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1、标准分享网 w w w . b z f x w . c o m 免费下载 Copyright 2006 American Association of Textile Chemists and Colorists AATCC Technical Manual/2007TM 189-2002355 Developed in 2000 by AATCC Commit- tee RA57; editorially revised and reaf- firmed 2001; reaffirmed 2002; editorially revised 2005. 1. Purpose and Scope
2、 1.1 This method is for determining the amount of fluorocarbon soil-resist agent present on carpet fibers by measurement of elemental fluorine on the pile fiber. It is useful for measurement of fluorocarbon present on carpet pile fiber as tested within the practical range of 100-1000 g/g (ppm). It m
3、ay also be used for yarns treated with fluorocarbon anti-soiling agents. 2. Principle 2.1 A weighed fiber specimen is burned in an oxygen combustion flask and the released hydrogen fluoride is ab- sorbed into a sodium hydroxide solution. The fluorine content is measured as dis- solved sodium fluorid
4、e at a constant pH and ionic strength using a fluoride ion ac- tivity electrode and a specific ion meter. 3. Terminology 3.1 fluorine content, n.in textile floor coverings, the ratio of the weight of total elemental fluorine to the total weight of carpet fibers. 3.2 soil resist agent, na material ap
5、- plied to, or incorporated in, carpet face fi- ber which retards and/or limits the build- up of soil. 4. Safety Precautions NOTE: These safety precautions are for information purposes only. The pre- cautions are ancillary to the testing proce- dures and are not intended to be all inclu- sive. It is
6、 the users responsibility to use safe and proper techniques in handling materials in this test method. Manufac- turers MUST be consulted for specific details such as material safety data sheets and other manufacturers recommenda- tions. All OSHA standards and rules must also be consulted and followe
7、d. 4.1 Good laboratory practices should be followed. Wear safety glasses in all laboratory areas. 4.2 All chemicals should be handled with care. Use chemical goggles or face shield, impervious gloves and an imper- vious apron during the dispensing and mixing of the fluoride and sodium hy- droxide st
8、andards. The standards should be made and dispensed in a hood. 4.3 An eyewash/safety shower should be located nearby and a self-contained breathing apparatus should be readily available for emergency use. 4.4 Exercise care in cutting the speci- mens with the scalpel or razor blade; pro- tective glov
9、es may provide additional protection. 4.5 Oxygen supply pressure from the pressure regulator should not exceed 14 kPa (2 psi). 4.6 Do not operate the test equipment until the manufacturers operating in- structions have been read and under- stood. It is the responsibility of whoever operates the test
10、 equipment to conform to the manufacturers directions for safe op- eration. 4.7 Exposure to chemicals used in this procedure must be controlled at or below levels set by governmental authorities (e.g., Occupational Safety and Health Administrations OSHA permissible exposure limits PEL as found in 29
11、 CFR 1910.1000 of January 1, 1989). Flu- oride salts and sodium hydroxides are listed with OSHA permissible exposure limits PEL. In addition, the American Conference of Governmental Industrial Hygienists (ACGIH) Threshold Limit Values (TLVs) comprised of time weighted averages (TLV-TWA), short term
12、exposure limits (TLV-STEL) and ceiling limits (TLV-C) are recommended as a general guide for air contaminant ex- posure which should be met (see 12.1). 5. Apparatus, Reagents, Materials 5.1 1000 mL combustion flask with ball stopper (with platinum wire hook) and clamp (one each per specimen; reus- a
13、ble). 5.2 Platinum carrier basket (one per sample; reusable). 5.3 Infrared ignition cabinet. 5.4 Black paper specimen wrappers (one per sample). 5.5 Specific ion meter. 5.6 Fluoride ion selective electrode. 5.7 Reference electrode. 5.8 0.001N Sodium Hydroxide (NaOH). 5.9 TISAB (Total Ionic Strength
14、Ad- justment Buffer with CDTA (1,2-cyclo- hexanediaminetetraacetic acid) or formu- lated for fluorine analysis to prevent aluminum interference) (see 12.2). 5.10 Re-pipette or bottle-top dispenser (optional). 5.11 Sodium Fluoride (NaF) standard (see Appendix A). 5.12 Mechanical shaker (optional). 6.
15、 Calibration 6.1 Calibrate the specific ion meter us- ing the procedures described in the opera- tion manuals for the fluoride ion activity electrode and the specific ion meter. Cali- brate the voltage output on the specific ion meter to read 40.0 for every 1 g/g (ppm) fluoride in the standard solut
16、ion (see 12.3, 12.4). Calibration should be done on a daily or every shift basis. 7. Sampling 7.1 Prepare the yarn sample by remov- ing the tufts from the carpet sample with a scalpel or razor blade. Cut the tufts as close to the primary backing as possible having a stubble not greater than 1 mm. Tw
17、enty to 40 tufts are required for a sin- gle sample, depending on carpet con- struction. Place the tufts in a paper enve- lope and identify by test number. 7.1.1 Sampling Option #1. To deter- mine an overall average fluorine content of carpet fibers, take samples from across the entire width of the
18、carpet to compen- sate for possible variability in application and combine the tufts in a single envelope. 7.1.2 Sampling Option #2. To deter- mine the variability of fluorine content across a carpet sample, take multiple samples from various areas of the carpet and analyze each set of carpet tufts
19、sepa- rately (see 12.5). 8. Procedure 8.1 Weigh samples using tared weigh- ing pans. Weigh between 0.110 g and 0.150 g of randomly selected tufts from each sample and record the weight. Fold all of the weighed tufts into the black pa- per sample holder and place the paper holder into the platinum ba
20、sket. Suspend the basket from the platinum wire hook on the flask stopper. 8.2 Number each combustion flask and plastic cup. 8.3 Pipette 20.0 mL of the 0.001N so- dium hydroxide solution into the oxygen combustion flask (see 12.6). 8.4 Turn on the oxygen supply. Place the flexible plastic tube into
21、the oxygen combustion flask. Turn on the pressure regulator and allow oxygen to fill the flask for about 5-20 s. Turn off the oxy- gen flow (see 12.7). 8.5 Immediately place the flask stopper with the platinum basket suspended from the hook on the flask and clamp in place. Do not allow the sample ba
22、sket to be- come wet or the sample will not ignite. AATCC Test Method 189-2002 Fluorine Content of Carpet Fibers Copyright The American Association of Textile Chemists and Colorists Provided by IHS under license with AATCC Licensee=Hong Kong Polytechnic Univ/9976803100 Not for Resale, 03/24/2007 04:
23、07:53 MDTNo reproduction or networking permitted without license from IHS -,-,- Copyright 2006 American Association of Textile Chemists and Colorists 356TM 189-2002AATCC Technical Manual/2007 8.6 Place the flask in the infrared igni- tion cabinet. Adjust the flask level so that the test specimen in
24、the suspended plati- num basket is in the center of the infrared light beam and the tab on the black paper exposed to the infrared light. Turn on the infrared light until the sample ignites. Turn off the infrared light once the sam- ple ignites. Allow the flame to burn out. Do not open the cabinet u
25、ntil the flaming has completely ceased. Confirm that the test specimen has burned completely. If any portion of the sample remains un- burned, abort the test. Remove the flask from the ignition cabinet using a flask grip or gloves, as the flask will be hot. 8.7 Shake the flask. 8.7.1 If a mechanical
26、 shaker is used, place the flask into the holder and secure into position. Turn on the mechanical shaker for 1.5-2 min. Remove the flask. 8.7.2 If shaking is done by hand, shake vigorously for a minimum of 1 min. 8.8 Open the flask and pour all of the sodium hydroxide solution into a 100 mL plastic
27、cup labeled with the test number. 8.9 Dispense 20.0 mL of TISAB into the empty flask. When dispensing, lift the flask stopper as little as possible to pre- vent any loss of gases. Replace the stop- per and clamp in place. Repeat step 8.7 above. Pour all of the TISAB solution into the cup containing
28、the sodium hy- droxide solution. 8.10 Remove the platinum basket from the solution using tweezers. Cover the cup and allow the mixture to cool by sit- ting at room temperature for a minimum of 30 min. 8.11 Place the fluoride ion activity and reference electrodes into the cup contain- ing the cooled
29、test solution from the flask. Stir slowly and allow the meter to stabilize. Read and record the meter read- ing alongside the sample weight (see 12.8). 8.12 Discard the solutions in the plastic cups and to prevent cross-contamination, do not reuse the cups. Wash the platinum baskets and glassware, r
30、inse with deion- ized or distilled water, and dry prior to using in a new test. 9. Calculation 9.1 Calculate the results as follows (if calibrated according to 6.1): Fluorine content on carpet fiber g/g (ppm) = 9.1.1 Measured levels of less than 100 g/g (ppm) fluorine are considered as background le
31、vels and below the detec- tion limit of this method. Meter reading (millivolt) from step 8.11 above sample weight (grams) - - 10. Precision tel: 513/742-2020. 12.2 Total Ionic Adjustment Buffer (TISAB) is available from most laboratory supply companies. The buffer solution con- tains the following:
32、sodium citrate, sodium hydroxide, acetic acid and water. 12.3 These calibrations of the electrode and meter simplify the calculations of fluorine content on carpet fibers. This 40:1 ratio ac- counts for the dilution of the hydrogen fluo- ride gas in the 40 mL of sodium hydroxide and TISAB solution.
33、12.4 In keeping with standard laboratory practices, two-point calibrations across the range to be tested give better precision and ac- curacy in determining fluoride content of solu- tions. For example, a two-point calibration may use 1 g/g (ppm) and 3 g/g (ppm) fluo- ride standards for 40.0 and 120
34、.0 voltage out- put meter readings, respectively. 12.5 In order to prevent confusion, a sam- ple numbering system should be established wherein all items to be used with a specific test specimen are numbered the same; i.e., pa- per envelopes, plastic cups, combustion flasks, etc. 12.6 For convenienc
35、e in processing large numbers of samples, re-pipette dispensers may be used for the stock solutions of sodium hydroxide and TISAB buffer. If so, they should be checked for calibration daily. 12.7 The pressure from the pressure regula- tor should not exceed 14 kPa (2 psi). Exces- Table IComponents of
36、 Variance for Fluorine Content (Expressed as Variances and Standard Deviationsa) ComponentVariance Standard Deviation g/g (ppm) Specimens within materials and laboratories630.025.1 Laboratories378.019.4 Interaction: Materials times laboratories59.67.7 aSquare roots of the components of variance are
37、reported to express the variability in the appropriate units of measure rather than as the squares of those units of measure. Table IICritical Differences for the Conditions Noted 95% Probability Level, Single Material Comparisons g/g (ppm) Fluorine Number of Test Results in each Average Within-Labo
38、ratory PrecisionBetween-Laboratory Precision Standard Error Critical Difference Standard Error Critical Difference 125.17031.788 217.84926.373 314.54024.267 412.63523.164 511.23122.462 79.52721.661 98.92321.259 NOTE 1The tabulated values of the critical differences should be considered to be a gener
39、al statement, particu- larly with respect to between-laboratory precision. Copyright The American Association of Textile Chemists and Colorists Provided by IHS under license with AATCC Licensee=Hong Kong Polytechnic Univ/9976803100 Not for Resale, 03/24/2007 04:07:53 MDTNo reproduction or networking
40、 permitted without license from IHS -,-,- Copyright 2006 American Association of Textile Chemists and Colorists AATCC Technical Manual/2007TM 189-2002357 sive pressure may cause splashing. 12.8 Keep the electrodes immersed in the 2 g/g (ppm) fluoride standard solution when not in use in order to mai
41、ntain electrode con- ditioning. Appendix AStandard Preparation A1 Examples of fluoride standards: A1.1 2000 g/g (ppm) fluoride stan- dard: Weigh 4.4200 0.0001 g of oven dried sodium fluoride (NaF) and transfer to a 1 L volumetric flask. Add distilled water to the 1 L mark and shake until dis- solved
42、. A1.2 20 g/g (ppm) fluoride standard: Pipette 10.0 mL of the above 2000 g/g (ppm) solution into a 1 L volumetric flask. Add distilled water to the 1 L mark and shake. A1.3 2 g/g (ppm) fluoride standard: Pipette 100.0 mL of the 20 g/g (ppm) fluoride solution into a 1 L volumetric flask. Add distille
43、d water to the 1 L mark and shake. A1.4 0.001N sodium hydroxide solu- tion: Pipette 2.00 mL of 0.500N NaOH into a 1 L volumetric flask. Fill to the 1 L mark with distilled water and shake. Appendix BMaintaining Laboratory Level B1 It is strongly suggested that nylon fiber with known amount of non-vo
44、latile fluorocarbon treatment be used to develop and maintain a control chart of testing. Copyright The American Association of Textile Chemists and Colorists Provided by IHS under license with AATCC Licensee=Hong Kong Polytechnic Univ/9976803100 Not for Resale, 03/24/2007 04:07:53 MDTNo reproduction or networking permitted without license from IHS -,-,-