Request for tender regarding the robustness validation of the draft methods for eluate and content analysis of inorganic substances

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1 Secretariat: Nederlands Normalisatie-instituut doc.nr. Vlinderweg 6 P.O. Box AX DELFT 2600 GB DELFT date The Netherlands The Netherlands Telephone: CEN/TC 351 N 0635 item nr. total pages : 19 supersedes document Mobile: Committee CEN/TC 351 Telefax: Construction products: [email protected] Assessment of release of dangerous substances Request for tender regarding the robustness validation of the draft methods for eluate and content analysis of inorganic substances For information For reply, if any, before: For approval before: (no reply will be considered as an abstention) For consideration during the next meeting Remarks For the robustness validation of the draft TSs and , being the 'umbrella standards' for analysis and content of inorganic substances in and from construction products, CEN/TC 351/WG 5 has prepared this request for tender. The most recent drafts (as confirmed by the members of WG 5 in September 2014) of both documents are available as CEN/TC 351 documents: N 0636 Analysis of inorganic substances in eluates (work item ) (CEN/TC 351/WG 5 N 274) N 0637 Methods for analysis of aqua regia digests (work item ) (CEN/TC 351/WG 5 N 278) The umbrella standards, by their nature, refer to existing and commonly used analysis methods which are assumed available with interested laboratories. The exceptions to this are the construction product specific methods for (N 0638) Digestion by aqua regia for subsequent analysis of the major, minor and trace elements (work item ) (CEN/TC 351/WG 5 N 275) (N 0639) Analysis by (work item ) (CEN/TC 351/WG 5 N 276) NB All plenary documents of CEN/TC 351 are available on CEN Livelink. Please refer to the administrator of the national standards authority in your country to get a login name and password and to add you to the CEN/TC 351 member list in the CEN Global Directory.

2 CEN/TC 351 N 0635 (N 0640) Analysis by (work item ) (CEN/TC 351/WG 5 N 277) A further exception is the hydride generation method which is expected to meet, in combination with, the required precision for As, Sb and Se. The document referred to here is not a formal standard. The reference can be found in section 5 'References'. It is also available as CEN/TC 351 document: N 0641 Elements with inductively coupled plasma Atomic emission spectrometry (ICP-AES) (CEN/TC 351/WG 5 N 306). In that method reference is made to yet another non-formal standard also made available as CEN/TC 351 document, notably: N 0642 Antimony, arsenic and selenium with hydride Atomic absorption spectrometry (Hydride-AAS) (CEN/TC 351/WG 5 N 307) The work The work consists of two parts: 1. Analysis of eluates for inorganic substances, and 2. Suitability for construction products of content analysis methods from other fields Offers for one of the parts or both are welcomed by the CEN/TC 351 secretariat by15 October 2015.

3 CEN/TC 351 N 0341 Annexes to this document Annex A to this document is the work programme for the robustness validation. Annex B to this document describes the procedure of assessment of the offers. Circulation This request is circulated in both the plenary CEN/TC 351 and its WG 5, and published on the websites of CEN and NEN ( NOTE With decision 224 (Stockholm 5 June 2014), CEN/TC 351 agreed "that WG 5 may combine the limited need for robustness testing with the precision testing (repeatability and reproducibility) for eluate analysis and content analysis of inorganic substances. The decision was taken by unanimity." [CEN/TC 351 N 0578] However, as the administrative arrangements for the robustness validation of the WG 3 and WG 5 methods are now settled (specific agreement CEN/ ) and as the round robin validation by JRC Geel is still under preparation, it is considered best to continue with the robustness validation and incorporate the results in the draft TSs that will be submitted for TC Approval, which is in line with the procedures followed for the other CEN/TC 351 TSs. 3

4 Annex A: Work programme for the robustness validation process for eluate and content analysis of inorganic substances in and from construction products 1. Introduction 1.1 General As stated in CEN/TR 16045:2010 a preference exists for multi-element and multimatrix methods to avoid unnecessary application of multiple protocols for the inorganic substances to be analysed. The present robustness validation project aims at establishing the suitability of the following two 'systems' of standards: 1. Analysis of inorganic substances in eluates from construction products; 2. Content of inorganic substances - Analysis of aqua regia digests from construction products. The main aspect to be covered is to ensure that methods selected are sufficiently sensitive to allow regulatory limits to be assessed with sufficient precision to draw conclusions on acceptability. The associated analytical methods need to be verified for suitability by carrying out repeatability measurements. Regarding the analysis of eluates, the robustness validation involves, besides existing established methods, the following newly developed draft standards of CEN/TC 351: N 0636 Analysis of inorganic substances in eluates (work item ); This is the 'umbrella standard'; N 0639 Analysis by (work item ); N 0640 Analysis by (work item ). Regarding the analysis of digests, the robustness validation involves, besides existing established methods, the following newly developed draft methods of CEN/TC 351: N 0638 Digestion by aqua regia for subsequent analysis of the major, minor and trace elements (WI ) N 0637 Methods for analysis of aqua regia digests (work item ); This is the 'umbrella standard'; N 0639 Analysis by (work item ); N 0640 Analysis by (work item ). 1.2 Eluate analysis for inorganic substances In the draft umbrella standard (CEN/TC 351 N 0636) no reference is made to the origin of the eluate. For the present robustness validation project eluates from 4

5 leaching tests according to CEN/TS :2014 and CEN/TS :2014 shall be used. It has been established that one of the preferred multi-element methods, notably, possibly can't meet the sensitivity requirement, to allow regulatory limits to be assessed with sufficient precision, for As, Sb and Se. Hence a corresponding hydride generation method ( 1 ) has been listed. It was identified that, in practice, indeed the hydride technique is used in combination with, but there is no formal standard (yet). A description of this method is publicly available at the VITO website and for convenience distributed as CEN/TC 351 document N 0641 (ICP-AES), which refers, for the generation of hydride, to N 0642 (Hydride-AAS). As discussed in CEN/TC 351/WG 5, it is necessary to demonstrate equivalence between and and the element specific methods, indicated as 'More sensitive methods', EN ISO and EN ISO spectrometers, also known as ICP-AES or ICP plasma spectrometers. 2 To allow the use of the same analytical equipment for a wider spectrum of substances. 5

6 2. Part 1: Eluate analysis for inorganic substances 2.1 Selection of materials for eluate generation For the robustness work the eluates and the SRM solution will be supplied. Test Eluate analysis Number of construction Quantity for producing products eluates 8 At least 1 kg for granular material. At least 5 units per monolithic product 3 The 8 construction products, with the accompanying hens and mandates are Granular product hen Mandate 1. Coal fly ash EN M/ Masonry product EN M/ Expanded clay EN M/103, M/ Natural aggregate EN M/125 Monolithic product hen Mandate 5. Clay masonry unit EN M/ Steel slag EN M/ Tiles or ceramic tiles EN M/119 EN Plastic product EN M/121 NOTE: The construction products in the table are selected as being representative for the various types of products covered by Mandate/366. Products have been selected based on relatively high and expected low concentrations of substances of interest. Masonry (recycled masonry aggregate) is added because it has measurable levels of As, Se and Sb. Methods to be used by element or element group Granular product Specific substances Methods to be used 1. Coal fly ash Cr, S, V, Zn 2- SO 4 EN ISO Cd EN ISO Hg 2. Masonry product As EN ISO and EN ISO For instance: If such situation occurs, at least 5 bricks shall be selected. 6

7 Sb, Se Al, Mo, Zn EN ISO See also section 2.4 below. EN ISO See also section 2.4 below. 3. Expanded clay As EN ISO Sb, Se See also section 2.4 below. EN ISO See also section 2.4 below. F - EN ISO SO 4 EN ISO S, V, Zn 4. Natural aggregate Cu, Zn As EN ISO See also section 2.4 below. Monolithic product Specific substances 5. Clay masonry unit As EN ISO See also section 2.4 below. Sb, Se EN ISO See also section 2.4 below. Mo, Zn 6. Steel slag Ba, Mg, S, V, Zn F - EN ISO SO 4 2- EN ISO Tiles or ceramic tiles Ca, Mo, Si, Zn 8. Plastic product # Cu, Pb, Zn Standard Reference Material (SRM) solution # Depending on stabiliser used. Zn, others (max. 6) to be decided when solution is available To be decided. 7

8 2.2 Preparation of eluates The selected materials shall be leached according to CEN/TS for monolithic products (analysis of fraction 1 and 3); and to prcen/ts in case of granular material, using fractions obtained at L/S=2 and L/S=10. These ratios are chosen to have two concentration levels for analysis, and these are the most used L/S ratios. 2.3 Robustness testing of analysis of eluates All analysis per method, per substance and per eluate shall be done in 5 fold. The repeatability of the measurements shall be presented in tabular form as well as in graphical form (percentage standard deviation on y-axis as a function of concentration in solution on x-axis). Comprehensive raw data shall be presented in an annex and in electronic form. The main topic for this study on robustness will be to demonstrate if the repeatability is good and the sensitivity of the methods proposed is adequate for the existing regulatory requirements in Europe. 2.4 Repeatability and suitability of the hydride generation- method for oxyanions As, Sb, Se To demonstrate suitability of hydride as alternative to Hydride Generation AAS for As determination and Grafite Furness AAS for Sb and Se determination, determination according to the method described in N 0651 shall be carried out in parallel with HG-AAS according to EN ISO 11969:1996 and GF-AAS according to EN ISO 15586:2003 respectively. This will be done on eluates obtained from - granular masonry as material with measurable levels of As, Se and Sb in eluates and - monolithic clay masonry product, - expanded clay and - granular natural aggregate (for As only). Again all analysis per method, per substance and per eluate shall be done in 5 fold. 2.5 Deliverables and reports The expected results and deliverables of the project are as follows: At least one progress report on the details of the action s implementation and its presentation in WG 5 (deadline for submission: 2 months after assignment). One final technical implementation report for the adaptation of the examined methods (work items , 017, 018, 019, 021 including precise proposals 8

9 for adjustment of these draft TS's on the basis of the results of the robustness validation (deadline for submission: 5 months after assignment). This final technical implementation report shall, in draft form, consist of a statistical evaluation of all data generated (e.g. informative annexes, tables of results, test reports, outlines and flowcharts of the procedures followed, conclusions on suitability of the methods and recommendations for improvement of the harmonised methods considered necessary), which can support the standardisation of the examined umbrella document and their publication as TS s. One comprehensive final report consisting, in their final form, of a series of all necessary data elaborated and analysed (e.g. informative annexes, tables of results, test reports, outlines and flowcharts of the procedures followed, conclusions and definitions to the pass/fail criteria of the methods, final drafts and design of any adjustments on the harmonised methods considered necessary), which can support the standardisation of the examined umbrella document and its publication as TS (deadline for submission: 8 months after assignment). 2.6 Budget Offers for part 1 (as described in clause 2) shall not exceed EUR (excl. VAT) including reporting. 9

10 3. Part 2: Suitability of content analysis methods from other fields for construction products 3.1 Selection of materials for content analysis For the robustness work sample material and a SRM will be supplied. The number and type of construction products and approximate quantities needed are given below: Test Digestion and digest analysis Number of construction Quantity products 11 1 kg per granular sample At least 5 units per monolithic product 4 The 11 construction products, with the accompanying hens and mandates are Granular product hen Mandate 1. Coal fly ash EN M/ Steel slag EN M/125 EN Reclaimed asphalt EN M/ Armour stone EN M/ Masonry product EN M/ Natural aggregate EN M/125 Monolithic product hen Mandate 7. Roofing felt (Bitumen shingles) EN 544 M/121, M/ Pure mineral based renders and EN M/116 mortars 9. Plastic product EN M/ Asphalt concrete EN M/ Treated wood * EN M/112 * Although treated wood is a relevant matrix with regard to organic substances (boron, copper), it is also listed here as an example of a non-mineral matrix. NOTE: The construction products in the table are selected as being representative for the various types of products covered by Mandate/366. All products will be supplied with size-reduced to 95 % < 0,25 mm. Methods to be used by element or element group Granular product Specific substances Methods to be used 1. Coal fly ash Cr, V, Zn 4 For instance: If such situation occurs, at least 5 bricks shall be selected. 10

11 As EN ISO See also section 2.4 above. Sb, Se EN ISO See also section 2.4 above. Cd EN ISO Hg EN ISO and EN ISO Steel slag Ba, Mo, V F - EN ISO Reclaimed asphalt Ba, S, V, Zn 2- SO 4 EN ISO Masonry product As EN ISO See also section 2.4 above. Sb, Se EN ISO See also section 2.4 above. Mo 5. Natural aggregate Al, Mn, Zn, As EN ISO See also section 2.4 above. Monolithic product Specific substances 6. Armour stone Minimal 30 major, minor and trace elements 7. Roofing felt As, Ba, S, V (Bitumen shingles) 8. Pure mineral based renders and mortars ## SO 4 2- Cr, V, Zn EN ISO Plastic product # Cu, Pb, Zn 10. Asphalt concrete Ba, Ca, Zn, S 2- SO 4 EN ISO

12 11. Treated wood (CCA) As, Cr, Cu Standard Reference Material (SRM) # Depending on stabiliser used. ## Depending on the render supplied To be decided when SRM material is known (max. 6 specific substances). 3.2 Robustness testing of digestion and subsequent content analysis Digestion Aqua regia digestion is most commonly used for content analysis of materials and as stated in CEN/TR it is the recommended procedure for construction products. In the protocol described in WI two methods are specified. It is necessary to do the tests on the selected construction products with both digestion methods in parallel to ensure comparability of data for using either digestion method Analysis All analyses per method, per substance and per digestion method shall be done in 5 fold. Both the combinations <digestion methods analytical methods> and the newly developed analytical methods themselves need to be verified for suitability for construction products by carrying out repeatability measurements. The repeatability of the measurements shall be presented in tabular form as well as in graphical form (percentage standard deviation on y-axis as a function of concentration in solution on x-axis). Comprehensive raw data shall be presented in an annex and made available in electronic form. The main topic for this study on robustness will be to demonstrate if the repeatability is good and the sensitivity of the methods proposed is adequate for the existing regulatory requirements in Europe. 3.3 Deliverables and reports The expected results and deliverables of the project are as follows: At least one progress report on the details of the action s implementation and its presentation in WG 5 (deadline for submission: 2 months after assignment); One final technical implementation report for the adaptation of the examined methods (work items , 017, 018, 019, 021 including precise proposals for adjustment of these draft TS's on the basis of the results of the robustness validation (deadline for submission: 5 months after assignment). This final technical implementation report shall, in draft form, consist of a statistical evaluation of all data generated (e.g. informative annexes, tables of results, test reports, outlines and flowcharts of the procedures followed, 12

13 conclusions on suitability of the methods and recommendations for improvement of the harmonised methods considered necessary), which can support the standardisation of the examined umbrella document and their publication as TS s. One comprehensive final report consisting, in their final form, of a series of all necessary data elaborated and analysed (e.g. informative annexes, tables of results, test reports, outlines and flowcharts of the procedures followed, conclusions and definitions to the pass/fail criteria of the methods, final drafts and design of any adjustments on the harmonised methods considered necessary), which can support the standardisation of the examined umbrella document and its publication as TS (deadline for submission: 8 months after assignment). 3.4 Budget Offers for this part (as described in clause 3) shall not exceed EUR (excl. VAT) including reporting. 13

14 4. Sampling requirements The samples needed for the robustness study are expected to be provided by producers/suppliers on behalf of a product TC. CEN/TC 351/WG 5 is responsible for contacting the proper organizations to provide the names of producers willing to supply their products for testing in the robustness validation. Sampling requirements are prepared under the responsibility of the evaluation team established at the WG 5 meeting in February This implies that testing material shall be ready by the time the tender process and contract negotiations are completed. 4.1 Eluate analysis Eluates from construction products are generally clean, hence very limited sample pre-treatment is expected. Eluates for testing shall be generated according to the methods in CEN/TS and prcen/ts Although the latter has not been completely finalised yet, this has no consequences for the eluate analysis robustness work. The construction products to be used for the robustness validation are listed in the table in 3.1. Eluates obtained by the specified methods will be supplied. 4.2 Content analysis For content analysis of construction products size reduction is required to 95 % < 250 micrometres. Draft standard WI on sample pre-treatment shall be applied. The materials as listed in the table in 2.1 shall be used for the robustness validation. Size reduced materials will be supplied. 14

15 5. References EN 544:2011, Bitumen shingles with mineral and/or synthetic reinforcements Product specification and test methods EN 771-1:2003, Specification for masonry units Part 1: Clay masonry units EN 998-1:2010, Specification for mortar for masonry Part 1: Rendering and plastering mortar EN 1484:1997, Water analysis Guidelines for the determination of total organic carbon (TOC) and dissolved organic carbon (DOC) EN :2006, Bituminous mixtures Material specifications Part 1: Asphalt Concrete EN 13242:2003+A1:2008, Aggregates for unbound and hydraulically bound materials for use in civil engineering work and road construction EN :2008, Plastics Unplasticized poly(vinyl chloride) (PVC-U) profiles for building applications Part 2: PVC-U profiles and PVC-UE profiles for internal and external wall and ceiling finishes EN :2002, Armourstone Part 1: Specification EN :2004, Terrazo tiles Part 2: Terrazzo tiles for external use EN 14229:2010, Structural timber Wood poles for overhead lines EN 14411:2012, Ceramic tiles Definitions, classification, characteristics, evaluation of conformity and marking EN 15732:2012, Light weight fill and thermal insulation products for civil engineering applications (CEA) Expanded clay lightweight aggregate products (LWA) EN 15824:2009, Specifications for external renders and internal plasters based on organic binders EN 16192:2011, Characterization of waste Analysis of eluates EN 27888:1993, Water quality Determination of electrical conductivity (ISO 2788:1985) EN ISO :2009, Water quality Determination of dissolved anions by liquid chromatography of ions Part 1: Determination of bromide, chloride, fluoride, nitrate, nitrite, phosphate and sulfate EN ISO 10523:2012, Water quality Determination of ph 15

16 EN ISO 11969:1996, Water quality Determination of arsenic Atomic absorption spectrometric method (hydride technique) EN ISO 12846:2012, Water quality Determination of mercury Method using atomic absorption spectrometry (AAS) with and without enrichment EN ISO 15586:2003, Water quality Determination of trace elements using atomic absorption spectrometry with graphite furnace EN ISO 17852:2008, Water quality Determination of mercury Method using atomic fluorescence spectrometry CEN/TR 16045:2010, Construction Products Assessment of release of dangerous substances - Content of regulated dangerous substances Selection of analytical methods CEN/TR 16220:2011 Construction products Assessment of release of dangerous substances Complement to sampling CEN/TS :2014, Construction products Assessment of release of dangerous substances Part 1: Guidance for the determination of leaching tests and additional testing steps CEN/TS :2014, Construction products Assessment of release of dangerous substances Part 2: Horizontal dynamic surface leaching test prcen/ts , Construction products Assessment of release of dangerous substances Part 3: Horizontal up-flow percolation test (under development in CEN/TC 351/WG 1) WI , Construction products Analysis of inorganic substances in eluates (under development in CEN/TC 351/WG 5) (CEN/TC 351 N 0636) WI , Construction products Assessment of release of dangerous substances Digestion of construction products by aqua regia (under development in CEN/TC 351/WG 5) (CEN/TC 351 N 0638) WI , Construction products Assessment of release of dangerous substances Analysis of inorganic substances in digests and eluates Part 1: Analysis by Inductive Coupled Plasma Optical Emission Spectrometry () (under development in CEN/TC 351/WG 5) (CEN/TC 351 N 0639) WI , Construction products Assessment of release of dangerous substances Analysis of major, minor and trace elements in digests and eluates by Inductively Coupled Plasma Mass Spectrometry () (under development in CEN/TC 351/WG 5) (CEN/TC 351 N 0640) WI , Construction products Methods for analysis of aqua regia digests (under development in CEN/TC 351/WG 5) (CEN/TC 351 N 0637) WI , Construction products Assessment of release of dangerous substances Preparation of test portions from the laboratory sample for analysis of eluates and digests (under development in CEN/TC 351/WG 5) (CEN/TC 351 N 0636) 16

17 Hjelmar, O., J. Hyks, M. Wahlström, J. Laine-Ylijoki, A. van Zomeren, R. Comans, U. Kalbe, U. Schoknecht, O. Krüger, P. Grathwohl, T. Wendel, M Abdelghafour, J. Méhu, N. Schiopu, M. Lupsea (2012) Robustness validation of TS-2 and TS-3 developed by CEN/TC351/WG1 to assess release from products to soil, surface water and groundwater. Available from Hjelmar, O., A. van Zomeren and U. Kalbe (2014), Additional Robustness Testing on TS-3 (CEN/TC 351/WG 1). Available from VITO, Elements with inductively coupled plasma Atomic emission spectrometry (ICP- AES) (CEN/TC 351/WG 5 N 306) (CEN/TC 351 N 0641) VITO, Antimony, arsenic and selenium with hydride Atomic absorption spectrometry (Hydride-AAS) (CEN/TC 351/WG 5 N 307) (CEN/TC 351 N 0642) 17

18 CEN/TC 351 N 0635 Annex B Annex B: Assessment procedure 1. Selection Criteria for the tendering process (1) Only projects that are strictly non-profit-making and/or whose immediate objective is non-commercial shall be eligible. Selection will be based on the following criteria: 1) Documented experience (maximum 45 points): number of years working in the field of eluate and content analysis from construction products number of years working in the field of analysis and data processing and/or number of completed projects/publications confirming related technical experience and activities number of years participating in European and/or international standardisation work in the field of Release of Dangerous Substances from Construction Products into Soil and Groundwater and/or list of completed and running standardisation projects confirming related experience description of actual experience in running European and/or international programs list of publications in the field of eluate and content from construction products and related materials in peer reviewed journals description of the quality assurance procedures for the required analyses 2) Organisation demonstration of ability and understanding of the project (maximum 35 points): proof of stable and sufficient sources of finance to ensure the continuity of the organisation throughout the project description of infrastructure; submission of curriculum vitae of every person to be performing work in connection with the robustness project; delineation of organisation of the measurements; proof of an established quality system. 3) Quotation price (maximum 20 points): Only offers that pass the selection criteria of scoring minimum 30 points under 1) and 20 points under 2) will be further evaluated. (2) The criteria shall be assessed on the basis of the documents supplied by the tender providers. The selection committee reserves the right to approach bidders previous customers for reference. The sum of points acquired under 1) and 2) is divided by the number of points scored for the quotation price for the lot under 3). The offer with the highest ratio will be selected. However, in case the ratio of 18

19 CEN/TC 351 N 0635 Annex B {1) + 2)}/3) of the two best offers differs less than 10 %, the evaluation committee may decide to choose the offer with the best value (i.e. the highest sum of 1) + 2)). (3) The selected offer is sent to the EC and to CEN/TC 351/WG 5 for confirmation. After confirmation, the work is assigned. 2 Replies to tender (1) Tenders can be sent (by mail or ) to the secretary of CEN/TC 351 as soon as possible, at the latest by 15 October Late delivery will lead to exclusion of the applicant from the award procedure. The tender shall contain a specified breakdown of tasks, costs and travel expenses and a planning for the execution of the tasks. (2) If necessary, additional information can be obtained by the secretary of CEN/TC 351, Ms Annemieke Venemans (Tel.: , [email protected]). (3) NEN as holder of the secretariat of CEN/TC 351 is responsible for execution of the order voucher for mandate M/366. In order to control the process, project management is held by NEN. The secretariat of CEN/TC 351/WG 5 Eluate and content analysis of construction products will be responsible for monitoring the technical progress. (4) This means that contract and financial matters as well as monitoring of the general progress of the project and the communication with CCMC and CEN/TC 351 are under responsibility of NEN. The technical work (robustness studies) is conducted by a consortium or individual subcontracted parties appointed by the tender procedure specified in the present document. 19