1、October 2016 English price group 9No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 13.340.40!%n8“2577521www.din.deDI
2、N EN 16778Protective gloves The determination of Dimethylformamide in gloves;English version EN 16778:2016,English translation of DIN EN 16778:2016-10Schutzhandschuhe Bestimmung von Dimethylformamid in Handschuhen;Englische Fassung EN 16778:2016,Englische bersetzung von DIN EN 16778:2016-10Gants de
3、protection Dtermination de la teneur en dimthylformamide dans les gants;Version anglaise EN 16778:2016,Traduction anglaise de DIN EN 16778:2016-10www.beuth.deDocument comprises 13 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative
4、.09.16 DIN EN 16778:2016-10 2 A comma is used as the decimal marker. National foreword This document (EN 16778:2016) has been prepared by Technical Committee CEN/TC 162 “Protective clothing including hand and arm protection and lifejackets” (Secretariat: DIN, Germany). The responsible German body in
5、volved in its preparation was DIN-Normenausschuss Persnliche Schutzausrstung (DIN Standards Committee Personal Protective Equipment), Working Committee NA 075-05-08 AA Handschutz. EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16778 March 2016 ICS 13.340.40 English Version Protective gloves -
6、The determination of Dimethylformamide in gloves Gants de protection - Dtermination de la teneur en dimthylformamide dans les gants Schutzhandschuhe - Bestimmung von Dimethylformamid in Handschuhen This European Standard was approved by CEN on 30 January 2016. CEN members are bound to comply with th
7、e CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Managemen
8、t Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status
9、as the official versions. CEN members are the national standards bodies of 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, N
10、etherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2016 CEN All
11、 rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16778:2016 EEN 16778:2016 (E) 2 Contents PageEuropean foreword . 3 1 Scope 3 2 Normative references 4 3 Principle . 4 4 Consumables . 4 4.1 Reagents . 4 4.2 Stock solutions . 4 4.2.1 Interna
12、l standard Stock solution (1000 mg/l) 4 4.2.2 Internal standard working solution (200 mg/l). 4 4.2.3 Target compound Stock solution (1000 mg/l) 5 4.2.4 Target compound working solution (200 mg/l) 5 4.2.5 Extraction solution containing 20 mg/l internal standard 5 5 Equipment . 5 6 Test procedure . 5
13、6.1 Sampling . 5 6.2 Conditioning 5 6.3 Preparation . 6 6.4 Extraction . 6 6.5 Determination with GC-MS 7 6.5.1 Calibration . 7 6.5.2 Examples of instrumental method 7 6.6 Quantification . 8 6.7 Results . 9 7 Performance of the method . 9 8 Test report . 9 Annex A (informative) Results of the interl
14、aboratory trial . 10 Bibliography . 11 DIN EN 16778:2016-10 EN 16778:2016 (E) 3 European foreword This document (EN 16778:2016) has been prepared by Technical Committee CEN/TC 162 “Protective clothing including hand and arm protection and lifejackets”, the secretariat of which is held by DIN. This E
15、uropean Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by September 2016, and conflicting national standards shall be withdrawn at the latest by September 2016. Attention is drawn to the possibility that some of
16、the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European
17、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
18、, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 16778:2016-10 EN 16778:2016 (E) 4 1 Scope This document specifies a test method for the determination of Dimethylformamide (DMFa CAS N 68-12-2) in glove materials. NOTE For Dimethylformamide the following abbreviations can be used:
19、DMF, DMFa DMFo. The test method is applicable for the following materials: polyurethane (PU) materials (except elastane), PU Coated material (textile, leather), PU foam, PU blended materials; adhesives; all materials manufactured with a dipping process using DMFa. 2 Normative references Not applicab
20、le. 3 Principle The sample is cut into small pieces and extracted with methanol in a sealed flask in an ultrasonic bath. An aliquot of the extract is analysed with GC-MS. 4 Consumables 4.1 Reagents The substances are given in Table 1. Table 1 Reagent used in analysis N Substances CAS-Nr. purity 1 N,
21、 N-Dimethylformamide (DMFa) 68122 Certified standard (purity 95 % at least) 2 Dimethylformamide-d7 (DMFa-d7) 4472417 Certified standard (purity 95 % at least) 3 Methanol 67561 analytical grade (purity 99 % at least) 4.2 Stock solutions 4.2.1 Internal standard Stock solution (1000 mg/l) 100 mg of DMF
22、a-d7 is weighed with an accuracy of 0,1 mg in a 100 ml volumetric flask and filled with methanol to the mark and stored at 4 C, for maximum 1 month. 4.2.2 Internal standard working solution (200 mg/l) The solution is prepared by 1:5 dilution of the stock solution (4.2.1) with methanol. Storage condi
23、tions maximum of 1 month at 4 C. DIN EN 16778:2016-10 EN 16778:2016 (E) 5 4.2.3 Target compound Stock solution (1000 mg/l) 100 mg of DMFa is weighed with an accuracy of 0,1 mg in a 100 ml volumetric flask and filled up to the mark with methanol and stored at 4 C for maximum 1 month. 4.2.4 Target com
24、pound working solution (200 mg/l) The solution is prepared by 1:5 dilution of the stock solution (4.2.3) with methanol. Storage conditions maximum of 1 month at 4 C. 4.2.5 Extraction solution containing 20 mg/l internal standard Add 100 ml internal standard working solution (4.2.2) in a 1000 ml volu
25、metric flask and fill it with Methanol to the 1000 ml calibration mark. This solution can be stored in a vessel at 4 C for 6 months. 5 Equipment Usual lab equipment, in addition: 5.1 analytical balance (precision at least 0,1 mg); 5.2 sealed flask (for instance, Erlenmeyer) with screw cap and polyte
26、trafluoroethylene (PTFE) seal, 250 ml; 5.3 ultrasonic bath capable of maintaining a temperature of (70 5) C; 5.4 PTFE-membrane filter pore width 0,45 m; 5.5 suitable sample vials with PTFE-capped for GC-MS analysis; 5.6 volumetric flask, 10 ml, 100 ml, 1000 ml; 5.7 range of micropipettes and dispens
27、er with volume between 20 l to 200 ml; 5.8 gas chromatograph with mass detector. 6 Test procedure 6.1 Sampling The sample shall consist of a least a pair of gloves. 6.2 Conditioning When the gloves are received, the laboratory shall package them into an airtight plastic sealed bag (e.g. polyethylene
28、 bag) before the start of the preparation steps. Vacuum sealer shall not be used. If stored for more than 24 h before testing, the gloves shall be kept at (4 3) C. NOTE During the validation interlaboratory test, it has been demonstrated that a15 days storage in sealed plastic bag at 4 C has shown n
29、o significant difference in results. The sample (in the seal plastic bag) shall be conditioned (24 1) hours at (23 2) C prior to the preparation. DIN EN 16778:2016-10 EN 16778:2016 (E) 6 6.3 Preparation The sample is removed from the plastic bag. Cut a piece as shown in Figure 1 from each glove of t
30、he pair to have 2 test pieces. Each test pieces is a full finger including the strips from the palm and the back of the glove. The sampling is carried out so that all materials are included. Cut each of the 2 test pieces into pieces of about 10 mm by 10 mm. Immediately after use an analytical balanc
31、e (5.1) to weigh each of the 2 cut up test pieces to an accuracy of 0,1 g. Key: 1 cut d (30 5) mm NOTE The shaded area is the test piece Figure 1 Cutting of the test piece 6.4 Extraction The extraction shall be started maximum (30 5) minutes after the weighing of the tests pieces. Each test piece is
32、 put in a 250 ml Erlenmeyer flask. (5.2). Add the stored extraction solution (4.2.5) at a ratio of 10,0 ml per 1,0 g cut up test piece. The closure is to maintain safe and gas tight, throughout the complete extraction. The sample is then extracted 30 min at a temperature of 70 C in an Ultrasonic bat
33、h. DIN EN 16778:2016-10 EN 16778:2016 (E) 7 WARNING Extraction at 70 C leads to overpressure and the risk of uncontrolled emission of Methanol and loss of DMFa. After cooling to room temperature, the solution is filtered through a PTFE membrane filter (5.4). An aliquot of the extract is transferred
34、to a GC-MS vial and sealed with a PTFE-cap (5.5). The sealing should be done by well-trained operator to avoid any leakage. 6.5 Determination with GC-MS 6.5.1 Calibration Five calibrations points are used to establish the calibration curve, they are all prepared in 10 ml volumetric flasks, as stated
35、 in Table 2. A 6th point, L0,a blank, shall be included in the calibration curve. Table 2 Preparation of calibration Standard L1 L2 L3 L4 L5 Volume of target compound working solution (4.2.4) in l 25 50 100 250 500 Conc. of target compound in the solution in mg/l 0,5 1 2 5 10 Volume of the of intern
36、al standard working solution (4.2.2) in l 1000 1000 1000 1000 1000 Concentration of the internal standard in mg/l 20 20 20 20 20 Standard L1L2L3L4L5Volumetric flasks are filled to the mark with methanol 6.5.2 Examples of instrumental method 6.5.2.1 Measuring method Suggested parameters for GC-MS det
37、ermination of DMFa. Measuring parameter: The DMFa is analysed by gas chromatography/mass spectrometry on a single quad/MS use in a simultaneous SIM/SCAN mode. 6.5.2.2 Chromatographic conditions a) COLUMN: polar stationary phase based on Polyethylene Glycol; length: 30 m; internal diameter: 250 m; DI
38、N EN 16778:2016-10 EN 16778:2016 (E) 8 film thickness: 0,5 m; (alternative column possible as long as it has the same properties). b) CARRIER GAS: helium. c) OVEN: 60 C during 2 min; 250 C at 20 C/min; 250 C during 2 min. d) INJECTOR: 240 C in splitless mode with an injection volume of 1 l. 6.5.2.3
39、Detection conditions a) TRANSFER LINE: 240 C: The single quad MS work in simultaneous SIM/SCAN mode; The mass SCAN range is between 40 to 200 uma. Table 3 The SIM mode focus on the following ions Compounds Ions DMFa 73 (quantifier) 44 (qualifier) DMFa-d7 80 (quantifier) 6.6 Quantification The DMFa c
40、ontent is calculated according to the following equation as a mass fraction w in mg/kg of glove. Set up the linear regression function by using the following ratio (Ae/Ais) and (Ce/Cis) with the help of the formula: =+ eeis isACab Where: Aeis the area of the peak of Dimethylformamide; Aisis the area
41、 of the peak of Dimethylformamide-D7; Ceis concentration of Dimethylformamide in the calibration standard in microgram per litter; CISis concentration of Dimethylformamide-D7 in the calibration standard in microgram per litter; a is the slope of the linear function; DIN EN 16778:2016-10 EN 16778:201
42、6 (E) 9 b is the ordinate intercept of the calibration curve, in mg/l. The content of DMFa is calculated according to the following equation as a mass fraction w in mg/l: =echisisAbAVWCmaWhere: W is the content of the Dimethylformamide in the specimen (mg/l); V is the volume of the solvent use for t
43、he extraction (ml) (in most cases, this value will be equal to 10 ml); m is the mass of the tested specimen (g); Aechis the area of the peak of Dimethylformamide in the sample; Aisis the area of the peak of Dimethylformamide-D7 in the sample; CISis concentration of Dimethylformamide-D7 in the sample
44、 in microgram per litter; a is the slope of the linear function; b is the ordinate intercept of the calibration curve. The units depend of the evaluation. 6.7 Results Each determination result shall be reported. The final result is the average (Mv) of the 2 values obtained on the 2 test pieces. 7 Pe
45、rformance of the method Quantification limit of this test method is 5 mg/kg of DMFa in gloves or glove components. 8 Test report The test report shall include at least the following: reference to this standard; description of the packaging at reception; all details necessary for complete identificat
46、ion of the sample tested; date of reception of the sample in the laboratory; date of the test; condition and time of storage before the test in the laboratory; used analytical technic; the determined content of the extracted DMFa is given in ppm (see 6.7); any deviation from the present standard. DI
47、N EN 16778:2016-10 EN 16778:2016 (E) 10 Annex A (informative) Results of the interlaboratory trial The following data have been obtained in a collaborative correlation trial organized by CEN/TC 162 WG 8 in November/December 2013 with a group of relevant laboratories (on demand from CEN/TC 162 secret
48、ariat). Table A.1 Results of correlation trial Number of laboratories Number of measurement per laboratory Average value Standard deviation Spiked sample with 10ppm 8 1 12,5 7,0 Spiked sample with 200ppm 5 1 197,7 8,0 Dipped Polyurethane test pieces with dynema 5 4 33,7 5,3 Dipped Polyurethane test
49、pieces with nylon 7 4 761,4 130,9 DIN EN 16778:2016-10 EN 16778:2016 (E) 11 Bibliography CEN ISO/TS 16189, Footwear - Critical substances potentially present in footwear and footwear components - Test method to quantitatively determine dimethylformamide in footwear materials (ISO/TS 16189:2013) DIN EN 16778:2016-10
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