Standard Method of Test for Sampling and Testing for Chloride lon in Concrete and Concrete Raw Materials aa oD AASHTO Designation: T 260-97 (2009) ¥ ae g 1. SCOPE 14 This method covers procedures for the determination of the acid-soluble chloride ion content or the water-soluble chloride ion content of ageregates, portland cement, mortar or concrete 1.2, ‘The total amount of chloride is usually equal to the acid-soluble chloride. However, organic additives or minerals that contain acid-insoluble chloride may be present in concrete and concrete raw materials. These constituents may become acid soluble during long-term exposure to the alkaline environment in concrete or mortar. 1.3. ‘The age of concrete mortar, or hydrated portland cement atthe time of sampling will have an affect on the water-soluble chloride ion content. Therefore, unless early age studies are desired, itis recommended that the material be well cured and at least 28 days of age before sampling. 14. This standard provides for the determination of chloride ion content by two procedures: Procedure A, Determination of Acid-Soluble Chloride fon Content and Water-Soluble Chloride Ton Content by Potentiometric Titration or Ton-Selective Electrode (Laboratory Test Method); and Procedure B, Acid-Soluble Chloride lon by Atomic Absorption (Laboratory Test Method). 15. Sulfides are known to interfere with the determination of chloride content. Blast-furnace slag aggregates and cements contain sulfide sulfur in concentrations that can cause such interference, ‘which can be eliminated by treatment as noted in the test procedures. Other materials that produce strong odor of HS when acid is acided to them should be similarly treated. 16. ‘The values stated in ST units are to be regarded as the preferred standard, PROCEDURE A—ACID-SOLUBLE CHLORIDE ION AND WATER- SOLUBLE CHLORIDE ION BY POTENTIOMETRIC TITRATION OR ION SELECTIVE ELECTRODE (LABORATORY TEST METHOD) 2. APPARATUS 24 ‘Sampling equipment for Procedures A and B are listed in Sections 2.4.1 or 2.1.2. 244 ‘Core drill 212 Rotary impact-type drill with a depth indicator and drill or pulverizing bits of sufficient diameter to provide a representative sample of sufficient size for testing. TS-30 T 260-41 ‘AASHTO 1 2010 by the American Assoeiation of State Highway and Transportation Officials. All rights reserved. Duplication isa violation of applicable law.2424 ‘Sample containers capable of maintaining the sample in an uncontaminated state. 2122 Spoons of adequate size to collect the sample from the drilled holes. 2123. A “blow out” bulb or other suitable means of removing excess pulverized material from the hole prior to re-drilling operations. 2124 ‘A device capable of determining the location and depth of steel reinforcement to #3 mm (#'/ in). 22. Equipment for Chemical Testing 224 Chloride ion or silver/sulfide ion selective electrode and manufacturer-recommencled filling solutions. Note 1—Suggested electrodes are the Orion 96-17 Combination Chloride Electrode or the Orion 94-6 Silver/Sulfide Electrode or equivalents. The Silver/Sulfide Electrode requires use of an appropriate reference electrode (Orion 90-02 or equivalent) 222 A millivolimeter compatible with the ion electrode. Note 2—Suggested millivaltmeter is the Orion Model 701 A Digital ph/mV meter or equivalent. 223. ‘Magnetic stirer and Teflon stirring bars. 224 ‘Burette with 0.l-mL graduations. 225. Balance complying with M231, Class A. 226. ‘Balance complying with M231, Class G 2. 227. Hot plate, 250 to 400°C heating surface temperature. 228. Glassware, 100 and 250-mL beakers, filter funnels, stirring rods, watch glasses, dropper, wash bottles. 229. Sieve, U.S. Standard 300 um (No. 50). 2.2.40. ‘Whatman No. 40 and No. 41 filter papers (or equivalent) Note 3—If equivalent filter papers are used, they should be checked to confirm they do not contain chloride, which will contaminate the sample. 3. REAGENTS 31 Concentrated HINOs (sp gr 1.42). 32 Sodium chloride, NaCl, reagent grade (primary standard) 33. Standard 0.01 normality NaCI solution. Dry reagent grade NaCl in an oven at 105°C. Cool, in a desiccator, determine the mass of approximately 0.5844 g to the nearest 0,001 g. dissolve in TS-3c T 260-2 ‘AASHTO 12010 by the American Assoclation of State Highway and Transportation Officials, llrightsreserved. Duplication sa wiolation of applicable law.a4, 36. 36. a7. 38. distilled HO, and transfer to a 1-L volumetric flask. Make up to the mark wil and mix. Calculate the exact normality as follows: Wess) 05844 distilled HO Nuucr = (020100) o where: Went = actual mass of NaCl, and Newt = normality of NaCl solution. Standard 0.01 normality AgNO. Determine the mass of 1.7 grams of reagent AgNO; dissolve in lled H,0, filter into a 1-L brown glass bottle fill, and mix thoroughly. Standardize against 25.00 mL. of the NaC solution by the titration method given in Section 5.4. Calculate the exact normality as follows: (cs (Nie) Vagwo, Napoy (ca) where: Nagno, = normality of AgNO: solution, Vasc = volume (mL) of NaCl solution, Nyse = normality of NaCI solution, and Vago, = volume (mL) of AgNO, solution. Distilled Water. Note 4—Deionized water may be used in place of distilled water for samples where extreme precision and accuracy are not demanded. Methyl orange indicator. Ethanol, denatured, or methanol, technical Hydrogen Peroxide (30 percent), 44 44a 412, 4424 METHOD OF SAMPLING Concrete Sample: Determine the depth within the conerete for which the chloride content is desired. Note 5—A convenient method of determining the location and depth of reinforcement bars is a pachometer capable of determining the location and depth of steel reinforcement to 43 mm (0.125 in), Core Method-—Drill the core to chosen depth and retrieve. ‘When samples are received in the laboratory in other than pulverized condition, the sample shall be crushed and ground to a powder. All sawing or crushing shall be done dry’ (‘e., without water) All material shall pass a 0.300-mm (No. 50) sieve. All pulverizing tools and sieves shall be washed with alcohol or distilled water and shall be dry before use with each separate sample. (See note following Section 4.1.3.7.) TS-3¢ 280-3 AASHTO 122010 by the American Association of Stato Highway and Transporation Officials, Allright eserved. Duplication is violation of applicblc law443. 413.4 4132. 413.8. 443.4. 4135. 4136. 441.37. 42. 424. 42.2. Pulverizing Method: Set the rotary hammer depth indicator so that it will drill to 13 mm (0.5 in.) above the desired deptin Using a drill or pulverizing bit, drill until the depth indicator seats itself on the concrete surface. Thoroughly clean the drilled hole and surrounding area. suitable means. izing the “blow out” bulb or other Reset the depth indicator to permit 13 mm (0.5 in.) additional drilling. Pulverize the concrete until the depth indicator again seats itself on the concrete. Note 6—Care must be exercised during this pulverizing operation to prevent the drill bit from abrading concrete from the sides of the hole above the sampling depth. To insure against this, some users utilize a 6-mm (0.25-in.) smaller diameter bit in this step than that used in Section 4.1.3.2. Collect at least 10 g of the material remaining in the hole using a spoon and place in the sample container. Ifthe sample, as collected, does not completely pass a 0.300-mm (No. 50) sieve, additional pulverizing shall be performed in the laboratory until the entire sample is finer ‘than 0.300-mm (No. 50). Note 7—During sample collection and pulverizing, personnel shall use caution to prevent contact of the sample with hands, or other sourees of body perspiration or contamination. Further, all sampling tools (dri bits, spoons, bottles, sieves, etc.) shall be washed with alcohol or distilled water and shall be dry prior to-use on each separate sample. Alcohol is normally preferred for washing because of the rapid drying, which naturally occurs. Raw Material Sample: Cement samples shall be taken and prepared as prescribed in T 127, Sampling and Amount of Testing Hydraulic Cement. Coarse and fine aggregate samples shall be taken as prescribed in T 2, Sampling of Aggregates. Samples shall be reduced in accordance with T 248, Reducing Samples of Aggregates to Testing Size. TS-20 T 260-4 AASHTO. 1B 2010}y the American Association of State Highway and Transportation Officials, Allright reserved. Duplication is violation of applicable4.23. 424. Test samples shall contain the following minimum sizes: Mm coment—100 g. m sand—300 g, coarse aggregate—3000 g. Coarse aggregate samples shall be crushed to pass a 4.75-mm (No. 4) sieve and then reduced down to about 300 g. The final 300 g of coarse or fine aggregate shall be ground to a minus 0.300-mm (No. 50) sieve. 54 5.2. 5.241. PROCEDURE ‘Two distinct procedures are presented here for determination of acid-soluble chloride ion or water-soluble chloride ion content. For acid-soluble chloride ion content follow Sections 5.1 and 5.2, then continue with Section 5.4. For water-soluble chloride ion content follow Sections 5.1 and 5.3, then continue with Section 5.4. Determine the mass to the nearest milligram of a 3-g powdered sample representative of the ‘material under tests. Note 8—Some users dry the sample to constant mass ina 105°C oven and determine the dry sample prior to analysis. This optional procedure provides a constant base for comparison of all results by eliminating moisture content as a variable. Itis generally believed that drying is only necessary when very high accuracy is desired. (See Reference 1 for data in this area.) Procedure for Acid-Soluble Chloride Ton Content: Transfer the sample quantitatively to a beaker; add 10 mL of distilled HO, swirling to bring the powder into suspension. Add 3 mL of concentrated HNO; with continued swirling until the ‘material is completely decomposed. Break up any lumps with a stirring rod and dilute with hot H,0 to 50 mL. Stir thoroughly to ensure complete sample digestion If the sample contains blast-furnace slag or other sulfide-bearing material, add 3 mL. of hydrogen peroxide (30 percent solution). Add five drops of methyl orange indicator and stir, If yellow to yellow-orange color appears, solution is not sufficiently acidic. Add additional concentrated HINO; dropwise with continuous stirring until a faint pink or red color persists in the solution. Cover with a watch glass, retaining the stirring rod in the beaker. Heat the acid solution or slurry to boiling on a hot plate at medium heat (250 to 400°C) and boil for about 1 minute. Remove from the hat plate, filter through double filter paper (Whatman No. 41 over No. 40 filter paper or equivalent) ‘Wash the filter paper 10 times with hot distilled HO, being careful not to lift the paper away from the funnel surface. Finally, lft the filter paper carefully from the funnel and wash the outside surface of the paper with hot distilled H,O: then wash the tip of the funnel. The final volume of the filtered solution should be 125 to 150 mL. Cover with a watch glass and allow to cool to room ‘temperature in an HCI fume-free atmosphere. Note 9—Due to the presence of relatively insoluble materials in the sample, the solution generally will have a strong gray color, making the detection of indicator color difficult at times. Rumning of several trial samples is suggested to give the analyst practice in detecting the indicator color. Note 10—A sample prepared to 100 percent passing 0.300-mm (No. 50) sieve should generally allow determination of any expected chloride level with adequate precision and accuracy. Samples containing highly siliceous aggregates may require finer grinding to minimize bumping during the TS-30 T 260-5 ‘AASHTO ©2010 by the American Association of State Highway and Transportation Official. All rights reserved. Duplication is violation of applicable law.5.3. 5.34 5.3.2. 54. 544 ‘procedure in Section 5.2. This may also be the case when the conerete contains modifiers such as latex or polymer. Procedure for Water-Soluble Chloride fon Consent: ‘Transfer the sample quantitatively to a beaker, add 60-70 mL. distilled HO. Cover the beaker with a watch glass and bring to a boil on a hot plate-magnetic stirrer using a small magnet. Boil for 5 minutes, then let stand for 24 hours in an FICI fume-free atmosphere. Filter the clear supernatant liquid in the beaker through double filter paper (Whatman No. 41 over ‘No. 40 or equivalent) into a 250-mL beaker; take care to quantitatively transfer any adhering drops on the watch glass, and use a stirring rod to aid transfer. Add sufficient hot distilled HO to cover any residue left in the original beaker, stir 1 minute on a magnetic stirrer, and filter into the: 280-mL beaker with a swirling action. Wash the beaker and the stirring rod once into the filter with hot distilled HO. Wash the filter paper once with hot distilled HO. Lift the filter paper carefully from the funnel and wash the outside surface of the paper with hot distilled HO. Set aside the paper and wash the interior of the funnel and its tip with hot distilled HzO. Finally, add 1-2 drops of methyl orange indicator to the 150-ml beaker: then add concentrated HNO dropwise with continuous stirring until a permanent pink to red color és obtained. If the sample contains blast-furnace slag or other sulfide-bearing material, add 3 mL. of hydrogen peroxide (30- percent solution). Make up the volume to 125 to 150 mL with distilled HO. “Three alternate methods are available to determine the CI” content of the solution. All methods utilize an ion selective electrode (Clr or Ag’) and all methods for the purpose of this analysis give results of essentially equal accuracy and precision. Method 1: Potentiometric Titration—Fill the Cl’ or the Ag* electrode with the solution(s) recommended by the manufacturer, plug it into the millivoltmeter (preferably the type with a digital rather than a dial readout), and determine the approximate equivalence point by immersing the electrode in a beaker of distilled F,0. Note the approximate millivoltmeter reading (which may be unsteady in HO). Take the cooled sample beaker from Section 5.3 and carefully add 4.00 mL. of 0.0100 normality NaCl, swirling constantly. Remove the beaker of distilled HO from the electrode, wipe the electrode with absorbent paper, and immerse the electrode in the sample solution. Place the entire beaker-electrode assembly on a magnetic stirrer and hegin gentle stirring. Using a calibrated buret, add gradually and record the amount of standard 0,01 normality AgNOs solution necessary to bring the millivoltmeter reading to 40 mV of the equivalence point determined in distilled H2@. Then add standard 0.01 normality AgNO; solution in 0.10 mL- increments recording the millivoltmeter reading after each addition. ‘As the equivalence point is approached, the equal additions of AgNOs solution will cause larger and larger changes in the millivolimeter reading. Past the equivalence point, the changes per unit volume will again decrease. Continue the titration until the millivoltmeter reading is at least 40 mV past the approximate equivalence point. The endpoint of the titration usually is near the approximate equivalence point in distilled water and may be determined by (1) plotting the volume of AgNO; solution added versus the millivoltmeter readings. The endpoint will correspond to the point of inflection of the resultant smooth curve, or (2) calculating the differences in millivoltmeter readings between successive AgNO; additions and caleulating the total volume of AgNO; that corresponds with each difference (ie., the midpoints between successive additions) TS-30 T 260-6 AASHTO 12.2010 by the American Association of State Highway and Transportation Officials, All rights reerved. Duplication is violation of applicable law.Raw Data Titrant Volume 42 mL 43m 4a mL 4S mL 64414 5.4.2, Millivolt Titrant —_Millivolt Reading Midpoints Difference 1300 4.25 mt, 50 1350 4.35 mt, 70 42.0 4.45 mL, oo 1520 ot. ‘The endpoint will be near the midpoint, which produced the largest change in millivoltmeter reading, It may be determined by plotting midpoints versus differences and defining the AgNO; volume, which corresponds to the maximum difference on a smooth, symmetrical curve drawn ‘through the points. However, it can usually be estimated accurately without plotting the curve by choosing the midpoint, which corresponds to the maximum difference and adjusting for asymmetry, if any. In other words, if the differences on each side of the largest difference are not symmetrical, adjust the endpoint mathematically in the direction of the largest differences, Detailed examples of this adjustment are contained in Reference 1. Caleulations: Determine the endpoint of the titration as described in Secti estimating from the numerical data. Calculate the percent CT (35453 (4N,-¥%) Cr percent = 0 3) 5.4.1 by either plotting a curve or mn from the equation: where: V, = endpoint in mLof AgNO: M, = normality of AgNO; W = mass of original concrete sample in grams; Vs = volume of NaC! solution added, in mL; and N= “normality of NaC! solution: ‘Method If: Gran Plot Methad—This method is compatible with either a Cor Ag* ion selective electrode. Attach the electrode of choice to a compatible digital millivoltmeter after filling the required solutions as per the electrode manufacturer's instructions. Clean the electrode with distilled HO and pat dry with absorbent paper. Determine the mass of the solution and beaker from Section 5.3 without the watch glass and record the mass. Using a calibrated buret, titrate the sample to 225 + 5 mV (CI electrode) or 3105 mY (Ag" electrode) with standard 0.01 normality AgNO} solution. Record the volume added and the millivolimeter reading. Continue to titrate in 0.50-mL. increments recording the volume added and the millivoltmeter reading for each increment, Add and record the data for at least five increments. Empty, clean, dry, and determine the mass of the beaker. Subtract beaker mass from beaker + solution mass determined above to define solution mass. Example shown in Figure 1. Additional information on the Gran Method is given in Reference 2. TS-30 T 260-7 AASHTO 122010 by the American Association of State Highvray and Transportation Oficial. All rights teenved. Duplication is «violation of applicse la,5 330 325 320 Elecvooe Potential, mv a3 310 308 300 295 lEndooint = 3.48 £0.02 mL] 3 4 5 8 T é mL ot AgNG, Salutian Figure 1—Use of Gran Method to Determine Endpoint in the Potentiometric Titration of an Acid Extract of Concrete 5421 Gran Method Calculations: Calculate corrected values for each of the volumes recorded in Section 5.4.2 by the equation: Veeco Veet = 4 et Gf t0b “@ Ww original solution mass in g, and ‘volumes recorded in mL. Tfany of the V correct values are greater than 10, see Section 5.42.2. If less than 10, plot these corrected values versus the: corresponding millivolt readings on Orion Gran Plot Paper (10 percent ‘volume corrected type with each major vertical scale division equal to five raillivolts) or ‘equivalent. Draw the best straight line through the points and read the endpoint at the intersection of the line with the horizontal axis of the graph. Calculate the actual endpoint by the equation: w 5) E, Actual Endpoint = E, (ms) 3) where: E, = endpoint determined from graph in mL, and W = mass of solution in g TS-30 T 260-8 ‘AASHTO 12.2010 by the American Association of State Highway and Transportation Offical llrightsreserved. Duplication is violation of applicable(6) E, = actual endpoint in mL, N= normality of AgNOs solution, and We = conerete sample mass in g. 5422 Suppiemensary Gran Method Calculations: When the V correct volumes determined in Section 5.4.2.1 are greater than 19, discard the values and follow the following procedure. Choose a constant which, when subtracted from all V record volumes, yields values less than 10m. Note 11—This constant, designated as X in the formulas below, is normally assigned an even value such as 5, 10, 15, 20, etc. Calculate a revised solution mass (Wi) as: W,=W+X a) where: W = original solution in g, and X= the constant, Then calculate corrected volumes for each recorded volume as: Vosnag tent =X (6) W,/100 Plot these values and determine the graph endpoint E, as described in Seetion 5.4.2.1. The actual endpoint (E,) is then z= {™)+x (9 «(i900 where: E, = actual endpoint in mL, E, = endpoint from graph in mL, W, = revised solution mass in g, and X= theconstant chosen above. Calculate the chloride content using the formula given in Section 5.4.2.1 543. Method If: Automatic Titrator—This method is compatible with either a CI-or Ag* ion-selective ‘electrode. The millivalt endpoint determination and testing procedure shall be in accordance with ‘the instrument manufacturer’s recommendation. 5434 Automatic Titrator Caleulations: ‘Having determined the endpoint with the automatic ttrator, calculations will be identical with Section 5.4.1.1 55. ‘The percent chloride may be converted to kg of Cl/m’ (Ib/yd") of concrete as follows: uw) kg Cl/m® = Percent Cif | 10) cg CI) if 00 J (70) TS-3e T 260-9 ‘AASHTO {2010 by the American Association of Stat Highway and Transportation Official All rights escrved. Duplication isa violation of applicable law.a UW Ib Cr, = Pe it Cl |—_ aL [ya = Percen (& ] ) where: UW = unitmass of concrete per cubic meter (cubie yard). Note 12—A unit mass of 2323 kg/m’ (3915 Ib/yd") is often assumed for normal structural mass concrete when the actual unit mass is unknown. 6. PRECISION 61. ‘The precision statements presented below are based on guidelines presented in ASTM C 670, Preparing Precision Statements for Test Methods for Construction Materials. They are, of necessity slightly different since the within-laboratory standard deviation was essentially constant over the chloride levels examined while the between-laboratory precision varied with chloride level. Both statements, however, are based on the difference two-sigma limit, (42s). The (42s) index is the difference between two individual test results that would be equaled or exceeded in the long run in only 1 ease in 20 in the normal and correct operation of the chemical analysis. 62. Single-Operator—The single-operator standard deviation has been found to be 0.0024 percent chloride.’ Therefore, results of two properly conducted tests by the same operator on the same ‘material should not differ by more than 0,0068-percent chloride.! 63. Multilaboratory Precision—Criteria for judging the acceptability of chloride ion concentration test results obtained by different laboratories by this test method are given in Table | Table 1—Multilaboratory Precision Percent Chloride ‘Acceptable Concentration Standard Range of Two Multilaboratory Precision Deviation® Results” ‘0.0176 0.0030" ‘0.0085 0.0268 0.0031 0.0088 0313 0.0032: ‘0.0091 0.05%, ‘0037 e010 0.1339 ‘00s 0.0136, 0.2618 10069. 0195 7 Ries asic pent egal ed) ns dno SHG, Racin ac or Ppang PS ‘oe The gues given in Crm. 2 athe arnt devine tht hay hen four tobe agpopineFor Ue horde tom cena deere in Cau 1. The igre ven in Colum 3 ete His tha shoul ate exceeded by thedferencehatvaee ti eal cf to papely corde. PROCEDURE B—ACID-SOLUBLE CHLORIDE ION BY ATOMIC ABSORPTION (LABORATORY TEST METHOD) 7. APPARATUS: 74 See Section 2.1 for sampling equipment. 72 Equipment for Chemical Testing: 724 Atomic Absorption Spectrophotometer. TS-30 T 260-10 AASHTO 2010 by the American Association of State Highway and Transportation Oticials Alrights reserved. Duplication is violation of applicable law.Note 13—The text of this method is most applicable to the use of a Perkin Elmer ‘Model 503 A.A., with a 50-mm (2-in.) path length burner and digital readout. Laboratories using {instruments other than Perkin Elmer should utilize the method to the fullest extent possible. 722 Millipore filter assembly No. XX 1104710 (47 mm in diameter), or equivalent. Millipore filter ‘membrane No. HAWPO4700 (0.45-wm membrane), or equivalent. Note 14—If equivalent filter membranes are used, they should be checked to confirm they do not contain chloride, which will contaminate the sample, 723, 100-mL. volumetric flasks with glass stoppers (clear glass) 724 100-mL. volumetric flasks (low actinic with glass stoppers) 725, Pipettes of suitable sizes, which meet or exceed the tolerances specified in NBS circular 602 for Class A Volumetricware. 726 “Analytical balance sensitive to 0,0001 g complying with M231, Class A. 727, Fisher filtrator (vacuum) with either a glass or plastic bell jar, tall enough to place a 100-mL. ‘volumetric flask underneath. 728, Hot plates (electric). 729 ‘Vacuum source. 7210 ‘Vinyl tubing 8. REAGENTS 84 Calcium carbonate, reagent grade. 82 Hydrogen peroxide (30 percent), 83. Methy/ orange. 84. Nitric acid, concentrated (sp gr 1.42). 85. Silver nitrate, reagent grade (primary standard). 86. Sodium chloride, reagent grade (primary standard). a7. Sodium nitrate, reagent grade. a8. Water, distilled TS-3¢ T 260-11 ‘AASHTO 19 2010 by the American Association of State Highway and Transpo Allright reserved. Duplication is violation of ppliabl9. METHOD OF SAMPLING oa. See Section 4 for method of sampling. 10. STANDARDIZATION 10.4 Dry a sufficient quantity of standard materials (AgNO, NaCl, CaCO, and NaNO;) at 105°C to constant mass. Cool and retain in a desiccator. 10.1.1 Determine the mass of a sufficient sample of each of the above standards to effect the Following, solutions m Ag’, 100 mg/L, m Cl; 100 mg/L, Na’, 100 mg/L, and m Ca", 500 mg/L. 10.2. Add 10 mL of 1 +9 HINO; to each of eight 100-mL. low actinie volumetric flasks. Aliquot sufficient chloride solution so that each flask will contain a chloride ion concentration of 0.0, 0.1, 0.25, 0.50, 0.75, 1.0, 2.0, and 3.0 mg/L, respectively. The 0.0 concentration will be the 1-mg/L, silver standard, 10.3. Proceed with the eight volumetric flasks following Sections 11.7.1 through 11.7.3 10.4. Set the operating parameters for A.A. in accordance with the manufacturer's procedures when using a silver lamp. 10.5. Aspirate the 10 mg/L Ag* standard with a zero chloride ion concentration, and set 10 mg/L in the readout window. 10.6. Aspirate the remaining seyen volumetries containing 0.1 through 3.0 mg/L chloride ion concentrations, and note the reaclings: Repeat this procedure at least three times on 3 different days to obtain an average reading. Develop the standardization data by aspirating randomly. 10.7. Prepare a curve on linear graph paper, plotting remaining Ag" ions determined by A.A. against the seven chloride standards. (See Figure 2a.) TS-3¢ T 260-12, AASHTO. 122010 by the American Association of State Highway and Transportation Officials. llrightsreserved. Duplication is violation of applicable law.80 10. 80 50 mgiL (Ag*) 49 30 20 10 0.0 Q Method B ‘Agt Concentration vs oF Gancanvation 10 20 30 mgt (") Figure 2a—Method B 11. PROCEDURE 14 ‘The sample as received shall be made to pass a 300-um (No. 50) sieve, after removing any free fron that may have been introduced in sample preparation: If received sample is excessively large, ‘quartering may be necessary before grinding. 11.2 Dry sample at 105°C to constant mass and cool in desiccator. 11.3 Determine the mass to the nearest mg of a one (I) g powdered sample representative of the ‘material under test. Transfer to a 150-ml beaker, and add 10 mL. of dilute nitric acid (1 +9) to dissolve as much of the sample as possible. Break up any lumps with a stirring rod, 11.4 Tf carbonates are present, let sample stand until all effervescence is completed, 11.5 Tf the solution is not acid at this point, add only enough nitric acid to produce a red color: methyl orange. 11.6. ‘Heat the slurry on a hot plate to just under boiling, and digest for 5 minutes or until all reaction ceases. Remove from hot plate and cool. Vacuum filter (Fisher filtrator or equivalent through 0.45-ym membrane (Millipore filter assembly No. XX1104710, Millipore filter membrane ‘No. HAWP04700, or equivalents) into a 100-mL volumetric flask. (See Figure: 2.) Wash the precipitate with three or four small portions of distilled water. Dilute to volume. TS-3c T 260-13 ‘AASHTO 1.2010 by the American Association of State Highway and Transportation Official, All rights reserved. Duplication is «violation of applicable la.Extension Tube Velumetre Flask 100 (mL) |_____“miipore” Funnel (Threaces) Filter Paper ‘Support (Threaded) Vecuur Tight Fit of Fiter ny Support te Botte ‘Tube of Sutficiont Length to Enter Nouth of Volumevic Flask: Vacuum Bote Rubber Cushioned Vecuum Plate n Vacuum Hole To Vecuum Source = Veeuum Central —__ Figure 2b—Schematic Sketch of Filtration Apparatus, Method B 117. 117.4 11.7.2. 14.7.3. 117.4. 12. Aliquot 10 mL of the filtered sample solution into a 100-mL. volumetric flask (low actinic). Save ‘balance of the sample; other dilutions may be needed if concentration is relatively high. Add 1.5-mL hydrogen peroxide and agitate for 1 minute. Add 10 miL of the 100 mg/L silver nitrate solution. Agitate the flask once again and let stand for 1 hour, ‘Vacuum filter, using above Millipore or equivalent equipment, into a 100-mL volumetric flask (low actinic) containing 5 mL. of the sodium solution and 1 mL. of the calcium solution. Wash the precipitate with three or four small portions of distilled water. Dilute to volume. This filtrate contains the unreacted silver ions from the silver chloride precipitation that are found by standard atomic absorption procedures for silver, including measurements of suitable standards during the determinations. Enter the curve (Figure 1) with Ag’ remaining, and determine the chloride concentration (mg/L). CALCULATION Calculate the percentage of chloride in the concrete or concrete raw material, as indicated below: _{1)(me/L er) Percent Cl -(f) (=a) (12) where: V_ = volume of aliquot used in Section 11.7, in mL; and W_ = massof original concrete sample, in g. This equation assumes that the aliquot is diluted to 100 mL. TS-3¢ T 260-14 ‘AASHTO 18 2010 by the American Associaton of State Highway and Transportation Offical All rights reserved. Duplication is «violation of applicable law13. PRECISION Data are being compiled that will be suitable for use in developing precision statements for ‘tis method. 14. REFERENCES 144 Clear, K. C. Evaluation of Portland Cement Concrete for Permanent Bridge Deck Repair. Report FHWA-RD-74-5. Federal Highway Administration, U.S. Department of Transportat February 1974. 142 Clemena, G. C., J. W. Reynolds, and R. M. McCormick. Comparative Studies of Chloride in Hardened Concrete. Report No. FHWA-RD-T7-84 T-RT. Vii Research Council, August 1976, nia Highway and Transportati ' ‘The numbers represent, respectively, the (1s) and (d2s) limits as described in ASTM C 670 for Preparing Precision Statements for Test Methods for Construction Materials, TS-3¢ T 260-15 ‘AASHTO 1 2010 by the American Association of State Highvray and Transportation Oficial All rights reserved. Duplication is violation of appliceble aw.