1、Designation: D 7076 05Standard 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 (e) 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 UnitsThe values stated in either SI units or inch-pounds are to be regarded s
3、eparately as a standard. The valuesstated in each system may not be exactly equivalent; therefore,each system shall be used independently of the other. Combin-ing values from the two systems may result in non-conformance with the standard.1.3 This standard does not purport to address all of thesafet
4、y 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 regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 6798 Terminology Related to Fla
5、x 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 compared to a reference file andthe value of shive reported as weight percent.4. Significance and Use4.1 Few s
6、tandards 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 whatproducts the fiber can be used. Spectroscopic data provide anaccurate
7、, 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,comparative tests should be performed by those laboratories todetermine if there is a statistical bias between th
8、em, 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 each labora-tory. These results from the two laboratories should be com
9、-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 adjusted in consideration of theknown bias.4.2 This test method gives da
10、ta 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 products, particularly their aesthetic properties; (3)adjusting processing
11、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 for the initial grinding.5.2 NIRSystems Model 6500 Monochrometer or equivalentinstrumentReference spectra
12、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 limited.6. Hazards6.1 When handling or grinding any flax material a bre
13、athingmask 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 upon between the purchaser and supplier.7.2 Take measurements at a minimum of five sites within asample, a
14、nd three measurements at each site. Means of thethree replicates constitute the site reading. For each specimen,report means of the five sites.7.3 Sample Handling and Preparation:1This test method is under the jurisdiction of ASTM Committee D13 on Textilesand is the direct responsibility of Subcommi
15、ttee D13.17 on Flax and Linen.Current edition approved Jan. 1, 2005. Published February 2005.2For 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
16、Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.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
17、for 3 min in a SPEX8000 mixer mill. 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 di
18、agnostics checking ofsignal to noise 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 handse
19、parating fiber and shive, grinding 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
20、-tical procedure. These are standard 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
21、using a grinder to providea uniform 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 in
22、strument. This isaccomplished by 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
23、becomes the calibrationfor the host 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 w
24、ill be preformed by exposing thesample at least 12 h.11. Procedure11.1 Perform routine analysis and diagnostics for NIRSys-tems model 6500 monochrometer.411.2 Clean quartz window with lens tissue to remove dustand streaks.11.3 Packing the Sample Cell:3Shenk, J. S., and Westerhaus, M. O., Crop Sci.,
25、31, 1991, p. 469.4Available from NIRSystems Inc., Silver Springs, MD, USA.TABLE 1 Mean, Standard Deviation and Within-LaboratoryRepeatability LimitsAfor Analysis of the Same Ground SpecimenRepeated 3 Times with Mixing Between AnalysesSpecimenBStatisticShive Content byNIRSystem 65001 Mean 1.76Standar
26、d deviation 0.283Repeatability Limit 0.7922 Mean 5.54Standard deviation 0.182Repeatability Limit 0.5093 Mean 11.46Standard deviation 0.193Repeatability Limit 0.544 Mean 15.30Standard deviation 0.081Repeatability Limit 0.2275 Mean 20.31Standard deviation 0.303Repeatability Limit 0.8486 Mean 30.08Stan
27、dard deviation 0.744Repeatability Limit 2.087 Mean 38.55Standard deviation 0.485Repeatability Limit 1.35AThe average and standard deviation (SD) are from analysis of the samespecimen as described in Section 7. The 95 % repeatability limit (RL) is derived bymultiplying 2.83 the sample SD in accordanc
28、e with Form and Style of ASTMStandards, section A21.2.5.BSamples were from a set of sequentially Shirley cleaned flax samples.TABLE 2 Mean, Standard Deviation and Within-LaboratoryRepeatability LimitsAfor Analysis of Three Specimens of the“As Is” SamplesSampleBStatisticShive Content byNIRSystem 6500
29、1 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 2.789Repeatability Limit 7.816
30、 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 deviation 1.02Repeatability Limit 2.8
31、8AThe 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 ASTM Standards, section A21.2.5.B
32、Samples were from a set of sequentially Shirley cleaned flax samples.D707605211.3.1 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
33、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 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 equ
34、ation 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 16 reps of internal standardbefore and after each sample (total sample scan time is about1 min).11.4.5 The spectrum of each spe
35、cimen 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 board andcarefully transfer the specimen to the original container.11.5 Vacuum the cell and spacer to remove dust and cleanthe qu
36、artz 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.12.2 Report the following:12.2.1 Type, variety and extent of retting (if known) for flaxmaterial according to Terminology D 6798.1
37、2.2.2 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 sampling.13. Precision and Bias13.1 PrecisionThe mean, standard deviation, and 95 %repeatability limit (2.83 sample standard devi
38、ation) of within-laboratory samples tested with the same method, equipment,laboratory, and operator for various flax fibers are shown inTables 1 and 2.13.2 BiasWith the limitation imposed by within-laboratory evaluation and triplicate evaluation of the samesample, this method has no bias.14. Keyword
39、s14.1 flax fiber; NIR; shive trashASTM International takes no position respecting the validity of any patent rights asserted in connection 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 risko
40、f infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible 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
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42、ur views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D7076053
