1、Designation: E2776 18Standard Guide forCorrelation of Results of Solid Particle Size MeasurementInstruments1This standard is issued under the fixed designation E2776; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last
2、 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 guide describes one methodology to correlate solidparticle analysis results between solid particle analysis instru-me
3、nts for user specified products of user specified particle sizesand distributions in order to expand the capability of particlemeasurement throughout the manufacturing process and pro-vide better control and efficiency. The guide is not limited toinstrument type or product type.1.2 WarningAll instru
4、ments may not correlate to allother instruments for various user specified products and sizeranges. Instruments may measure different particle features,and they may also measure the same particle features differ-ently and thus correlating the results of any two may bepossible for some products but n
5、ot possible for others. It is alsothe case that certain materials can be altered by the instrumentsmeasuring them which would eliminate them from consider-ation under this guide if the instruments results are determinedbased on measurements made after the instrument has alteredthe user specified pro
6、duct.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 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
7、 appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for
8、theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Terminology2.1 Definitions of Terms Specific to This Standard:2.1.1 bin, na user specified division of the overall particlesize range of a user
9、specified product.2.1.2 correlation, nmathematical equation(s) relating oneset of numerical values to another.2.1.3 particle analysis instrument, nany instrument of anytype that can produce a particle size distribution measurementof a product. There is no restriction on technology or method-ology us
10、ed by the instrument to measure particles nor is thereany restriction of particle characteristics used to report resultsof the measurement.2.1.4 user specified product, nindicates a product manu-factured by the user to a specified size distribution, usuallyindicated by common sieve screen sizes.3. S
11、ummary of Guide3.1 This guide describes a method which can be used tocorrelate results between instruments which measure particlesize, and distribution, of materials by the same or differentparameters and principles.3.2 The primary interest is the correlation of particle sizemeasurements of user spe
12、cified products.3.3 This guide can be used for any two particle measuringinstruments which output a user specified distribution and havethe capacity to shift bin boundaries within the software.Therefore, a set of sieves cannot correlate to anotherinstrument, but another instrument may correlate to t
13、he set ofsieves. Ideally the bin boundaries for the correlating instrumentwould match the bin boundaries of the primary instrument, orif correlating to sieves, match the range of each correspondingsieve, but if they do not, the method described in this documentcould be used to adjust the individual
14、bin boundaries used bythe correlating instrument to make the volume percent detectedfor each bin closely match the percent retained by eachcorresponding bin of the primary instrument or set of sieves.3.4 The guide is valid for any two instruments as long as itcan be demonstrated that the correlation
15、 results are useful tothe user.1This guide is under the jurisdiction of ASTM Committee E29 on Particle andSpray Characterization and is the direct responsibility of Subcommittee E29.02 onNon-Sieving Methods.Current edition approved April 1, 2018. Published May 2018. DOI: 10.1520/E2776-18.Copyright A
16、STM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International St
17、andards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.14. Significance and Use4.1 It is useful to be able to obtain particle size measurementresults of a user specified product from multiple instrumentsand to be able to correlate the r
18、esults of the measurements. Thiscapability can be advantageous in expanding the use ofdifferent technologies to make a measurement or simply tocorrelate results between instruments of the same technology.An example might be comparing in-process particle sizemeasurements to final inspection particle
19、size measurements.4.2 The viability of this guide will need to be tested on acase-by-case basis as various products may present measure-ment challenges for some instruments and not all results fromall instruments may be able to be correlated to all other resultsfrom all other instruments. In additio
20、n, positive results shouldbe confirmed and improved with continued data comparisonsover time using process measurements from the instrumentsselected.5. ProcedureNOTE 1Depending on instrument type and features this proceduremight not exactly match the steps required to create a correlation on apartic
21、ular instrument. The steps referenced herein are meant to guide theuser toward creating a correlation by following similar logic appropriateto the instrument selected.5.1 The first step is for the user to select a particularmanufactured product which has a defined particle size rangeand distribution
22、 already determined by the users sieves orother instrument.NOTE 2Ideally distributions will be reported in discrete gradationshowever this guide can also be used where the determination of thedistribution is a continuous curve.5.2 The procedure requires the gathering of twenty-onerepresentative samp
23、les of the user specified product which willbe used to determine a correlation which can be used for futuremeasurements.5.3 The sample size (mass) can be determined by assessingthe statistical particle count for the largest bin size that willyield a particular confidence level. The example in Annex
24、A1illustrates the exercise in a straight forward manner.5.4 Using the gradations indicated in the users productspecification, determine the particle size distribution of eachsample using the primary instrument of measure. Confirm thatthe instrument is in good calibration in accordance with themanufa
25、cturers instructions or a standard procedure appropri-ate to the industry.5.5 Run one sample through the correlating instrument threetimes and create a correlation by shifting the bin boundaries sothe result closely matches the primary instrument result.5.6 Calculate the variation and average repeat
26、ability of thecorrelating instrument based on these results. Ideally therepeatability would be better than5%inthehighly populatedbins. The user will have to make a judgment on the applica-bility of any correlation based on the accuracy and repeatabilityof the correlating instrument involved and the
27、precision neededto control the process.5.7 If the results are acceptable, then verify the set up byrunning the remaining twenty samples. If adjustments arerequired, make them and then re verify. Determine the finalaccuracy and repeatability of the correlation and determine if itis adequate for measu
28、ring the process.5.8 Once the correlation is confirmed, the software file ofthe correlating instrument must be saved as a unique filecontaining the fixed settings and correlation for the particularuser specified product tested. If either the primary or correlat-ing instrument are altered in a way th
29、at might affect measure-ment results this entire procedure must be repeated.5.9 It is recommended that the correlation be tested near thespecification boundaries.An example is given in Appendix X3.6. Report6.1 The particle distribution produced by the correlatinginstrument should be reported using t
30、he gradations identifiedfor the user specified product.NOTE 3Changing the bin boundaries will not change the name of thebin. For example, a 325 mesh bin might have its boundary shifted from 44m to 35 m, but it is still identified as the 325 mesh bin.6.2 Report the correlating instrument model and so
31、ftwareversion as well as the file name and version containing thecorrelation. Include a statement indicating the instrument isreporting results correlated to another instrument per thisguide. Indicate the primary instrument and reference thisdocument. It may also be informative to include the correl
32、ationresults in a format similar to the tables presented in SectionX2.1. An example report format follows:Correlation ReportPrimary Instrument: (include identifying information; model #, serial numberetc.)Correlating Instrument: (include identifying information; model, serial numberetc.)Sample: (inc
33、lude sample product name, lot, date run and any other identifyingcodes as appropriate)Results: (report size distribution of sample in tabular or graphical form)7. Keywords7.1 bin; correlation; distribution; particle sizeE2776 182ANNEX(Mandatory Information)A1. DETERMINATION OF SAMPLE SIZEA1.1 As ind
34、icated in 5.3, it is important to select a samplesize that will yield a high enough number of particles forstatistical significance. A straight forward way to do this isdetailed in this annex by means of an example.A1.2 AssumptionsA1.2.1 Particle range: 1 m 100 m.A1.2.2 Five gradations (bins) as fol
35、lows with 20 % by massin each: pan, 20 m, 40 m, 60 m, and 80 m. Fewest numberof particles will reside in the 80-m bin, so using that as thelimiting factor of the analysis, compute the number, and thenmass, of sample required.A1.3 MethodA1.3.1 Select a standard error (Sn) allowable. The standarderror
36、 is the measured standard deviation of a sample. For thisexample, 5 % will be used.A1.3.2 Calculate the number of particles required in thelargest bin. Assume all particles at the median bin size, in thiscase 90 microns.Sn 5 1n12!n 5 number of particlesn 5 1 0.05!2n 5 400 particles required(A1.1)A1.
37、3.3 With the number of particles now calculated for thetop bin, a minimum sample mass can be projected for the entiresample by converting the 20 % bin mass to 100 %. Assume theproduct density is 1 g/cm3.Sample Mass 5 400 3 100 20! 3 Pi 6! 3 90 3 1024!3cm3#31gcm35 0.00076g (A1.2)One must still ensure
38、 that the correlating instrument actuallymeasures the minimum number of particles (n).APPENDIXES(Nonmandatory Information)X1. SAMPLE CORRELATIONX1.1 Sample DescriptionX1.1.1 The sample used in this illustration of the correlationis silica frac sand. Correlation is between a sieve stack and animaging
39、 system.X1.2 User Specified DistributionX1.2.1 Sieves that makeup the distribution of this sand areas follows:(1) 20 USS,(2) 30 USS,(3) 35 USS,(4) 40 USS,(5) 45 USS,(6) 50 USS,(7) 70 USS, and(8) PAN.X1.2.2 Product distribution is defined as follows:(1) 90 % passing 30 screen and retained above 50 sc
40、reen,(2) No more than 0.1 % on 20 screen, and(3) No more than1%on70screen.X1.3 Analysis of Sample 1X1.3.1 Sample 1 is taken from production inventory at asand manufacturing facility. Table X1.1 shows the percentagein each bin as sieved (on the left) and the raw correlatinginstrument results after th
41、ree runs (on the right) and thecorrelated values in bold type in Column 4 of Table X1.1.Correlation is within 1.5 % for each bin.TABLE X1.1 Sample 1Sample 1Sieve ResultsSample 1UncalibratedInstrument ResultsBin Grams % Recal Run Run 1 Run 2 Run 3 Std Dev r (%)20 USS 0.05 0.05 0 20 USS 1.09 0.74 0.78
42、 0.19 42.9430 USS 2.67 2.72 2.43 30 USS 21.03 19.48 17.49 1.77 17.9735 USS 16.69 17.03 16.07 35 USS 39.98 39.51 38.00 1.03 5.1740 USS 51.10 52.13 51.25 40 USS 30.41 31.65 33.75 1.69 10.3745 USS 22.70 23.16 24.64 45 USS 6.79 7.56 8.75 0.99 25.2050 USS 4.21 4.29 4.92 50 USS 0.51 0.76 0.88 0.19 50.8870
43、 USS 0.56 0.57 0.61 70 USS 0.16 0.25 0.28 0.06 52.65Pan 0.05 0.05 0.06 Pan 0.03 0.05 0.06 0.02 68.87Total 98.03 100.00E2776 183X1.3.2 In this example, the boundaries of the bins used bythe correlating instrument were adjusted so that the totalpercent mass of each bin matched closely with the corresp
44、ond-ing gradation of the primary instrument, in this case a sieve.The data captured in the sample runs was used by the softwareto compare one gradation at a time to its corresponding sieve.A sieve was selected to match and the instrument boundariescorresponding to that sieve were adjusted to include
45、 a revisednumber of particles to better match the percent retained on thecorresponding sieve. The remaining gradations were thenadjusted to match the sieves they correspond to. In thisparticular case the boundary changes were made by thesoftware, however manual changes could also have been made.Chan
46、ges may need to occur on an iterative basis.X1.4 Analysis of Sample 2X1.4.1 Sample 2 is the same type of sand as in Sample 1,however it was taken from a different production lot severalweeks later. The same software correlation is used to run thissample through the correlating instrument. Column 3 o
47、f TableX1.2 shows the sieve percent in each bin and Column 4 ofTable X1.2 shows the correlating instrument percent for eachbin.X2. MULTI SAMPLE DATAX2.1 Correlated Sieve Results from Multiple SamplesX2.1.1 Another 30/50 silica frac sand was used for testing.Twenty samples from a lot of approved sand
48、 was analyzedusing the correlation determined in Appendix X1. See TablesX2.1-X2.20.X2.2 Correlation of Abrasive SampleX2.2.1 A silicon carbide material was correlated to a sievemeasurement and then a fresh sample was tested. The specifi-cation and result are shown in Table X2.21 and Table X2.22,resp
49、ectively.TABLE X1.2 Sample 2Bin Mass (g) %CorrelatingInstrument20 USS 0.05 0.05 030 USS 2.26 2.39 3.8135 USS 20.46 21.60 18.8240 USS 49.69 52.46 51.145 USS 19.28 20.35 22.350 USS 2.78 2.93 3.7370 USS 0.20 0.21 0.22Pan 0.00 0.00 0.01Total 94.72 100.00TABLE X2.1 Sample 1Instrument %Mass in Grams Sieve % Run 1 Run 2 Run 3 Std Dev r20 0.02 0.02 0.00 0.00 0.00 0.00 0.0030 2.68 2.33 1.93 1.78 1.81 0.08 0.2235 19.76 17.20 16.06 14.96 14.65 0.74 2.0840 59.95 52.18 52.55 51.34 51.89 0.16 1.7045 26.18 22.79 24.08 25.82 25.27 0.89 2.4950 5.14 4.47 4.58 5.2
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