vu sip Designation: D 3230—89 (Reapproved 1997)** Standard Test Method for Salts in Crude Oil (Electrometric Method)' ‘Ties sardal i wend the Med desipaioe 3230; the ruber emeditly flowing the designation ideas the year oF sii adopn fhe ease of fein, We yea as vein number i parentheses wads he yer of as reapcoval. A Sapp qtr (eats on eta ese since she at eis of rear, Ths samt ha horn approved for me hy ences ofthe Diners of Dxfse © Nive Siccon 12 yan added ediavily fy November 1597 Seope LU This test method covers the determination of salts in crude vit [2 The accepted concentration units are pounds NaCl per 000 bibl of enude oil 3 This standard dines wot purport to aaddress all of the mas, if any, ussociated wit its use. It (s the responsibiliwy of the user of this standard 10 esiablish appro- priate vafoty and health practices and determine the applic Biliy of regulurory limitations prior to use. For specific precautionary statements, sce 6.3, 6.4, and 6.11 2. Rel 2 enced Docu 457M Standards: 191 Test Method for Preeipitarion Nuniber of Lubricating 0 D381 Test Meth Evaporation? D 843 Specification for Nitration Grade Xylene? 1D.1193 Specification for Reagent Water’ 1D 4037 Practice for Manual Sampling of Petroleum snd Tetroleum Products D4177 Practice for Autonntic Sampling of Petroleum and Peiroleum Products® summary of Test Method 3.1 This teat method is based on the conductivity of a Solution of crude oil in a polar solvent when subjected to an Alternating electrical stress (Note 1), The sample is dissolved in 4 mixed solvent and placed ina test cell consisting of a beaker anid two parallel stainless steel plates. An alternating voltoge is impressed oa the plates and the resulting current flow is shown ‘ona milliammeter, The selt content is obtained by reference to calibration curve of current versvs salt content of known 1d for Existent Gi > This tes med. i ander the jsicive of ASTM Commitee 9-2-08 evalu Products ad Lubes the cite esponsiiy of Subcomnatee ‘a2dSae Elemental Arye ‘Coren etiam apstoved Ost. 27, 989. Sb Decebr 1989, Originally Misiod as D 323072 Last evasion D 2230-83 os lok of SAF Stanton Wl O50 Ait Yook of ASTM Suda, Yo! UGO Srna Dok of STM Suan NON 1.0L Manat ik of ASTM Std NOS 02 20 Nott [This tat method will measure concsivity duc to the salt in the grude oil, Caliration curves are based on standards prepared 10 approximate the type and eancentmation of salts in the erude ols being tested 4, Significance and Use 4.1 This test method is used to determine the salt content of cnide oils, a knowledge of which is important in deciding whether oF not the crude needs desalting. Excessive salt left in the erude frequenily results in higher corrosion rates in refining units. 5. Apparatus S.A Assemble the apparatus as described in Annex AI. 6. Reagents and Materials 6. Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, iti intended that all reagents shall conform to the specifications of the Cornmit tee on Analytical Reagents of the American Chemical Society, ‘where sueit specifications are evatlable.® Other grades may be used, provided it is first ascertained that the reagent is of suflicienily high purity to permit its use without lessening the accuracy of the determination. 62 Purity of Water—Unless otherwise indicated, references to water shall be understood fo mean reagent water as defined by Type Il of Specification D 1193. 63 Alcohol Solvent Mixed Solution, (Warning—See Note 2) Mix 63 volumes of 1-butanol and 37 volumes of absolute ‘methanol; to each litre of this mixture, add 3 mL of water lammable, Liguid causes eve bums. Vapor hirn- ful, May be Fatal or ease bliraness if swallowed of inhaled Camiot be rmade nan poisonous, ‘art 3—The mined aleghol solvet is suitable for use if its conduc: Lig {less hun 0.25 ma when indicated electrode voltage is 125 V a. Reauings greater than 025 mAat 125 Va-c may be due excessive water inthe solvert and indicate that mettavol isnot anhydrous. “enge Chewicals, Amedean Chemical Seciey Speeation.” An. Chery Sex, Wishnton, DC: For stggesions onthe esting of rogers os ise by the Aisilen Chena! Sore, ee Ander Souder fo LaboartoryChenteat, BDI iit, Poole, Dont UK, and the Unt State Plarnacopei and Ntinal Friary 1S. Prarmcopeil Convento, le, (USC), Reekile, MO,4 ASTM Preciptiation Naphtha, (Warning —Seo Note 4), conforming to the requirements of Test Method D 91. Non (Warning: Baremely Flammable, Harm fi may cause fash fire 65 Calcium Chloride Salution (10 g/.)—Transfer 1,000 of calenim chloride (CaCl), oF the equivalent weight of 2 hydrated salt into a 100-mL volumetric ask and dissolve in 25 mil. of water, Dilute o the mark with mixed alechol solvent, 640 Magnesiuat Chloride Solution (10 ws.) —Transfer 1.600 g of magnesium chloride (MyCh, or the equivalent weight of hydrated salt), into 8 100-m. volumetric Nas: and dissolve in 25 mL of water. Dilute to the mark with miixed alcohol solvent. 67 Oil, Refined Neutral—Any refined salt-eer oil of ap- proximately 100 SUS viseosity at 38°C (00°F) and free of auditive. 6.8 Salts, Mixed Solution (Concentrated Sotution)— Combine 10.0 mL. of the CaCl, solution, 200 ml. of the MaCl, solution, and 70.0 ml of the NaCT solution and mix thoroughly. led. Vapors Nore $—The 10:20:70 proportions are sepresenative of the salts prszont in a wade range of ena oils. Whon the slative proportions of fleur, magnesium and sodrn clerides ae Knevwn for given eile ‘ik such proportions sha be usel for most accurate sess, 69 Salis, Mixed Solution (Dilute Solution) —Transfer 10.0 iL of the concentrated mixed salts solution {ao a 1000-mL. volumetric flask and dilute to the mark willy mixed atcotol salvent 6.10 Sodium Chloride Solution (10 g/L) Transfer 1.000 g of sodium chtoride (NaC!) into 4 100-mL volumetric flask and dissolve in 25 ml, of water. Dilute to the niark with mixed alcohol solvent, 6.11 Xylene (Warning—See Note 6) nitration grade, con- forming to the requirements of Specification D 843 (Nove 6 Waraings Planmabie: Vapoe tarmfa 7. Sampling 7.1 Take the summple in accordance with Practice D 4057, or by Method D 4177, 8. Standardization of the Eleetrometric Salt Decerminator Tustrument 81 Connect the eleetrometric salt determinaior instrument (AL1) toa 110-V, 50 0r 60-Hlz source. Ser togate switch $2 s0 that the 25 000 81 (0.5 %) noninductive precision resistor is in the circuit. Set togele switch SI to the high scale (I) and turn switch $3 to the ON position. Adjust the voltage to 125 V sc, Press switch $4 and adjust the 25-2 potentiometer so that the milliammeter is deflected to 0.1 mA. Release switch $4. Change toggle switch St to the tow scale (L). Press switch S4 and adjust the 50-01 poteatiometer so that the pointer is deflccied to full scale (1.0 mA). Rekease switch $$, Tu switch, S3 to the OFF position. Tum switch $2 to the electrode position, Nore 7—The low seal (L) is intended foc use with samples of low salt content and is thos move sersive than the high sete (H), The fll seale reading ofthe millammeer when toggle switch SU is in the L pesition is 1.0'mA, fll seal note indication when switch St isn the Ut position is Wma. 300 TP Yocou 9, Calibration 9.L The apparatus and procedure are calibrated against solutions of neutral oi and mixed salts solution in xylene because of the extreme difficulties in keeping enude oil-brine ‘mixtures homogencous, The calibration may be confirmed, if desired, by careful replicate analysis of enude-oil samples by exhaustive extraction of salts with hot water followed by hiration of the halides in the extract, in calibrating over a wide range of salt contents, it is necessary to apply voltages other than the standardizing voltage (125 V a-e) to obtain current readings within the limit of the instrument (0 i 19 mA) Higher voltages are applied for low standards. and lower voliages are applied fur tigh standards. Do not disturb the smndardization of the instrument when using oder applied voliages, The conductivity of solutions is affected by the temperature at which measurenseats are made. The temperature of samples a the ime of current measurement must be within 3°C (5°F) of the temperature at which the calibration curves ‘were made, 9.2 Runa blank by following the procedure in 93 and 9.4 omitting the mixed salis solution. If the indicated electrode current is greater than 0.23 mA at 123 V a-c, water or another conductive impurity is present and its source must be found and climinated before calibration can be completed, Determine aa blank cach tine fresh xylene or mixed solvent is used 913 Into a dey 100-mL praduated, glass-stoppered mixing cylinder, add 1S ml. of xylene. From a fo contain pipet add 10 iL of noutral oil. Wash the pipet with xylene until free of oil. ‘Make up to 50 mL with xylene, Stopper and shake the eylinder vigorously for at least 60 s to effect solution, Add a quantity oF dilute mixed salts solution ia aecocdance with Table 1 appro: priate to the range of salt contents to be measured. Dilute 10 100 mL with mixed alcohol solvent. Again shake the cylinder vigorously for 30 s to effect solution and allow the solution to stand 5 min. Pour the solution into a dry clectrode beaker. 94 Immediately place the electrodes in the beaker making sure that the upper edge of the electrode is at Rast Ysa in. (1.6 mu) below the surface of the liquid. Set toggle switch SI to high (H) position, Conncet the etzcirodes to the instrument Tura switcl $3 to ON position. Acjust the indicated electrode volings to a series of values, for example 25, $0, 125, 200 and 250 Vae. At each voltage, press S4 and note the milliammeter TABLE 1 Standard Samples ak as Wah Pounds per 100 ined a blot Cada Or Saison 70 03 30 03 30 1s 100 2 38 150 a 200 50 280 a 200 oo soo 0 fo 158 eso 13s 70 Bs a0 as ‘090 ano 0BERa eH ee kmmm & ee é ¢ ih 93230 ng hl eeord (0 Hie wRSL OYL mA, Hie reading, Nowe 9S rine ay be aed he walls of is isd tion, R trodes: fram solution, rinse with xylene — “e*hel solvent este esr or WO avate peso. Th voltig? from the current reading oF te sample 0 sci he lst ny be a ge 259 V 2 tas he net curent reading. Frem the calibration graph (9.6) ead ated salt content corresponding t0 the net milliampete the ad Bias 11, Precision he blank from the Mat This rethod hat been extensively tested ia a . ‘dard samples and plot the rumuber of laboratories and fourid wo give results comparable 10 ampere reading (ah those from other procedures for determining salt in crude ai paper Exact precision dats have not beon derived beoause of inability to obvain stable, homogeneous, and representative samples for ooperative testing. 00-ral. graduated, plasestoppered eylinder yy 9 responsible ASTM 2.03 study group is currently nethod to determine precision values fd 15 mil. of xylene and, by means of to contain pipet, 10 4 re-evaluating nL of crude oil sample. W u me and to 1e scope of the test method to sllow use ee HE modern commercial conductance apparatus. sti fot LL3. The bias for deyernining.the salt content of enide oils owing the solution tostand ‘or 3 min, pour t into BY this test method cannot be determined sincs a suitabl the diy elect " dare in.9.4 to gbtain —siandar material is not availabl i roading at te voltage, Record th wa vusrent 49 thy st 0.01 mA at 12, Keywords fokage, If necessury. recont the temperature of the solution 12.1 conduetivityy emade oil; salt ANNEX (Mandatory formation) AL, APPARATUS ALA Electrometric Salt Determinator (ESD) Components AlL# Variable Voltage Autotransformer, input 102-117 (Fig. ALL, Note ALLL) VSC/60 Hz, output 0-132 V, 1.75 A capacity LL Aditammeten, O-| made with 0-1 mA a-c seale, ALLS Transformer, plate supply 240 V, ccater tap 5060 2 intemal ce Hz, 250 mA dc capacity (filament voliage 5 V, 3.0 A not 7 ‘i apacity at 60 used),!? cinta amperasine Peat Reverse Al-L6 Poteutiometer, 25 0, ten turns |! ‘ ALL? Poteutiometer, 509, ten turns.!? 11.3-AC Fatuneier, rectifier type, 2600 (HV, 0 10 300- Nor AI.I—An equivalent part may Se substituiel in: eich ease siancar WOL4e, av SuncorBlccroic, Manetng Divison olg (§h D 3230 | PIY Switeh (PRESS To MAKE) U5 vac — To Elecirades 60 Herts [OTurn,5 Watt Potentiomaters FIG. Ats1 250 oF 540 Voit opposed and 0.2 uyanylen or TE in handling th mszlignment Fie os areniat —4YLON on weTTER si»jh D 3230 ‘Tre Amancan Seay lor Taig ac Matar talue ne peciionrorpecting he valdiy olay plan ight atzated in cennseson sae any tam montanes nie etandard sore a the tancard ae npsnenysaised iat datormnafon of easly Of ay ah ‘Baor hs, and ho rk of inkingorore of sac rhs. se orey er am respensblty, ‘The stance eutoa to rovison at any tine by the respensbetechicalcammiton and must be revioned ever tha youre and ‘trot raised. ether veapvovedorwitdeann. Your commenisare nite ete ierreislo ol hie standarorlor aaional ardarde “and shouldbe atcressed to ASTI Headausriers. Your eameris wil recov carol cnaieraion ala mest of e roxponsbie feohncal commitae, which you may anend Ifyou falta jour eammants have ne recaved a fal hoaing ye should make your rs kroun 19th AST Contos on Sardis 100 Bar Haraor Dive, Wat Conshehackon, PA 1422,