples should be as similar as possible to real samples handled routinely by the laboratory and the laboratory should use their normal procedures in handling and analysing the PT samples. However, real samples are often unstable and may have very low concentrations of the determinands of interest. Therefore, there is a conflict between providing a real sample and providing a sample of sufficient stability, homogeneity and determinand concentration. The Aquacheck scheme has developed its products over a period of nearly 20 years to find an acceptable compromise between these conflicting demands.


Aquacheck offers Groups to suit the following general sample classes;

� Clean waters - suitable for potable waters, river and groundwater � Waste waters - suitable for domestic and industrial waste water � Agricultural soils � Sewage sludge � Ecotoxicology

The use of real samples ensures that matrix effects are fully represented. Where it is not possible to use real samples, we either use a synthetic matrix or use a surrogate material which will at least represent some of the matrix effects likely to occur in real samples. 3.1 Quality Control Aquacheck test materials are prepared using well defined and tested procedures and employing stringent process quality control to ensure adequate homogeneity and stability. Many samples are true solutions and as such by definition are of suitable homogeneity for the purposes of the Scheme. 3.2 Determinands Aquacheck uses the term determinand for “that which is determined in the analysis or test”. Most of the determinands in Aquacheck have been selected because they are important for operational or regulatory purposes. The list of determinands and matrices has expanded in response to requests from customers and is continually evolving in response to changing needs. For non specific determinands, such as Kjeldahl nitrogen, the determinand is operationally defined. We try to select chemicals which most closely meet participants’ needs and inform them how the particular samples are constituted in order to help should they have analytical problems. Most determinands have a published maximum concentration (Max) and samples will normally be provided with concentrations between 20% and 100% of this value. This maximum value is derived either from regulations, when the maximum is set at 1.2 times the standard, or from experience and the requirements of Aquacheck participants. Exceptions to this general rule apply when participants request modified concentration ranges which fit better with their normal samples. For some determinands, where the expected concentration range in samples is wider than 20-100% of the Max value, a specific minimum concentration is also listed. These concentration ranges are indicative only, as occasionally concentrations outside the stated range will be provided, as will occur with real samples. When the Aquacheck samples are based on real samples the concentration range will obviously vary with the sample chosen. In these cases we provide an indication of the likely concentration range or the likely Max values by specifying the historic concentrations in the Group Descriptions in Appendix B. Some Aquacheck Groups are designed to assess laboratory performance in the detection and identification of problems and contaminants in water. Such Groups are referred to as Qualitative Groups. In 2007/8 the Qualitative Groups are Groups 22, 22A and 25. The more usual Groups involve quantification of defined contaminant levels, these Groups are referred to as Quantitative Groups.


The determinands, normal concentration ranges and the precise materials provided are listed in the Group Descriptions (Appendix B). 3.3 Methods of analysis Aquacheck publishes “standard deviations for proficiency test performance” as error target thresholds. Participants may use any analytical method they believe meets these performance targets. In some cases the test methods are specified in more detail to ensure comparability of results. 4 Participant Results Participants are all given free software to enter, return and store their results and the performance assessments provided by Aquacheck. This software is known as ADARS2. Results can also be returned using a spreadsheet provided to all participants. 4.1 Reporting format Participants report a single result to Aquacheck for each determinand. This result must be reported in the units specified by Aquacheck. However ADARS2 contains a simple unit conversion facility and it also allows replicate determinations to be entered for calculation of the simple mean as the result returned to Aquacheck. Participants are encouraged to report actual measured values and to report data to 3 significant figures. We will accept < values but do not use such values in any aggregate statistics or report any Z-scores for such data returns. We will flag < values in the following cases

� If the reported less than value is smaller than the Reference value by more than three times the error target threshold. For example, if the reported value <X is such that had X been reported it would have been awarded a Z score of less than -3 then the <X result will be single flagged with no Z score awarded.

� If the reported value is greater than the highest concentration normally used in the sample (i.e. the Max value) the result will be flagged because the method used is clearly not appropriate for this type of sample. For example if the reported value is <X and the Max value is M then if X>M the result is single flagged but no Z score is awarded.

We will not allow a single 0 (zero) as a valid data return because some participants have started to use 0 as a not analysed response which can bias the statistics. If labs wish to return a zero result they should use 0.0. 4.2 Reference (Assigned) value After the scheme round has closed, all results are collated, the data is then analysed and the assigned value is determined. This is the value assigned by Aquacheck as being the correct or target value for the sample in question. The source of assigned values to be used is detailed in Appendix B. Any deviations from this will be accounted for and explained in reports provided to participants. An Aquacheck Z-score for each participant result is then calculated. The Aquacheck Z-score is a performance score which compares the difference between each participants result and the assigned value in terms of the acceptable spread of results or error target thresholds. Thus: Z = x – X Where: x = participant result s X = assigned value s = target error threshold


Assigned values based on the median of reported results will be fixed at the time of reporting so late results do not affect Z-scores. The estimated relative standard uncertainty for median assigned values is calculated by the robust rsd divided by the square root of the number of labs reporting. For Spike assigned values, the various stages of sample formulation are used to estimate, by simulation, the standard uncertainty. As an initial target we are revising all sample preparation procedures to ensure that the standard relative uncertainty of all spike assigned values is less than 3%, based on ISO 13528 (2005) which has an acceptance criterion for the stability and homogeneity of PT samples of 3% and therefore seems an acceptable value to use initially. 4.3 Performance assessment 4.3.1 Target error thresholds Aquacheck sets target error thresholds for all determinands based on the expected purpose of the analyses. This means there are fixed criteria against which the results of laboratories are judged and, in principle, all laboratories could either pass or fail in a given test. Aquacheck provides assessments of results against these criteria but also allows participants to establish their own criteria and to evaluate results against these criteria, using the ADARS2 software provided. It is the practice in Aquacheck to flag results which exceed the target error thresholds in order to draw them to the attention of participants. In order to comply with current practice in proficiency testing the approach used to set target error thresholds is as follows:

� Thresholds are defined as a maximum percentage error (P) and as a fixed value (C). The larger of these two thresholds is applied in calculation of the Aquacheck Z-Score. This is to allow for the fact that at concentrations low in the range of interest a percentage threshold is unnecessarily demanding. Commonly, the threshold used is either 10% of the assigned value or one twentieth of the relevant quality limit, for example, an Environmental Quality Standard. With P at 10% and a quality limit value of 1.0, the fixed error threshold of 1.0/20 = 0.05 will apply at concentrations below 0.5.

� The threshold is set at a value which is half the error considered to be the maximum tolerable for fitness for purpose. Thus, the above thresholds of 10% or 0.05 would correspond to flags being applied to reported results which were in error by more than 20% or 0.1 concentration units.

4.3.2 Flagging of results In order to draw attention to unsatisfactory or questionable results based on the Z-scores a flagging system will be used in reports. A single flag is attached to laboratory results with Z-Scores greater than or equal to 2.00 or less than or equal to -2.00 and two or double flags are attached to results greater than or equal to 3.01 and less than or equal to -3.01. Flagged results exceed the error thresholds assigned by Aquacheck and the analytical process for these determinands therefore deserves consideration by the laboratory producing the results. Flagged determinands are designated by flag symbols in the Laboratory Report ( ) and double flagged results are designated by ( ) in Laboratory Reports. In some cases, flagging is suspended for a particular determinand in a distribution. In this case the determinand has an exclamation mark printed beside it in the laboratory report regardless of

the laboratory Z-Score ( )


4.3.3 Suspension of flagging In 2007/8 flagging for determinands based on median of laboratories will be suspended automatically if the estimated uncertainty of the median reference value of a determinand is greater than the error threshold which applies at the median concentration. In other cases all flagging suspensions will be justified and the technical reasons for the action taken explained in the report. Also, flagging will be suspended for all determinands that use an assigned value based on a median of results when there are less than 5 results because of the uncertainty associated with the estimation of the median. For determinands based on a median with numbers of results between 5 and 7 flagging will be suspended if there are any flagged results present. Participants should always be wary of median assigned values that are based on small numbers of results. When the number of results is less than 8 and the assigned value is based on the median of reported results participants should always be aware that a good Z-score might only indicate reasonable comparability with other labs. 4.4 Reports Reports are issued by Aquacheck within 4 working days of the reporting deadline. Reports are issued using the Aquacheck reporting software ADARS. Paper and PDF reports are available on request at an extra charge.

Appendix A

Aquacheck Distribution Schedule

2007/2008

Renewal Grid

Dist Distribution Date Reporting Deadline Ecotox

324 23 April 2007 11 May 2007 4G 5G 6A 6B 6C 7A 7B 7C 7D 8 9 22 22A 25

325 8 May 25 May 1 2 2A 3 4 5 5A 5B 5C 14

326 21 May 8 June 1A 3A 3B 6A 6C 7A 7B 7C 7D 8 9 18A 18B 18C 19A 19B 19C 19D 20 20A 21 50

327 4 June (5th Eire) 22 June 10 11 12 12C 17A 17B 17C 17D 13

328 18 June 6 July 6A 6C 7A 7B 7C 7D 8 8B 9 22 25

329 16 July 3 August 1 2 3 4 5 5B 5C 14

330 30 July 17 August 1A 3A 3B 6A 6C 7A 7B 7C 7D 8 9 18A 18C 19A 19B 19C 19D 20 20A 21 50

331 13 August 31 August 10 11 12 12C 17A 17B 17C 17D 13

332 28 August 14 September 6A 6C 7A 7B 7C 7D 8 8B 9 22 25

333 10 September 28 September 1 2 2A 3 4 5 5A 5B 5C 14

334 24 September 12 October 1A 3A 3B 6A 6C 7A 7B 7C 7D 8 9 18A 18B 18C 19A 19B 19C 19D 20 20A 21 50

335 8 October 26 October 10 11 12 12C 17A 17B 17C 17D 13

336 22 October 9 November 4G 5G 6A 6B 6C 7A 7B 7C 7D 8 9 22 22A 25

337 5 November 23 November 1 2 3 4 5 5B 5C 14

338 19 November 7 December 1A 3A 3B 6A 6C 7A 7B 7C 7D 8 9 18A 18C 19A 19B 19C 19D 20 20A 21 50

339 3 December 11 January 2008 10 11 12 12C 17A 17B 17C 17D 13

340 14 January 2008 1 February 4G 5G 6A 6B 6C 7A 7B 7C 7D 8 8B 9 22 22A 25

341 28 January 15 February 1 2 2A 3 4 5 5A 5B 5C 14

342 11 February 29 February 1A 3A 3B 6A 6C 7A 7B 7C 7D 8 9 18A 18B 18C 19A 19B 19C 19D 20 20A 21 50

343 25 February 14 March 10 11 12 12C 17A 17B 17C 17D 13

New GroupsMaximum number of distributions is three

CONTEST Contaminated Land PT scheme. Register through Aquacheck. For more information please contact AquacheckMaterials Not Available

April 2007-March 2008

Soils & Sludge

CONTEST

Clean Waters Waste Waters

Sample Type & Groups Included

CONTEST

CONTEST

CONTEST

CONTEST

Appendix B

Description of Aquacheck Groups

2007/2008


1. The Aquacheck Scheme Groups

An Aquacheck Group comprises of a set of samples of defined determinands in specified matrices. Where possible, the Groups are provided as made-up samples, ready for analysis. However, in some cases, sample instability is too great so the determinand is provided in a preserved spiking solution with instructions on sample preparation. The following information indicates the determinands offered along with details on the assigned value source, concentration ranges, error thresholds and reporting units for each determinand. 2. Aquacheck Matrices Groups 1-5B use a filtered river water matrix as such it is suitable for drinking water and surface water matrices. Customers are required to choose between hard and soft water options for Groups 1 and 2 and specify the choice for each sample distribution. Groups 4G and 5G will be provided in a groundwater matrix. Groups 6-9 are offered with a groundwater matrix to which the spiking solutions are added, by the participant, before sample analysis. This matrix is suitable for drinking and surface water analyses. Waste water groups are supplied with a waste water matrix solution to which the spiking solutions are added. This solution has been designed to be representative of sewage treatment plant effluents in relation to the substances which may interfere with analytical procedures, but to have good medium term stability. It is a synthetic solution made up in Deionised Water and contains organic material, nutrients and salts at levels considered to be typical of such waste waters. The solution is acidified to aid sample stability. The waste water matrix will be provided at 4 different concentrations during 2007/8 to provide customers with a more realistic varying matrix. The spiking solution provided in distributions where both clean and waste water organic groups are offered will be the same for corresponding groups. The difference between the samples will be in the matrix water supplied and the laboratory instructions participants are required to follow. For example, for Groups 6A and 18A in the same distribution, the spiking solutions will be prepared with the same concentrations of determinands. Participants ordering both groups should be aware of this. All inorganic spiking solutions are prepared in Deionised Water. The metal groups are provided in 0.5% acidified solutions. All organic solutions are provided in Methanol, Deionised Water or Dichloromethane (see the Group instructions in ADARS2 Help).


3. Abbreviations Used in Group Descriptions Assigned Value (Asg Value) M denotes that the median of laboratory results will be used as the assigned value and S denotes the use of an assigned value derived from sample preparation. Max This indicates the maximum concentration normally supplied for this determinand. The minimum value will usually be 20% of the maximum value. Where a range of values different from the 20-100% maximum is used, this is quoted as a Range in the Group Contents table. C Value This indicates the fixed error threshold for the determinand. This is usually set at a level which is half the limit of detection considered to be appropriate for these determinands in the type concerned. The Percentage Error Threshold (P Value) is generally 10%. Any exceptions to the 10% values are specifically noted in the C Value column of the group description table as, for example, P=0%. Units This indicates the Aquacheck units for the determinand. These are the units in which participants should report their results. CAS Numbers CAS Numbers are unique numerical identifiers for chemical compounds. They have been provided for some groups whose determinands may have names which are ambiguous.


Index to Description of Aquacheck Groups

Group Name of Group Page 1H Major Inorganic Components (Hard Water) 13 1S Major Inorganic Components (Soft Water) 13 1A Major Ions in Higher Salinity Water 14 2H Nutrients and Others (Hard Water) 14 2S Nutrients and Others (Soft Water) 15 2A pH in Poorly Buffered Waters 15 3 Non Specific Determinands 15 3A Inorganic Disinfection By-products 16 3B Free chlorine 16 4 Metals (Preserved in 0.5% Nitric Acid) 16 4G Metals in Groundwater (Preserved in 0.5% Nitric Acid) 17 5 Toxic Metals (Preserved in 0.5% Nitric Acid) 17 5C Chromium (VI) clean water 17 5G Toxic Metals in Groundwater(Preserved in 0.5% Nitric Acid) 18 5A Metals for Hydride Generation (Preserved in 0.5% Hydrochloric Acid) 18 5B EQS Metals (Preserved in 0.5% Nitric Acid) 18 6A Haloforms and Chlorinated Solvents 19 6B Phenols 19 6C Benzene, Toluene and Xylenes 19 7A Organochlorine Pesticides 20 7B Chlorinated Solvents 20 7C1 Polycyclic Aromatic Hydrocarbons (1 Spike) 20 7C2 Polycyclic Aromatic Hydrocarbons (2 Spikes) 21 7D Polychlorinated Biphenyls 21 8 Triazines, Urons and Acid Herbicides 22 8B Newer herbicides 22 9 Organophosphorus Pesticides 23 10 Nutrients 23 11 Non Specific Determinands 23 12 Metals (Preserved in 0.5% Nitric Acid) 24 12C Chromium (VI) in waste water 24 13 Sewage Sludge Inorganics 25 14 Agricultural Soil Inorganics 26 17A Major waste water determinands 27 17B Total Phenol, Cyanide and Sulphate 27 17C Metals (Preserved in 0.5% Nitric Acid) 27 17D Ammonia, Phosphate and Nitrogen 28 18A Haloforms and Chlorinated Solvents 28 18B Phenols 28 18C Benzene, Toluene and Xylenes 29 19A Organochlorine Pesticides 29 19B Chlorinated Solvents 29 19C1 Polyaromatic Hydrocarbons (1 Spike) 30 19C2 Polyaromatic Hydrocarbons (2 Spikes) 30 19D Polychlorinated Biphenyls 31 20 Triazines, Urons and Acid Herbicides 31 20A Mineral Oil 32 21 Organophosphorus Pesticides 32 22 Qualitative Organics by GCMS 33 22A Qualitative Organics by Purge and Trap GCMS 33 25 Qualitative Determination in Clean Water 33 50 Ecotoxicology Tests 34


Description of Aquacheck Groups Group 1H Major Inorganic Components (in Hard Water) Participants will receive: 2 x 1L Hard Water Sample

2 x 30ml Samples (Kjeldahl Nitrogen & Total Phosphorous) Determinand Asg Value Range C Value Units Calcium M 70-110 1 mg Ca/l Magnesium M 2-10 0.25 mg Mg/l Total Hardness M 50-120 3 mg Ca/l Alkalinity M 150-300 1.5 mg HCO3/l Potassium M 1-3 0.25 mg K/l Sodium M 10-25 0.25 mg Na/l Chloride M 20-45 1 mg Cl/l Sulphate M 10-35 1 mg SO4/l Fluoride M 1800 75 µg F/l Conductivity (20C) M 300-540 5 µS/cm Kjeldahl Nitrogen S 5 0.05 mg N/l Total Phosphorus M 2.6 0.025 mg P/l Barium M 20-180 5 µg Ba/l

This Group uses real water samples and the values given above are indicative, based on the range of waters used in the past. Single values in this table are maximum values. Group 1S Major Inorganic Components (in Soft Water) Participants will receive: 2 x 1L Soft Water Sample

2 x 30ml Samples (Kjeldahl Nitrogen & Total Phosphorous) Determinand Asg Value Range C Value Units Calcium M 6-30 1 mg Ca/l Magnesium M 0.5-6 0.25 mg Mg/l Total Hardness M 6-40 3 mg Ca/l Alkalinity M 15-90 1.5 mg HCO3/l Potassium M 0.3-4 0.25 mg K/l Sodium M 5-30 0.25 mg Na/l Chloride M 5-45 1 mg Cl/l Sulphate M 3-40 1 mg SO4/l Fluoride M 1800 75 µg F/l Conductivity (20C) M 100-400 5 µS/cm Kjeldahl Nitrogen S 5 0.05 mg N/l Total Phosphorus M 2.6 0.025 mg P/l Barium M 20-100 5 µg Ba/l

This Group uses real water samples and the values given above are indicative, based on the range of waters used in the past. Single values in this table are maximum values.


Group 1A Major Ions in Higher Salinity Potable Water Participants will receive: 1 x 1L Spiked Matrix Water Sample

1 x 25ml TOC Sample 1 x 500ml pH Sample

Determinand Asg Value Max C Value Units Sodium S 240 0.5 mg Na/l Magnesium S 60 0.25 mg Mg/l Chloride S 300 2.5 mg Cl/l Sulphate S 300 2.5 mg SO4/l pH M Range 4-10 0.1 (P=0%) pH unit Conductivity (20C) M 3000 5 µS/cm Total organic carbon (TOC) M 10 0.25 mg C/l Total Dissolved Solids (180C) M 2000 10 mg/l

Group 2H Nutrients and Others (in Hard Water) Participants will receive: 1 x 1L Hard Water Sample

7 x 30ml Samples (Nitrite, Ammonia, SR Phosphate, Colour, PI, Total Cyanide, Free Cyanide)

1 x 500ml pH Sample Determinand Asg Value Range C Value Units Total oxidised nitrogen (TON) M 10-25 0.1 mg NO3/l Silicate M 5-25 0.1 mg SiO2/l Nitrite S 0.35 0.005 mg NO2/l Ammonia M 0.6 0.025 mg NH4 /l Soluble reactive phosporus M 2600 10 µg P/l pH at 20-25C M 4-10 0.1 (P=0%) pH unit Colour S 24 1 Hazen Permanganate index (PI) S 6 0.25 mg O2/l Total Cyanide S 60 2.5 µg CN/l Free Cyanide S 60 2.5 µg CN/l Nitrate M 10-25 0.1 mg NO3/l Total Dissolved Solids (180C) M 1000 10 mg/l

This Group uses real water samples and the values given above are indicative, based on the range of waters used in the past. Single values in this table are maximum values.


Group 2S Nutrients and Others (in Soft Water) Participants will receive: 1 x 1L Soft Water Sample

8 x 30ml Samples (Nitrite, Nitrate, Ammonia, SR Phosphate, Colour, PI, Total Cyanide, Free Cyanide)

1 x 500ml pH Sample Determinand Asg Value Range C Value Units Total oxidised nitrogen (TON) M 0.3-15 0.1 mg NO3/l Silicate M 4-10 0.1 mg SiO2/l Nitrite S 0.35 0.005 mg NO2/l Ammonia M 0.6 0.025 mg NH4 /l Soluble reactive phosporus M 2600 10 µg P/l pH at 20-25C M 4-10 0.1 (P=0%) pH unit Colour S 24 1 Hazen Permanganate index (PI) S 6 0.25 mg O2/l Total Cyanide S 60 2.5 µg CN/l Free Cyanide S 60 2.5 µg CN/l Nitrate S 1-30 0.1 mg NO3/l Total Dissolved Solids (180C) M 1000 10 mg/l

This Group uses real water samples and the values given above are indicative, based on the range of waters used in the past. Single values in this table are maximum values. Group 2A pH in Poorly Buffered Waters Participants will receive: 2 x 500ml pH Samples Determinand Asg Value Range C Value Units pH at 20-25C -Low See below 3-5 0.1 (P=0%) pH unit pH at 20-25C -High See below 6-9 0.1 (P=0%) pH unit

The Reference value used will depend on the sample. If the sample has been well characterized we may use a published reference value, otherwise it will be the median of reported values. Group 3 Non-Specific Determinands Participants will receive: 5 x 30ml Samples (BOD, COD, Suspended Solids, MBAS,

Turbidity) 1 x 25ml Sample (DOC)

Determinand Asg Value Max C Value Units BOD (5 day) S Range 1-6 0.25 mg O2/l COD S 250 10 mg O2/l Suspended solids M 30 1 mg/l Methylene blue active substances (MBAS)

S 240 10 µg LS/l

Dissolved organic carbon S 5 0.5 mg C/l Turbidity M 4.8 0.2 NTU


Group 3A Inorganic Disinfection By-products Participants will receive: 3 x 30ml Samples (Chlorate/Chlorite, Bromide, Bromate) Determinand Asg Value Max C Value Units Bromide S 100 2.5 µg Br/l Bromate S 12 0.5 µg BrO3/l Chlorate S 100 2.5 µg ClO3/l Chlorite S 100 1.5 µg ClO2/l

Group 3B Free Chlorine Participants will receive: 1 x 500ml Matrix Water Sample 1 x 10ml Free Chlorine Spiking Solution Determinand Asg Value Max C Value Units Free Chlorine M 0.5 0.03 mgCl2/l

Group 4 Metals (Preserved in 0.5% Nitric Acid) Participants will receive: 1 x 500ml Metals Sample (all determinands except silver)

1 x 30ml Silver Sample Determinand Asg Value Max C Value Units Iron M 240 10 µg/l Manganese M 60 2.5 µg/l Copper M 500 5 µg/l Aluminium M 240 10 µg/l Zinc M 500 5 µg/l Silver M 12 0.5 µg/l Barium M 500 50 µg/l Boron M 1200 50 µg/l Strontium M 500 50 µg/l Lithium M 50 5 µg/l


Group 4G Metals in groundwater (Preserved in 0.5% Nitric Acid) Participants will receive: 1 x 500ml Metals Sample (all determinands except silver)

1 x 30ml Silver Sample Determinand Asg Value Max C Value Units Iron M 1000 10 µg/l Manganese M 100 2.5 µg/l Copper M 50 1 µg/l Aluminium M 100 5 µg/l Zinc M 30 1 µg/l Silver M 10 0.5 µg/l Barium M 500 50 µg/l Boron M 500 50 µg/l Strontium M 500 50 µg/l Lithium M 50 5 µg/l

Group 5 Toxic Metals (Preserved in 0.5% Nitric Acid) Participants will receive: 1 x 500ml Metals Sample (all determinands except mercury and tin)

1 x 30ml Mercury Sample 1 x 30ml Tin Sample

Determinand Asg Value Max C Value Units Cadmium M 6 0.25 µg/l Lead M 25 0.5 µg/l Nickel M 24 1 µg/l Selenium M 12 0.5 µg/l Arsenic M 12 0.5 µg/l Antimony M 6 0.25 µg/l Mercury M 1.2 0.05 µg/l Cobalt M 25 1 µg/l Vanadium M 25 1 µg/l Chromium M 60 2.5 µg/l Molybdenum M 25 2.5 µg/l Tin M 100 1 µg/l Beryllium M 5 0.25 µg/l

Group 5C Chromium (VI) in clean water Participants will receive: 1 x 30ml Spiking Solution Determinand Asg Value Max C Value Units Chromium (VI) S 20 0.5 µg/l


Group 5G Toxic Metals in groundwater (Preserved in 0.5% Nitric Acid) Participants will receive: 1 x 500ml Metals Sample (all determinands except mercury and tin) 1 x 30ml Mercury Sample

1 x 30ml Tin Sample Determinand Asg Value Max C Value Units Cadmium M 5 0.25 µg/l Lead M 50 0.5 µg/l Nickel M 20 1 µg/l Selenium M 5 0.5 µg/l Arsenic M 10 0.5 µg/l Antimony M 5 0.25 µg/l Mercury M 5 0.05 µg/l Cobalt M 10 1 µg/l Vanadium M 10 1 µg/l Chromium M 25 2.5 µg/l Molybdenum M 25 2.5 µg/l Tin M 20 1 µg/l Beryllium M 10 1 µg/l

Group 5A Metals for Hydride Generation (Preserved in 0.5% Hydrochloric Acid) Participants will receive: 1 x 500ml Metals Sample (all determinands) Determinand Asg Value Max C Value Units Arsenic See below 12 0.5 µg/l Selenium See below 12 0.5 µg/l Antimony See below 6 0.25 µg/l Tin See below 100 1 µg/l

A median reference value will be used unless to do so would mean that flagging would be suspended in which case the Spike value will be used as a Reference value. Group 5B EQS Metals (Preserved in 0.5% Nitric Acid) Participants will receive: 1 x 500ml Metals Sample (all determinands except mercury)

1 x 30ml Mercury Sample Determinand Asg Value Max C Value Units Cadmium M 1 0.05 µg/l Copper M 5 0.05 µg/l Total Chromium M 2.5 0.1 µg/l Lead M 2.5 0.1 µg/l Nickel M 12.5 2.5 µg/l Zinc M 10 0.5 µg/l Vanadium M 10 1 µg/l Mercury M 0.5 0.05 µg/l


Group 6A Haloforms and Chlorinated Solvents Participants will receive: 1 x 2L Groundwater Sample

1 x 10ml Spiking Solution Determinand Asg Value Max C Value Units Chloroform S 120 2.5 µg/l Bromodichloromethane S 120 2.5 µg/l Dibromochloromethane S 120 2.5 µg/l Bromoform S 120 2.5 µg/l Trichloroethene S 12 0.5 µg/l Tetrachloroethene S 12 0.5 µg/l Carbon Tetrachloride S 3.6 0.15 µg/l 1,2 dichloroethane S 3.6 0.15 µg/l

Group 6B Phenols Participants will receive: 1 x 2LGroundwater Sample

1 x 10ml Spiking Solution Determinand Asg Value Max C Value Units Pentachlorophenol S 600 25 ng/l Trichlorophenol S 600 25 ng/l Phenol S 600 25 ng/l 2-Chlorophenol S 600 25 ng/l 4-Chlorophenol S 600 25 ng/l 2,4-Dichlorophenol S 600 25 ng/l

Group 6C Benzene, Toluene and Xylenes Participants will receive: 1 x 2L Groundwater Sample

1 x 10ml Spiking Solution Determinand Asg Value Max C Value Units Benzene S 1.2 0.05 µg/l Toluene S 3 0.05 µg/l Ethylbenzene S 3 0.05 µg/l Styrene S 3 0.05 µg/l o-xylene S 3 0.05 µg/l m-xylene S 3 0.05 µg/l p-xylene S 3 0.05 µg/l Total xylene S 9 0.15 µg/l m- + p-xylene S 6 0.1 µg/l


Group 7A Organochlorine Pesticides Participants will receive: 1 x 2L Groundwater Sample

1 x 10ml Spiking Solution Determinand CAS No. Asg Value Max C Value Units Endrin 72-20-8 S 120 5 ng/l Dieldrin 60-57-1 S 50 1.5 ng/l Aldrin 309-00-2 S 50 1.5 ng/l pp’ DDT 50-29-3 S 120 5 ng/l Lindane 58-89-9 S 120 5 ng/l Trifluralin 1582-09-8 S 120 5 ng/l Alpha Endosulphan 959-98-8 S 120 5 ng/l Beta Endosulphan 33213-65-9 S 120 5 ng/l Hexachlorobenzene 118-74-1 S 120 5 ng/l Heptachlor 76-44-8 S 50 1.5 ng/l Heptachlor epoxide 1024-57-3 S 50 1.5 ng/l Pentachlorobenzene 608-93-5 S 120 5 ng/l

Group 7B Chlorinated Solvents Participants will receive: 1 x 2L Groundwater Sample

1 x 10ml Spiking Solution Determinand Asg Value Max C Value Units Hexachlorobutadiene S 400 25 ng/l CarbonTetrachloride S 400 25 ng/l Tetrachloroethene S 400 25 ng/l 1,2,4 Trichlorobenzene S 400 25 ng/l Trichloroethene S 400 25 ng/l 1,1,1-Trichloroethane S 400 25 ng/l 1,3,5-Trichlorobenzene S 400 25 ng/l 1,2,3-Trichlorobenzene S 400 25 ng/l 1,2-Dichloroethane S 400 25 ng/l Chloroform S 400 25 ng/l

Group 7C1 Polycyclic Aromatic Hydrocarbons (1 Spike) Participants will receive: 1 x 2L Groundwater Sample 1 x 10ml Spiking Solution Determinand CAS No. Asg Value Max C Value Units Fluoranthene 206-44-0 S 50 2 ng/l Benzo(b)fluoranthene 205-99-2 S 25 2 ng/l Benzo(k)fluoranthene 207-08-9 S 25 2 ng/l Benzo(a)pyrene 50-32-8 S 12 0.5 ng/l Benzo(ghi)perylene 191-24-2 S 25 2 ng/l Indeno(1,2,3-cd)pyrene 193-39-5 S 25 2 ng/l


Group 7C2 Polycyclic Aromatic Hydrocarbons (2 Spikes) Participants will receive: 1 x 2L Groundwater Sample 2 x 10ml Spiking Solutions Spiking solution 7C1 Determinand CAS No. Asg Value Max C Value Units Fluoranthene 206-44-0 S 50 2 ng/l Benzo(b)fluoranthene 205-99-2 S 25 2 ng/l Benzo(k)fluoranthene 207-08-9 S 25 2 ng/l Benzo(a)pyrene 50-32-8 S 12 0.5 ng/l Benzo(ghi)perylene 191-24-2 S 25 2 ng/l Indeno(1,2,3-cd)pyrene 193-39-5 S 25 2 ng/l

Spiking solution 7C2 Determinand CAS No. Asg Value Max C Value Units Acenaphthene 83-32-9 S 25 2 ng/l Acenaphthylene 208-96-8 S 25 2 ng/l Anthracene 120-12-7 S 25 2 ng/l Benz(a)anthracene 56-55-3 S 25 2 ng/l Chrysene 218-01-9 S 25 2 ng/l Dibenz(ah)anthracene 53-70-3 S 25 2 ng/l Fluorene 86-73-7 S 25 2 ng/l Naphthalene 91-20-3 S 25 2 ng/l Perylene 198-55-0 S 25 2 ng/l Phenanthrene 85-01-8 S 25 2 ng/l Pyrene 129-00-0 S 25 2 ng/l

Group 7D Polychlorinated Biphenyls Participants will receive: 1 x 2LGroundwater Sample

1 x 10ml Spiking Solution Determinand CAS No. Asg Value Max C Value Units PCB (28) 7012-37-5 S 100 1 ng/l PCB (52) 35693-99-3 S 100 1 ng/l PCB (101) 37680-73-2 S 100 1 ng/l PCB (118) 31508-00-6 S 100 1 ng/l PCB (138) 35065-28-2 S 100 1 ng/l PCB (153) 35065-27-1 S 100 1 ng/l PCB (180) 35065-29-3 S 100 1 ng/l


Group 8 Triazines, Urons and Acid Herbicides Participants will receive: 1 x 2LGroundwater Sample

2 x 10ml Spiking Solutions Spiking solution 8(1) Determinand CAS No. Asg Value Max C Value Units Simazine 122-34-9 S 120 5 ng/l Atrazine 1912-24-9 S 120 5 ng/l Propazine 139-40-2 S 120 5 ng/l MCPA 94-74-6 S 120 5 ng/l MCPB 94-81-5 S 120 5 ng/l Mecoprop 7085-19-0 S 120 5 ng/l 2,4 D 94-75-7 S 120 5 ng/l Isoproturon 34123-59-6 S 120 5 ng/l Diuron 330-54-1 S 120 5 ng/l Linuron 330-55-2 S 120 5 ng/l Chlortoluron 15545-48-9 S 120 5 ng/l Bentazone 25057-89-0 S 120 5 ng/l

Spiking solution 8(2) Determinand CAS No. Asg Value Max C Value Units Glyphosate 1071-83-6 S 120 5 ng/l

Group 8B Newer herbicides Participants will receive: 1 x 2LGroundwater Sample

2 x 10ml Spiking Solutions Spiking solution 8B(1) Determinand CAS Number Asg Value Max C Value Units Monuron 150-68-5 S 120 5 ng/l Propyzamide 23950-58-5 S 120 5 ng/l Ioxynil 1689-83-4 S 120 5 ng/l Bromoxynil 1689-84-5 S 120 5 ng/l

Spiking solution 8B2 Determinand CAS Number Asg Value Max C Value Units Dichlorprop 120-36-5 S 120 5 ng/l Dicamba 1918-00-9 S 120 5 ng/l 2,4-DB 94-82-6 S 120 5 ng/l Trichlopyr 55335-06-3 S 120 5 ng/l


Group 9 Organophosphorus Pesticides Participants will receive: 1 x 2LGroundwater Sample

1 x 10ml Spiking Solution Determinand CAS No. Asg Value Max C Value Units Azinphos-methyl 86-50-0 S 120 5 ng/l Azinphos-ethyl 2642-71-9 S 120 5 ng/l Dichlorvos 62-73-7 S 120 5 ng/l Fenitrothion 122-14-5 S 120 5 ng/l Malathion 121-75-5 S 120 5 ng/l Mevinphos 7786-34-7 S 120 5 ng/l Chlorfenvinphos 470-90-6 S 120 5 ng/l Diazinon 333-41-5 S 120 5 ng/l Fenthion 55-38-9 S 120 5 ng/l Parathion-ethyl 56-38-2 S 120 5 ng/l Parathion-methyl 298-00-0 S 120 5 ng/l

Group 10 Nutrients Participants will receive: 6 x 30ml Samples (Nitrate/Nitrite/Ammonia, Silicate, SR

phosphate/Chloride, Total Cyanide, Free Cyanide, Kjeldahl N/Total P)

Determinand Asg Value Max C Value Units Total oxidised nitrogen (TON) S 10 0.25 mg N/l Nitrate S 7.5 0.25 mg N/l Nitrite S 2.5 0.05 mg N/l Ammonia S 20 0.25 mg N/l Silicate S 25 0.25 mg SiO2/l Soluble reactive Phosphorus S 10 0.25 mg P/l Chloride S 50 1 mg Cl/l Total Cyanide S 2.5 0.05 mg CN/l Kjeldahl Nitrogen S 25 0.25 mg N/l Free Cyanide S 2.5 0.05 mg CN/l Total Nitrogen S 55 0.5 mg N/l Total Phosphorus S 20 0.05 mg P/l

Group 11 Non-Specific Determinands Participants will receive: 5 x 30ml Samples (BOD, COD, MBAS, DOC/TOC, Susp. Solids) Determinand Asg Value Max C Value Units BOD (5 day) S 200 0.25 mg O2/l COD S 250 10 mg O2/l Suspended solids M 50 1 mg/l Methylene blue active substances (MBAS)

S 75 0.01 mg LS/l

Dissolved/Total organic carbon S 250 0.5 mg C/l


Group 12 Metals (Preserved in 0.5% Nitric Acid) Participants will receive: 1 x 250ml Concentrated Synthetic Effluent Sample

1 x 125ml Metals Sample (all determinands except mercury) 1 x 30ml Mercury Sample

Determinand Asg Value Max C Value Units Arsenic S 50 2 µg/l Aluminium S 2.5 0.01 mg/l Chromium S 0.25 0.01 mg/l Iron S 5 0.01 mg/l Manganese S 2.5 0.01 mg/l Cadmium S 50 0.5 µg/l Copper S 0.25 0.01 mg/l Lead S 0.25 0.01 mg/l Nickel S 1 0.01 mg/l Zinc S 5 0.01 mg/l Mercury S 25 0.5 µg/l Selenium S 50 2.5 µg/l *Sodium *Potassium *Calcium *Magnesium

Determinands marked with a star (*) will only be included if more than 6 customers specifically request them Group 12C Chromium (VI) in waste water Participants will receive: 1 x 30ml Spiking Solution 1 x 500ml synthetic waste water Determinand Asg Value Max C Value Units Chromium (VI) S 200 5 µg/l


Group 13 Sewage Sludge Inorganics Participants will receive: 1 x 20g Sludge Sample Determinand Asg Value Likely Range C Value Units Arsenic M 1-20 0.5 µg/g Cadmium M 1-30 0.25 µg/g Chromium M 50-400 5 µg/g Copper M 200-500 12.5 µg/g Lead M 100-500 12.5 µg/g Mercury M 1-5 0.05 µg/g Molybdenum M 4-10 1.5 µg/g Nickel M 20-150 5 µg/g Vanadium M 10-100 1 µg/g Zinc M 500-2000 25 µg/g Selenium M 1-3 0.25 µg/g Total Boron M 10-60 1 µg/g Fluoride M 100-3000 25 µg/g Total Nitrogen M 1-5 0.3 % N Total Phosphorus M 1-3 0.1 % P Total Potassium M 0.1-0.5 0.05 % K Cobalt M 5-100 1 µg/g Iron M 10000-100000 50 µg/g Manganese M 100-1000 1 µg/g *Aluminium *Antimony *Barium *Tin *Titanium

Determinands marked with a star (*) will only be included if more than 6 customers specifically request them Group 13 uses real sludge samples from different sources the range figures given above provide an indication of the concentrations that may be supplied, they are values from a range of recent samples provided by Aquacheck.


Group 14 Agricultural Soil Inorganics Participants will receive: 1 x 100g Soil Sample Determinand Asg Value Likely Max C Value Units Arsenic M 20 2.5 µg/g Cadmium M 1 0.15 µg/g Chromium M 60 12.5 µg/g Copper M 30 4 µg/g Lead M 50 15 µg/g Mercury M 0.5 0.05 µg/g Molybdenum M 4 0.2 µg/g Nickel M 40 2.5 µg/g Vanadium M 50 2.5 µg/g Zinc M 100 10 µg/g Selenium M 1 0.15 µg/g Total Boron M 100 1 µg/g Water Extractable Boron M 100 1 µg/g Fluoride M 100 25 µg/g Total Nitrogen M 4000 20 µg/g Total Phosphorus M 1000 10 µg/g Total Potassium M 5000 10 µg/g Cobalt M 20 1 µg/g Iron M 30,000 50 µg/g Manganese M 1000 1 µg/g Dry matter (105±5C) M TBA 1 (P=0%) % Loss on ignition (550±25C) M 10 2.5 (P=0%) % pH (2.5:1 water:soil) M TBA 0.2 (P=0%) pH units *Aluminium *Antimony *Barium *Tin *Titanium

Determinands marked with a star (*) will only be included if more than 6 customers specifically request them Group 14 uses real soil samples. The “Likely Max” values listed above are the highest values provided in recent distributions of these samples or from other data.


Group 17A Major waste water determinands Participants will receive: 1 x 1L Sample Determinand Asg Value Max C Value Units pH at 20-25C M Range 3-10 0.1 (P=0%) pH units Settled Chemical oxygen demand (COD)

M 1000 10 mg O2/l

Total COD S 2100 10 mg O2/l Suspended Solids M 1000 2.5 mg/l Conductivity (20C) M Range 0.5-45 0.01 mS/cm Total dissolved solids (180C) M Range 0.3-30 0.05 g/l Non filterable COD M 1000 10 mg O2/l

Group 17B Total Phenol, Cyanide and Sulphate Participants will receive: 1 x 250ml Sample (Phenol and Sulphate)

1 x 125ml (Cyanide)

Determinand Asg Value Max C Value Units Total Phenol S 50 0.05 mg/l Cyanide S 25 0.05 mg CN/l Sulphate S 1000 25 mg SO4/l

Group 17C Metals (Preserved in 0.5% Nitric Acid) Participants will receive: 1 x 250ml Metals Sample

1 x 30ml Mercury Sample 1 x 30ml Tin Sample 1 x 30ml Silver Sample

Determinand Asg Value Max C Value Units Chromium S 25 0.0125 mg/l Cadmium S 500 0.25 µg/l Copper S 25 0.0125 mg/l Lead S 25 0.0125 mg/l Nickel S 25 0.0125 mg/l Zinc S 25 0.0125 mg/l Mercury S 250 0.5 µg/l Silver S 0.5 0.005 mg/l Tin S 0.5 0.025 mg/l Iron S 50 0.025 mg/l


Group 17D Ammonia, Phosphate and Nitrogen Participants will receive: 3 x 125ml Samples (Ammonia/SRP, Total Phosphorus, Total

Nitrogen) Determinand Asg Value Max C Value Units Ammonia S 25 0.25 mg N/l Soluble reactive Phosphorus S 125 0.25 mg P/l Total Phosphorus S 125 0.25 mg P/l Total Nitrogen S 125 0.25 mg N/l

Group 18A Haloforms and Chlorinated Solvents Participants will receive: 1 x 500ml Concentrated Synthetic Effluent Sample

1 x 10ml Spiking Solution Determinand Asg Value Max C Value Units Chloroform S 1200 12.5 µg/l Bromodichloromethane S 1200 12.5 µg/l Dibromochloromethane S 1200 12.5 µg/l Bromoform S 1200 12.5 µg/l Trichloroethene S 120 10 µg/l Tetrachloroethene S 120 10 µg/l Carbon Tetrachloride S 36 3 µg/l 1,2 dichloroethane S 36 3 µg/l

Group 18B Phenols Participants will receive: 1 x 500ml Concentrated Synthetic Effluent Sample

1 x 10ml Spiking Solution Determinand Asg Value Max C Value Units Pentachlorophenol S 6000 50 ng/l Trichlorophenol S 6000 50 ng/l Phenol S 6000 50 ng/l 2-Chlorophenol S 6000 50 ng/l 4-Chlorophenol S 6000 50 ng/l 2,4-Dichlorophenol S 6000 50 ng/l


Group 18C Benzene, Toluene and Xylenes Participants will receive: 1 x 500ml Concentrated Synthetic Effluent Sample

1 x 10ml Spiking Solution Determinand Asg Value Max C Value Units Benzene S 24 1 µg/l Toluene S 60 3 µg/l Ethylbenzene S 60 3 µg/l Styrene S 60 3 µg/l o-Xylene S 60 3 µg/l m-Xylene S 60 3 µg/l p-xylene S 60 3 µg/l Total Xylene S 180 9 µg/l m- + p-xylene S 120 6 µg/l

Group 19A Organochlorine Pesticides Participants will receive: 1 x 500ml Concentrated Synthetic Effluent Sample

1 x 10ml Spiking Solution Determinand CAS No. Asg Value Max C Value Units Endrin 72-20-8 S 1200 50 ng/l Dieldrin 60-57-1 S 500 50 ng/l Aldrin 309-00-2 S 500 50 ng/l p’p DDT 50-29-3 S 1200 50 ng/l Lindane 58-89-9 S 1200 50 ng/l Trifluralin 1582-09-8 S 1200 50 ng/l Alpha Endosulphan 959-98-8 S 1200 50 ng/l Beta Endosulphan 33213-65-9 S 1200 50 ng/l Hexachlorobenzene 118-74-1 S 1200 50 ng/l Heptachlor 76-44-8 S 500 50 ng/l Heptachlor epoxide 1024-57-3 S 500 50 ng/l Pentachlorobenzene 608-93-5 S 1200 50 ng/l

Group 19B Chlorinated Solvents Participants will receive: 1 x 500ml Concentrated Synthetic Effluent Sample

1 x 10ml Spiking Solution Determinand Asg Value Max C Value Units Hexachlorobutadiene S 4000 250 ng/l CarbonTetrachloride S 4000 250 ng/l Tetrachloroethene S 4000 250 ng/l 1,2,4 Trichlorobenzene S 4000 250 ng/l Trichloroethene S 4000 250 ng/l 1,1,1-Trichloroethane S 4000 250 ng/l 1,3,5-Trichlorobenzene S 4000 250 ng/l 1,2,3-Trichlorobenzene S 4000 250 ng/l 1,2-Dichloroethane S 4000 250 ng/l Chloroform S 4000 250 ng/l


Group 19C1 Polyaromatic Hydrocarbons (1 Spike) Participants will receive: 1 x 500ml Concentrated Synthetic Effluent Sample

1 x 10ml Spiking Solution Determinand CAS No. Asg Value Max C Value Units Fluoranthene 206-44-0 S 500 20 ng/l Benzo(b)fluoranthene 205-99-2 S 250 20 ng/l Benzo(k)fluoranthene 207-08-9 S 250 20 ng/l Benzo(a)pyrene 50-32-8 S 120 5 ng/l Benzo(ghi)perylene 191-24-2 S 250 20 ng/l Indeno(1,2,3-cd)pyrene 193-39-5 S 250 20 ng/l

Group 19C2 Polyaromatic Hydrocarbons (2 Spikes) Participants will receive: 1 x 500ml Concentrated Synthetic Effluent Sample

2 x 10ml Spiking Solution Spiking solution 19C1 Determinand CAS No. Asg Value Max C Value Units Fluoranthene 206-44-0 S 500 20 ng/l Benzo(b)fluoranthene 205-99-2 S 250 20 ng/l Benzo(k)fluoranthene 207-08-9 S 250 20 ng/l Benzo(a)pyrene 50-32-8 S 120 5 ng/l Benzo(ghi)perylene 191-24-2 S 250 20 ng/l Indeno(1,2,3-cd)pyrene 193-39-5 S 250 20 ng/l

Spiking solution 19C2 Determinand CAS No. Asg Value Max C Value Units Acenaphthene 83-32-9 S 250 20 ng/l Acenaphthylene 208-96-8 S 250 20 ng/l Anthracene 120-12-7 S 250 20 ng/l Benz(a)anthracene 56-55-3 S 250 20 ng/l Chrysene 218-01-9 S 250 20 ng/l Dibenz(ah)anthracene 53-70-3 S 250 20 ng/l Fluorene 86-73-7 S 250 20 ng/l Naphthalene 91-20-3 S 250 20 ng/l Perylene 198-55-0 S 250 20 ng/l Phenanthrene 85-01-8 S 250 20 ng/l Pyrene 129-00-0 S 250 20 ng/l


Group 19D Polychlorinated Biphenyls (PCBs) Participants will receive: 1 x 500ml Concentrated Synthetic Effluent Sample

1 x 10ml Spiking Solution Determinand CAS No. Asg Value Max C Value Units PCB (28) 7012-37-5 S 1000 10 ng/l PCB (52) 35693-99-3 S 1000 10 ng/l PCB (101) 37680-73-2 S 1000 10 ng/l PCB (118) 31508-00-6 S 1000 10 ng/l PCB (138) 35065-28-2 S 1000 10 ng/l PCB (153) 35065-27-1 S 1000 10 ng/l PCB (180) 35065-29-3 S 1000 10 ng/l

Group 20 Triazines, Urons and Acid Herbicides Participants will receive: 1 x 500ml Concentrated Synthetic Effluent Sample

2 x 10ml Spiking Solutions Spiking solution 20(1) Determinand CAS No. Asg Value Max C Value Units Simazine 122-34-9 S 1200 50 ng/l Atrazine 1912-24-9 S 1200 50 ng/l Propazine 139-40-2 S 1200 50 ng/l MCPA 94-74-6 S 1200 50 ng/l MCPB 94-81-5 S 1200 50 ng/l Mecoprop 7085-19-0 S 1200 50 ng/l 2,4 D 94-75-7 S 1200 50 ng/l Isoproturon 34123-59-6 S 1200 50 ng/l Diuron 330-54-1 S 1200 50 ng/l Linuron 330-55-2 S 1200 50 ng/l Chlortoluron 15545-48-9 S 1200 50 ng/l Bentazone 25057-89-0 S 1200 50 ng/l

Spiking solution 20(2) Determinand CAS No. Asg Value Max C Value Units Glyphosate 1071-83-6 S 1200 50 ng/l


Group 20A Mineral Oil in Water Participants will receive: 1 variable volume sample (pH<2) in a I litre glass bottle Determinand Asg Value Max C Value Units Total Hydrocarbons by GC Analysis S 50 1

(P=15%) mg/l

Total Hydrocarbons by IR Analysis S 50

1 (P=15%) mg/l

Total Hydrocarbons by Gravimetric Analysis S 50

1 (P=15%) mg/l

Volume of sample provided S Range 0.75 – 0.9 5% l

Recovery adjusted Total hydrocarbons by GC S 50 1

(P=15%) mg/l

Recovery adjusted total hydrocarbons by IR S 50

1 (P=15%) mg/l

This Group compares the Total Hydrocarbon Content values obtained from an in-situ extraction of a one litre sample of water contaminated with Mineral Oil. A Type A mineral oil will be used to prepare these samples. This is designed to match the needs of ISO 9377 with a carbon range of C10 to C40. The “Recovery adjusted” values are for those labs that have determined recovery factors for the Type A mineral oil and wish to report adjusted values that allow for this recovery factor. Group 21 Organophosphorus Pesticides Participants will receive: 1 x 500ml Concentrated Synthetic Effluent Sample

1 x 10ml Spiking Solution Determinand CAS No. Asg Value Max C Value Units Azinphos-methyl 86-50-0 S 1200 50 ng/l Azinphos-ethyl 2642-71-9 S 1200 50 ng/l Dichlorvos 62-73-7 S 1200 50 ng/l Fenitrothion 122-14-5 S 1200 50 ng/l Malathion 121-75-5 S 1200 50 ng/l Mevinphos 7786-34-7 S 1200 50 ng/l Chlorfenvinphos 470-90-6 S 1200 50 ng/l Diazinon 333-41-5 S 1200 50 ng/l Fenthion 55-38-9 S 1200 50 ng/l Parathion-ethyl 56-38-2 S 1200 50 ng/l Parathion-methyl 298-00-0 S 1200 50 ng/l


Group 22 Qualitative Organics by GCMS Participants will receive: 2 x 2ml Samples (Sample and Blank) Ten organic determinands are provided for qualitative identification. This group is designed to test the ability of laboratories to identify organic compounds via GCMS analysis. Participants are provided with a solution containing ten organic compounds. The test requires that participants identify the ten compounds present. Marks are awarded on the basis of correctly identifying both the compound and if necessary the specific isomer present by identifying the correct CAS number. Participants are also provided with a solvent blank. The choice of the ten organic compounds is designed to avoid the formation of reaction by-products. Group 22A Qualitative Organics by Purge and Trap GCMS Participants will receive: 2 x 40ml Samples (Sample + Blank) Six organic determinands are provided for qualitative identification. This group is designed to test the ability of laboratories to identify organic compounds via purge and trap GCMS analysis. Participants are provided with a solution containing six organic compounds. The test requires that participants identify the six compounds present. Marks are awarded on the basis of correctly identifying both the compound and if necessary the specific isomer present by identifying the correct CAS number. Participants are also provided with a solvent blank. The choice of the 6 organic compounds is designed to avoid the formation of reaction by-products. Group 25 Qualitative Determination in Clean Water Participants will receive: 1 x 2L Sample The intent of this Group is to test the ability of laboratories to detect and identify an unknown contaminant in surface/potable waters. This group is designed for laboratories which may be involved in investigating potentially contaminated potable or surface waters and tests both the extraction and identification stages of investigations. Participants are provided with a two litre water sample and one or more 'indicators' of a potential problem, e.g. water is discoloured or has an oily sheen. Participants are asked to identify the contaminating substance(s).


Group 50 Ecotoxicology Participants will receive: 1 x 500ml Sample Determinand Asg Value P Value Units Daphnia Magna 48hr EC50 S 30% % Dilution Vibrio Fischeri 30 minute IC50 (ISO 11348-3) S 30% % Dilution Other 30 min luminescent bacteria IC50 tests S 30% % Dilution 15 minute luminescent bacteria IC50 tests M 30% % Dilution Tisbe battagliai 48 hour mortality test S 30% % Dilution Oyster 24 hour embryo-larval development test (Crassostrea gigas) S 30% % Dilution

Freshwater algae growth inhibition test -biomass reduction (Pseudokirschneriella subcapitata)

S 30% % Dilution

Marine algae growth inhibition test (Skeletonema costatum) M 30% % Dilution

Participants are required to dilute the sample provided in line with their usual practice, and to determine the EC50 (or IC50) dilution using any or all of the ecotoxicity tests listed. The solution will contain zinc sulphate at a concentration in the range 10 to 200mg Zn/l. The % dilutions to produce on EC50 returned, will be converted to mg Zn/l and Z-scores awarded based on a suitable reference value with a percentage error target of 30%.

aquacheckuzmanakreditasyon.com/dosya/aquacheck_test_plan_2007_8.pdf · 2014. 11. 9. · aquacheck...

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