Wood preservatives - Determination of the toxic values against larvae of Hylotrupes bajulus (Linnaeus) - (Laboratory method)

This document specifies a method for the determination of the toxic values of a wood preservative against the larvae of Hylotrupes bajulus (Linnaeus), introduced into wood treated previously by full impregnation. This method is applicable to: ¾ water-insoluble chemicals which are being studied as active insecticides; ¾ organic formulations, as supplied or as prepared in the laboratory by dilution of concentrates; ¾ organic water-dispersible formulations as supplied or as prepared in the laboratory by dilution of concentrates; ¾ water-soluble materials, for example salts. The method is applicable whether or not the test specimens have been subjected to appropriate ageing procedures.

Holzschutzmittel - Bestimmung der Grenze der Wirksamkeit gegenüber Larven von Hylotrupes bajulus (Linnaeus) - (Laboratoriumsverfahren)

Diese Europäische Norm legt ein Verfahren zur Bestimmung der Grenze der Wirksamkeit eines Holzschutzmittels gegenüber Larven von Hylotrupes bajulus (Linnaeus) fest, die in Holz eingesetzt wurden, das zuvor durch Volltränkung behandelt wurde.
Das Verfahren gilt für:
-   wasserunlösliche Chemikalien, die als wirksame Insektizide untersucht werden;
-   organische Formulierungen im Anlieferungszustand oder in Form von im Laboratorium hergestellten Verdünnungen von Konzentraten;
-   organische, in Wasser dispergierbare Formulierungen im Anlieferungszustand oder in Form von im Laboratorium hergestellten Verdünnungen von Konzentraten; und
-   wasserlösliche Stoffe, zum Beispiel Salze.
Das Verfahren gilt unabhängig davon, ob die Proben einer angemessenen Alterungsbeanspruchung ausgesetzt wurden oder nicht.

Produits de préservation du bois - Détermination du seuil d'efficacité contre les larves d'Hylotrupes bajulus (Linnaeus) - (Méthode de laboratoire)

La norme européenne définit une méthode de détermination du seuil d’efficacité d'un produit de préservation du bois contre les larves d’Hylotrupes bajulus (Linnaeus) après leur introduction dans du bois traité préalablement par imprégnation totale.
La présente méthode est applicable :
-   aux produits chimiques non hydrosolubles étudiés en tant que matières actives insecticides ;
-   aux formules organiques telles qu'elles sont fournies ou préparées en laboratoire par dilution de concentrés ;
-   aux formulations organiques hydrodispersables telles qu'elles sont fournies ou préparées en laboratoire par dilution de concentrés ; et,
-   aux produits solubles dans l’eau, par exemple aux sels.
Cette méthode s’applique à des éprouvettes ayant subi ou non des épreuves de vieillissement appropriées.

Biocidni proizvodi za zaščito lesa - Ugotavljanje toksičnih vrednosti proti ličinkam hišnega kozlička Hylotrupes bajulus (Linnaeus) (laboratorijska metoda)

Ta dokument določa metodo za ugotavljanje toksičnih vrednosti biocidnega proizvoda za zaščito lesa proti ličinkam hišnega kozlička Hylotrupes bajulus (Linnaeus), uporabljenega na lesu, ki je bil obdelan s popolno impregnacijo. Ta metoda se uporablja za: ¾ v vodi netopne kemikalije, ki se preučujejo kot aktivni insekticidi; ¾ organske formulacije, ki so dobavljene ali pripravljene v laboratoriju z redčenjem koncentratov; ¾ organske formulacije, ki se razpršijo v vodi in so dobavljene ali pripravljene v laboratoriju z redčenjem koncentratov; ¾ v vodi topne materiale, na primer sol. Metoda se uporablja ne glede na to, ali so preskušanci izpostavljeni ustreznim postopkom staranja ali ne.

General Information

Status
Withdrawn
Publication Date
29-Nov-2017
Withdrawal Date
27-Feb-2017
Current Stage
9060 - Closure of 2 Year Review Enquiry - Review Enquiry
Start Date
04-Mar-2022
Completion Date
04-Mar-2022

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.WRGDHolzschutzmittel - Bestimmung der Grenze der Wirksamkeit gegenüber Larven von Hylotrupes bajulus (Linnaeus) - (Laboratoriumsverfahren)Produits de préservation des bois - Détermination des valeurs toxiques contre les larves d'Hylotrupes bajulus (Linnaeus) - (Méthode de laboratoire)Wood preservatives - Determination of the toxic values against larvae of Hylotrupes bajulus (Linnaeus) - (Laboratory method)71.100.50Wood-protecting chemicalsICS:Ta slovenski standard je istoveten z:EN 47:2016SIST EN 47:2017en,fr,de01-januar-2017SIST EN 47:2017SLOVENSKI

STANDARDSIST EN 47:2005/AC:2007SIST EN 47:20051DGRPHãþD
SIST EN 47:2017
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 47
August
t r s x ICS
y sä s r rä w r Supersedes EN
v yã t r r wEnglish Version

Wood preservatives æ Determination of the toxic values Produits de préservation du bois æ Détermination du seuil d 5efficacité contre les larves d 5Hylotrupes bajulus

Holzschutzmittel æ Bestimmung der Grenze der Wirksamkeit gegenüber Larven von Hylotrupes bajulus This European Standard was approved by CEN on

t January
t r s yä

egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä

translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä

CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey andUnited Kingdomä

EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels

t r s x CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN

v yã t r s x ESIST EN 47:2017

EN 47:2016 (E) 2 Contents Page European foreword ....................................................................................................................................................... 3 Introduction .................................................................................................................................................................... 4 1 Scope .................................................................................................................................................................... 5 2 Normative reference ...................................................................................................................................... 5 3 Terms and definitions ................................................................................................................................... 5 4 Principle ............................................................................................................................................................. 5 5 Test materials ................................................................................................................................................... 6 6 Sampling ............................................................................................................................................................. 8 7 Test specimens ................................................................................................................................................. 9 8 Procedure........................................................................................................................................................ 10 9 Expression of results ................................................................................................................................... 14 10 Test report ...................................................................................................................................................... 14 Annex A (informative)

Example of a test report ............................................................................................ 16 Annex B (informative)

Technique for culturing Hylotrupes bajulus (Linnaeus) ................................ 18 Annex C (normative)

Differentiation of heartwood and sapwood in Pinus species .......................... 21 Annex D (informative)

Environmental, health and safety precautions within chemical/biological laboratory .............................................................................................................. 22 Bibliography ................................................................................................................................................................. 23

SIST EN 47:2017

EN 47:2016 (E) 3 European foreword This document (EN 47:2016) has been prepared by Technical Committee CEN/TC 38 “Durability of wood and wood-based products”, the secretariat of which is held by AFNOR. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by February 2017, and conflicting national standards shall be withdrawn at the latest by February 2017. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 47:2005. The significant technical difference between this document and EN 47:2005 is as follows: — introduction of new harmonized specifications for wood quality. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 47:2017

EN 47:2016 (E) 4 Introduction This document describes a laboratory method of testing which gives a basis for the general assessment of the effectiveness of a wood preservative against Hylotrupes bajulus by determination and comparison with different classes of larvae, of the concentration at which the product prevents their survival in totally impregnated wood of a susceptible species. In this respect it differs from the method specified in EN 46-1 which is intended to determine whether a preservative applied to the surface is capable of preventing infestation of wood by these larvae. This laboratory method provides a criterion by which the value of a preservative can be assessed. In making this assessment the methods by which the preservative may be applied should be taken into account. It is further recommended that results from this test should be supplemented by those from other appropriate tests and, above all, by comparison with practical experience. When products which are very active at very low concentration are used, it is very important to take suitable precautions to isolate and separate, as far as possible, operations involving chemical products, other products, treated wood, laboratory apparatus and clothing. Suitable precautions should include the use of separate rooms, areas within rooms, extraction facilities, conditioning chambers and special training for personnel (see also Annex D for environmental, health and safety precautions). SIST EN 47:2017

EN 47:2016 (E) 5 1 Scope This European Standard specifies a method for the determination of the toxic values of a wood preservative against the larvae of Hylotrupes bajulus (Linnaeus), introduced into wood treated previously by full impregnation. This method is applicable to: — water-insoluble chemicals which are being studied as active insecticides; — organic formulations, as supplied or as prepared in the laboratory by dilution of concentrates; — organic water-dispersible formulations as supplied or as prepared in the laboratory by dilution of concentrates; and — water-soluble materials, for example salts. The method is applicable whether or not the test specimens have been subjected to appropriate ageing procedures. 2 Normative reference The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696) 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 representative sample sample having its physical or chemical characteristics identical to the volumetric average characteristics of the total volume being sampled [SOURCE: EN 1001-2:2005, 4.71] 3.2 supplier sponsor of the test (person or company providing the sample of wood preservative to be tested) Note 1 to entry: Adapted from EN 1001–2:2005, 4.83. 4 Principle Impregnation of several sets of test specimens of susceptible wood species with a series of concentrations of the preservative. Introduction of Hylotrupes bajulus larvae of a given category into these test specimens and determination of their survival rate at fixed intervals of time. SIST EN 47:2017

EN 47:2016 (E) 6 Comparison of the results with those obtained with untreated and solvent or diluent-treated control test specimens. Derivation of the toxic values of the product under test for the category of larvae in question. 5 Test materials 5.1 Biological material 5.1.1 Hylotrupes bajulus (Linnaeus) larvae — Category 1 (obligatory test): larvae within a maximum of 3 days of hatching; — Category 2 (optional additional test): larvae with masses in the range 50 mg to 150 mg. 5.1.2 Source of larvae The larvae shall preferably be obtained from cultures reared according to the method described in Annex B. Otherwise larvae in Category 2 can be taken from naturally infested wood, in which case they should be transferred into sapwood of pine and stored for at least 4 weeks under the rearing conditions specified in Annex B. Do not use the larvae in the test if they have not fed normally during this storage period. 5.1.3 Provision of larvae Collect larvae in Category 1 from eggs laid by different females. Carefully cut out the larvae in Category 2 from the culture blocks and keep them separated from one another for 2 days to 3 days in the culturing chamber (5.3.1) to check that they are healthy. 5.1.4 Choice of larvae in Category 2 Use only healthy larvae in the test. NOTE A healthy larva can be recognized by its ivory-white colour, its firm consistency and rounded appearance, and by the absence of wounds or bites which show up as dark marks. Healthy larvae react to the touch by vigorous movement and attempts to bite. Reject any larvae which are shrunken or aged, which have recently moulted, or which are in a pre-pupal stage. 5.1.5 Number of larvae The number of larvae per treated and control test specimen shall be six of Category 1 or one of Category 2. Sort the larvae retained in Category 2 mentioned above. Do not use larvae weighing more than 150 mg as they may pupate and therefore interfere with the test. For a single test, use a mixed batch of larvae of Category 1 and for Category 2, as far as possible, use larvae of similar masses. The number of larvae necessary is given in Table 1. SIST EN 47:2017

EN 47:2016 (E) 7 Table 1 — Number of larvae and test specimens Type of test specimen Concentrations of preservatives Mass fraction Larvae in Category 1 Larvae in Category 2 Without radiography With radiography a Number of test specimens Number of larvae Number of test specimens Number of larvae Number of test specimens Number of larvae Treated test specimens 1 5 30 10 10 7 7 _ 2 5 30 10 10 7 7 _ 3 5 30 10 10 7 7 _ 4 5 30 10 10 7 7 _ 5 5 30 10 10 7 7 etc.

Untreated control test specimens 0 5 30 10 10 7 7 Solvent or diluent control test specimens (including water) 0 5 30 10 10 7 7 Total for 5 concentrations 35 210 70 70 49 49 a The use of radiography is only recommended in the case of tests with larvae in Category 2. 5.2 Products and reagents 5.2.1 Xylene, technical grade, mixed isomers. 5.2.2 Water, complying with grade 3 of EN ISO 3696. 5.2.3 Solvent or diluent, a volatile liquid that will dissolve or dilute the preservative but does not leave a residue in the wood at the end of the post-treatment conditioning period that has a toxic effect on the insects. CAUTION — Do not use benzene or other solvents which pose a health risk. 5.2.4 Cellulose or absorbent cotton wool and filter paper 5.3 Apparatus 5.3.1 Culturing chamber, with air circulation, and controlled at (28 ± 2) °C and at relative humidity (70 ± 5) %. 5.3.2 Conditioning chamber, well ventilated and controlled at (20 ± 2) °C and at relative humidity (65 ± 5) %. NOTE The conditioning of test specimens can be carried out in the laboratory work area (see 5.3.3) provided that this has the conditions specified for the conditioning chamber (see 5.3.2). 5.3.3 Laboratory work area, well ventilated, where treatment of the test specimens is carried out. SIST EN 47:2017

EN 47:2016 (E) 8 CAUTION — It is essential to follow safety procedures for handling flammable and toxic materials. Avoid excessive exposure of operators to solvents or their vapours. 5.3.4 Testing chamber, ventilated and air-conditioned, controlled at (22 ± 2) °C and at a relative humidity of (70 ± 5) %. 5.3.5 Treatment vessels, of a material that does not react with the preservative under test, for example of glass for organic products and of polyethylene for salts containing fluorine. 5.3.6 Weights, to provide ballast for the test specimens. The weights shall not react with any materials with which they come into contact during the test. 5.3.7 Safety equipment and protective clothing, appropriate for the test product and the test solvent, to ensure the safety of the operator. 5.3.8 Vacuum vessel(s), fitted with stopcocks, capable of receiving the treatment vessels (5.3.5). 5.3.9 Vacuum pump, fitted with a pressure gauge and capable of maintaining a pressure of 700 Pa1). 5.3.10 Drying vessel(s), capable of holding sets of five test specimens (7.5), provided with a close-fitting cover and containing supports that will give minimum contact with treated test specimens to be placed on them. The vessels and supports shall be of a material that does not react with the preservative under test, for example glass for organic compounds and polyethylene for products containing fluorine. 5.3.11 Drill and twist drills, approximately 3,0 mm to 4,5 mm in diameter, and a fine awl. In all cases, the number of bits shall be sufficient to drill holes to the size of the larvae available; in the case of larvae of Category 1, use a steel awl. 5.3.12 Ordinary laboratory equipment, including a balance capable of weighing to an accuracy of 0,01 g. 5.3.13 X-ray apparatus (optional) with tungsten target and beryllium window, with voltage and current continuously variable in the following ranges: — voltages: 10 kV to 50 kV; — current: 0 mA to 15 mA. 5.3.14

Protective gloves 6 Sampling The sample of preservative shall be representative of the product to be tested. Samples shall be stored and handled in accordance with any written recommendations from the supplier. For the sampling of preservatives from bulk supplies, the procedure given in EN 212 should be used.

1) 100 Pa = 1 mbar. SIST EN 47:2017

EN 47:2016 (E) 9 7 Test specimens 7.1 Species of wood The reference species is Scots pine (Pinus sylvestris Linnaeus)2). Additional tests may be carried out using other species but, if so, this should be stated in the test report. 7.2 Wood quality The wood shall be free from visible cracks, stain, decay, insect damage and other defects. The wood shall not have been water-stored, floated, chemically treated or steamed. The wood shall originate from trees preferably felled in winter. The trees shall be cut immediately after felling and the timber rapidly air-dried or kiln dried at temperatures below 60 °C. The wood shall not have been stored for more than five years. The wood shall be exclusively sapwood containing little resin and having between 2,5 annual rings per 10 mm and eight annual rings per 10 mm. The proportion of latewood in the annual rings shall not exceed 30 % of the whole. It is recommended to use test specimens of similar growth rate within a single test. 7.3 Provision of test specimens Prepare planed strips having a cross-section of (25 ± 0,5) mm × (15 ± 0,5) mm removing a minimum of 2 mm from any faces exposed during drying. The longitudinal faces shall be parallel to the direction of the grain. The annual rings shall have a contact angle of greater than 10° to the faces of the test specimens. Make transverse cuts, neatly to give sharp edges and a fine-sawn finish to the end-grain surfaces, to give test specimens (50 ± 0,5) mm long. The specimens shall originate from a minimum of three trees or shall be taken at random from a stock originally of more than 500 test specimens. 7.4 Dimensions of test specimens The dimensions of each test specimen after reaching equilibrium in the conditioning chamber (5.3.2) shall be (50 ± 0,5) mm × (25 ± 0,5) mm × (15 ± 0,5) mm. For the purposes of calculating the mass of preservative retained per unit volume of wood (8.1.2.2) the nominal volume of each test specimen shall be taken as 18,75 cm3. Mark each test specimen so that it can be identified throughout the test. 7.5 Number of test specimens The number of test specimens required is given in Table 1. It is advisable to treat more than the specified number of test specimens so that, after weighing, any test specimens with abnormally high or low retentions can be rejected from the batch.

2) In southern European countries the species of pine most frequently infested by Hylotrupes bajulus may be used as an alternative, provided that the suitability of the species for use in the tests specified in this document has been demonstrated in all aspects (development of larvae, resistance to impregnation, etc.). SIST EN 47:2017

EN 47:2016 (E) 10 8 Procedure 8.1 Preparation of test specimens 8.1.1 Conditioning of test specimens before treatment Allow the test specimens to condition in the conditioning chamber (5.3.2), for a minimum of two weeks. 8.1.2 Treatment of the test specimens 8.1.2.1 Preparation of the treatment solutions 8.1.2.1.1 Solid preservatives Water-soluble preservatives: — dissolve the preservative in the water (5.2.2) in a series of concentrations. Non-water-soluble preservatives: — dissolve the preservative in an appropriate solvent (5.2.3) in a series of concentrations. 8.1.2.1.2 Liquid preservatives If appropriate, use the preservative without further preparation other than any necessary stirring. If it is a concentrate, dilute the preservative with the diluent to the required working concentration, using the procedure specified by the manufacturer. All treatment solutions shall be freshly prepared. 8.1.2.1.3 Preparation Prepare a series of at least five concentrations by mass, distributed evenly about the expected toxic values. A solvent or diluent control, i.e. treatment at concentration = 0, shall also be used. If the approximate toxic values are unknown, the concentrations shall form a widely spaced geometric progression for a first test and a more closely spaced geometric or arithmetic progression for subsequent tests. All treatment solutions shall be freshly prepared. 8.1.2.2 Impregnation Carry out impregnation in ascending order of concentration, starting with the solvent control (concentration = 0). The following procedure ensures the required complete impregnation of test specimens by the test solutions. For each concentration weigh each test specimen, to the nearest 0,05 g, and then stack the test specimens in one of the treatment vessels (5.3.5) so that as much of their surface as possible is exposed (e.g. by piling them crosswise). Ballast the stack of test specimens with the weights (5.3.6) to prevent them from floating later when the liquid is admitted. Place each beaker in one of the vacuum vessels (5.3.8), attach the vacuum pump (5.3.9) and reduce the pressure to 700 Pa. Maintain it for 15 min. Observe the proper safety measures for vacuum vessels. After this period, close the stopcock to the vacuum pump (5.3.9) and

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