This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D3230 − 19
Standard Test Method for
Salts in Crude Oil (Electrometric Method)1 This standard is issued under the fixed designation D3230; 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.
1. Sco Scope* pe* 1.1 1. 1 Th This is tes testt met metho hod d co cove vers rs the de dete term rmin inati ation on of the approximate chloride (salts) concentration approximate concentration in crude oil. The range of concentration covered is 3.5 mg ⁄kg to 500 mg ⁄kg or 1.0 1. 0 lb ⁄1 ⁄100 000 0 bb bbll to 15 150 0 lb ⁄1 ⁄100 000 0 bb bbll (P (PTB TB)) as ch chlo lori ride de concentration concen tration/volum /volumee of crude oil. 1.2 This test method measures measures conductivity conductivity in the crude oil due to the pre presen sence ce of com common mon chlorides chlorides,, suc such h as sod sodium ium,, calcium, and magnesium. Other conductive materials may also be present in the crude oil. 1.3 Th 1.3 Thee va valu lues es sta stated ted 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. 1.3.1 Exception— Acceptable Acceptable concentration concentration units are g/m3 or PTB (lb/1000 bbl). 1.4 This standar standard d doe doess not purport purport to add addre ress ss all of the safet sa fetyy co conc ncer erns ns,, if an anyy, as asso socia ciate ted d wi with th its us use. e. It is th thee responsibility of the user of this standard to establish appro priate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific warning statements, see see 7.3 7.3,, 7.4 7.4,, and and 7.11 7.11.. 1.5 This int intern ernati ationa onall sta standa ndard rd was dev develo eloped ped in acc accor or-dance with internationally recognized principles on standardizatio iza tion n es esta tabl blis ishe hed d in th thee De Decis cisio ion n on Pr Prin incip ciple less fo forr th thee Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee. 2. Referenc Referenced ed Documents Documents 2.1 ASTM Standards:2 D381 Test D381 Test Method for Gum Content in Fuels by Jet Evaporation 1
Thiss tes Thi testt met method hod is und under er the jur jurisd isdict iction ion of AST ASTM M Com Commit mittee tee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee D02.03 Subcommittee D02.03 on on Elemental Analysis. Curren Cur rentt edi editio tion n app approv roved ed May 1, 201 2019. 9. Pub Publis lished hed May 201 2019. 9. Ori Origin ginall ally y approved in 1973. Last previous edition approved in 2018 as D3230 – 13 (2018). DOI: 10.1520/D3230-19. 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.
D1193 Specification for Reagent Water D1193 D4928 Test D4928 Test Method for Water in Crude Oils by Coulometric Karl Fische Fischerr Titr Titration ation D5002 Test D5002 Test Method for Density, Relative Density, and API Gravity of Crude Oils by Digital Density Analyzer 3. Terminology 3.1 Definitions of Terms Specific to This Standard: 3.1.1 PTB— lb/1000 lb/1000 bbl. 3.1.2 salts commonly nly,, chlor chlorides ides of sodiu sodium, m, salts in cru crude de oil— commo calcium, and magnesium dissolved in crude oil. Other inorganic chlorides may also be present. 4. Summ Summary ary of Test Test Method 4.1 This test method measures measures the conductivity conductivity of a solution of crude oil in a mixed alcohol solvent when subjected to an electrical stress. This test method measures conductivity due to the pre presen sence ce of ino inorg rganic anic chl chlori orides des,, and oth other er con conduc ductive tive materia mate rial, l, in the cru crude de oil. A hom homoge ogenize nized d test specimen specimen is dissolved in a mixed alcohol solvent and placed in a test cell consisting of a beaker and a set of electrodes. A voltage is impressed on the electrodes, and the resulting current flow is measured. The chloride (salt) content is obtained by reference to a calibration curve of current versus chloride concentration of known mixtures. Calibration curves are based on standards prepared to crude approximate thetested. type and concentration of chlorides in the oils being 5. Signi Significanc ficancee and Use 5.1 This test method is used to determine the approximate approximate chlo ch lori ride de co cont nten entt of cr crud udee oi oils ls,, a kn know owle ledg dgee of wh whic ich h is impo im porta rtant nt in de decid cidin ing g wh whet ethe herr or no nott th thee cr crud udee oi oill ne need edss desalting. The efficiency of the process desalter can also be evaluated. 5.2 Excess Excessive ive chloride chloride left in the crude oil frequently frequently results in hi high gher er co corr rros osio ion n ra rate tess in re refin finin ing g un unit itss an and d al also so ha hass detrimental effects on catalysts used in these units. 5.3 This test method provides provides a rapid and convenient convenient means of determining the approximate content of chlorides in crude oil and is useful to crude oil processors.
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D3230 − 19 6. Appar Apparatus atus 6.1 The apparatus apparatus (see (see Annex Annex A1) A1) shall consist of a control unit capable of producing and displaying several voltage levels for applying stress to a set of electrodes suspended in a test beak be aker er co cont ntain ainin ing g a te test st so solu lutio tion. n. Th Thee ap appa para ratu tuss sh shall all be capable cap able of meas measuri uring ng and dis displa playin ying g the cur curren rentt (mA (mA)) con con-ducted through the test solution between the electrodes at each voltagee level. voltag NOTE 1—Some apparatus are capable of measuring voltage and current internally and, after comparison to internal calibration curves, of displaying the resul resultant tant concen concentratio tration. n.
6.2 Test Beaker— See Annex See Annex A1. A1. 6.3 Pipet, 10 mL (total delivery), shall be used in 10.3 10.3 and 11.1 when when th thee vi visc scos osity ity of th thee cr crud udee oi oill mat mater erial ial be bein ing g analyzed is suitable to transfer the required volume for use in the test (see 6.3.1 (see 6.3.1)). The type of pipet to use is one that is able to be ri rins nsed ed to en ensu sure re th thee en entir tiree vo volu lume me of th thee ma mater teria iall is contained in the intended volume. 6.3.1 In some cases, the viscosity viscosity of the crude oil makes it difficult and impractical to transfer 10 mL of sample using a pipet. In such cases, it is permissible to use a 10 mL graduated cylinder in place of the pipet to transfer the neutral oil (10.3 ( 10.3)) and crude oil sample (11.1 ( 11.1)) to ensure consistency. The current ` , , , ` , , ` ` ` ` ` ` , ` ` ` , , , ` ` ` ` ` , ` ` ` , , , ` -
precision statements are based on the use of 10 mL pipets only. 6.4 Cylinders, 100 mL, stoppered. 6.5 Other volumetric and graduated pipets and volumetric flasks. 7. Reag Reagents ents and Materials Materials 7.1 Purity of Reagents— Reagent Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all reagents shall conform conform to the specifications specifications of the America American n Chemicall Societ Chemica Society y, where such specifi specification cationss are availab available. le.3 Other grades may be used, provided it is first ascertained that thee re th reag agen entt is of su sufffici icien ently tly hi high gh pu puri rity ty to pe perm rmit it its us usee without lessening the accuracy of the determination. 7.2 Purity of Water— Unless Unless otherwise indicated, references to water shall be understood to mean reagent water as defined by Type II in Specification D1193 D1193.. 7.3 Mixed Alcohol Solvent— Mix Mix 63 volumes of 1-butanol and 37 volum volumes es of absolu absolute te methyl alcohol (anhy (anhydrou drous). s). To each litre of this mixture, add 3 mL of water. (Warning— ( Warning— Flammable. Liquid causes eye burns. Vapor harmful. May be fatal or cause blindness if swallowed or inhaled.) NOTE 2—The mixed alcohol solvent is suitable for use if its conductivity tivit y is le less ss th than an 0. 0.25 25 mA at 12 125 5 V ac (o (orr 2 mi micr cros osie ieme mens ns). ). Hi High gh conductivity can be due to excess water in the solvent and can indicate that the methyl alcohol used is not anhydrous.
7.4 Hexa Extremely Hexanes, nes, Reag Reagent ent Gra Grade, de, ( Warning— Warning—Extremely flammable, harmful if inhaled.) 3
Reagent Chemicals, American Chemical Society Specifications, Americ American an
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed by the American American Chemi Chemical cal Society, Society, see Annual Standa Standards rds for Labor Laboratory atory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
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NOTE 3—Hexanes solvent is sometimes referred to or sold by other names, such as petroleum naphtha, petroleum ether, ligroine, petroleum benzin ben zin,, and ind indust ustria riall nap naphth htha. a. One should should con confirm firm that it mee meets ts the requirements of 7.4. 7.4 .
7.5 Calcium Chloride (CaCl2) Solution (10 g ⁄L) — Transfer Transfer 1.00 g 6 0.01 0.01 g of Ca CaCl Cl2, or th thee eq equi uiva vale lent nt we weig ight ht of a hydrated salt, into a 100 mL volumetric flask and dissolve in 25 mL of water. Dilute to the mark with mixed alcohol solvent. 7.6 Magne Magnesiu sium m Chl Chlori oride de (Mg (MgCl Cl2) So Solu lutio tion n (1 (10 0 g ⁄L ⁄L)— )— 6 2 Transfer 1.00 g into 0.01 g of MgCl , or theflask equivalent weight of a hydrated salt, 100 mL volumetric and dissolve in 25 mL of water. Dilute to the mark with mixed alcohol solvent.
7.7 Sodium Sodium Chl Chlori oride de (Na (NaCl) Cl) Sol Soluti ution on (10 g ⁄L) ⁄L)— — Transfer 1.00 g 6 0.01 g of NaCl into a 100 mL volumetric flask and dissolve in 25 mL of water. Dilute to the mark with mixed alcohol solvent. 7.8 Oil, Refined Neutral— Any Any refined chloride-free oil of approximately 20 mm2 /sec (cSt) viscosity at 40 °C and free of additive. 7.9 Salt Salts, s, Mixe Mixed d Solu Solution tion (Co (Concen ncentrat trated ed Sol Solutio ution)— n)— Combinee 10.0 mL of the CaCl2 solutio Combin solution, n, 20.0 mL of the MgCl2 soluti sol ution, on, and 70. 70.0 0 mL of the NaC NaCll sol solutio ution, n, and mix tho thorroughly. NOTE 4—The 10:20:70 proportions are representative of the chlorides present in a number of common crude oils. When the relative proportions of calcium, magnesium, and sodium chlorides are known for a given crude oil, such proportions should be used for most the accurate results.
7.10 Salts, Mixed Soluti Solution on (Dilut (Dilutee Solut Solution)— ion)— Tra Transfer nsfer 10 mL of th thee co conc ncen entr trate ated d mi mixe xed d ch chlo lori ride dess so solu luti tion on in into to a 1000 mL volumetric flask, and dilute to the mark with mixed alcohol solvent. 7.11 Xylene, reagent grade, minimum purity. (Warning— ( Warning— Flammable. Vapor harmful.) 8. Sampl Sampling ing 8.1 Obtain a sample and test specimen in accordance accordance with Test Metho Method d D4928. D4928. Ensure Ensure tha thatt the sam sample ple is com comple pletely tely homogenized with a suitable mixer. See Test Method D4928 for suitable apparatus and proving. 8.2 Sample Sampless of very viscous materials may be warmed until they are reasonably fluid before they are sampled; however, no sample shall be heated more than is necessary to lower the viscosity to a manageable level. 8.3 Sample Sampless of crude oil contain water water and sediment sediment and are inhomogeneous by nature. The presence of water and sediment will influence the conductivity of the sample. The utmost care shall sha ll be tak taken en in obt obtain aining ing hom homog ogeniz enized ed rep repres resent entativ ativee samples. 9. Preparat Preparation ion of Apparatus Apparatus 9.1 Suppo Support rt the apparatus apparatus on a level, steady steady surface, such as a table. 9.2 Prepar Preparee the appar apparatus atus for operation operation in accord accordance ance with the manufacturer’s instructions for calibrating, checking, and operating the equipment. (Warning— (Warning—The The voltage applied to the electrodes can be as great as 250 V ac, and hazardous.) Number: 02260707 2Order Sold to:SERVICES INTER LAB DE MEXICO [700168] -
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D3230 − 19 Thoroughl oughly y clean and dry all parts of the test beaker, beaker, the 9.3 Thor electrodes, and its accessories before starting the test, being sure to remove any solvent that had been used to clean the apparatus. 10. Cali Calibrati bration on
since the electronics are built-in for auto-ranging. Determination of the blank and the calibration standard responses are the same.
10.5 Repeat the procedure procedure in 10.3 in 10.3,, using other volumes of mixed salts solution (dilute solution) as needed to cover the range of chloride contents of interest.
10.1 The conductivity conductivity of soluti solutions ons is af affected fected by the temperature of the specimen when measurements are made. The temperature of the test specimen at the time of measurement
10.6 Subtr Subtract act the value obtained for the blank measurement measurement from the indicated current readings of each standard sample, and plo plott the chl chlori oride de con conten tentt (or (ordin dinate) ate) aga agains instt net cur curren rentt (mA)) rea (mA readin dings gs (ab (abscis scissa) sa) for eac each h vol voltag tagee on 3 by 3 cyc cycle le
shall bewere within 3 °C of the temperature temperature at which the calibration calibration curves made.
log-log paper, or other suitable format.
10.2 Establi Establish sh a blank measurement measurement by following following the procedure ced ure in 10.3 and 10.4, 10.4, omitting omitting the mix mixed ed salt saltss sol solutio ution. n. When the indicated electrode electrode current is greater than 0.25 mA at 125 V ac, water or another conductive impurity is present and its source must be found and eliminated before calibration can be completed. Determine a blank measurement each time fresh xylene or mixed solvent is used. 10.3 Into a dry dry,, 100 mL graduated, graduated, glass-stopper glass-stoppered ed mixing cylin cy linde derr, ad add d 15 mL of xy xylen lene. e. Fr From om a 10 mL pi pipe pett (t (tot otal al delivery deliver y, see 6.3 6.3), ), or 10 mL gra gradua duated ted cyl cylind inder er (se (seee 6.3.1) 6.3.1) when applicable, add 10 mL of neutral oil. Rinse the 10 mL pipet or 10 mL graduated graduated cylinder with xylene until free of oil. Make up to 50 mL with xylene. Stopper and shake the cylinder vigoro vig orousl usly y for app approx roxima imately tely 60 s to ef effec fectt sol solutio ution. n. Add a quanti qua ntity ty of dil dilute ute mix mixed ed salt saltss sol soluti ution, on, in acco accorda rdance nce with Table 1, 1, that is appropriate to the range of salt contents to be measured. measur ed. Dilute to 100 mL with mixed alcohol solvent. solvent. Again shake the cylinder vigorously for approximately 30 s to effect solution, and allow the solution to stand approximately 5 min. Pour the solution into a dry test beaker. 10.4 Immedi Immediately ately place the electro electrodes des into the solutio solution n in the beaker, making sure that the upper edge of the electrode plate pl atess ar aree be belo low w th thee su surf rface ace of th thee so solu lutio tion. n. Adjust Adjust th thee indicated electrode voltage to a series of values, for example 25 V, 50 V, 125 V, 200 V, and 250 V ac. At each voltage, note the current reading and record the voltage displayed and the current to the nearest 0.01 mA. Remove the electrodes from the solutio sol ution, n, rin rinse se with xylene followed followed by nap naphth htha, a, and allo allow w them to dry. NOTE 5—With some apparatus, the detailed settings will not be required TABLE 1 Standard Samples Salt, g/m3 of Crude Oil
Salt, lb/1000 bbl of Crude Oil
Mixed Salts Solution (dilute), mL
3 9 15 30 45 60 75 90 115 145 190 215 245 290 430
1.0 3.0 5.0 10.0 16.0 21.0 26.0 31.0 40.0 51.0 66.0 75.0 86.00 101.0 151.0
0.3 1.0 1.5 3.0 4.5 6.0 8.0 9.5 12.0 15.0 20.0 22.5 25.5 30.5 45.0
NOTE 6—Some apparatus are capable of internally recording the current readings, standard concentration, and blank, and they provide an output in direct concentration units. Alternatively, some apparatus are also capable of int intern ernall ally y con conver vertin ting g and dis displa playin ying g the mea measur sured ed cur curren rents ts int into o conductivity units of microsiemens, µS, although the precision of such instruments was not evaluated in the 1997 interlaboratory study identified in Section 14 Section 14,, Precision and Bias. NOTE 7—The apparatus apparatus are calibr calibrated ated against stand standard ard solut solutions ions of neutrall oil and mixed chloride solutions neutra solutions in xylene because because of the extreme difficulties in keeping crude oil-brine mixtures homogeneous. The calibratio bra tion n may be con confirm firmed, ed, if des desire ired, d, by car carefu efull rep replica licate te ana analys lysis is of crudecru de-oil oil sam sample pless by exh exhaus austiv tivee ext extrac ractio tion n of sal salts ts wit with h hot wat water er,, followed by titration of the chlorides in the extract. NOTE 8—In calibrating over a wide range of chloride concentrations, it may be necessary to apply several voltages to obtain current readings within the limit of the apparatus current level display (0 mA to 10 mA). Higher voltages are applied for low concentrations and lower voltages are applied for high concentrations.
11. Proced Procedure ure 11.1 To a dry 11.1 dry,, 100 mL graduated, graduated, glassglass-stopp stoppered ered cylinder, cylinder, add ad d 15 mL of xy xylen lenee an and, d, us usin ing g th thee sam samee ty type pe of vo volu lume me transferring device used in 10.3 10.3 (that is, either a 10 mL pipet (total delive delivery ry,, see 6.3 6.3)), or 10 mL gra gradua duated ted cyl cylind inder er (se (seee 6.3.1)) when applicable), transfer 10 mL of the crude oil sample 6.3.1 into the 100 mL graduated, glass-stoppered cylinder. Rinse the 10 mL pipet or 10 mL gradu graduated ated cylinder cylinder with xylene xylene until free of oil. Make up to 50 mL with xylene. Stopper and shake the cylinder vigorously for approximately 60 s. Dilute to 100 mL with wit h mix mixed ed alco alcohol hol sol solven vent, t, and aga again in sha shake ke vig vigoro orousl usly y for approx app roximat imately ely 30 s. Aft After er allo allowin wing g the sol solutio ution n to sta stand nd for approximately 5 min, pour it into the dry test beaker. 11.2 11 .2 Fol Follow low the pro proced cedure ure in 10.4 to obt obtain ain vol voltage tage and current readings. Record the indicated electrode current to the nearest 0.01 mA and the nearest voltage (see Note 6) 6). 11.3 Remove the electrodes 11.3 electrodes from the sample solution, solution, and clean the apparatus. 12. Calc Calculat ulation ion 12.1 Subtr Subtract act the value obtained for the blank measurement measurement from the value obtained from the specimen measurement to obtain the net current reading. From the calibration graph, read thee in th indi dicat cated ed sa salt lt co conc ncen entr trati ation on co corr rres espo pond ndin ing g to th thee ne nett 6). current (mA) reading of the sample (see Note 6). 12.2 12. 2 Calc Calcula ulate te the con concen centra tration tion in mg/ mg/kg kg by usi using ng the appropriate equation given below: Salt, mg/kg 5
1000 X d
Salt, mg/kg 5 2853 Y / d --`,,,`,,``````,```,,,``-`-``,```,,,`---
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(1 )
(2 )
D3230 − 19 where: measured ed salt salt concentrat concentration ion in g/m3, X = measur measured ed salt salt concentrat concentration ion in PTB, and and Y = measur 3 d = spe specime cimen n density density at at 15 C in kg/m kg/m .
Y = the avera average ge of two test test result resultss in lb/1000 lb/1000 bbl bbl (PTB). (PTB).
NOTE 9—The density of the specimen can be determined by various methods, method s, suc such h as Test Met Method hod D5002 or other density measu measuremen rementt methods.
14.1.2 Reproducibility— The The difference between two single and independent results, obtained by different operators working in different laboratories on identical material, would in the long lo ng ru run, n, ex excee ceed d th thee fo foll llow owin ing g va valu lues es in on only ly on onee cas casee in twenty.
13. Repor Reportt 13.1 Report the following information: The concentration concentration in mg/kg as electrometric chloride in crude oil per Test Method D3230. Alternately, report report the concentration directly in g/m3 or lb/1000 bbl, if so required. NOTE 10—F 10—For or rep report orting ing pur purpos poses, es, the val values ues sta stated ted in PTB are the preferred units in the United States; in other countries, their common units can be used.
14. Pre Precisi cision on and Bias4 14.1 Precision— The The precision of this test method as determined by the statistical examination of the 1997 interlaboratory test results is as follows: 14.1.1 Repeatability— The The dif differ ferenc encee betw between een suc succes cessiv sivee results,, obtain results obtained ed by the same opera operator tor with the same appar apparatus atus under constant operating conditions on identical test material, would in the long run, in the normal and correct operation of the test method, exceed the following values in one case in twenty. ` , , , ` , , ` ` ` ` ` ` , ` ` ` , , , ` ` ` ` ` , ` ` ` , , , ` -
r ~ ~ mg/kg! 5 0.3401 X 0.75
(3 )
r ~ ~ lb/1000 bbl! 5 0.2531 Y 0.75
(4 )
where: X = the avera average ge of two two test test results results in mg/k mg/kg, g, and and
R ~ mg/kg! 5 2.7803 X 0.75
(5 )
R ~ lb/1000 bbl! 5 2.069 Y 0.75
(6 )
where: X = the avera average ge of two te test st result resultss in mg/k mg/kg, g, and Y = the avera average ge of two test test resu results lts in lb/1000 lb/1000 bb bbll (PTB). (PTB). NOTE 11—Since all instruments in the 1997 interlaboratory cooperative test program were calibrated in PTB and results reported in PTB, the precision statement was directly obtained in PTB. The resulting precision dataa hav dat havee bee been n mat mathem hemati aticall cally y con conver verted ted int into o pre precis cision ion in mg/ mg/kg, kg, assuming an average density of the crude oil samples of 0.875 kg ⁄L.
14.2 Bias— The The procedure procedure in Test Method D3230 D3230 has no bias bi as sin since ce sa salt lt co cont nten entt is de defin fined ed on only ly in ter terms ms of th this is tes testt method meth od and cert certified ified ref referen erence ce mate materia rials ls are una unavai vailabl lable. e. Howeve How everr, sin since ce the sam sample pless fro from m the int interl erlabo aborat ratory ory stu study dy were neat desalted crudes, spiked with known quantities of salt (as sea water and formation water), bias might be defined as percent recovery of halide added. Over the range from 5 g ⁄m3 3
to 500 gto⁄m (1.5 (1. 5 PTB PTB to 150 PTB)) salt PTB added, add ed, the93rec recove ry proved be approximately constant and averaged %.overy 14.3 14. 3 The precision precision statements statements were der derive ived d fro from m a 199 1997 7 interlaboratory cooperative test program. Participants analyzed eight sample sets comprised of crude oils with various concentrations of chlorides. Thirteen laboratories participated with the commercial available apparatus. See 6.3 and 6.3.1 for additional information about the precision statements. 15. Keyw Keywords ords
4
Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1470. Contact ASTM Customer Service at
[email protected].
15.1 chlor chlorides; ides; crude oil; electrometric; electrometric; halide halides; s; petroleum; salt in crude
ANNEX (Mandatory Information) A1. APPARA APPARATUS TUS
A1.1 Electro Electrometr metric ic Chlo Chloride ride Apparatus Apparatus (Cust (Custom om Manufacture) (see (see Fig. Fig. A1.1 a and nd Note Note A1.1) A1.1) A1.1.1 Milliammeter, 0 mA to 1 mA dc with 0 mA to 1 mA ac scale, 88 Ω internal resistance. A1.1.2 Bridge Bridge Rectifie Rectifierr, full-wav full-wave, e, 0.7 0.75 5 A cap capacit acity y at 60 Hz, amb ambien ientt temp tempera eratur ture; e; min minimu imum m of 400 PR PRV V (Pe (Peak ak Reverse Voltage). A1.1.3 AC Voltmeter, rectifier type, 2000 range.
Ω
A1.1.5 Transformer, plate supply 240 V, center tap, 50/60 Hz, 250 mA dc capacity. A1.1.6 Potentiometer, 25 Ω, ten turn. A1.1.7 Potentiometer, 50 ohm, ten turn. NOTE A1.1— A1.1—An An equ equiva ivalen lentt par partt can be sub substi stitut tuted ed in each cas case, e, provided the electri provided electrical cal characteristics characteristics of the entire circui circuitt remai remain n unchanged and the inductive effects and stray currents are avoided.
⁄V,, 0 V to 300 V ⁄V
A1.2 T est A1.2) Cell) Comp Component onentss (Cust (Custom om Manuf Manufactu acture) re) (see Fig. A1.2
A1.1.4 Variable Variable Voltage Autotransformer Autotransformer,, input input 10 105 5 V to 117 V, 50/60 Hz, output 0 V to 132 V, 1.75 A capacity.
A1.2.1 Beaker, 100 mL tall form without lip, as described for use in Test Method D381. D381.
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D3230 − 19 in Fig. A1.2 and A1.2 and Fig. A1.2.2 Electrode Assembly, as shown in Fig. A1.3. The elec A1.3. electro trodes des mou mounte nted d in par paralle allell pos positio ition, n, exa exactly ctly opposed and 6.4 mm 6 0.1 mm apart, and electrically separated by a nylon or TFE-fluorocarbon spacer.
A1.4 Test Cell Components (Commercial Manufacture) Manufacture)
A1.3 Electr Electrome ometri tricc Chlo Chlorid ridee Appa Apparat ratus us (Com (Commer mercia ciall 4 Manufacture)
A1.4.1 Beaker, 100 mL tall form without lip, as described for use in Test Method D381, D381, is commo commonly nly used; however, however, minor variations on dimensions are acceptable to accommodate differ dif ferent ent man manufa ufactu cturin ring g spe specifi cifics. cs. The bea beaker ker pur purpos posee is to provide for containment of the specimen.
A1.3.1 A1.3. 1 The apparatus apparatus shall consist of a contro controll unit capable of producing and displaying several voltage levels for applying
A1.4.2 Electrode Assembly, shown by example in Fig. in Fig. A1.2 and Fig. A1.3. A1.3. The electrode assembly dimensional require-
st stre ress ss to aa se set t of elec el ectr trod odes es apparatus susp su spen ende ded dshall in abete test st be beak aker er containing test solution. The capable of measuring and displaying the current (mA) conducted through the test solution between the electrodes at each voltage level (see Note (see Note 6). 6).
ments and means of support in the beaker are not critical to the applica app licatio tion n as lon long g as each ind indivi ividua duall com compon ponent ent rem remain ainss specific to the given manufactured apparatus.
NOTE A1.2—S A1.2—Some ome app appara aratus tus is cap capabl ablee of mea measur suring ing vol voltag tagee and current intern current internally ally and after comparison comparison to intern internal al calibr calibration ation curves, display the resultant concentration.
A1.3.2 A1.3. 2 The actual constr construction uction specifics specifics of the appar apparatus, atus, such as voltages utilized and means of displaying or recording the voltage, displa displaying ying or recor recording ding the curren currentt condu conduction, ction, or calcula calc ulatin ting g and dis displa playin ying g the cali calibra bratio tion n cur curves ves/sp /specim ecimen en measurements, or combination thereof, are not critical to the applica app licatio tion n as lon long g as eac each h ind individ ividual ual com compon ponent ent rem remain ainss specific to the given manufactured apparatus (see Note 6). 6).
FIG. A1.1 250 Volt or 540 Volt Transformer
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D3230 − 19
FIG. A1.2 Test Cell ` , , , ` ` ` , ` ` ` ` ` , , , ` ` ` , ` ` ` ` ` ` , , ` , , , ` -
FIG. A1.3 Electrode Assembly
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D3230 − 19
SUMMARY OF CHANGES Subcommittee D02.03 has identified the location of selected changes to this standard since the last issue (D3230 – 13 (2018)) that may impact the use of this standard. (Approved May 1, 2019.) (1) Revised subsection subsection 1.1 1.1.. 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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