aay Designation: 0 6 ~ 8 (Reapproved 1808) Designation: MPMS Chapter 10.4 Standard Test Method for Water and Sediment in Crude Oil by Centrifuge Method (Field Procedure)" Mpa a arssus ern yr ‘ied efi ney en npn Fe Med an 1 1. Seope LI This test method covers the centiyge method for etemining seiment and eter in erode ot during Bed ‘custody transfer. This test method may nt always provide te ‘ost aoorate rel, bt i is coosidered the mow prac) ‘method for feld determination of sdiment and wate When iher degree of accuracy is equred, th laboratory proces Aeserbed in Test Methods D 4008, D377 ce D473 should be ea ove 1M by ison nl aime y exon ecm co te out ms cds of rng ofc ae wt 1.2 This standard does not purport to adress al of the safety concer, fay, sociated with tune Iti the responsibilty of the user of this sandod 9ecablich opp rate aft a health pracces and determine the epic iy of regulatory linia prior to use 2. Referenced Documents 21 ASTM Standart 1235 Specieaton for Mineral Spits Pewoleum Spr) (ydoearton Dryleanng Spits) 1362 Specification for Industial Grade Toluene 1D 473 Test Method for Sediment in Crude Oils and Fuel Oils by the Extraction Method 1 846 Speciation for Ten-Degree Xylene? 1209 Test Method for Color of Clear igus (Pati ‘Cobalt Sele md mc A Su 13689 Specitcaton for Kersinc* 1 40n6 Test Meth for Water n Crate Oi by Distiain® 14057 Practice for Manual Sampling of Pevoleam and Pesroleum Prodics™ 4177 Practice fr Automatic Sampling of Peso and Peiroleom Produc” D377 Test Method for Water in Crate Oils by Poentio. ‘ere Kart Feener Titan ET Specification for ASTM Thermometesst FE 5a2 Practice for Calibration of Volume Ware* 22. API Sandon” Mont of Porteun Moasunment Standards (Chapce 8. Sampling Peleum and Pevolcum Preducs ‘Chaper10, Sediment and Wate 3. Summary of est Method 2.1 Kaown volumes of ede oil and solvent (water sat ‘aid if eid) ate placed i a cantige abe and Heed to GO°C = 3°C (40°F © $°F. Alter centitugaton, th volume ofthe Sedimenand-wair Laer the eter of the Tube Is ‘ead tus of 7-0 1G wig ye ae me tw yas ply th hye mor meso essen sta Wome tn 67°C (47 nay cme spe hey ye ed wh te cart of eps oe, we trot 4 Slgnicance and Use UA detemsinaion of sediment and water content is requited wo determine acurtly the et volumes of ena il involved sles. ation, exchinges, venir, arcu vans An excessive amount of sediment and wate nena 2A of rss Wa AACA Air es@ 096 cil signifcatbaeause i can vate corsion of equipment and problems in processing and transporting and ray violate Feder, or manic elon S. Apparates 51 Conrige—A censifge sal be capable of soning ‘ov or more centifige tesa speed tat cn be controled {orgie a minimum relative const force of 500 at etn ofthe tubes. The rotation sped necessary 0 prduce a relive tiga force of 500 fr various diameters of swing canbe ‘etemined from Table I or fom one of the following uations: os ya © sie = 255 / @ ‘eaton speed, in rvotions per mines Featve ceil force, ‘hamster of swing in tan (Ea 1) of i, (EQ 2, measured beiveen the sof oposite ues when there ae in thi oting poner. ‘The revolving. ead, wansion rng, and tension cops ‘nclaing the cushions, shall be comtrced o wind the ‘animum conga fore ep of being delivered by the power source. The unnion eups and ensions shall tnty poor te tabes when the centifuge is in motion. Tae foniifuge stl be enclosed by a meal eld or ee trong Enc contain yng dari in the vent abe breaks oe enunfuge maluretions Sut Te centage sal be hate sn sal be capable of raining the sample a a temperature of 60 = 3°C (iao"E= SF). The minimum allowable temperate inthe fol shal be 32°C (125°) 52 Conrfge Taber 521 Catrifgetbes sal cone shaped an 203 mm ( in) ce 167 mm (6) i length. Tuber stall conform tothe mansions give i Bg 1 (203 mm) a Fg, 2167 me) and stall be mage of thoroughly anealed gas. A20G part be ‘al confom io the dimensions sven fo Fi. 2, ith the marking foreach division multiplied by 2 (or example, 25 mL = 30 pars). The mouth ofeach tke shal be consticed 4 ‘TABLE 1 Rotation Spads Necessary to Produce a lave cent! Ftc oS tor cenufages ot Varous States at ‘Sng amare aa Raima aes ten Faas on oppo oar Fae EIS eae 000775 mm 00 16.1 Conehaped Contage Tae, 23m (in), Forclosure with a topper Graduations fc the 203-me (in) and. 167mm (Gin) tubes shall bo ip secordance with the ‘quirements of Tale 2 and Table 3, especvely. The scale (tors for a centifge cae sll not exsoed the wolranocs Specied in Table 2 and Table 3. The graduation requiemens ‘hu scale-arortlarance Bown ia Tab Zang Table 3 apply { calibatios made by reading the botlom of the shaded ‘enous of sete water ata emperatre of 20°C (68°F). The ‘raduatons om each tbe sal he lay aambored 3 shown fg. ant Fg. 2 522 The ube graguation marks” accuracy shall be vols ialyverifed or gravimetrically certified efor fll ose ‘ofthe tube, n osordaes th Practice E'542 uring Nation! Insite of Standards end Techacogy-taceele equipment ‘The version or cerification sal! incl a alibation check at each ark up trough te 0.5-mL (part) mak atthe 1.15 and 2 Qa par marks: and athe 50-and ‘o-ma (100 and 200-prt) mss. The be sal nat be sedmate sont 1,2 Coneshspes Carritug Tbe, 167 mm (6a) JTASLE® Hinmum Graduation Reuremen an axiom aura Tolrancss fo 8-nm (in) Cone Sopes abe ‘ifthe scale era ny mark exceeds the applicable oerace fom Tale 20° 3. 5.3 Preteater—the pretest stall be ete «metal bck ‘oc guid bath of silent poh wo peri inuetsion ofthe feniioge tube in the vera! positon to the 10m. lie (200,part) mak and capble of Heating the sample to °C = Bc (lanes 54 Thermomet: shall ave geauatons at neva of FC (2°F) or less and shall be secrate (01°C (227), A thermometer suchas ASTM IC of 1F i stab shown in Speciation 6, Reagents 6.1 The reagent listed i thi ston ae sift for we in eld testing. 182 Demuljfier—Whennacesay, a cemulsor should be sed to promote te spuration of waz fom th sample, ‘revent Water fom the sample, clinging to the wall of te eaiige tbe, and to enlance the distnctvenes of the ‘wae interface: In Sore cass a demulifr i aquired © ‘ain agreement withthe ba meted (ee Note 1) When 3 muster is wed, ie sbould be mised scoring wo the ‘manufac recommendations and shoul ver ad to he volume of sediment apd water étemined. The denulsier "ok soltion ore preined withthe solve tbe used inthe 153 Kerosine(SpecfeaionD 3699) 53:1 Thetypcalchuracetses of kerosine area disilaon range of 205-300°C (401-572°F), a maximum eezing pono 30°C (-22°F, anda minimum Nash pia of 38°C (100°, 632 Stodéard solvent and keosia. do not have 19 be satrted with wate, since to sla selves snot sigalicsnc at 60°C (140 Nore 3Maring: Kee ie oni Se ALD, 4 Stoddard Solves (Speciation D 235) 464.1 The typical charoctersis of Stoddard solvent ae a Ailton range of 148-208°C 200-407"), a minima fash point of 38°C (10°F), and aromatics plas is content of Tos han 205% by volume Now Warning: Soir stent contuil (SA., 642 See63.2 65 Toluene (Specfcaion D 362: 65.1 The ypialetoraceistcs of oluere are x molecular ‘weight of 82, an American Pali Health Association (APH) oor of 10 (in aecortance wih Tes Method D128), boing ‘ange inital to dy pint) of 20°C (35°F [recone boing Pointe 110.6% (23. 1°), ané 0001 residue afer evapo ration Toluene pases the American Chemis Society (ACS) ten for subaanees darkened by #50, None SWarings Tene male (eA). 652 Toluene and xylene shall be saturaed with water at0 60°C = 2°C (140°F = 5°) and msi a this temperate ni use procedure forthe station of sovensie sven in the appendix. The water-saturated solvent sil be fie fom suspended water atte time of ase. Tolvene and xylene at ‘eeommended for semenand-seter determinations fv ing splenic eu oe. “58 pene (Speifomion D 46 55.1 The uplea eharacerisis of xylene ae @ moseuer weight of 105, an APHA color of oat snore than 1D Cn steonance with Tet Method D 1208) a balls ange of (37 {o 148°C (279 t0 291°), aod 0.002 5 residue after evapora: Vion. Xylene pases the ACS test fr substances darkened by selfrc ace ‘Nove 6—Marnng: Xe ama (Se ALA, 652 See652, 1, Sampling 74 Sampling is dofined as all sepa required to obtain a representative quant of th entent of any pple, tank, ot ‘ther sytem and to place it in an epprorat confage be 72 The sample shall be thoroughly represettve of the creo in question andthe parton he ape wed othe Sedinert and water determination cl be hora epe= Sentatve of te sample isa Ian stoma etd taneer (ACT unit i invalid, vigorous agitation ofthe sample container is equied Before the sarple i anseed tothe eoeiige tbe tubes Only representative samples obsied fs speted in Pracices D0ST or D177 stall be wed for Procedure 81 Fl ach of wo corifuge testo exaety the S0-mL (100) mak with ample taken direct frm the sampling ‘oviee (Tor example, thief bottle, beaker, or LACT sample consign or the container in which the sample was collect. ‘Then fil eh ube wih solvent to erally the 1OO-mL (200-part ark. Read ihe tp a the meniscus tbat he 30- snd 100m (100: nd 200 pt) mas expen nese ‘hata demulsier is reqsited ané one hae nt aleady een det the slvest, at each abe quantity of demi. Selvent stock solution that hse previously been determined to be satisfactory forthe end oil under et, Stopes each tbe ‘iahly and invert he tes minima of 10 tes fo ensure "har ihe olan solver re wiformly mixed Nore 7—Contn ua pi me doctansa aPC (40%) aproniaty doe he tae GONE). Ce ‘get. Shoal ays be ed aon bw eve BLL Whee the cud iis very viscous an mixing ofthe solver with dhe il dial dhe Solver may be et the etrtuge tube prior oth ot ite ming, this car, texeme care must be ken to fl the oenuge tbe to exacly ‘he 0-m (100-ar mark with slven and ten exactly he 1m (200 pare mack with the same 182 Loosen the oppers to prevent pes buildup ding bong nd mere the toes fo the [Om (200-9) mk Ina preesir Hest he coments to SO°C = 3°C (aD SF). 83 Seow the stoppers and agai invert the tubes (0 cms to ena wiform mbsng ofthe land solvent, 84 Place the tes the tunnion cups on oposite sides of the cette to establish a Balanced condition, Regen the Hoppe and spin for at lest $ mines a minim eae emg fore of 500, 5 Imei afer the cemifage comes to ees, esfy the temperate. Do not isu he o- waz eta ih the thermometer The tat is nv if he fil temperature afer cetigation is below 52°C (25°F) Nore 31 he na enpete et be iow °C (128%, sje te cere Sa nee tel gee ed ‘hetero, beng ih 82 35.1 Real and record the combined volume of sediment dwar atthe buon af each abe a indexed in Table and Fig. 3 (Table Sand Fi 4Tor200 par tuber) Reheat oth ube © 60°C = 3C (40°F © 57, rewrD the bes witout ‘gation 1 he cen, and spin Fr another 5 min atthe sme ate. Repeat tis operation wot two consecive consis teat eadings te obiined on ach tbe. ‘8 Forthotest tobe considered valida cler interface must be observed betwoan he ol lyer and he separated water, No ‘denise layering ati, an emulsion) shouldbe present immediately above the ol water interface, In such ese. on ‘or mor of the following remedies may be eetive: 61 Shake he mist between whiings i the centfuge Jus enough o dager the emulsion 162 Use a diferent ora inerensd amount of densi (The demas sould ot however, conte othe volume of sient and water) 63 Use'adifaent or an incened amount of sven. Aller satfatorygrocedre for patil ipe ofl bas bean worked out, twill snarl be suitable fr al samples ofthe same cra i. 9 Calenlaion snd Report 9:1 Compare the readings of the Wo tubes. If he dilerence tecnee theo readings is grea tan ne subdlvson on the enefge tube Gee Table or 3) 0025 mL (0.08 5 for part tbes) fr readings of 0.10 mL (0.20% for 200-pat tubes) and below, the readings ae ieadmisible and ‘he ‘etrminton shall be repented ‘9.2 Tf bes graduated In 100 mi. have been wed for he etrmination, er the sum of he fil vom of semen ad water in each tube obtained, a spied in Section 8, td ‘epom this som as tbe pecenage of sediment and water (ee Fig 3 for eading en epoting sediment anc water when ving 1O0.mL cone-shaped cntfuge wber. Report the rele at shown in Table 55 If deceeaing 200-prt wes have Been sed fr the eceminaon, th porentage of sefiment and water fe the verge, 10 thee decimal ples, of te values read rely ffom the two tubes. The percentage can only be read dey roma 200-pr te the tube contain 30 ro 100 pst of al TABLE 4 Procedure for Resting a 106m CaneShaped Tue7.3 Poseduo for Ruodng Sesion’ en tr When Using "Tne Reasig 00 7a, «Pract fr ei Sede nd er Whe sg = paces enter earn pee 94 We mest peueartsstens0mL ota ae i Bs per cana Be bavcage ine ewes Fy Fs ‘tows ES i ea Sie ma p= (9 18 eas fa ae o ee A te 3 volume of sient an water, mor prs and = volume of ol ested, mL ot pas. For example, if te ttl volume of ol tested (¥) i 20 mL andthe volume of saement and wate (5) 80.13 mb Selina snd waee = @1520)x100=075 95 If the test conditions outlined i Section 6 are sat followed exactly, the following must also be reported: 951 The solvent wed andthe water strain cepts 9532 The pe end amour of damulsier Gt used). 953 The tnpetues of the sample and solvent the poheuer temper, the ceaiuge tampon, and he tempertre ofthe final mitre afer cenriuping. 9554 The nberof samples or bes used in the determi- 10, Precisbn and Bias 1011 Precision The precision ofthis est method is being etemined 102 Biar—Since thee is no aceped reference mata suitable for determining the bias no Satemet about bis Is being made@ 06 1 Keywords LT centage: centriige tbe; crue i eld procedure: sampling sediment and water elven ANNEX (andatary Infra) Al PRECAUTIONARY STATEMENTS ALI Kevusine Keep avay fom hes, spk, or open flame. Keep conainor cloned when ot in ane. Keresne’s ‘vapors harmful. Provide adequate venation when Heroine [sused Nether an Occupational Safty and Heath Adminie ‘ation permissible expose lini nor an American Confrence of Governmental Insta Hens tesold lit valve fas been esablished for leone Ingestion of Kerosine rey ese ition of the digestive act ingestion of large nouns may cause signs of cena eros sytem depression. ‘Apion ofthis mater int the nevons system depression. Repetitive applications of Kerosive circtly to the skin of laboratory animals over thoi fetes fa resem skin ‘encer in the annals. Peoleum hydrocarbons of salar omposidon and boiling range have bn shown (0 prodice Lidey damage and more in iaborstory animal. Avoid skin sonaat wih Kerosine. Prolonged repented skin contact ay ‘aus dating and drying ofthe sin AL2. Stoddard Solvent—Keap away from hes, sparks, oF ‘open fame Is cotinr soul be Kap loss hen ‘ie. The salen’ vapor is harmful Adogeate vetilation Should be provided whe the solvent is uied, and siome concentrations shouldbe kept below the established exposare Tints. Tae permissive expose limit etabished by the (Occupational Safety and Health Admiistation fr Sloddir selvent is 500 parsmilin. The American Conference of Governmental inurl Hygienists has established a tveshold Timi aloe of 100 pets pee malion. Inkastion of vapors of Spray mist should be avoided. Acute overxponi may rel I teacon ofthe throat and lung. High consnrtons may ‘aase cena porous system depression, pian of this Ite noth lngs may cause ceria preston. Long term exposure can enuse chronic health effects. Carooke ‘overexposure ha esl in ve, hea, and Blood disorder. Inns apd preracied exposure tothe solvent maybe asso sd wi an increased risk of Key canoe, Kidney dese, and nerve and train damage Avoid skin contact withthe Solvent Prolonged or repeated contact with the iui can ‘esi in drying and éefating ofthe skin that may result in Ieation snd dermis. AL3 Toluene Keep away from heat, sparks, oF ope ‘tame, Keep container close when natin ae. Tobe’ vee ist. Provide adequate venation whos toluene used, and alvbome oncenzatons should be Kept teow the est Tshed exposure limits. The Occupational Safety and Health ‘Administaor bas established a permissible exposie limit of 200 parsmilion, with an aocepable cling’ of 300 parts milion and unacceptable maxima peak of 50 partion for 10 min. The American Conference of Govermectel Tusa Hyglenists hs established a thesbld Uni vale of 100 partsiniion, with a shoe expesie limit of 150, ttn fr | min, Prolonged ovecexposur trugh ink Inson may case coughing, shores of rest, Gziness and Icaion. Aspiration of this materia nko th figs may ase chemical pneumonia. Long-term exposure to this mie Fal may cause choni hein eect. Toluene may remove fas from the skin and cause chronic dermatitis. ter potetal hzarde include posible ver, kidney, and nervous aystem amigo and cardiac snsization wo einpicine I enn, toluene ts been shown tbe tact the embyo a fest high concearaans in anal experimen, however, sich state have filed to demonstrate frank bith defects. Pro. longed or reese skin contact may cause Skin wo become Sy orercted, [AL X9lene—Keepamay from hee, sparks, o open Ame. Keep container close when not in use. Xylene vapor is harm Povide adequate Velation when xylene i ed, ane ep atormeconcerations below entablshod exposure lit its The Occupation Safty and Health Admaisation's esis exposure it or xylene i100 partion. Tae “American Conference of Governmental Inautal Hygienists av esablised a theshod init value of 100 pation with 2 USmin short-term exposure mit of 150 parsinilion Overeposure though intlation may cause sorte of beat, dzziness, ification, and ealase. Aspiration o this ‘material into the fungs may cause coma poeumnis. Long: {Gem expo otis material can cause chron ath es Prolonged, repeated exposure thigh lees of syle can induce cenal nervous sytem problems and may che ver tnd kidney damage. Avis prolonged or repesed skin contact wt xylene. Skin contac may esa delayed skin tation tn blero,XU ter Saturation of Solvents XI Filleachoftwocetifuge tubes tothe 2 (par) rat wih water and hen to the 100ml (20-pa) mask wih the solvent e arated, YU.2 Stopper the thes and shake vigorously for 30s, oii ie rbes below eye level, to disperse the Watt in he tole, Laoren the stoners. XL13 Place the bes cooling the wedolvent iu inco a Sample preheater or hewed (conspnaing) confuse aained ata terpertre of GC (40°F) ora minimum of 30 min, XLL4 Inspect the watdsolvent mitue for suspended vate droplets before use. fan suspended waters vil, he Tubes mos be centfged at a temperate of 60°C (40°F) for Sin ata sped suffcteat vee elaivecemifugal fre of 50 atthe be XLS Use the top 30 ml (100 pars ofthe mixture fom cach abe Forest purposes. Take particule ae nto pour any (Of the ee wae in the ip ofeach tbe int the sample X12 Demir: X11 Aldous a good commerial crude demolsifer wl work eectively wile s wide range of era oi there ae th 096 APPENDIX (Nomandtory intention) ‘XL, DEMULSIFIERS AND WATER SATURATION OF SOLVENTS Some crus for which one demulsifr i more eee han note Ifthe selec dems does a provide the cesied ‘esl others shoul bet X12 Overweuiment wit @ demulsiter can aid erone- ously woth appre seine and water level, Dents 3o bot ie gone contin wate, bu they have lined Solu tn the sovenesampie and, if added in excessive ‘quae, can show up aller conifveing ax 2 spate Immiseblecemponont athe botom ofthe he, To reve this problem he denulssershoald aways bo ed in he Form ofa demulsirsolvent stack solution or shoul be premixed ith the solvent to be sed in the test In ter ease, he ‘uamiy of mule co be added to the solvent shoud be based on tess forte parton desir solvent combi tion. The demir manufeetarer'sintractions shuld be followed when a demulsier soltion i prepred X13_Demlsfrs and demulsifersolven solutions should always be sored in acordance wih the manufacure's re ‘ommendations Each consnerveed to sore dali or ‘Semolsiiersovent solton shoul be dtd, andthe cotets Should be cscarded wien tey reach the demulsier manuf turers recommended tel Iie ‘ce Sy aaron cn tay a etn ccon says etd saat Cine on ayo te aye ‘ops it tony ey ey etme a arent Yas eas ete eat onset Soba ae