1、Designation: D7076 10 (Reapproved 2015)1Standard Test Method forMeasurement of Shives in Retted Flax1This standard is issued under the fixed designation D7076; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisi
2、on. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTEThe terminology section was added editorially in April 2015.1. Scope1.1 This test method covers the measurement of shives inretted flax.
3、1.2 The values stated in SI units are to be regarded asstandard. No other units of 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 appr
4、o-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D123 Terminology Relating to TextilesD6798 Terminology Relating to Flax and Linen3. Summary of Test Method3.1 The sample to be evaluated is to be gr
5、ound and theresulting mixture placed in the appropriate NIR cell and thespectra taken.3.2 The data will then be compared to a reference file andthe value of shive reported as weight percent.4. Terminology4.1 For all terminology related to Flax, see TerminologyD6798.4.2 For definitions of all other t
6、extile terminology, seeTerminology D123.5. Significance and Use5.1 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 processing and can determine in w
7、hatproducts the fiber can be used. Spectroscopic data provide anaccurate, precise and rapid determination of the amount ofshive in flax fiber.5.1.1 If there are differences of practical significance be-tween reported test results for two or more laboratories,comparative tests should be performed by
8、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 randomly assigned in equal numbers to
9、 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 forthat fiber sample type must be
10、adjusted in consideration of theknown bias.5.2 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, predicting the qualityof flax pro
11、ducts, particularly their aesthetic properties; (3)adjusting processing machinery for maximum efficiency incleaning; and (4) relating shive content to end-product qualityand processing efficiency.6. Apparatus6.1 GrinderSPEX 8000 mixer mill or equivalent instru-ment for the initial grinding.6.2 NIRSy
12、stems 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.d. spacerring if sample size is
13、 limited.7. Hazards7.1 When handling or grinding any flax material a breathingmask should be worn.1This test method is under the jurisdiction ofASTM Committee D13 on Textilesand is the direct responsibility of Subcommittee D13.17 on Flax and Linen.Current edition approved Feb. 1, 2015. Published Apr
14、il 2015. Originallyapproved in 2005. Last previous edition approved in 2010 as D707610. DOI:10.1520/D7076-10R15E01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to t
15、he standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States18. Sampling, Test Specimens, and Test Units8.1 For acceptable testing, take a lot sample from shippingcontainer as directed in an ap
16、plicable specification, or asagreed upon between the purchaser and supplier.8.2 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.8.3 Sample Hand
17、ling and Preparation:8.3.1 Each specimen to be analyzed should be at least2ginweight. Care should be taken not to loose any free shive.8.3.2 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 separate
18、grinding.9. Preparation of Apparatus9.1 Turn on 6500 and computer and allow enough time forwarm up that 12.1 is satisfied.9.2 Start software.9.3 Begin scan program running diagnostics checking ofsignal to noise ratio and wave length accuracy.9.4 Enter routine scan mode.10. Calibration and Standardiz
19、ation10.1 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 ofkno
20、wn 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 obtainedfro
21、m the manufacturer.10.2 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 spectral da
22、ta obtained to accountfor differences in particle size produced by the grinder.10.3 Alternatively the calibration file from the USDA in-strument can be transferred to the host instrument. This isaccomplished by using a set of standardization samples ob-tained from the manufacturer (Foss in this case
23、) 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 10.1.311. Conditioning11
24、.1 Do not precondition the test sample.11.2 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.12. Procedure12.1 Perform routine analysis and diagnostics for NIRSy
25、s-tems model 6500 monochrometer.412.2 Clean quartz window with lens tissue to remove dustand streaks.12.3 Packing the Sample Cell:12.3.1 Mix the specimen thoroughly.12.3.2 Using a spatula carefully remove a small amount ofthe material from the sample bottle and gently place in the cell(5 cm o.d.) or
26、 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.12.3.3 Place a white foam board (3 mm thick, previously cutto fit) into the loaded cell.12.3.4 Label specimen number on the back of the foamboard.12.4 Scannin
27、g the Sample:12.4.1 Load scan program appropriate equation file (.eqa).12.4.2 Scan using the spinning cell attachment with quartzwindow.12.4.3 Place the loaded cell in the spinning cell apparatus.12.4.4 Set instrument to scan 16 reps of internal standardbefore and after each sample (total sample sca
28、n time is about1 min).3Shenk, 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 forMeasurement of Shive Content (%) in Retted FlaxSampleAverageRepeatabilityStandardDeviationsrReproducibili
29、tyStandardDeviation xsRRepeatabilityLimitrReproducibilityLimitR1 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
30、 3.71538 69.99 0.3623 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.
31、07 0.5855 1.9470 1.6394 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 4.5
32、512 9.2063 12.7434 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 25.4335D7076 10 (2015)1212.4.5 The spectrum of each specimen has reflectance data(log 1/R) for every 2 nm from 400 to 2498 nm (1050 p
33、oints).12.4.6 Remove loaded cell from apparatus.12.4.7 Using a thin spatula, remove the foam board andcarefully transfer the specimen to the original container.12.5 Vacuum the cell and spacer to remove dust and cleanthe quartz window with lens tissue.12.6 Steps 12.3-12.5 are repeated three times. Sh
34、ive valuewill be displayed after each scan.13. Report13.1 State the calibration method used.13.2 Report the following:13.2.1 Type, variety and extent of retting (if known) for flaxmaterial according to Terminology D6798.13.2.2 Type of flax processing and cleaning (if known).13.2.3 Identification of
35、the samples by shipment, mark, lotnumber or bale, which ever is applicable.13.2.4 Method of sampling.14. Precision and Bias14.1 PrecisionThe average, standard deviation, and 95 %repeatability limit (2.8 sample standard deviation) of inter-laboratory samples tested with the same method for variousfla
36、x fibers samples are shown in Table 1.14.2 BiasError analysis shows that the absolute value ofthe maximum systematic error that could result from aninstrument and other tolerances specified in the test method is1.6 % of the test result.15. Keywords15.1 flax fiber; NIR; shive trashASTM International
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