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    Agua y sedimento en petróleo crudo por el método de centrífuga

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    ASTM D96-88 -Water & Sediment in Crude Oil

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    Agua y sedimento en petróleo crudo por el método de centrífuga

    Copyright:

    © All Rights Reserved
    Download as PDF or read online from Scribd
    Flag for inappropriate content
    Download as pdf
    369 views7 pages

    ASTM D96-88 - Water & Sediment in Crude Oil

    Uploaded by

    pefevago
    Agua y sedimento en petróleo crudo por el método de centrífuga

    Copyright:

    © All Rights Reserved
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    fl) Designation: D 96 ~ 88 (Reapproved 1998) Es Designation: MPMS Chapter 10.4 Peps foment ap OAT Standard Test Method for Water and Sediment in Crude Oil by Centrifuge Method (Field Procedure)’ “isan iad rt rd desiain DD aerial olving ke eno ini i eof isi di tageay Un enerc tr too ye pos connie ose Comper Seiten aon eh ‘ri aha as ho ied for goat replace Mathd 30 of dee Tew Mee Srna Na 7816, 1. Scope LI This test method covers the centrifuge method for otcrmining sediment and water in crude oil during feld castody transfor, This test method may not always provide the ‘most accurate results, but itis considered the most practical ‘method for fled determination of sediment and water. When & higher degree of accuracy is required, the laboratory procedure described in Test Methods D 4006, D 4377 or D473 should be sed, Nore 1_Watr by dsilation and sediment by extraction are eoside ‘ere the mest accurate mets of determining sedi ard wae fn Snide oil As sich, thee methods shuld be employed to resolve Siersoees in teats fom variations ofthis procedure or between this ‘prosede ond eter methods, oa te case af a dispute botween pts This standart does not purport to address all of the safety concerns, if any. associated with its use. tt is the responsibilty ofthe user of this standard 10 establish appro priate safety and health practices and determine the applica- Dility of regulators limitations prior 10 use. 2. Referenced Documents 2.1 ASTM Standard: D235 Specification for Mineral Spirits (Petroleum Spits) (Hydrocarbon Dryeleaning Spirits)? D362 Specification for Industrial Grae Toluenc* D473 ‘Test Method for Sediment in Crude Oils and Fuel Oils by the Extraction Method" 1D 846. Specification for Ten-Degree Xylene 1D 1209 Test Method for Color of Clear Liquids (Platinurn- Cobalt Seale?™ "hist msds une he jin of Cmte 2 on Reem (DO202 08 Seinen! er en ASTM. Cura skon sproed Mani 25.18, Pla Deer 8, Ciginly phe DO -e5r Lat pean eon DST oe ‘Anne Bot 9 AST Sana el 8604 > ame Rast of ATH Sarde, Nl O80 er vrs endl be cad rece eon oe 1D 2699 Specification for Kerosine* ‘1D 4006 Test Mechod for Water in Crude Oil by Distillation? D408? Practice for Manual Sampling of Petroleum and Petroleum Products" 14177 Pructice for Automatic Sampling of Petroleum and Petroleum Products* D437? Test Method for Water in Crude Oils by Potentio- rmettic Karl Fischer Titration* E I Specification for ASTM Thermometers! E542 Practice for Calibration of Volumetric Ware® 22. APY Standards:? ‘Manual of Petroleum Measuremest Standards Chapter 8, Sampling Petroleum and Petroleum Products Chapter 10, Sediment and Water 43. Summary of Test Method 3.1 Known volumes of crude oil and solvent (water satu rated if required) are placed in a centrifuge tube and heated (0 60°C = °C (140"F * °F). After conrifugaton, the volume of the sediment-and-water layer atthe bottom of the tube is read Nove 2—It as been observed that for sone waxy crue oils, tmp tures oF 71°C (180°) ar hiahr may be required To melt he ws eres completely 0 that they are not mesuret a seit. If enperances Fier than °C (L40°F) are nacesay amine this problem, they may be used with the consent ofthe pres nvoled, I wer sstuston ‘fhe solvents rogied mest be done at he sams tempers. 4, Significance and Use 4.1 A determination of sediment and water content is required to determine accuratly the net volumes of erude oil involved in sales, taxation, exchanges, inventories, and custody transfers, An excossive amourt of sediment and water in end * Aaa Boo of ASTM Stunned 14.08 ‘Ae! Boo of AST Stands 81 ingwe, DC 2005, - ib D 96 oil is significant because it can cause corrosion of equipment and problems in processing and warsporting and may violmo {edera, state, or municipal regulations 5. Apparatus 5.1 Centviigo—A centrifuge shall be capable of spioning ‘wo oF more centrifuge tubes ata speed that can be controlled to give a minimum relative centrifugal fores of $00 at the tip Of the thes. The rotation speed necessary to produce a relative centrifugal force of $00 for various diameters of swing can be determined from ‘Table 1 or from one of the following equations: iin = 1235 VF o in = 266 -YRFE a where: rpm. = rojation speed, in revolutions per mioute rulative centrifugal force, iameter of swing, in mm (Eg 1) oF in. (Eq 2), ‘measured between the tips of opposite tuhes when the tubes are in their rotating position ‘The revolving head, (runnion rings, and cunnien cups, including the cushions, shall be constructed to withstand the maximum centifugal force capable of being delivered by the power source. The tunnion cups and cushions shall firmly support the tubes when the centrifuge is in motion. The centrifuge shall be enclosed by a metal shield or case strong igh to contain ying debs in dhe event a tube breaks or the centrifuge malfunctions. S.1.1 The centrifuge shall be heated and shall be capable of maintaining the sample at a temperature of BOC 3°C (40°F S°F). The minimum allowable temperature in the field shall be 52°C (125°F), 5.2 Centrifuge Tubes: 52.1 Centrifuge thes shall be cone shaped and 203 mm (8 in) oF 167 mm (6 in.) in length, Tubes shall conform to the dimensions given in Fig. 1 (203 mm) or Fig. 2 (167 mm) and shall be made of thoroughly annealed glass. A200-parl tbe shall conform co the dimensions shown in Fig. 2, with the ‘marking for esch division muldptied by 2 (For example, 25 rm = 50 parts). The mouth of each tube shall be constricted ‘TABLE 1 Rotation Speeds Necessary to Produce a Relative Contitugal Force of 50 for Contituges of Various Dlametars of Swing Dias Sy ‘eon Sed Tames Tec ‘erin we " 1899 % 103 “Rissa baweanita tal te opproinuies when ies are Poe 7 2 mmo 96.0¢-97.75 mm OD INSIDE TAPER SHAPE FIG. 1 Cone-Shaped Centrifuge Tube 203 mm (8 in) {or closure with a stopper. Graduations fer the 203-mm (8-in.) and 167-nira (G-in.) tubes shall be in accordance with the requirements of Table 2 and Table 3, espectively. The scale errors for a cencrifuge tube shall not ecceed the colerances specified in Table 2 and Table 3. The graduation requirements and scale-erzor tolerances shown in Table 2 and Table 3 apply ‘o calibrations made by reading the botlom of the shaced meniscus of ue-free water ata empecature of 20°C (68°F). The _graduations on cach tube shall be clearly cumbered as shown in Fig. Land Fig. 2 5.22 The tube graduation marks’ accuracy shall be volu- rmewically verified or gravimetrically cared before fleld use OF the tube, in accoréanee with Practice E542 using National Instiwte oF Standards and Technology-raesable equipment The voriliestion or cetificuion shall include a calibration check at exch mark up through the 0.-mL (L-part) mark at the 1 5, and 2emL. (2- 3+, and 4-part) marks: and 2: the 50- and 100-mi. (100- and 260-pant) marks. The tbe shall not be used Moe 17 = 1 44-46 mm 00 ‘Sige of taoer 82-89 aime must be straight FIG. 2 Cone-Shaped Centituge Tube, 167 mm (6 in) ‘TABLE 2 Minimum Graduation Requirements and Méeximum Calitation Tolerances for 9-mm (ein) Gane-Shaped Tubes ange, Sitchin, mt van, Sete ono S030 o8 as 100 2 iF the seale error at any mark exceeds the appticable tglergnee from Table 2 oF 3. 5.3 Preheater—The preheater shall be ether a metal block ‘or a Liquid bath of suficienc depth co permit immersion of the centrifuge tube in the vertical position to the 10kmt. lire (200-part) mark ad capable of heating the sample 10 60 3°C (40°F = $°F), 54 Thermometer shall have greduations at intervals of 1°C (2°E) or less and shall be accurate 10 21°C (22°F), A TABLE 3 tnimum Graduation Roqulroments and Maximum Calloraton Totrances far 187-14 (in) Cone- Shaped Tubes Tee __ Sabie ners Fears soa ba soe ate ae Tors Fea, eatatore = a 100 thermometer such as ASTM IC of 1F is suitable as shown in ‘Speeltcaton E 1. 6, Reagents 6.1. The reagents ised in his section are satisfactory for so in field testing, 62 Denuisifer—When necessary, a demulsifier should be used to promote the separation of water from the sample, 22 provent water from the sample, clinging to the walls of the centrifuge tube, and to eclsanes the distinctiveness of the wateroil interface. In some eases a demulsilir is required ied (See Note 1). When a emulsifier is used, it should be mixed according to the manufacturer's recommendations and should never add tothe volume of sediment and water determined. The emulsifier should always be used in the form of 2 demuisifersoivent stock selution or be premixed with the solvent co be used inthe test. 63 Kerosine (Specification D 3699) 6.2.1 The typical characteristics of kerasine are a distillation ange of 205-300°C (401-872"F), a maximum freezing point of 30°C 22°F), and a minimum ash poiat of 38°C (100°F), 6.3.2 Stoddard solvent and kerosine do not have to be soturated with water, since the solubility oF water in these solvents is n0t significant at 60°C (140°), Nore 3-Warning: Kevin is combust (Se AL}. 64 Stoddard Solvent (Specification D 225}: 6.4.1 The typical characteristics of Stoddard solvent are a silaion range of 149-208°C (300-407°F), 2 minimum fash Point of 38°C (10°F), and aromaties plus olefins content of Tess than 20 9 by volume, None Warning? Sted solves combusible (See A.D. 642 See 63.2. 65 Toluene (Specification D 362): 65.1 The typical characteristics of foluene are a molecular ‘weight of 82, an Atneriean Public Health Association (APHA) color of 10 (in accordance with Test Method D1206), a boiling ange (intial 10 dry point) of 2.0°C 3.6°F) [reeorted boiling point of 110.62C (231.1°Fy, and 0.001 % residue after evapo ration. Toluene passes the American Chemical Society (ACS) test for substances derkened by H,S0,, Nowe 5Wa ing: Toluene is Ramamable (S82 AI 3) 65.2 Toluene and xylene shall be saturated with water at dh ves 60°C * 3°C (140°F = S°F) and mainuained a this temperature uni used. A procedure forthe saturation of solvent is given in te appendix. The watcrsaturaed solvent shall be free from suspended water at the time of use, Toluene and xylene are recommended for sedirsentand-waler determinations invely- ing asphaltenie rude oils. 56 Xplene (Specification D 846) 56.1 The typical characteristics of xylene are» molecular ‘weight of 106, a0 APHA color of not more than 10 (ia accordance with Test Method D 1209), a boiling range of 137 {0 144°C (279 to 291°F), and 0.002 % residue alter evapora- tion. Xylene passes the ACS test for substances darkened by sali sei. Nove 6—Warning: Xe is Cammable (Sse Al), 662 See 652. Sampling 11 Sampling is dainad ax all steps roquined to obtain a rejeesentaive quantity ofthe eantents of any pipeline, tank. or ‘otter sysiem and to pines icin an appropriate contifuze tube, 1. The sample shall be thoroughly representative of the crude ol in question, and he portion ofthe sample used for the seciment and water determination shall be thoroughly repre- sertative ofthe sample itself. fan automatic custody transfor (LACT) unit is involved, vigorous agitation af the sample ‘container is requited before the sample is transferred to the ceitifuge tube or tubes. Only representative samples obtained as specified in Practices D 4057 or D177 shall be used for this tost metho. 1 8. Procedure 8.1 Fill each of two centrifuge tubes to exactly the SO-mL. ({Gikpart} mark witha sample taken diretly from the sampling Gevice (Tor example, » thief bottle, beaker, or LACT sample cortsiner) or the container in which the summple was eolected, Then fil each ube with solvent 10 exactly the 100-mL (200-parp mark, Read the top of the meniscus at both the 30- tne 100-mL. (100- and 200-part) marks. f experience indicates tha, a demulsiier is required and one ns not slreudy been raced to the solvent, add t0 each tube quantity of demasifiet= solvent stock solution that has previously bean determined to be satisfactory fer the crude oil under test. Stopper each tube tighdy and invert the tubes a minimum of 10 times to ensure tha the oil and solvent are uniformly mixed. ove 7—Caution: a genom, the var pes of hycrocuroas | OC (HOF) are eprosimatty deuble hose ne 40°C (10°F, Con ‘ven, bes Spel alvays bo inverted 3 pion below eye lve. LLL Where the erude oil is very viscous and mixing of dhe soltent with the ol is dificult, the solvent may be eed to the centrifuge tube prior to the of o Facilitate mixing. La this ease, ‘exe eae musi be taken to fill the centrifuge tube t9 exactly ‘the $0-mL. (100-part) mark with solvent and then to exactly the LOCemb. (200-part) mark with the sample, 82 Loosen the stoppers to prevent pressure buildup during beating and immerse the cubes to the 10Q-mL (200-part) mark in preheater. Hear the contents to 60°C © 3°C (L20°F = 5°F), 83 Secure the stoppers and again invert dhe tubes 10 times ‘o ensure uniform mixing of the bil and solvent, 84 Place the tzhes in the runnion cups on opposite sides of the centrifuge to establish a balanced condition. Retighten the stoppers and spin for atleast $ mauve at a minimury relative centrifupal force of $00, 8.5 Invmodiately after the centrifuge comes to rest, verity the temperatare. Do not distur the oilewater imterface with the Ahermometer. The test is invalid ifthe final temporaure afer centrifugation is below 52°C (125°F, Nore If the final tener is found be below 52°C (RSP). aljus he couuge hetero increase the final tet tmperaure ant reinile the procede. Beginning with 82, 85.1 Read and record the combined volume of sediment and water atthe Bottom of esc ube as indicated in Table and ig. 3 (Table Sand Fig 4 for 200-part tubes). Reheat both tubes fo 60°C = HC (40F = 5, retum the tubes without asitation to the centrifuge, and. spin for another 5 min atthe same rate, Repeat this operation tnt 1wo consecutive eon 8.6 For he test robe considered valid «clear interface must be observed between the ol layer and the separated water. No jentfiable layering (that is, an emulsion) should be present immediately abowe the oil-vater interface. fn such eases, one or more of the following remedivs may be effective: 8.6.1 Shake the mixture between whilings inthe esntefuse Just enough to disperse the emulsion, 8.6.2 Use a diferent or an increased amount of demulsife. (The demulsifier should noe, however, conubute to the volume of sediment and water) 8.6.3 Use a diferent or an increased amount of solvent. After satisfactory procedure for 2 particular type of oil has been worked ont, i¢ will ordinarily be suitable for all samples of the same crude il 9. Calculation and Repoct 9.1 Compare the readings ofthe two tubes. If the dieronce. bbeween the two reading i grester than one subdivision am the centrifuge tube (see Table 2 of 3) oF 0.025 mL (0.05 % for 200-part tubes) for readings of 0.10 mL (0.20 % for 200-part tubes) and below, the readings are inadmissible andthe

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