Designation: D1322 − 15
An American National Standard
Designation: 598/12
Standard Test Method for
Smoke Point of Kerosine and Aviation Turbine Fuel 1 This standard is issued under the fixed designation D1322; the number immediately following the designation indicates the year of original origin al adoption or, in the case of revis revision, ion, the year of last revision. revision. A number in paren parenthese thesess indicates the year of last reappr reapproval. oval. A superscript epsilon (´) indicates an editorial change since the last revision or reapproval. This standard has been approved for use by agencies of the U.S. Department of Defense.
2.2 Energy Institute Standard:3 IP 367 Petroleum 367 Petroleum products - Determination and application of precision data in relation to methods of test IP 598 P 598 Petro etroleu leum m pro produc ducts ts - Det Determ erminat ination ion of the smo smoke ke point of kerosine, manual and automated method
1. Sco Scope* pe* 1.1 This test method covers two procedures procedures for determ determinaination of the smoke point of kerosine and aviation turbine fuel, a manual man ual pro proced cedure ure and an aut automa omated ted pro proced cedure ure,, whi which ch giv givee results with different precision.
NOTE 1—Only IP 598 published in 2012 by the Institute of Petroleum (now Energy Institute) is equivalent to D1322; IP 57 is not equivalent.
1.2 An inte interla rlabor borato atory ry stu study dy was con conduc ducted ted in 201 2012 2 (se (seee ASTM RR:D02-1747 for supporting data) involving 11 manual laboratories and 13 automated laboratories, with 15 samples tested test ed in blin blind d dup duplica licate. te. The aut automa omated ted pro proced cedure ure dem demononstrated stra ted obj objecti ective ve rati rating ng and sup superio eriorr con contro troll and sho should uld be considered the preferred approach.
3. Terminology 3.1 Definitions: 3.1.1 aviation turbine fuel, n— refined refined petroleum distillate, generally used as a fuel for aviation gas turbines. 3.1.1.1 Discussion— Different Different grades are charac characterized terized by volatility ranges, freeze point, and by flash point.
1.3 1. 3 Th Thee va valu lues es sta state ted d in SI un units its are to be re rega gard rded ed as standard. No other units of measurement are included in this standard.
kerosine, n— refined 3.1.2 kerosine, refined petroleum distillate, boiling between 140 and 300°C, generally used in lighting and heating applications. 3.1.2.1 Discussion— Different Different grades are charac characterized terized by volatility ranges and sulfur content.
1.4 This standar standard d doe doess not purport purport to add addre ress ss all of the safetyy co safet conc ncer erns ns,, if an anyy, as asso socia ciated ted wi with th it itss us use. e. It is th thee responsibility of the user of this standard to establish appro priate safety and health practices and determine the applicability of regulatory limitations prior to use.
3.2 Definitions of Terms Specific to This Standard: 3.2.1 smoke point, n— the the maximum height, in millimetres, of a smokeless flame of fuel burned in a wick-fed lamp of specified design.
2. Referenc Referenced ed Documents Documents 2.1 ASTM Standards:2 D4057 Pr Pract actice ice fo forr Ma Manu nual al Sa Samp mplin ling g of Pe Petro troleu leum m an and d Petroleum Products D6299 Practice D6299 Practice for Applying Statistical Quality Assurance and Control Charting Techniques to Evaluate Analytical Measurement System Performance
4. Summ Summary ary of Test Test Method 4.1 The sample is burned burned in an enclosed wick-fed wick-fed lamp that is calibrated against pure hydrocarbon blends of known smoke point.. The maximu point maximum m height of flame that can be achieved with the test fue fuell wit withou houtt smo smokin king g is det determ ermine ined d to the nearest nearest 0.5 mm with the manual apparatus and to the nearest 0.1 mm with the automated apparatus.
1
Thiss tes Thi testt met method hod is und under er the jur jurisd isdict iction ion of ASTM Com Commit mittee tee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee D02.J0.03 Subcommittee D02.J0.03 on Combustion and Thermal Properties. Curren Cur rentt edi edition tion app approve roved d Apr April il 1, 201 2015. 5. Pub Publis lished hed Jun Junee 201 2015. 5. Ori Origin ginall ally y approved in 1954. Last previous edition approved in 2014 as D1322 – 14a. DOI: 10.1520/D1322-15. 2 For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at
[email protected]. For Annual Book of ASTM Standards volume information, refer to the standard’s Document Summary page on the ASTM website.
5. Signi Significanc ficancee and Use 5.1 This test method provides provides an indication of the relative smoke producing properties of kerosines and aviation turbine 3 Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR, U.K., http://www.ene http://www.energyinst.org.uk. rgyinst.org.uk.
*A Summary of Changes section appears at the end of this standard Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
D1322 − 15
FIG. 2 Smoke Point Princi Principle ple (Aut (Automated omated))
Smoke Poi Point nt Lam Lamp p (Au (Autom tomated ated))4, in ad 6.2 Smoke addi diti tion on to th thee basic components components descri described bed in Annex A1, A1 , as shown in Fig. in Fig. 2, 2, automated units also shall be equipped with a digital camera connected to a computer to analyze and record the height of the flame, a candle displacement system to adjust the height of the flame, and a barometric pressure acquisition system associated to a calibra calibration tion database to select the right calibration value for the automatic calculation of the correction factor defined in 10.1.2.. 10.1.2 6.2.1 The digital camera camera associated to its dedicated software software shall have a minimum resolution of 0.05 mm for the flame height measurement. 6.2.2 6.2 .2 Due to the vas vastly tly sup superi erior or res resolu olution tion of the dig digital ital camera cam era compared compared to the human eye, smo smoke ke poi point nt sha shall ll be measur mea sured ed by the aut automa omated ted unit whe when n ava availab ilable. le. In cas casee of dispute between results from manual and automated methods, the referee shall be considered the automated method.
FIG. 1 Smoke Point Point Lamp (Manual) (Manual)
fuels in a diffusion flame. The smoke point is related to the hydroc hyd rocarb arbon on typ typee com compos positio ition n of suc such h fue fuels. ls. Gen Genera erally lly the more aromatic the fuel the smokier the flame. A high smoke point indicates a fuel of low smoke producing tendency.
6.3 Barometer— With With accuracy of 60.5 kPa. 6.4 Wick, of woven solid circular cotton of ordinary quality, having the follow having following ing charac characteristic teristics: s:
5.2 The smoke point point is quant quantitativel itatively y related to the potential radiant heat transfer from the combustion products of the fuel. Because radiant heat transfer exerts a strong influence on the metal temperature of combustor liners and other hot section parts par ts of gas turbines turbines,, the smoke point provide providess a bas basis is for correlation of fuel characteristics with the life of these components.
Casing Filling Weft Pi c k s
17 en d s , 66 t ex b y 3 9 e n d s , 1 0 0 te x b y 4 4 0 te x b y 2 6 per centimetre
6.5 Pipettes or Burettes, Class A. 4
The sole source of supply of the automated apparatus known to the committee at this time is AD systems (www.adsystems-sa.com), model SP 10 – Smoke Point, available from AD systems, Allée de Cindais, P.A. Portes de la Suisse Normande, 14320 Saint-André-s Saint-André-sur-Orn ur-Orne, e, France. If you are aware of altern alternative ative suppliers, suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible technical committee,1 which you may attend.
6. Appar Apparatus atus 6.1 Smoke Point Lamp (Manual), as shown in Fig. 1 and described in detail in Annex in Annex A1. A1 .
2
D1322 − 15 TABLE 1 Reference Fuel Blends Standard Smoke Point at 101.3 kPa
Tol olue uene ne
2,2, 2, 2,44-tr trim imet ethy hylp lpen enta tane ne
mm 1 4 .7 2 0 .2 2 2 .7 2 5 .8 3 0 .2 3 5 .4 4 2 .8
% (V/V) 40 25 20 15 10 5 0
% (V/V) 60 75 80 85 90 95 10 0
9.3 Extra 9.3 Extract ct al alll wi wick cks, s, ei eith ther er ne new w or fr from om a pr prev evio ious us determination, for at least 25 cycles in an extractor, using a mixturee of equal volum mixtur volumes es of toluene and anhyd anhydrous rous methanol. Allow the wicks to dry partial partially ly in a hood before placing in the oven, or use a forced-draft and explosion-proof oven for drying wicks, or both. Dry for 30 min at 100 to 110°C, and store in a dessicator until used. 9.3.1 Extrac Extracted ted wicks are commer commercially cially available available and may be us used ed,, pr prov ovid ided ed th that at th they ey ha have ve be been en ce certi rtifie fied d as be bein ing g extrac ext racted ted by the pro proced cedure ure out outline lined d in 9.3 9.3.. Store purchased purchased extracted wicks in a desiccator over desiccant until use. After use, extract these wicks as in 9.3 9.3 before before using again.
7. Reag Reagents ents and Materials Materials 7.1 Toluene, ASTM ASTM Re Refe fere renc ncee Fu Fuel el gr grad ade. e. (Warning— Flammable, vapor harmful. (See Annex A2.1 A2.1..))
10. Cali Calibrat bration ion of Appar Apparatus atus Manual Apparatus
2,2,4-trimethylpentane tane (isooctane) (isooctane),, minimum 7.2 2,2,4-trimethylpen minimum pur purity ity 99.75 mass %. (Warning— ( Warning—Flammable, Flammable, vapor harmful. (See Annex A2.2 Annex A2.2..))
10.1 10. 1 Con Confirm firm cali calibra bratio tion n of the app appara aratus tus in acco accorda rdance nce with 10.1.3 or calibrate, if needed, in accordance with 10.1.1 with 10.1.3 with 10.1.1 prior to first use of the day. Recalibrate when there has been a change in the apparatus or operator, or when a change of more than 0.7 kPa occurs in the barometric pressure reading.
7.3 Metha anhydrous. us. ( Warning— Methanol nol (methy (methyll alcoh alcohol), ol), anhydro Flammable, vapor harmful. (See Annex A2.3 A2.3..)) 7.4 Reference Fuel Blends, appropriate to the fuels under test,, pr test prep epar ared ed ac accu currat atel ely y fr from om to tolu luen enee an and d 2, 2,2, 2,44trimethylpentane, in accordance with the compositions given in Table 1, 1, by means of calibrated burettes or pipettes, with a precision precisi on of 60.2% or better.
10.1.1 Calibra 10.1.1 Calibrate te the appar apparatus atus by testing two of the reference fuel blends specified in 7.4 in 7.4,, using the procedure specified in Section 11 Section 11 and, and, if possible, bracketing the smoke point of the sample. If this is not possible, use the two test blends having their smoke points nearest to the smoke point of the sample. 10.1.2 10.1. 2 Determi Determine ne the correc correction tion factor, factor, f , for the apparatus from the equation:
7.5 Heptane, mini minimu mum m pu puri rity ty 99 mas masss %. (Warning— Extremely flammable, vapor harmful if inhaled. (See Annex A2.4..)) A2.4
f 5
8. Samp Sampling ling and Preparatio Preparation n of Samples 8.1 It is re 8.1 reco comm mmen ende ded d sa samp mple less sh shal alll be ta take ken n by th thee procedures proced ures descri described bed in Practic Practicee D4057. D4057. Use the sample as received. Allow all samples to come to ambient temperature (20 6 5°C), without artificial heating. If the sample is hazy or appears to contain foreign material, filter through qualitative filter paper.
~ A
s ⁄ A d ! 1 ~ B s ⁄ B d !
2
(1 )
where: As
= the standar standard d smoke point point of the first referenc referencee fue fuell blend, smoke point point determined determined for for the first first reference reference fuel fuel Ad = the smoke blend, Bs = the standard standard smoke smoke point point of the the second refer reference ence fuel fuel blend, and smoke point determin determined ed for the second second reference reference Bd = the smoke fuel blend.
9. Pre Prepara paration tion of Apparatus Apparatus Manual Apparatus 9.1 Place the lamp in a vertical position position in a room where it can be completely protected from drafts. Carefully inspect each new lamp to ensure that the air holes in the gallery and the air inlets to the candle holder are all clean, unrestricted, and of proper size. The gallery shall be so located that the air holes are completely unobstructed.
If th thee sm smok okee po poin intt de deter termin mined ed fo forr th thee tes testt fu fuel el ex exac actly tly matches the smoke point determined for a reference fuel blend, use as the second bracketing reference fuel the reference fuel blen bl end d wi with th th thee ne next xt hi high gher er sm smok okee po poin int, t, if th ther eree is on one. e. Otherwise, use the one with the next closest smoke point. 10.1.3 An alternative 10.1.3 alternative approach to confirm calibration calibration of the apparatus is for each operator to run a control sample each day the apparatus is in use. Record the results and compare the average from the database of the control sample using control charts cha rts or equ equiva ivalen lentt sta statist tistica icall tech techniq niques ues.. If the dif differ ferenc encee exceeds the control limits or when new apparatus is used, then the apparatus must be recalibrated.
NOTE 2—Slight variations in these items all have a marked effect on the precision of the result obtained.
9.1.1 If the room is not completely completely draft-free, draft-free, place place the lamp in a ver vertica ticall pos positio ition n in a box construc constructed ted of hea heat-r t-resis esistan tantt material (not containing asbestos), open at the front. The top of the box shall be at least 150 mm above the top of the chimney and the inside of the box painted dull black.
Automated Apparatus
Automated Apparatus
10.2 The apparatus apparatus shall have a calibration database database for the storage of the reference fuel blends values specified in Table 1. 1. Each calibration test performed with the reference fuel blends
9.2 Prepa Prepare re the appara apparatus tus according to the manufacturer’ manufacturer’ss instructions. 3
D1322 − 15 shall be stored in this database in addition with the barometric pressu pre ssure re obs observ erved ed at the mom moment ent the cali calibra bration tion was per per-formed. 10.2.1 10.2. 1 The apparatus apparatus shall have the capability to automatically calculate the correc correction tion factor f according according to Eq 1 by automatically selecting in its calibration database the reference fuel blends values specified in Table Table 1, using the procedure specified specifie d in Sectio Section n 11 11 and and the calculation specified in Section 12 and, 12 and, if possible, bracketing the smoke point of the sample. If this is not possible, it shall use the two test blend results having their smoke points nearest to the smoke point of the sample. NOTE 3—The digital camera and the associated software replace the operator operat or eye eyess for the obs observ ervatio ation n of the flam flame. e. Con Conseq sequen uently tly it is not necessary to recalibrate the apparatus when there has been a change in the operator.
10.2.2 Record 10.2.2 Record the bar barome ometri tricc pre pressu ssure re and che check ck in the calibration database that the instrument has been calibrated at that recorded pressure 60.7 kPa. If no calibration values exist forr th fo thee se seve ven n bl blen ends ds sp spec ecifie ified d in Tabl Tablee 1 at the pre pressu ssure re observed 60.7 kPa, calibrate the apparatus in accordance with 10.2.3.. If calibration values exist for the seven blends specified 10.2.3 in Table in Table 1, 1, in other words, if the instrument has been already calibra cali brated ted at the pre pressu ssure re obs observ erved, ed, che check ck the app appara aratus tus in accordance with 10.2.4 with 10.2.4.. NOTE 4—Because 4—Because the autom automated ated apparatus stores the smok smokee points obtained with the reference fuels at different barometric pressures, it is not necessary to recalibrate the apparatus when a change of more than 0.7 kPa occurs in the barometric pressure reading. Depending on the barometric pressure entered at the test initiation, the apparatus will automatically use the cor correc rectt sto stored red values obtained obtained with the fuel ble blends nds.. If the correct correct values are not yet stored, the apparatus will prompt the operator in order to perform the calibration at the pressure observed.
10.2.3 Calibra 10.2.3 Calibrate te the apparatus by testing the seven reference reference fuel blends specified in 7.4 7.4,, using the procedure specified in Section 11 Section 11.. 10.2.4 10.2. 4 At regular intervals intervals of not more than seven days or when there has been a change in the apparatus, verify that the appara app aratus tus is per perfor formin ming g pro proper perly ly by usi using ng a qua quality lity con contro troll (QC)) sam (QC sample ple that is rep repres resent entativ ativee of the fue fuel(s l(s)) rou routin tinely ely tested test ed by the laborator laboratory y to con confirm firm that the apparatu apparatuss is in statistical statistic al contro controll follow following ing the guide guidelines lines given in Practice D6299.. If the difference D6299 difference exceeds the contr control ol limits, recalibrate recalibrate the appara apparatus. tus. 11. Procedur Proceduree 11.1 Soak a piece of extracted and dried 11.1 dried wick, not less than 125 mm long, in the sample and place it in the wick tube of the candle (Fig. (Fig. 3). 3). Carefully ease out any twists arising from this operation. In cases of dispute, or of referee tests, always use a new wick, prepared in the manner specified in 9.3 9.3.. 11.1.1 11 .1.1 It is advisable to resoak the burning-end burning-end of the wick in the sample after the wick is inserted in the wick tube.
FIG. 3 Wick Tube
assembly is not being used, cut the wick horizontally and trim it free of frayed ends so that 6 mm projects from the end of the candle. Use a clean razor blade or other sharp instrument. 11.3.1 11 .3.1 Some razor blades blades have a protec protective tive coating; coating; in such cases, remove the coating with a solvent before using the blade. 11.3.2 11 .3.2 An alte alterna rnative tive method method of pre prepar paring ing a wick free of twists and frayed ends utilizes a wick-trimmer assembly ( assembly (Fig. Fig. 4). The wick-trimmer holder is inserted over the top of the wick tube (Fig. (Fig. 5—Step 5—Step 1) and the long-nosed triceps are inserted throug thr ough h the tube and holder holder ( Fig. 5—S 5—Ste tep p 2) 2).. Th Thee wi wick ck is
11.2 11 .2 Intro Introduce duce as near to 20 mL of the prepared sample sample as available, but not less than 10 mL, at room temperature, into the clean, dry candle. 11.3 Place the wick tube in the candle and screw home. Take Take care that the candle air vent is free from fuel. If a wick-trimmer 4
D1322 − 15 11.6.1 Key in all sample details, enter the current current barometric pressu pre ssure re and initiate initiate the test. For more details, details, ref refer er to the instruction instru ction manual of the appar apparatus atus manuf manufacture acturer. r. 11.6.2 11 .6.2 The candle is automa automatically tically introduced introduced in the lamp and lit. 11.6.3 11 .6.3 The candle level is automatically automatically adjusted so that the flame is approximately 10 mm high and the lamp burns for 5 min. 11. 1.6. 6.4 4 Af After ter th thee 5 mi min n st stab abili ilizat zatio ion n tim time, e, th thee ca cand ndle le is auto au toma matic ticall ally y ra rais ised ed un until til a sm smok oky y ta tail il ap appe pear ars, s, th then en it is lowered slowly. The apparatus software analyses flame images taken by the digital camera. It automatically detects the flame shap sh apee co corr rres espo pond ndin ing g to Fla Flame me B ac acco cord rdin ing g to 11.5.3. 11.5.3. It determines the height of Flame B to the nearest 0.1 mm. The apparatus records the height observed. The candle conveyor lowerss the candle, the flame is automa lower automatically tically extinguished, extinguished, and the conveyor comes back to its rest position.
FIG. 4 Wick Trimmer Assembly Assembly
grasped (Fig. (Fig. 5—Step 5—Step 3) and carefully pulled through the tube without twisting (Fig. (Fig. 5—Step 5—Step 4). The tube is then inserted into the candle and screwed home (Fig. ( Fig. 5—Step 5—Step 5). A new, clean, sharp razor is used to cut the wick at the face of the holder and remove rem ove wisps and fra frayed yed ends ( Fig. 5—Ste 5—Step p 6). When the holder is removed, the wick will be at the correct height in the tube (Fig. 5—Step 5—Step 7).
NOTE 5—Due to the flame height resolution of the digital camera, the flame height is recorded to the nearest 0.1 mm.
11.6.5 The apparatus makes three separate observations 11.6.5 observations of the flame height at the smoke point by repeating the flameappearance appear ance sequen sequence ce specifie specified d in 11.5. 11.5. If the these se val values ues var vary y over a range greater than 1.0 mm, the apparatus shall warn the operator. The test is repeated with a fresh sample and another wick. 11.6.6 11 .6.6 Rem Remove ove the can candle dle fro from m the con convey veyor or,, rin rinse se wit with h heptane, and purge with air to make ready for reuse.
Manual Apparatus 11.4 11 .4 Inser Insertt the candle into the lamp. 11.5 Light the candle and adjust 11.5 adjust the wick so that the flame is approximately 10 mm high and allow the lamp to burn for 5 min. (See Fig. (See Fig. 6 and 6 and Fig. Fig. 7. 7.) Raise the candle until until a smoky tail appears, then lower the candle slowly through the following stages of flame appearance: 11.5.1 11 .5.1 A long tip; smoke slightly visible; visible; erratic and jumpy flame. 11.5 1.5.2 .2 An elongated elongated,, poi pointe nted d tip with the sid sides es of the tip appearing concave upward as shown in Fig. 6 (Flame A). 11. 1.5. 5.3 3 The po poin inte ted d tip ju just st di disap sappe pear ars, s, le leav avin ing g a ve very ry slightly blunted flame as shown in Fig. 6 (Flame B). Jagged, erratic, luminous flames are sometimes observed near the true flame tip; these shall be disregarded. 11.5 1.5.4 .4 A well rounded rounded tip as sho shown wn in Fig. 6 (Flame C). Determine the height of Flame B to the nearest 0.5 mm. Record the height observed. 11.5.4.1 11 .5.4.1 To eliminate errors due to parallax, the eye of the observer shall be slightly to one side of the centerline, so that a reflected image of the flame is seen on the scale on one side of the central vertical white line, and the flame itself is seen again ag ainst st th thee ot othe herr sid sidee of th thee sc scal ale. e. Th Thee re read adin ing g fo forr bo both th observations shall be identical. 11.5.5 11 .5.5 Make three separate separate observations observations of the flame height at the smoke point by repeating the flame-appearance sequence specified in 11.5 in 11.5.. If these values vary over a range greater than 1.0 mm, repeat the test with a fresh sample and another wick. 11. 1.5. 5.6 6 Remov Removee th thee ca cand ndle le fr from om th thee la lamp mp,, ri rins nsee wi with th heptane, and purge with air to make ready for reuse.
12. Calc Calculat ulation ion 12.1 Manual Apparatus— Calculate Calculate the smoke point, to the nearest 0.1 mm, from the equation: Smoke point 5 L 3 f
(2 )
where: L f
= the average average of three three individua individuall readings, readings, and = the correc correctio tion n factor factor (se (seee 10.1.2 10.1.2). ).
12.2 Automated Apparatus— The The smoke point is automatically calculated by the apparatus according to 12.1 to 12.1.. 13. Repo Report rt 13.1 Manual Apparatus— Report Report the result, rounded to the nearest 0.1 mm, as the smoke point of the sample obtained by the manual procedure, and reference this Test Method D1322, manual procedure. Automated Appar Apparatus— atus— Repor 13.2 Automated R eportt th thee re resu sult lt fr from om th thee appara app aratus tus to the nearest nearest 01. mm as the smoke point of the sample obtained by the automa automated ted procedure, procedure, and reference this Test Method D1322, automated procedure.
14. Pre Precisi cision on and Bias 5 Fig. 9) 9) Manual Apparatus (see Table 2 and and Fig. Repeatability,, r— The 14.1 Repeatability The differen difference ce betwee between n success successive ive testt re tes resu sults lts ob obta tain ined ed by th thee sam samee op oper erato atorr wi with th th thee sa same me
Automated Apparatus 11.6 Positio 11.6 Position n the candle on the conveyor of the analyzer as shown on Fig. 8, 8, Steps 1, 2 and 3.
5
Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1178.
5
D1322 − 15
FIG. 5 Wick Positioning Steps
where: r = repea repeatability tability,, and x = smoke point point,, in millimet millimetres. res.
14.2 Reproducibility, R— The The difference between two single and independent results obtained by different operators working in different laboratories on nominally identical test material would, in the long run, in the normal and correct operation of the test method, exceed the follo following wing value in only one case in 20: R 5 0.09363~ x 1 16!
where:
reproducib ducibility ility,, and and R = repro millimetres. es. x = smoke point, in millimetr Fig. 9) 9) Automated Apparatus (see Table 2 and and Fig. 14.3 Repeatability The dif differen ference ce betwee between n success successive ive Repeatability,, r— The testt re tes resu sults lts ob obta tain ined ed by th thee sam samee op oper erato atorr wi with th th thee sa same me appara app aratus tus und under er con constan stantt ope operat rating ing con condit dition ionss on iden identica ticall materia mate riall wou would, ld, in the long run, in the normal normal and correct correct operation of the test method, exceed the following value in only one case in 20: r 5 0.02231 x
where: r = repea repeatability tability,, and x = smoke point point,, in millimet millimetres. res.
14.4 Reproducibility, R— The The difference between two single and independent results obtained by different operators working in different laboratories on nominally identical test material would, in the long run, in the normal and correct operation of the test method, exceed the follo following wing value in only one case in 20:
FIG. 6 Typical Flame Appearances
R 5 0.01651~ x 1 30!
apparatus appara tus und under er con constan stantt ope operat rating ing con conditi ditions ons on ide identi ntical cal material mate rial would, would, in the long run, in the normal normal and correct correct operation of the test method, exceed the following value in only one case in 20:
where: Reproducibili ucibility ty,, and and R = Reprod = smoke point, in millimetres. millimetr es. x
r 5 0.06840~ x 1 16!
NOTE 6—Prec 6—Precisi ision on val values ues wer weree dete determ rmined ined by a joi joint nt EI/ EI/AST ASTM M
6
D1322 − 15
FIG. 7 Examples of Typical Flame Appearances
FIG. 8 Candle Positioning with Automated Apparatus TABLE 2 Typical Precision Values
14.5.1 14.5. 1 The procedure procedure in Test Method D1322 for measuring the smoke point of kerosines and aviation turbine fuels has no bias because the value of the smoke point can only be defined in terms of a test method. 14.5.2 14. 5.2 A relative relative bia biass exis exists ts bet betwee ween n the manual and the automated procedures. The bias takes the form of an approximatel ma tely y un unif ifor orm m ra ratio tio,, ap appl plic icab able le ov over er th thee wh whol olee ra rang ngee of results. The corresponding bias relationship is:
NOTE 1—r = repeatability; R = reproducibility Mean Result 15 20 25 30 35 40 42
Manu Ma nual al Pr Proc oced edur ure e
Auto Au toma mate ted d Pr Proc oced edur ure e
r
R
r
R
2. 12 2. 46 2. 80 3. 15 3. 49 3. 83 3. 97
2. 90 3. 37 3. 84 4. 31 4. 78 5. 24 5. 43
0. 33 0. 45 0. 56 0. 67 0. 78 0. 89 0. 94
0 .7 4 0 .8 3 0 .9 1 0 .9 9 1 .0 7 1 .1 6 1 .1 9
~ A
1
16! 5 ~ M 1 16! ⁄1.016
(3 )
where: M = man manual ual res result ults, s, and and automated result results. s. A = automated
program in 2012,6 with 11 manual labs, 13 automated labs and 15 different samples tested in blind duplicates. The results were evaluated for precision according to the statistical procedures given in IP 367 as implemented in ASTM D02 computer program D2PP.
14.5.3 Results 14.5.3 Results usi using ng the aut automa omated ted ins instru trumen mentt sha shall ll be reported without correction for bias.
14.5 Bias:
15. Keyw Keywords ords 15.1 aviatio aviation n turbine fuel; combu combustion stion properties; properties; jet fuel; kerosine; radiant heat; smoke point
6
Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1747.
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D1322 − 15
FIG. 9 Graph Graphical ical Repre Representat sentation ion of the Precisions
ANNEXES (Mandatory Information) A1. APPARA APPARATUS TUS
Smoke Point Lamp, as shown in Fig. 1, A1.1 Smoke 1, complying with the dimens dimensional ional requirements requirements given in in Table Table A1.1 and A1.1 and as shown sho wn in Fig. A1.1 and Fig. A1.2. A1.2. The follo following wing essent essential ial requirements shall be met:
shall have a range of 50 mm graduated in 1 mm intervals, figured at each 10 mm and with longer lines at each 5 mm.
NOTE A1.1—A medium-density cobalt glass may be used to reduce eye fatigue when viewing the flame.
A1.1.3 An efficient efficient device for raising or lowering the flame shall be provided. The total distance of travel shall be not less than 10 mm and the movement shall be smooth and regular.
A1.1.1 The top of the wick guide shall be exactly level A1.1.1 level with the zero mark on the scale.
A1.1.4 A1. 1.4 The glass window window of the door shall be cur curved ved to prevent the formation of multiple images.
A1.1.2 A1. 1.2 The scale shall be mar marked ked in whi white te lines on bla black ck glass on each side of a white or black strip 2 mm in width. It
A1.1.5 A1. 1.5 The joint between between the bas basee of the can candle dle and the candle body shall be oil-tight.
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D1322 − 15 TABLE A1.1 Critical Dimensions of Smoke Point Lamp Dimension, mm Lamp Body ( Body (Fig. Fig. A1.1) A1.1) Candle Socket (C) Internal diameter Wick Guide (D) Internal diameter Air Inlets (20 in number) (E) Diameter Gallery (F) External diameter Air inlets (20 in number), diameter Lamp Body (G) Internal diameter Internal depth Chimney (H) Internal diameter Height, top of chimney to center of lamp body Candle ( Candle (Fig. Fig. A1.2) A1.2) Candle Body Internal diameter External diameter Length, without cap Thread on cap Wick Tube (A) Internal diameter External diameter L e n g th Air-Vent (B) Internal diameter L e n g th † Editorially corrected.
Tolerance, mm
2 3. 8
± 0. 05
6 .0
± 0 .0 2
2. 9
± 0. 05
3 5 .0 3 .5
± 0 .0 5 ± 0 .0 5
8 1. 0 8 1. 0
± 1. 0 ± 1 .0
4 0. 0 13 0
± 1. 0 ± 1 .0
2 1. 25 .. . sliding fit in candle holder 10 9† ± 0 .0 5 9.5 mm dia screwe screwed d 1.0 mm pitch 4 .7 ± 0 .0 5 c l o s e fi t i n fl a m e gu i d e 8 2. 0 ± 0 .0 5 3 .5 9 0. 0
9
± 0 .0 5 ± 0 .0 5
D1322 − 15
NOTE 1—Dimensions are millimetres. FIG. A1.1 Lamp Body
10
D1322 − 15
FIG. A1.2 Candl Candle e
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D1322 − 15 A2. WARNING STATEMENTS STATEMENTS
A2.1 Toluene
nonpoisonous. Keep away from heat, sparks and open flame. Keep container closed. Avoid contact with eyes and skin. Avoid breathing of vapor or spray mist. Use with adequate ventilation. Do not take internally.
A2.1.1 Warning—Flammable. Warning—Flammable. Vapor harmful. Keep away from heat, sparks and open flame. Keep container closed. Use with adequate ventilation. Avoid breathing of vapor or spray mist. Avoid prolonged or repeated skin contact.
A2.4 Hept Heptane ane
A2.2 2,2,4-T 2,2,4-Trimethylpe rimethylpentane ntane (Isooctane)
A2.4.1 Warning—Ext remely ely flamm flammabl able. e. Har Harmfu mfull if inWarning—Extrem haled. Vapor may cause flash fire. Keep away from heat, sparks and open flam flame. e. Kee Keep p con contain tainer er clo closed sed.. Use wit with h ade adequa quate te ventilation. Avoid build-up of vapors and eliminate all sources of ignition, especially nonexplosion-proof electrical apparatus and hea heaters ters.. Avoi void d bre breath athing ing of vap vapor or or spr spray ay mis mist. t. Avoi void d prolonged or repeated skin contact.
A2.2.1 Warning—Extr emely y flam flammab mable. le. Har Harmfu mfull if inWarning—Extremel haled. Vapor may cause flash fire. Keep away from heat, sparks and ope open n flam flame. e. Kee Keep p con contain tainer er clo closed sed.. Use with ade adequa quate te ventilation. Avoid buildup of vapors and eliminate all sources of ignition, especially nonexplosion-proof electrical apparatus and hea heater ters. s. Avoi void d bre breath athing ing of vap vapor or or spr spray ay mist mist.. Avoi void d prolonged or repeated skin contact. A2.3 Metha Methanol nol (Met (Methyl hyl Alcohol) Alcohol) A2.3.1 Warning—Flammable. Warning—Flammable. Vapor harmful. May be fatal or cause blindness if swallowed or inhaled. Cannot be made
APPENDIX (Nonmandatory Information) X1. HELPFUL INFORMATION INFORMATION ON WICK EXTRACTION AND CYCLE TIMES TO AVOID CONSTANT CONSTANT ATTENDANC ATTENDANCE E
X1.1 Extra X1.1 Extract ct all wick wicks, s, eit eithe herr ne new w or fr from om a pr prev evio ious us determination determi nation using the following following proced procedure: ure:
taken for two complete filling and emptying cycles be determined. Then the time for 25 cycles may be calculated. The wick(s) should then be extracted for at least this period of time.
X1.1.1 X1. 1.1 Place the wic wick(s k(s)) in an ext extrac ractor tor and ext extrac ractt the wick(s) wick( s) wi with th a mi mixt xtur uree of eq equa uall vo volu lumes mes of to tolu luen enee an and d anhydrous methanol for at least 25 filling and emptying cycles. Soxhlet or similar extraction apparatus are permitted.
X1.1.3 Drain the wick(s) wick(s) and place on absorbent absorbent paper in a fume hood and allow to dry. After drying, place wick(s) in a suit su itab able le ov oven en at 10 100° 0°C C to 110 10°C °C fo forr 30 mi min. n. St Stor oree in a desiccator until required.
X1.1.2 X1. 1.2 In order to ove overco rcome me the need for an ope operat rator or to stand and count 25 cycles, it is recommended that the time
SUMMARY OF CHANGES Subcommittee D02.J0 has identified the location of selected changes to this standard since the last issue (D1322 – 14a) that may impact the use of this standard. (Approved April 1, 2015.) (1) Revised Revised 10.2.1 10.2.1,, 12.1 12.1,, 13.1 13.1,, and 13.2 and 13.2;; added new subsection 12.2.. 12.2
Subcommittee D02.J0 has identified the location of selected changes to this standard since the last issue (D1322 – 14) that may impact the use of this standard. (Approved Dec. 1, 2014.) (1) Added Added 6.2.2 6.2.2..
Subcommittee D02.J0 has identified the location of selected changes to this standard since the last issue (D1322 – 12 1) that may impact the use of this standard. (Approved Oct. 1, 2014.) ε
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D1322 − 15 Added Appendix Appendix X1. X1 . (1) Added ASTM International International takes no positi position on respecting the validi validity ty of any patent rights assert asserted ed in connec connection tion with any item mentio mentioned ned in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk of 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 and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible respon sible technical technical committee, which you may attend. If you feel that your comments have not receiv received ed a fair hearing you should make your 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 above address addr ess or at 610610-832832-9585 9585 (pho (phone), ne), 610610-832832-9555 9555 (fax (fax), ), or serv service@ ice@astm astm.org .org (e-m (e-mail) ail);; or thro through ugh the ASTM webs website ite (www.astm. (www .astm.org). org). Permission Permission rights to photocopy the standa standard rd may also be secure secured d from the Copyri Copyright ght Clearance Center, Center, 222 Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/
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