1、Designation: D 6404 99 (Reapproved 2009)Standard Practice forSampling Vegetable Materials Containing Tannin1This standard is issued under the fixed designation D 6404; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of las
2、t revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This practice covers obtaining representative samplesfrom shipment lots of botanical materials containing tannin.1.2 The
3、values stated in SI units are to be regarded as thestandard. The inch-pound units given in parentheses are forinformation only.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 a
4、ppro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1517 Terminology Relating to Leather2.2 ALCA Method:J10 Sampling Vegetable Materials Containing Tannin33. Terminology3.1 Definitions:3.1.1 For
5、definitions of general leather and tanning termsused in this practice refer to Terminology D 1517.3.1.2 quarteringthe term applied to a method described inthis practice of reducing the size of samples without impairingtheir representative quality.3.1.3 tanninan astringent substance found in the vari
6、ousparts of plants such as bark, wood, leaves, nuts, fruits, roots,etc.3.1.4 vegetable tanninsmixtures of substances (naturalproducts) obtained from plant tissues by water extractionwhich have the chemical and physical properties necessary toconvert animal hides and skins into leather.4. Summary of
7、Practice4.1 This practice describes methods for obtaining represen-tative samples for analysis from shipments of vegetable tan-ning materials and tannin extracts.5. Significance and Use5.1 This practice provides standard procedures for obtainingrepresentative samples of various materials used as a s
8、ource oftannins for the tanning industry.5.2 Procedures are described for obtaining representativesamples of economical and convenient quantities from a lot, orsections of a lot, of material for examination and analysis sothat agreement may be reached with regard to the extent ofvariation of quality
9、 in different portions of a lot and the averagequality of the entire lot of material.5.3 No directions for sampling, however explicit, can takethe place of judgment, skill, and previous experience on thepart of persons actually engaged in the sampling or thesupervision of the sampling. These directi
10、ons are intended tosupplement that experience and, particularly, to serve as aguide in the selection of the method which is to be used, incommon, by each of two or more contracting parties.5.4 Tanning materials contain moisture in varying amounts,depending both on the nature of the material and on t
11、heclimatic conditions, so that sampling must be carried out asquickly as is consistent with thoroughness in order to avoidchanges in moisture content.6. Apparatus6.1 Balance, analytical balance which will weigh the quan-tity of material specified in this practice to an accuracy of 610g(6 0.35 oz).6.
12、2 Canvas, 11-oz weight and of sufficient size (as deter-mined by the discretion of the sampler or analyst) for use inmixing and quartering samples.6.3 Sieve, with round openings 1.27 cm (0.50 in.) indiameter.6.4 Sampling Tool, this tool shall be made of brass or othercorrosion-resistant metal tubing
13、, with solid handle attached,similar to that described below and illustrated in Fig. 1.1This practice is under the jurisdiction ofASTM Committee D31 on Leather andis the direct responsibility of Subcommittee D31.01 on Vegetable Leather. This testmethod has been adapted from and is a replacement for
14、Method J10 of the OfficialMethods of the American Leather Chemists Association.Current edition approved April 1, 2009. Published July 2009. Originallyapproved in 1999. Last previous edition approved in 2004 as D 6404 99 (2004).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orc
15、ontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Official Methods of the American Leather Chemists Association. Availablefrom the American Leather Chemists Association, University of
16、 Cincinnati, P.O.Box 210014, Cincinnati, OH 45221-0014.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.4.1 Thin brass or other corrosion-resistant metal tubing,37 cm long and 17.5 mm diameter, is used.Asolid steel handle,6 cm long,
17、 is welded to one end of the tube. A section 11 mmwide and 30 cm long is cut out of the side of the tube and theedges of this opening sharply beveled. The working end is cutto a sharp point for piercing sacks, or other tough materials,like plantation gambier.7. Quartering Samples7.1 “Quartering” is
18、a term applied to the following methodof reducing the size of samples without impairing theirrepresentative quality.7.1.1 All of the material, taken from the various containersor parts of the shipment of solid material being sampled, shallbe immediately and thoroughly mixed on a square piece of 11oz
19、 canvas. In the case of solid extracts, large pieces shall havebeen broken previously so as to pass a screen having roundopenings 1.27 cm (0.50 in.) in diameter. The pile shall bedivided into four equal portions and quarters A and B shall bediscarded as illustrated in diagram X of Fig. 2. The remain
20、ingtwo quarters shall then be re-mixed thoroughly and againdivided into four equal portions and quarters C and D shall bediscarded as illustrated in diagram Y of Fig. 2. This processshall be repeated until the mixture of any two remainingquarters of the sample be of sufficient size to secure theindi
21、vidual samples as specified below. The individual samplesshall be obtained by thoroughly mixing the two remainingquarters and dividing the mixture into as many uniformsections as necessary, such that each section will be largeenough to fill one of the required number of containers. Allfine, powdery
22、material in each section shall be completelyremoved with its respective section, whether the section isdiscarded or placed in a sample container.8. Filling Containers8.1 Immediately after the final samples are obtained, theyshall be put into clean, dry containers, closed airtight, sealed,and labeled
23、 as described in the procedure (11.11).8.2 Liquid and powdered extracts and tannery liquorsamples shall be put into stoppered glass bottles of the requiredsize.8.3 Solid and pasty extracts shall be wrapped in aluminumfoil and put into Mason-type jars or tin cans of the requiredsize.8.4 Cut bark, fru
24、its, roots, galls, nuts, leaves, etc., and spentmaterials, shall be placed in lacquered, pressed-top tins of therequired size, which close airtight. Boxes or bags must not beused as containers.8.5 Sample containers shall be of no greater capacity thanwill conveniently be filled by the sample taken.9
25、. Number of Packages to be Sampled9.1 The number of packages to be sampled from any givenlot of tanning material composed of solid, powdered or pastyextract, crude or manufactured tanning materials, in bales,boxes, bags, barrels, or similar packages, shall be as shown inTable 1. The samples shall be
26、 selected from as uniformlydistributed parts of the lot as is possible at the time ofweighing.9.1.1 Where the shipment exceeds 10 000 packages, it shallbe divided into as few, equal, sections (of not more than 10 000packages each) as possible and each section shall be sampledand analyzed as if it we
27、re an individual shipment. In such case,the mean of the analyses of the sections shall constitute theanalysis of the shipment.10. Number of Samples10.1 In addition to the representative samples for submis-sion to the contracting parties, at least one extra sample shall betaken and held in reserve by
28、 the sampler, in case one of theregular samples is lost or damaged.11. Procedure11.1 Solid ExtractsCut a suitable triangular opening in themiddle of the exposed side of the package to be sampled. Thencut a V-shaped wedge, 10 to 12.5 cm (4 to 5 in.) in width on thesurface of the exposed side of the p
29、ackage, as near to themiddle as possible and to the depth shown in the diagramillustrated in Fig. 3.11.1.1 Remove this piece, including any dry or crumblyexterior portion of it, place on the quartering canvas andcovered to prevent loss of moisture. Promptly break theV-shaped samples from all the sel
30、ected packages to a sizewhich will pass the sieve (6.3). Quarter the mixture and sampleas described in Section 7. Each final sample shall weighapproximately 225 g (8 oz) and shall be packaged as describedin 8.3.11.2 Powdered ExtractsDraw a portion from each of thespecified number of bags, using the
31、sampling tool (6.4). Laythe bags horizontally, with the narrow side exposed, and insertthe sampling tool into the middle of the exposed side and to thecenter of the bag. The portions removed shall be of equalquantity, thoroughly mixed, and the mixture quartered andsampled as described in Section 7.
32、Each sample shall weighapproximately 170 g (6 oz.) and be packaged as described in8.2.FIG. 1 Sampling ToolFIG. 2 Quartering SamplesD 6404 99 (2009)211.3 Barks, Roots, Galls, Nuts, etc., in BagsDraw samplesas under “Powdered Extracts” (11.2), using a scoop, whennecessary, instead of the sampling tool
33、. Thoroughly mix theportions and quarter and sample the mixture as described inSection 7. Each sample shall consist of enough material to filla 3.8 L (1 gal) container, at least, and be packaged as describedin 8.4.11.3.1 In sampling Valonia cups and beards, take threeportions from each of the specif
34、ied number of bags, one fromthe middle, one midway between the middle and one end, andthe third between the middle and the other end. Thoroughlymix the portions and quarter and sample the mixture asdescribed in 11.3.11.3.1.1 In case of disagreement, or when agreed uponbetween buyer and seller, the f
35、ollowing method may be used:the specified number of bags shall be screened through thesieve (6.3) in their entirety and the percentage of cups andbeards determined by weighing. Draw samples of each bymixing and quartering, etc., as described in 11.3. State therelative proportions of cups and beards,
36、 found by weighing, onthe label and the same proportions taken for analysis.11.4 Bark and Wood in BalesSample chopped bark orsimilar material in bales by cutting a 15 cm (6 in.) slit in theapproximate middle of the covering of the bale. Using a meathook about 25 cm (10 in.) long, dig out the materia
37、l through theslit as deeply as possible. Thoroughly mix and sample theseportions as described in Section 7. Each final sample shallconsist of enough material to fill a 3.8 L (1 gal) container, atleast, and be packaged as described in 8.4.11.5 Bark and Wood in Sticks or Logs, Bulk ShipmentSelect the
38、required number of pieces and saw or break intosmaller pieces, each representing in relative size, as nearly asis practicable, the piece from which it was taken. The sawingmust be done so as to avoid iron contamination of the samplefrom the saw or other cutting instrument. Overheating of thesample b
39、ecause of friction from the cutting tool must beavoided. Thoroughly mix and sample the sample portionsobtained as described in Section 7. Each final sample shallconsist of enough material to fill a 3.8 L (1 gal) container, atleast, and be packaged as described in 8.4.11.6 Wood as Chips (from Chipper
40、)Take chips from thechipping machine at regular intervals during the run beingexamined and immediately place in a suitable, closed con-tainer. Thoroughly mix and sample these portions as describedin Section 7. Each final sample shall consist of enough materialto fill a 3.8 L (1 gal) container, at le
41、ast, and be packaged asdescribed in 8.4. Samples are not representative when water isused to lay the dust in chipping.11.7 Spent MaterialsMix a portion of material from theinner and outer areas of the top, middle, and bottom of theleach for sampling, or take five portions from the pitch-hole asthe s
42、pent material leaves the hole. Take the first portion 5 minafter starting to pitch and the last portion 5 min before pitchingis completed. Take the intermediate portions at equal timeintervals between the first and the last portions. Each portionshall be of approximately equal size. Sample autoclave
43、sTABLE 1 Sampling QuantitiesNumber ofPackagesin LotNumber ofPackages toBe SampledNumber ofPackagesin LotNumber ofPackages toBe SampledNumber ofPackagesin LotNumber ofPackages toBe Sampled1 to 3 each 1201 to 1300 25 4551 to 4700 483 to 24 3 1301 to 1400 26 4701 to 4900 4925 to 40 4 1401 to 1510 27 49
44、01 to 5100 5041 to 60 5 1511 to 1640 28 5101 to 5300 5161 to 84 6 1641 to 1730 29 5301 to 5520 5285 to 112 7 1731 to 1860 30 5521 to 5720 53113 to 144 8 1861 to 1980 31 5721 to 5940 54145 to 180 9 1861 to 1980 32 5941 to 6160 55181 to 220 10 2101 to 2240 33 6161 to 6380 56221 to 264 11 2241 to 2380
45、34 6381 to 6600 57265 to 312 12 2381 to 2520 35 6601 to 6840 58313 to 364 13 2521 to 2660 36 6841 to 7080 59365 to 420 14 2661 to 2810 37 7081 to 7320 60421 to 480 15 2811 to 2960 38 7321 to 7560 61481 to 544 16 2961 to 3120 39 7561 to 7800 62545 to 612 17 3121 to 3280 40 7801 to 8060 63613 to 684 1
46、8 3281 to 3440 41 8061 to 8320 64685 to 760 19 3441 to 3610 42 8321 to 8580 65761 to 840 20 3611 to 3780 43 8581 to 8840 66841 to 920 21 3781 to 3960 44 8841 to 9120 67921 to 1010 22 3961 to 4140 45 9121 to 9400 681011 to 1100 23 4141 to 4320 46 9401 to 9660 691101 to 1200 24 4321 to 4550 47 9661 to
47、 10 000 70FIG. 3 Package CuttingD 6404 99 (2009)3continuously from the spent material conveyor. Thoroughlymix and sample these portions as described in Section 7. Eachfinal sample shall consist of enough material to fill a 3.8 L (1gal) container, at least, and be packaged as described in 8.4.11.8 Pa
48、sty ExtractsSelect the number of packages re-quired for sampling. Insert a sampling tool (6.4) to the middleof each selected package three times, side by side, and emptythe samples obtained into a suitable container. If the samplingtool fails, use a scoop or hatchet. Cut all portions into cubes ofap
49、proximately 1.27 cm (0.50 in.) sides and thoroughly mix andsample as described in Section 7. Each final sample shall be ofsufficient size to fill a 1.9 L (2 qt) Mason jar and packaged asdescribed in 8.3.11.9 Liquid Extracts:11.9.1 Samples of liquid extracts are not representativewhen they have been frozen, or when steam has been passeddirectly into the extract. Add a suitable preservative to samplesof liquid extract which are prone to ferment. Seal all samplesimmediately to prevent loss of moisture.11.9.2 Liquid Extracts in BarrelsDetermine the numberof barrels to be s
