1、 FORD LABORATORY TEST METHOD BZ 108-01 Date Action Revisions 2017 01 23 Released D. Stark, NA Controlled document at www.MATS Copyright 2017, Ford Global Technologies, LLC Page 1 of 6 10-L BAG METHOD FOR MEASURING VOC EMISSIONS FROM VEHICLE INTERIOR MATERIALS Application This procedure is used as a
2、material-level screening method for the emissions of selected volatile organic compounds (VOCs) and total volatile organic compounds (TVOCs). Apparatus and Materials Required Gas Chromatograph Mass Spectrometer (GC-MS) Agilent GC6890N(7890A)/MS5975B (or equivalent) High Performance Liquid Chromatogr
3、aphy (HPLC) Agilent 1100 or 1260 from , Shimadzu LC20A from , Thermo U-3000 from (or equivalent) Thermal Desorption Markes TD-100 (or equivalent) Thermal Desorption Unit (TDU) Gerstel Twister (or equivalent) with CIS4 cold injection system and 012440-004-00 straight liner, no packing Thermal Desorp
4、tion System Autosampler (TDSA) Gerstel TDSA2 with CIS4 cold injection system and 013238-005-00 straight liner packed with 10 mg Tenax TA (or equivalent) Note: This system should not be used for the testing of leather Mechanical convection oven Capable of maintaining a temperature of 100 0.5 C, typic
5、al chamber size is 0.4 m3 10 Liter Sample bag 10-L polyvinyl fluoride (PVF) Tedlar bag with Polytetrafluoroethylene (PTFE), stainless steel, or polypropylene (PP) valves, typical bag size is approximately 33 cm x 50 cm or 30 cm x 56 cm. The bags should be capable of being sealed with either plastic
6、locking rail or heat seal. Alternative bag material must demonstrate equivalency. Purchasing pre-cleaned sample bags is recommended. Suitable suppliers for sampling bags: Dalian Delin Gas Packaging Co., Ltd. 240 Sanyuan St, Xigang District, Dalian, Liaoning, China Tel: 86-0411-83703385 or 86-0411-83
7、671536 Fax: 86-0411-83706065 Sampling Bag Technologies, LLC 27491 Schoolcraft, Livonia, MI 48150 734-525-8600 FORD LABORATORY TEST METHOD BZ 108-01 Controlled document at www.MATS Copyright 2017, Ford Global Technologies, LLC Page 2 of 6 Restek Corporation, U.S. Catalog #: 22053 110 Benner Circle,
8、 Bellefonte, PA 16823 1-800-356-1688, ext. 3 William Vecere S 248-866-3913 Troy, MI USA Jensen Inert Products Catalog #: GSTP0101219LJCP 3773 NW 126th Avenue #1 Coral Springs, FL 33065 954-344-2006 Thermal Desorption (TD) Tube Gerstel TDU Tubes - Gerstel Carbopack B / Carbopack X (part number: 01
9、5954-005-00) Note: Preferred for the testing of leather Gerstel TDSA Tubes - Tenax TA or Carbotrap 300 Note: Carbotrap 300 should not be used for the testing of leather Markes TD Tubes - Tenax TA 2,4-dinitrophenylhydrazine (DNPH) Cartridge Waters Corporation: Sep-Pak silica cartridge, catalogue numb
10、er WAT037500 (or equivalent) Bonna-Agela Technologies: Cleanert IC-DNPH (or equivalent) Sampling pump, such as Gillian IAQ-Pro (or equivalent) Gas flow meter, such as Bios International Corp. DCL-M (or equivalent) Mass flow controller, such as Brooks Instrument 5850E, use a mass flow controller wi
11、th a 1 to 3 LPM flowrate to fill the bags Vacuum pump, such as Jin Teng GM-1.0A from (or equivalent) TD tube conditioning chamber, Markes TC-20 for Markes tubes, ; Gerstel tube conditioner for Gerstal tubes, Sampling Assembly Transfer lines, PTFE or equivalent material; Outside diameter: 6 mm; Ins
12、ide diameter: 4 mm Connection fit, such as Ultra-Torr Vacuum Fittings with O-rings, Part No. SS-4-UT-6 from (or equivalent) Sealing strips: for sealing the sampling bag; or other sealing methods as long as the bag passes a leak check. Ultra High Purity (UHP) Nitrogen (N2): 99.999% purity, hydrocarb
13、on concentration 0.5 ppm Ultra High Purity (UHP) Helium (He): 99.999% purity, hydrocarbon concentration 0.5 ppm FORD LABORATORY TEST METHOD BZ 108-01 Controlled document at www.MATS Copyright 2017, Ford Global Technologies, LLC Page 3 of 6 Bag Cleaning Procedure The following cleaning procedure can
14、be used if pre-cleaned 10-L PVF Tedlar bags are not available for purchase: 1. Heat the bag to100 C for 24 hours. 2. After heating the bag, install the sample port, seal, and evacuate the bag. Evacuation of the bag should take no longer than one minute and maintain consistent evacuation time from ba
15、g to bag. 3. Test bags should be cleaned in lots. Mark the bags to insure from the same lot. 4. Each lot of bags shall be comprised from the same material roll, heated, sealed, and evacuated as a group. Conditioning of Materials and Specimen Preparation Note: Whenever handling the specimens, samples
16、, and sampling bags, nitrile gloves shall be worn. 1) Cut 10 x 20 cm test specimens and begin conditioning for 14 28 days at 23 2 C and 50% relative humidity and pressure. 2) After conditioning for 14 28 days, the test specimens must either be tested immediately or placed in a new polyethylene (PE)
17、coated aluminium bag, or wrapped tightly in silicone-free aluminum foil then placed in a new PE bag, until testing. Note: Any samples bagged and not immediately tested should go back in the conditioning room/chamber at 23 2 C and 50% relative humidity until testing begins. Note: Suppliers shall subm
18、it a minimum of two (2) specimens per test. One (1) specimen per test will be used as backup. Samples should not be exposed to air in contaminated locations or locations with poor air quality (such as paint shops, etc.) The entire surface area of the test specimen should be exposed to air (i.e. leat
19、her should not be folded to itself) 10 L Sample Bag Procedure NOTE: Sampling procedure steps 1 10 shall be performed concurrently, without interruption. 1. Use conditioned TD tubes and a properly stored DNPH cartridge. The sampling system transfer lines shall be as short as possible. 2. Record the s
20、pecimen dimensions (cm) and mass (g). Open the sampling bag. Place the specimen into the sampling bag. Immediately seal the sampling bag. Photograph the specimen in the bag. Note: The specimen shall be put into the bag with the “A” surface facing up. The “A” surface is defined as the surface exposed
21、 to the customer in a vehicle. 3. Evacuate until all the air is removed from the bag (approximately 10 seconds). 4. Leak check the bag with a vacuum gauge. 5. Fill the bag with 6.0 L 0.2 L of N2. 6. Place the sample bag into the pre-heated oven at 65 2 C. Each bag shall be positioned flat on the rac
22、ks and attach to the sampling assembly. The bag is not allowed to touch the inner side of the oven or other bags. 7. Heat the sample for 2 hours 2 minutes. FORD LABORATORY TEST METHOD BZ 108-01 Controlled document at www.MATS Copyright 2017, Ford Global Technologies, LLC Page 4 of 6 8. Use Table 1 b
23、elow to select the appropriate sampling pump flow rates. Table 1 Sampling Conditions Item 10L bag Sampling media Two (2) TD Tubes DNPH Cartridge Flow rate (mL/min) 100 to 200 500 to 850 Sampling volume (L)* 1 L per tube 3 *Use the final collected sample volume in the calculations to determine collec
24、ted mass and bag concentrations 9. Collect the evolved samples from the sample bag. 10. Once sampling is completed, remove the TD tubes and DNPH cartridge. Cap and seal the TD tubes. Place the DNPH cartridge inside a sealed aluminized Mylar bag. Store the sealed TD tubes and DNPH cartridge at 4 2 C.
25、 The analysis of the TD tubes and DNPH cartridge must be performed within 7 days. 11. Analyze the TD tubes using the following references: a. ISO/DIS 16000-6: Indoor Air part 6: Determination of Volatile Organic Compounds in Indoor and Test Chamber Air by Active Sampling on Tenax TA Sorbent, Thermal
26、 Desorption and Gas Chromatography MS/FID. International Organization for Standardization, Geneva, Switzerland b. Compendium TO-17: Determination of Volatile Organic Compounds in Ambient Air Using Active Sampling Onto Sorbent Tubes. Compendium of Methods for the Determination of Toxic Organic Compou
27、nds in Ambient Air, Second Edition, Center for Environmental Research Information, Office of Research and Development, U.S. Environmental Protection Agency 12. Analyze the DNPH cartridge using the following references: a. ISO/DIS 16000-3: Indoor Air part 3: Determination of Formaldehyde and Other Ca
28、rbonyl Compounds in Indoor Air and Test Chamber Air Active Sampling Method. International Organization for Standardization, Geneva, Switzerland b. Compendium TO-11A: Determination of Formaldehyde in Ambient Air Using Adsorbent Cartridge Followed by High Performance Liquid Chromatography (HPLC) (Acti
29、ve Sampling Methodology). Compendium of Methods for the Determination of Toxic Organic Compounds in Ambient Air, Second Edition, Center for Environmental Research Information, Office of Research and Development, U.S. Environmental Protection Agency 13. Calculate VOC and Aldehyde results per Appendix
30、 1. 14. Record the results using the Data Sheet in Appendix 2. FORD LABORATORY TEST METHOD BZ 108-01 Controlled document at www.MATS Copyright 2017, Ford Global Technologies, LLC Page 5 of 6 Appendix 1: Calculations for Target Compounds and TVOC 1. Target VOC compound concentrations: Cs= (MA /VT) -
31、CB Cs: concentration of each target compound in the 10-L sample bag, g/m3 MA: mass of each target compound in the sampling volume, ng VT: sampling volume of TD tube at standard temperature and pressure, L CB: concentration of each target compound in the 10-L blank bag, g/m3 2. Calculation for TVOC a
32、s toluene equivalent. TVOC area is based on the peak area integration of the VOCs between Hexane and N-hexadecane (C6C16) on the chromatogram: CT= (MT /VT) - CTB CT: concentration of TVOC in the 10-L sample bag, g/m3 MT: mass of TVOC in the sampling volume, ng VT: sampling volume of TD tube, L CTB:
33、concentration of TVOC in the 10-L blank bag, g/m3 FORD LABORATORY TEST METHOD BZ 108-01 Controlled document at www.MATS Copyright 2017, Ford Global Technologies, LLC Page 6 of 6 Appendix 2 Test Report Requirements FLTM BZ 108-01 TEST REPORT* Sample ID: Conditioning Period (Dates): Test Date: Test Sp
34、ecimen Length x Width x Thickness (mm): Test Specimen Mass (g): Sampling Conditions Sampling Bag Volume (L) TD Tube Sampling Flow Rate (mL/min) N2 Volume in the Sample Bag (L) TD Tube Sampling Volume (L) Oven Heating Temperature (C) DNPH Cartridge Sampling Flow Rate (mL/min) Heating Time (minutes) D
35、NPH Cartridge Sampling Volume (L) Test Results g/m3 Compounds Bag Detection Limits TD Tube 1 Data TD Tube 2 Data DNPH Cartridge Data Formaldehyde Acetaldehyde Acrolein Benzene Toluene o-, p-Xylenes m-Xylene Ethylbenzene Styrene Total VOC as Toluene Equivalent *NOTE: Include information recorded on M
36、ATERIAL INFORMATION LABEL. If the label was not included with shipped sample, then contact material supplier for the following information: Material type (fabric, leather, vinyl, etc) Supplier name, contact and contact information Product code/trade name Manufacturing location Ford material specification Ford vehicle program code (if applicable) Material manufacturing date Material packaging date Material ship date
