1、 FORD LABORATORY TEST METHOD FLTM BZ 157-01 Date Action Revisions Rev. 1 2011 03 11 Revised Added preferred use of GC/MSS. S.Riewer, FOE 2009 01 03 Activated S.Riewer, FOE Printed copies are uncontrolled Copyright 2011, Ford Global Technologies, LLC Page 1 of 4 DETERMINATION OF ORGANIC EMISSIONS FRO
2、M NON-METALLIC MATERIALS IN VEHICLE INTERIORS BY HEADSPACE GAS CHROMATOGRAPHY Application This test method is used to determine emissions of organic compounds (TVOC = total volatile organic compounds) which are given off from non-metallic materials in the immediate vicinity of or inside vehicle inte
3、riors. The sum of individual substances according to a gas chromatography analysis and detection with a flame ionization detector (GC/FID) or mass selective detector (GC/MS) is used as a measure of the total emission of a material. It is preferred to use GC/MS as this technology delivers more accura
4、te and more reliable results. Usage of GC/FID must be agreed by Ford Materials Engineering prior to testing. The test is performed using Head-Space technique after tempering at 120 C. The relevant sampling points, requirements and special provisions relating to the execution of the test can be found
5、 in the appropriate specifications and drawings, etc. If components are made up of a number of different materials, separate tests may be required for each individual material. Apparatus and Materials Required Acetone p.a. Butanol p.a. Gas Chromatograph for capillary column operation with Head-Space
6、 test vessel, flame ionization detector (FID) or mass selective detector (MSD) and computer/integrator. WCOT capillary column with a separation phase of 100 % polyethylene glycol (so-called wax type, e.g. DB wax, Carbowax, etc.), 0.25 mm internal diameter, 0.25 um film thickness and 30 m length. Ana
7、lytical balance with an accuracy of 0.1 mg Micro liter syringe, 5 L Beakers Graduated flasks FORD LABORATORY TEST METHOD FLTM BZ 157-01 Printed copies are uncontrolled Copyright 2011, Ford Global Technologies, LLC Page 2 of 4 Conditioning and Test Conditions Transport and storage of the samples shal
8、l take place in an aluminium-clad polyethylene bag. Sampling shall take place immediately after delivery or in a condition equivalent to that status. The dates of delivery and sampling shall be recorded. Conditioning of the sample is not normally required. One exception is natural materials (cotton,
9、 wood, leather, wool). These materials must be divided up into small pieces, dried for 24 h over calcium chloride (CaCI2) and then weighed. The sample must be taken at the stipulated point over the entire section of the component. It must be broken (without causing it to heat up) into pieces weighin
10、g between 10 mg and 25 mg. Other types of sample preparation may be indicated, if necessary, on the drawing or in the Technical Regulation (TR). This must be stated in the report of the results. The test quantity to be weighed depends on the size of the Head-Space vessel, which shall have a minimum
11、volume of 5 ml. For a 10 ml Head-Space vessel, 1,000 g 0.001 g (i.e. a maximum weighing error of 0.1 %) of the sample shall be weighed. Metal parts shall be removed before weighing. Organic substances such as paint and adhesive, etc., which are firmly attached to metal parts shall be removed by mech
12、anical means and then weighed. The sample is weighed in the Head-Space vessel (at least three Head-Space vessels per sample). The Head-Space vessel is then sealed in a gas-tight fashion with the help of a septum, with the Teflon coating on the side facing the interior of the Head-Space vessel. Metho
13、d Immediately before the measurement, the Head-Space vial is tempered to 120 + 1 C. The test period in the Head-Space is 5 h 5 min at 120 1 C, and the analysis shall take place immediately thereafter. At least three samples of each material shall be analyzed. The blind value is determined by means o
14、f the mean value from at least three measurements with empty Head-Space vessels. Metering shall take place in an identical and reproducible fashion in conjunction with all analyses of samples, blind values and calibration solutions. The column shall be burned off once a week by heating the column to
15、 its maximum operating temperature for 15 minutes. GC oven temperature Program: 3 min isothermal at 50 C Heating to 200 C at a rate of 12 C/min 4 min isothermal at 200 C Injector temperature: 200 C Detector temperature: 250 C Split ratio: approx. 1 : 20 Carrier gas: helium Mean carrier gas velocity:
16、 approx, 22 - 27 cm/s Note: The substance 2.6-di-tertiary-butyl-methylphenol (BHT) shall exhibit a retention time of less than 16 minutes. FORD LABORATORY TEST METHOD FLTM BZ 157-01 Printed copies are uncontrolled Copyright 2011, Ford Global Technologies, LLC Page 3 of 4 Calibration Calibration curv
17、es according to the “External Standard“ method are used for the quantitative determination of TVOC emissions and the quantity of individual sub-stances. Acetone is used as the calibration substance for TVOC emissions, and the substances themselves are used for the individual substances. After instal
18、lation of a new column or other modification to the equipment, a basic calibration shall be performed with seven calibration concentrations. A control calibration shall also be carried out at least every 4 weeks with at least three concentrations. For the basic calibration of the acetone, seven diff
19、erent calibration solutions shall be prepared with concentrations of 0.1 / 0.5 /1 / 5 /10 / 50 and 100 g of acetone per liter in n-butanol. A control calibration shall have been carried out beforehand with the three concentrations 0.5 / 5 and 50 g of acetone per liter. The reason for this is to ensu
20、re in advance that no peaks occur in the n-butanol at the same time as acetone. Calibration Solutions in the same concentrations as for the acetone control calibration shall be prepared for the individual substances, in conjunction with which a solvent with a boiling point below 120 C shall always b
21、e used. The solvent must not exhibit peaks at the same time as the individual substance, All the substances used for calibration shall be of at least analytically pure quality (pro analysis, p.a.). The calibration measurement is performed by using a 5 L syringe to inject 2 L 0, 02 L (i.e. max. 1 % i
22、njection error) per 10 ml of tube volume into an empty, open Head-Space vessel. When filling the syringe, attention must be paid to ensuring that no air bubbles are present inside the cylinder. The vessel shall be sealed immediately. The calibration samples are tempered for 1 h at 120 C in the Head-
23、Space vessel and are then analyzed in accordance with the general testing instructions, in conjunction with which the temperature program of the gas chromatograph can be interrupted after elution of the solvent. Each calibration solution shall be analysed at least 3 times. The areas found for each c
24、alibration substance are plotted on the y-axis as an function of the concentration of the calibration Solutions (in g/l). This produces a straight line, the slope of which represents the calibration factor k (k(G) for the total emission, and k(i) for the emissions of individual substances. These sha
25、ll be estimated using the least squares method. The correlation coefficient k shall be greater than 0.995 in this case. Evaluation It shall be possible to read off from the data recorded on the gas chromatogram the total area of the peaks and the areas for the individual substances indicated on the
26、drawing or in the TR. Only peaks that fulfil the following criteria shall be included in the calculation of the total area: - peaks, whose height exceeds the noise of the base line by at least 3 times, and whose area is greater than 10 % of the peak for the acetone area, where the concentration in t
27、he calibration solution was 0.5 g/L. The detection limit of the analytical procedure shall give a peak area and a peak height that are at all times less than 10 % of the actual value obtained with acetone for an analysis of a calibration solution with a concentration of 0.5 g/L of acetone. FORD LABO
28、RATORY TEST METHOD FLTM BZ 157-01 Printed copies are uncontrolled Copyright 2011, Ford Global Technologies, LLC Page 4 of 4 The desired emission values can be found from the measurement results, as follows: Total carbon emission, EG: EG is calculated from the total area obtained from the analysis of
29、 the samples (ATS) minus the total area of the blank (ATB ) and the calibration factor k(G) from the acetone calibration The unit is gC/g (g carbon per g sample). The factor 2 arises from the relationship to “g sample“ and is obtained by placing 1 g of sample, but 2 L of calibration solution, in a 1
30、0 mL test vessel. The factor 0.6204 is the proportion of carbon by mass in the acetone (3*M(C)/M(C3H6O). Emissions of individual substances Ei: Eis are calculated from the peak area obtained from the analysis of the samples for the substance under investigation (Ai ), and from the calibration factor
31、 k(i) from the calibration of the individual substance The unit is g/g (g substance per g sample). The factor 2 relates to “g sample“ and is obtained by placing 1 g of sample, but 2 L of calibration solution, in a 10 mL test vessel. The results of the three measurements performed on a component may
32、not be used to determine the mean values, but all three measured values shall fulfil the requirements. This is necessary in order to be able to guarantee that the requirements are fulfilled in all areas on the component. Test Report The test report shall include the following: 1. Reference to this s
33、tandard 2. All the necessary details for identifying the test object 3. Documented results for each test, also indicating a mean value 4. Any special characteristics of the samples noted during testing and their condition 5. Date of manufacture and manufacturer of the test material, if known 6. Date of sampling. 6204.02)( = Gk AAE TBTSG2)( = ikAE ii
