1、Designation: D7076 091Standard 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 revision. A number in pa
2、rentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTEThe title of Table 1 was corrected editorially in June 2010.1. Scope1.1 This test method covers the measurement of shives inretted flax.1.2 The values sta
3、ted 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 appro-priate safety an
4、d health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D6798 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
5、 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. 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 dete
6、rmination. Shive content will vary de-pending on the stage of processing 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-twe
7、en reported test results for two or more laboratories,comparative 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 f
8、rom which the disputed test results were obtained,and are randomly 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, eitheri
9、ts cause must be found and corrected, or future test results forthat 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 obtaina
10、ble from retted flaxfiber; (2) along with other measurements, predicting 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. Appara
11、tus5.1 GrinderSPEX 8000 mixer mill or equivalent instru-ment for 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
12、minicup with aquartz window is used and equipped with a 15 mm i.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 shippingconta
13、iner as directed in an applicable specification, or asagreed upon 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 f
14、ive sites.1This test method is under the jurisdiction of ASTM Committee 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
15、. DOI:10.1520/D7076-091.2For 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 the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Ba
16、rr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7.3 Sample 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 mil
17、l. If the grinder cannot hold all 2 g, the aliquotsare to be thoroughly mixed after separate 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 no
18、ise ratio and wave length accuracy.8.4 Enter routine scan mode.9. Calibration and Standardization9.1 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, grindin
19、g each fraction and preparingblended shive/fiber samples of known composition samples 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 stand
20、ard chemometric algorithmswhich will be part of the instrument software package obtainedfrom 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 unifo
21、rm particle size. These data will be plotted and aslope/bias correction to the spectral 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
22、using a set of standardization samples ob-tained from the manufacturer (Foss in this case) 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 ho
23、st instrument and a deterministic model developed asdescribed in 9.1.310. Conditioning10.1 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 thes
24、ample at least 12 h.11. Procedure11.1 Perform routine analysis and diagnostics for NIRSys-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 forMeasur
25、ement of Shive Content (%) in Retted FlaxSampleAveragexRepeatabilityStandardDeviationsrReproducibilityStandardDeviationsRRepeatabilityLimitrReproducibilityLimitR1 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 5.3251
26、5 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 0.3623 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
27、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 1.6394 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.
28、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 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 Devia
29、tion and Within-LaboratoryRepeatability LimitsAfor Analysis of Three Specimens of the“As Is” SamplesSampleBStatisticShive 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 1.0
30、63Repeatability Limit 2.974 Mean 3.775Standard deviation 1.529Repeatability Limit 4.285 Mean 10.1Standard deviation 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 4.6
31、18Repeatability Limit 12.99 Mean 21.727Standard deviation 7.042Repeatability Limit 19.710 Mean 4.618Standard deviation 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. T
32、he95 % repeatability limit (RL) is derived by multiplying 2.83 the sample SD inaccordance with Form and Style of ASTM Standards, section A21.2.5.BSamples were from a set of sequentially Shirley cleaned flax samples.D7076 091211.2 Clean quartz window with lens tissue to remove dustand streaks.11.3 Pa
33、cking the Sample Cell:11.3.1 Mix the specimen thoroughly.11.3.2 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 the spacer ring (15 mm i.d.) for specimens lessthat 2 g, until a small mound covers the ring opening. Do no
34、tpack or shake the ground mixture.11.3.3 Place a white foam board (3 mm thick, previously cutto fit) into the loaded cell.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 a
35、ttachment with quartzwindow.11.4.3 Place the loaded cell in the spinning cell apparatus.11.4.4 Set instrument to scan 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
36、 400 to 2498 nm (1050 points).11.4.6 Remove loaded cell from apparatus.11.4.7 Using a thin spatula, remove the foam board 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 r
37、epeated three times. Shive valuewill be displayed after each scan.12. Report12.1 State the calibration method used.12.2 Report the following:12.2.1 Type, variety and extent of retting (if known) for flaxmaterial according to Terminology D6798.12.2.2 Type of flax processing and cleaning (if known).12
38、.2.3 Identification of the samples by shipment, mark, lotnumber or bale, which ever is applicable.12.2.4 Method of sampling.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 sa
39、me method for variousflax fibers samples are shown in Table 1 and Table 2 .13.2 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.14. Keywords14.1 flax fiber
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