1、Designation: D 7076 09Standard Test Method forMeasurement of Shives in Retted Flax1This standard is issued under the fixed designation D 7076; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in p
2、arentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the measurement of shives inretted flax.1.2 The values stated in SI units are to be regarded asstandard. No other units of
3、 measurement are included in thisstandard.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulator
4、y limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 6798 Terminology Relating to Flax and Linen3. Summary of Test Method3.1 The sample to be evaluated is to be ground and theresulting mixture placed in the appropriate NIR cell and thespectra taken.3.2 The data will then be compar
5、ed to a reference file andthe value of shive reported as weight percent.4. Significance and Use4.1 Few standards exist to objectively determine flax qual-ity. Shive is the woody core of the stem and has an importanteffect on quality determination. Shive content will vary de-pending on the stage of p
6、rocessing and can determine in whatproducts the fiber can be used. Spectroscopic data provide anaccurate, precise and rapid determination of the amount ofshive in flax fiber.4.1.1 If there are differences of practical significance be-tween reported test results for two or more laboratories,comparati
7、ve tests should be performed by those laboratories todetermine if there is a statistical bias between them, usingcompetent statistical assistance. As a minimum, test samplesthat are as homogeneous as possible are drawn from thematerial from which the disputed test results were obtained,and are rando
8、mly assigned in equal numbers to each labora-tory. These results from the two laboratories should be com-pared using a statistical test for unpaired data, a possibilitylevel chosen prior to the testing series. If a bias is found, eitherits cause must be found and corrected, or future test results fo
9、rthat fiber sample type must be adjusted in consideration of theknown bias.4.2 This test method gives data on shive content of rettedflax fiber which can be used as a basis for: (1) estimating thenet amount of manufacturing fiber obtainable from retted flaxfiber; (2) along with other measurements, p
10、redicting the qualityof flax products, particularly their aesthetic properties; (3)adjusting processing machinery for maximum efficiency incleaning; and (4) relating shive content to end-product qualityand processing efficiency.5. Apparatus5.1 GrinderSPEX 8000 mixer mill or equivalent instru-ment fo
11、r the initial grinding.5.2 NIRSystems Model 6500 Monochrometer or equivalentinstrumentReference spectra scanned over the range 400 to2498 nm at 2 nm intervals and stored as log (1/R), where R isreflectance. Standard 50 mm diameter black minicup with aquartz window is used and equipped with a 15 mm i
12、.d. spacerring if sample size is limited.6. Hazards6.1 When handling or grinding any flax material a breathingmask should be worn.7. Sampling, Test Specimens, and Test Units7.1 For acceptable testing, take a lot sample from shippingcontainer as directed in an applicable specification, or asagreed up
13、on between the purchaser and supplier.7.2 Take measurements at a minimum of five sites within asample, and three measurements at each site. Means of thethree replicates constitute the site reading. For each specimen,report means of the five sites.1This test method is under the jurisdiction of ASTM C
14、ommittee D13 on Textilesand is the direct responsibility of Subcommittee D13.17 on Flax and Linen.Current edition approved July 1, 2009. Published August 2009. Originallyapproved in 2005. Last previous edition approved in 2005 as D707605.2For referenced ASTM standards, visit the ASTM website, www.as
15、tm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7.3 Samp
16、le Handling and Preparation:7.3.1 Each specimen to be analyzed should be at least2ginweight. Care should be taken not to loose any free shive.7.3.2 Each 2-g aliquot is to be ground for 3 min in a SPEX8000 mixer mill. If the grinder cannot hold all 2 g, the aliquotsare to be thoroughly mixed after se
17、parate grinding.8. Preparation of Apparatus8.1 Turn on 6500 and computer and allow enough time forwarm up that 11.1 is satisfied.8.2 Start software.8.3 Begin scan program running diagnostics checking ofsignal to noise ratio and wave length accuracy.8.4 Enter routine scan mode.9. Calibration and Stan
18、dardization9.1 The NIR instrument should be standardized with acalibration set which contains samples with a shive contentranging from 0 to 100 %. This set can be prepared by handseparating fiber and shive, grinding each fraction and preparingblended shive/fiber samples of known composition samples
19、ofknown weight. A calibration equation will be prepared fromthese samples through the use of Partial Least Squares (PLS1),Multiple Linear Regression (MLR) or another suitable statis-tical procedure. These are standard chemometric algorithmswhich will be part of the instrument software package obtain
20、edfrom the manufacturer.9.2 To verify or to account for a difference in particle sizeproduced by a second grinder, a second set of standard sampleswill be run which has been ground using a grinder to providea uniform particle size. These data will be plotted and aslope/bias correction to the spectra
21、l data obtained to accountfor differences in particle size produced by the grinder.9.3 Alternatively the calibration file from the USDA instru-ment can be transferred to the host instrument. This isaccomplished by using a set of standardization samples ob-tained from the manufacturer (Foss in this c
22、ase) and scanningthem on both instruments. A standardization file is built withthe standardization routines in the instrument software andapplied to the calibration file. This file becomes the calibrationfor the host instrument and a deterministic model developed asdescribed in 9.1.310. Conditioning
23、10.1 Do not precondition the test sample.10.2 Bring the laboratory sample from prevailing atmo-sphere to approximate moisture equilibrium with the air of theroom in which the test will be preformed by exposing thesample at least 12 h.11. Procedure11.1 Perform routine analysis and diagnostics for NIR
24、Sys-tems model 6500 monochrometer.43Shenk, J. S., and Westerhaus, M. O., Crop Sci., 31, 1991, p. 469.4Available from NIRSystems Inc., Silver Springs, MD, USA.TABLE 1 Summary of Precision and Bias Analysis for FinenessOption 1SampleAveragexRepeatabilityStandardDeviationsrReproducibilityStandardDeviat
25、ionsRRepeatabilityLimitrReproducibilityLimitR1 0.15 0.5618 1.3999 1.5731 3.91982 10.88 0.7949 1.4153 2.2257 3.96303 20.14 0.6897 1.1416 1.9312 3.19654 31.13 0.2448 1.9018 0.6854 5.32515 40.73 0.6555 2.0239 1.8353 5.66686 51.37 0.5044 2.4763 1.4123 6.93367 60.31 0.4011 1.3269 1.1232 3.71538 69.99 0.3
26、623 2.7942 1.0146 7.82369 79.77 0.5672 2.8398 1.5883 7.951410 89.41 1.3213 4.0920 3.6996 11.457611 98.57 0.5887 3.4107 1.6484 9.549912 19.21 0.3332 0.8894 0.9329 2.490313 27.15 0.5076 0.7963 1.4212 2.229514 35.36 0.6395 0.9469 1.7906 2.651315 51.78 0.4892 0.8152 1.3697 2.282516 66.07 0.5855 1.9470 1
27、.6394 5.451717 34.90 0.2710 0.8698 0.7587 2.435518 23.06 0.6322 1.5068 1.7702 4.219119 38.02 1.7109 8.6843 4.7906 24.315920 18.53 1.9017 8.1436 5.3248 22.802221 49.23 2.0655 10.6839 5.7834 29.915022 9.26 2.8163 11.3705 7.8856 31.837523 2.24 2.2125 12.5514 6.1951 35.144024 13.32 4.5512 9.2063 12.7434
28、 25.777725 7.31 2.4626 4.1993 6.8954 11.758026 3.77 1.4387 4.1103 4.0283 11.508927 45.09 3.6865 7.8500 10.3221 21.980128 39.36 4.8082 9.0834 13.4629 25.4335TABLE 2 Mean, Standard Deviation and Within-LaboratoryRepeatability LimitsAfor Analysis of Three Specimens of the“As Is” SamplesSampleBStatistic
29、Shive Content byNIRSystem 65001 Mean 7.425Standard deviation 2.303Repeatability Limit 6.442 Mean 0.391Standard deviation 0.369Repeatability Limit 1.033 Mean 6.147Standard deviation 1.063Repeatability Limit 2.974 Mean 3.775Standard deviation 1.529Repeatability Limit 4.285 Mean 10.1Standard deviation
30、2.789Repeatability Limit 7.816 Mean 9.78Standard deviation 1.127Repeatability Limit 3.157 Mean 21.746Standard deviation 8.376Repeatability Limit 23.48 Mean 33.190Standard deviation 4.618Repeatability Limit 12.99 Mean 21.727Standard deviation 7.042Repeatability Limit 19.710 Mean 4.618Standard deviati
31、on 1.02Repeatability Limit 2.88AThe average and standard deviation (SD) are from three specimens from thesame “as is” sample described in Section 7, to illustrate sampling variation. The95 % repeatability limit (RL) is derived by multiplying 2.83 the sample SD inaccordance with Form and Style of AST
32、M Standards, section A21.2.5.BSamples were from a set of sequentially Shirley cleaned flax samples.D707609211.2 Clean quartz window with lens tissue to remove dustand streaks.11.3 Packing the Sample Cell:11.3.1 Mix the specimen thoroughly.11.3.2 Using a spatula carefully remove a small amount ofthe
33、material from the sample bottle and gently place in the cell(5 cm o.d.) or the spacer ring (15 mm i.d.) for specimens lessthat 2 g, until a small mound covers the ring opening. Do notpack or shake the ground mixture.11.3.3 Place a white foam board (3 mm thick, previously cutto fit) into the loaded c
34、ell.11.3.4 Label specimen number on the back of the foamboard.11.4 Scanning the Sample:11.4.1 Load scan program appropriate equation file (.eqa).11.4.2 Scan using the spinning cell attachment with quartzwindow.11.4.3 Place the loaded cell in the spinning cell apparatus.11.4.4 Set instrument to scan
35、16 reps of internal standardbefore and after each sample (total sample scan time is about1 min).11.4.5 The spectrum of each specimen has reflectance data(log 1/R) for every 2 nm from 400 to 2498 nm (1050 points).11.4.6 Remove loaded cell from apparatus.11.4.7 Using a thin spatula, remove the foam bo
36、ard andcarefully transfer the specimen to the original container.11.5 Vacuum the cell and spacer to remove dust and cleanthe quartz window with lens tissue.11.6 Steps 11.3-11.5 are repeated three times. Shive valuewill be displayed after each scan.12. Report12.1 State the calibration method used.12.
37、2 Report the following:12.2.1 Type, variety and extent of retting (if known) for flaxmaterial according to Terminology D 6798.12.2.2 Type of flax processing and cleaning (if known).12.2.3 Identification of the samples by shipment, mark, lotnumber or bale, which ever is applicable.12.2.4 Method of sa
38、mpling.13. Precision and Bias13.1 PrecisionThe average, standard deviation, and 95 %repeatability limit (2.8X sample standard deviation) of inter-laboratory samples tested with the same method for variousflax fibers samples are shown in Table 1 and Table 2 .13.2 BiasError analysis shows that the abs
39、olute value ofthe maximum systematic error that could result from aninstrument and other tolerances specified in the test method is1.6 % of the test result.14. Keywords14.1 flax fiber; NIR; shive trashASTM International takes no position respecting the validity of any patent rights asserted in conne
40、ction with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsi
41、ble technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful co
42、nsideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100
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