A number in parentheses indicates the year of last reapproval. In Hardened Concrete in Constructions most cases, acid-soluble chloride is equivalent to total chloride. Significance and Use fication E The alternative designation in parentheses is for information only and does not represent a different standard sieve size.
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A number in parentheses indicates the year of last reapproval. Inmost cases, acid-soluble chloride is equivalent to total chloride. Some values haveonly SI units because the inch-pound equivalents are not usedin practice. The alternative designation in parentheses is for informationonly and does not represent a different standard sieve size. These notes and foot-notes shall not be considered as requirements of this standard. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.
Referenced Documents2. Significance and Use3. However, some organic substances that may be intro-duced into mortar or concrete contain chloride that is initiallyacid-insoluble that can eventually ionize and thus becomeacid-soluble or water-soluble after a period of exposure in thevery alkaline cement system.
Blast-furnace slag aggregates and cementscontain sulfide sulfur in concentrations that can cause suchinterference and produce erroneously high test results. Treat-ment with hydrogen peroxide, as discussed in Test MethodsC, is used to eliminate such interference. Such chloride will be detected by theuse of this method. Current edition approved Dec. Published January Originallyapproved in Hope, John A.
Page and John S. United States Direct-reading balances shall have a sensitivity not exceeding 0. Conventional two-pan balances shall have a maximumsensibility reciprocal of 0.
Any rapid weighing devicethat may be provided, such as a chain, damped motion, orheavy riders, shall not increase the basic inaccuracy by morethan 0. A digital readout is preferred but not required.
Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee onAnalytical Reagents of theAmerican Chemical Society5. Other grades may be used, provided it is first ascertained thatthe reagent is of sufficiently high purity to permit its usewithout lessening the accuracy of the determination.
Weigh 2. Dissolve in water and diluteto exactly 1 L in a volumetric flask and mix thoroughly. Thissolution is the standard and requires no further standardization. Dilute to 1 L in avolumetric flask and mix thoroughly. Standardize against 5. Commercially available standard solutions may be usedprovided the normality is checked according to the standard-ization procedure. Concrete farthest from a surface into which chloride has penetrated oftenprovides chloride data close to that of the originally placed fresh concrete.
The cooling water from core cutting may dissolve some of the chloride. Such samples maybe unrepresentative, especially when the nominal maximumcoarse aggregate size is 25 mm 1 in. Thus, severalsuch samples should be combined, or the data used with care. Procedures for this method of sampling are as follows To prevent sample contamination, avoidcontact of sample with hands and other sources of perspiration. Pharmaceutical Convention, Inc. No lubricants shall be used during drilling.
NOTE 4—Sampling tools may be cleaned with a brush, cloth, ethylalcohol rinse, water rinse, or other method that will not contaminate thesample. Sample Preparation7. Disperse thesample with 75 mL of water. If the smell of hydrogen sulfide is strongly present, add3 mL of hydrogen peroxide See Note 5. Add 3 drops ofmethyl orange indicator to the beaker and stir.
Cover the beakerwith a watch glass and allow to stand for 1 to 2 minutes. If thesolution above the settled solids is not pink colored, add morenitric acid dropwise while stirring until a pink or reddish colorpersists, then add 10 additional drops of nitric acid and stir. Heat the covered beaker rapidly to boiling and remove fromhot plate.
Do not allow sample to boil more than a few seconds See Note 6. Make a blank determination using 75 mL ofwater in place of sample. NOTE 5—Slags and slag cements contain sulfide sulfur in concentra-tions that can interfere with chloride determination unless oxidized withhydrogen peroxide. NOTE 6—To prevent loss of chloride by volatilization, it is important tokeep the beaker covered during heating and digestion. Ten seconds ofboiling is sufficient.
Excessive amounts of acid can erode the silverchloride coating on the silver billet electrode prematurely. A slurry that isonly slightly acidic is sufficient. Rinse the beaker and the filter paper twicewith small portions of water. Transfer the filtrate from the flaskto a mL beaker and rinse the flask once with water. Theoriginal beaker may be used See Note 7. Cool the filtrate toroom temperature. The volume should not exceed mL. NOTE 7—It is not necessary to clean all the slurry residue from the sidesof the beaker, nor is it necessary that the filter remove all the fine material.
The titration may take place in a solution that contains a small amount ofsolid matter. Recordthe approximate millivoltmeter reading. Remove the beakerand wipe the electrodes with absorbent paper. Place the beaker on amagnetic stirrer and add a TFE-fluorocarbon coated stir bar. Immerse the electrodes into the solution, taking care that thestir bar does not strike the electrodes. Begin stirring gently. Place the delivery tip of the 10 mL buret filled to the zero markwith standardized 0.
NOTE 8—It is advisable to maintain constant temperature duringmeasurement, as the solubility of silver chloride varies markedly withtemperature at low concentrations.
NOTE 9—If the tip of the buret is out of the solution, any adheringdroplet should be rinsed into the beaker with a few millilitres of waterfollowing each titration increment. Recordthe buret reading and the corresponding millivoltmeter reading.
Allow sufficient time between each addition for the electrodesto reach equilibrium with the sample solution See Note NOTE 10—Experience has shown that acceptable readings are obtainedwhen the minimum scale reading does not change within a 5-s period.
More C However, some organic substances that may be introduced into mortar or concrete contain chloride that is initially acid-insoluble that can eventually ionize and thus become acid-soluble or water-soluble after a period of exposure in the very alkaline cement system. Blast-furnace slag aggregates and cements contain sulfide sulfur in concentrations that can cause such interference and produce erroneously high test results. Treatment with hydrogen peroxide, as discussed in Test Methods C , is used to eliminate such interference. Such chloride will be detected by the use of this method. Scope 1.