Product Safety Reference Manual Book 5 - Laboratory Policies and Procedures C17-1 2003-01-20Part B: Test Methods Section, Method C-17DETECTION OF CELLULOSE NITRATE IN CHILDRENS OPTICAL FRAMES, TOYS AND OTHER CONSUMER PRODUCTS 30 1 SCOPE1.1 This method describes a general procedure for the detection of cellulose nitrate in childrensoptical frames, toys and other consumer products applicable as per items 6 and 7 of Part Iof Schedule I of the Hazardous Products Act.2 APPLICABLE DOCUMENTS2.1 ASTM Standard test method for quantitative determination of cellulose nitrate in alkydmodified lacquers by infrared spectrophotometry, D-3133, 1996.2.2 J. Haslaw, H.A. Willis and D.C.H. Squirrel, Identification and Analysis of Plastics, 2nd edition,Butlerworth and Co., Chapter 2, 1972.2.3 Project report 98-0467 “Determination of cellulose nitrate in childrens toys.”2.4 B. Sguin “Revision of Method C17 - Detection of cellulose nitrate in childrens optical frames,toys, and other consumer products”, Health Canada, PSL, Project report no. 2002-0712(2003).3 REAGENTS AND APPARATUS3.1 Infrared spectrophotometer equipped with Fourier Transform acquisition system3.2 Electric grinder3.3 Infrared lamp3.4 Acetone, A.C.S. Certified3.5 Dichloromethane, Optima Grade3.6 Tetrahydrofuran, HPLC Grade3.7 Aluminium platter (weighing pan)3.8 Potassium bromide (KBr), IR Grade3.9 Hydraulic Press used for making KBr pellets (maximum pressure 25 tons)3.10 Cellulose nitrate filters (Whatman 0.45 :m, 25 mmn)3.11 KBr die kit3.12 Polystyrene NIST standards4 EXPERIMENTAL PROCEDURE4.1 Cut sample in small fragments. Deposit the sample fragments on an aluminium platter anddissolve them using acetone, dichloromethane, or tetrahydrofuran, depending on the type ofplastic. Allow the organic solvent to evaporate at room temperature in order to collect theplastic film that is formed using this procedure. An infrared lamp may be used to reduce thedrying time. Product Safety Reference Manual Book 5 - Laboratory Policies and Procedures C17-2 2003-01-20Part B: Test Methods Section, Method C-17DETECTION OF CELLULOSE NITRATE IN CHILDRENS OPTICAL FRAMES, TOYS AND OTHER CONSUMER PRODUCTS 30 4.2 If a film is produced it can be used in the sample holder (section 4.4). If no film is produced,ground in fine particles, the plastic material using an electric grinder and follow theinstructions of section 4.2.1. 4.2.1 Disc preparationFor better results, drying of KBr powder is best done by leaving it in a shallow dishin an oven at 120/C for approximately 24 hours. It may then be transferred in abottle and kept in a dessicator.The preparation of a disc without adding any sample is prepared to check thebackground signal.- Place 3 micro-spatula scoops (approximately 0.225 g) of KBr in the mortar. Smashand mix the mixture using the mortar and pestle. - Use the KBr die kit (See Appendix) to form a disc. Before preparing the discs,make sure that all parts of the die assembly are clean and dry. Use a Kimwipe orother suitable tissue and water to clean them. - Assemble the base and cylinder.- Place one of the pellets polished face up into the cylinder. - Place a quantity of powder into the cylinder, enough to cover the pellet. - Distribute the powder as evenly as possible by lightly shaking. - Drop the top pellet into the cylinder (polished surface down) and press down lightlywith the plunger. - Place the die under the pellet press and adjust the height by turning the blackwheel at the surface of the press. - Operate the handle until the pressure is 5 tons, wait 5 minutes. - Release the pressure slowly to zero.- Operate the handle until the pressure is 10 tons with the handle and wait anadditional 10 minutes.- Release the pressure slowly to zero.- Remove the die from the press- Invert and support the rest of the assembly on the plunger- Remove the base slowly- On a counter, slowly apply a pressure on the plunger until it moves up through thecylinder lifting the lower pellet and the KBr disc clear of cylinder- Place the disc on the support for analysisNote: It is advisable to handle the discs with tweezers, NEVER touch disc with barehands. Product Safety Reference Manual Book 5 - Laboratory Policies and Procedures C17-3 2003-01-20Part B: Test Methods Section, Method C-17DETECTION OF CELLULOSE NITRATE IN CHILDRENS OPTICAL FRAMES, TOYS AND OTHER CONSUMER PRODUCTS 30 4.2.2 Preparation of a sample disc- Mix the sample with some KBr in a approximate proportion of 1 part sample: 3parts KBr (1:3) and follow the instructions as above (section 4.2.1).- The sample is then ready for analysis (see section 4.4).4.3 FT-IR Instrument set-up parametersSelect the following experiment “C17- Detection of cellulose n