D15.04 - Chemical Properties

SIGNIFICANCE AND USE
5.1 This test method is for the quantitative determination of fluoride and glycol degradation products in engine coolants. By this method, analysis can be performed directly without pretreatment, other than dilution, as required by the linear ranges of the equipment. Table 1 indicates applicable analytes and approximate detection limits. (A) Sample diluted 1/10 with reagent water, suppressed conductivity detection, IonPac AS20 column with AG20 guard column. Other systems will require MQL determinations using chosen dilution factors, eluents, columns, and detector.
SCOPE
1.1 This test method covers the determination of fluoride in engine coolants by ion chromatography. Several glycol degradation products (different carboxylates including, but not limited to, formate and glycolate) can be determined by this test method.  
1.2 This test method applies to both new and used engine coolants.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
4.1 Knowledge of an approved method is required to establish whether the product meets the requirements of its specifications. The use of glycols in the reference sample is not intended to suggest the presence of glycol (EG, PG and DPG) impurities, but to demonstrate and quantify the separation of commonly used Engine Coolant glycols from PDO.
SCOPE
1.1 This test method describes the gas chromatographic determination of purity for 1,3-propanediol (PDO). This test method was originally developed to determine the purity of 1,3-propanediol used for the application as the freeze point depressant base fluid in formulated PDO engine coolants. Use of the method for purity of PDO for other applications may be viable.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.2.1 Exception—Inch-pound units (psi) are used in Table 1, Pressure Program, Options A and B.  
1.3 Review the current Material Safety Data Sheets (MSDS) for detailed information concerning toxicity, first aid procedures, and safety precautions.  
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
4.1 This test method provides for the qualitative and quantitative determination of denatonium benzoate in engine coolant in milligrams per litre to low percent range and requires approximately 1 mL per test, with results available in less than 10 min. Denatonium benzoate is a compound composed of a quaternary ammonium cation, denatonium and an inert anion, benzoate. In solution the denatonium benzoate exists in equilibrium between the denatonium benzoate compound, the denatonium cation and benzoate anion. By slightly adjusting the pH of the solution to be more acidic (≈ pH 4.6) the equilibrium will be shifted to the direction of forming more denatonium and benzoate ions in the solution.
SCOPE
1.1 This test method covers the chemical analysis of engine coolant for denatonium benzoate (DNB) by high-performance liquid chromatography (HPLC). DNB is added to potentially render engine coolant unpalatable to animals and humans. This analytical method was designed for the analysis of DNB and is not valid for any other bittering agents such as denatonium saccharide.  
1.2 This test method is applicable to both new and used coolants.  
1.3 Coelution of other ions may cause interferences in the detection of the denatonium cation. In the case of unfamiliar formulations, identification verification should be performed by either or both fortification and dilution of the sample matrix with denatonium ion.  
1.4 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.  
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.6 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.

SIGNIFICANCE AND USE
5.1 The total apparent water in engine coolant concentrate as determined by Karl Fischer titrations consists of the following: (1) water present in the original glycol base; (2) water added (for example, inhibitor solutions); (3) water of hydration of inhibitors (for example, Na2B4O7·5H2O); (4) water formed in the chemical reaction between borate and ethylene glycol, producing boratediol condensate and water; and (5) quantitative interference by the reaction of the reagent with inhibitors such as tetraborate or sodium hydroxide.
SCOPE
1.1 These test methods cover the determination of the water present in new or unused glycol-based coolant concentrates using a volumetric (Test Method A) or an automatic coulometric titrator procedure (Test Method B).  
1.2 Many carbonyl compounds react slowly with the Fischer reagent, causing a fading end point and leading to high results. A modified Fischer reagent procedure is included that minimizes these undesirable and interfering reactions.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazards statements see Sections 8 and 16.  
1.5 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.

SIGNIFICANCE AND USE
4.1 This test method provides for the qualitative and quantitative determination of common anions in engine coolant in the milligrams per litre to low percent range and requires only a few millilitres or microlitres of sample per test, with results available in less than 30 min. Acceptable levels of chloride and other anions vary with manufacturer's blending specifications and applicable ASTM minimum or maximum specifications.
SCOPE
1.1 This test method covers the chemical analysis of engine coolant for chloride ion by high-performance ion chromatography (HPIC). Several other common anions found in engine coolant can be determined in one chromatographic analysis by this test method.  
1.2 This test method is applicable to both new and used engine coolant.  
1.3 Coelution of other ions may cause interferences for any of the listed anions. In the case of unfamiliar formulations, identification verification should be performed by either or both fortification and dilution of the sample matrix with the anions of interest.  
1.4 Analysis can be performed directly by this test method without pretreatment, other than dilution, as required by the linear ranges of the equipment. Table 1 indicates several applicable anions and approximate detection limits.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to its use.  
1.7 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.

SIGNIFICANCE AND USE
5.1 This test method is designed to aid in identifying types of coolants. While the ash is primarily due to the inorganic inhibitors used, it is not a measure of the total inhibitor concentration because of the loss of organic inhibitors.  
5.2 An ash content greater than that stated in Specification D3306 may indicate a salt-based product.
SCOPE
1.1 This test method covers the determination of ash content after ignition of commercial engine coolants and antirusts, as packaged or after use.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific warning statements are given in 7.1 and 7.3.  
1.4 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.

SIGNIFICANCE AND USE
4.1 This test method permits the determination of very low levels of chloride ion in engine coolants containing the common corrosion inhibitor, mercaptobenzothiazole, or related mercaptans, which would normally interfere with the titration by also forming insoluble silver salts with silver nitrate.
SCOPE
1.1 This test method covers the determination of chloride ion in engine coolants in the range from 5 ppm to 200 ppm in the presence of up to 0.6 weight % mercaptobenzothiazole.  
1.2 Other materials that react with silver ion will interfere.  
1.3 Chloride in engine coolants containing an aryltriazole instead of mercaptobenzothiazole can be determined directly by this test method without pretreatment with hydrogen peroxide.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific hazards statements are given in Section 7.  
1.6 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.

ABSTRACT
This standard test method covers the determination of silicon in engine coolant concentrates by atomic absorption spectroscopy. Apparatus and reagents used for this test method include atomic absorption spectrometer, hollow-cathode lamp, reagent grade chemicals, standard silicon solution, ethylene glycol or propylene glycol, and sodium hydroxide. Silicon content shall be determined from an established standard curve and an atomic absorption spectrometer. A nitrous oxide-acetylene flame shall be used.
SCOPE
1.1 This test method covers the determination of silicon in the range from 200 ppm to 500 ppm in engine coolant concentrates by atomic absorption. This method is as accurate and precise as photometric methods, while requiring considerably less operator time and avoiding problems with reagent instability.  
1.1.1 Coolants with silicon content outside of this range may be analyzed by this method by suitably adjusting the sample size. Care should be taken to ensure that the glycol content of the working standards corresponds to that of the sample solution being analyzed.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 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.

SIGNIFICANCE AND USE
4.1 Any residual fatty acid and esters (FA&E) should be present only at very low levels in purified glycerine.  
4.2 This procedure requires the addition of a measured volume of sodium hydroxide, in excess of the amount actually needed to react with FA&E in the glycerine sample. After boiling, the excess sodium hydroxide is back titrated with standardized hydrochloric acid. The quantity of the substance being titrated is calculated as the difference between the volumes of the sodium hydroxide solution originally added, corrected by means of a blank titration, and that was consumed by the titrant in the back titration.
Note 1: The standardized solutions for sodium hydroxide and hydrochloric acid are commercially available.
SCOPE
1.1 This test method provides the quantitative determination of the fatty acid and ester content in purified glycerin by the titrimetric method.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 This standard may involve hazardous materials, operations and equipment. This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautions are listed in Section 8.  
1.4 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.

SIGNIFICANCE AND USE
4.1 This test method is based on the cold oxidation of the glycerol by sodium metaperiodate in a strong acidic medium. Formaldehyde and formic acid are produced in this reaction and the latter is used to measure the glycerol content by titration with standard sodium hydroxide solution, to a pH 8.1 ± 0.1. The glycerol content is expressed as a percentage (m/m).
4.2 Interferences—The glycerin sample should be free of organic compounds with more than two hydroxyl groups on adjacent carbon atoms (for example, sugars, glycols). These types of compounds may produce formic acid which interferes with the determination of the glycerol content.
SCOPE
1.1 This test method provides the quantitative determination of glycerin by the titrimetric method. It is applicable to all glycerin or glycerin/water mixtures >75 %.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 This standard may involve hazardous materials, operations, and equipment. This standard does not purport to address all of the safety concerns associated with its use. It is the responsibility of the user of this standard to consult the established and appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautions are listed in Section 8.  
1.4 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.

SIGNIFICANCE AND USE
5.1 Reserve alkalinity is the number of millilitres, to the nearest 0.1 mL of 0.100 N hydrochloric acid (HCl) required for the titration to a pH of 5.5 of a 10 mL sample of an undiluted, unused coolant, antirust, or coolant additive, and unused or used solutions thereof.  
5.2 Reserve alkalinity is a term applied to engine coolants and antirusts to indicate the amount of alkaline components present in the product. It is frequently used for quality control during production, and values are often listed in specifications. When applied to used solutions, reserve alkalinity gives an approximate indication of the amount of remaining alkaline components. Unfortunately, the term is sometimes misused in that its numerical value is said to be directly related to coolant quality, the higher the number, the better the coolant. ASTM Committee D15 on Engine Coolants believes there is a need to correct some misconceptions and place the term in its proper perspective.  
5.3 Reserve alkalinity (R.A.) as defined in Section 3 of this method is the number of millilitres of 0.1 N hydrochloric acid required to titrate 10 mL of concentrated coolant to a pH of 5.5. The term is not a completely accurate description of the property being measured because “alkalinity” usually refers to the pH range above 7.0.  
5.4 A review of the origin of the term may be helpful in attempting to understand its proper use. When ethylene glycol was first used as an engine coolant, it was uninhibited. The need for inhibition soon became apparent and triethanolamine was incorporated. When solutions of this inhibited glycol were titrated with dilute hydrochloric acid, it was found that the steepest part of the neutralization curve occurred at a pH of about 5.0. Following the introduction of triethanolamine, other buffers, such as borates and phosphates, have been used. Titration to 5.5 was employed with these buffers which have an end point close to 5.5.  
5.5 Generally, most metals in an automotive cooling...
SCOPE
1.1 This test method covers the determination of the reserve alkalinity of new, unused engine coolants, and liquid antirusts as received, of used or unused aqueous dilutions of the concentrated materials, and of aqueous dilutions of solid antirusts.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 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.

SIGNIFICANCE AND USE
4.1 pH is a measure of the hydrogen ion concentration and indicates whether an engine coolant, antirust, or a solution of these compounds is acidic, alkaline, or neutral.  
4.2 The pH range includes values from 0 to 14. Values from 0 to 7 represent the acidic half of the scale. Values from 7 to 14 represent the alkaline or basic half of the scale. The pH value 7 is considered neutral, as it is neither acidic nor alkaline.  
4.3 pH is sometimes used for production quality control. It is generally desirable that engine coolants have an alkaline pH.  
4.4 pH is not significant from the standpoint of predicting service life. The pH of used engine coolants or antirust solutions is not a dependable indication of either existing effectiveness or remaining life of the solution.
SCOPE
1.1 This test method covers the determination of the pH of unused engine coolants and antirusts, and used or unused aqueous dilutions of the concentrated products.  
Note 1: Antirusts in solid form are not included in this test method.
Note 2: It is believed that this procedure gives all the information required for determining the pH of samples of engine coolant or antirust likely to be encountered. Should additional information on pH determinations be needed, reference should be made to Test Method E70.  
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.3 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.

SIGNIFICANCE AND USE
5.1 Methanol content reflects the quality of glycerin for use as an engine coolant. The current specification for the maximum methanol content is 0.1 % weight to weight (w/w).
SCOPE
1.1 This test method provides for the quantitative determination of residual methanol in glycerin by gas chromatography. The range of detection for residual methanol is 0.02 to 0.60 mass %.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 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.

SIGNIFICANCE AND USE
4.1 Some engine coolants are formulated with silicon containing additives. This test method provides a means of determining the concentration of dissolved or dispersed elements which give an indication of this additive content in the engine coolant.
SCOPE
1.1 This test method covers the determination of silicon in engine coolant by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). Silicon can be determined as low as the range of 5 ppm by this test method. Other elements also found in engine coolant can be determined by this method. This test method is applicable to the determination of dissolved or dispersed elements.  
1.2 This test method is applicable to both new and used engine coolant.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
5.1 The total apparent water in engine coolant concentrate as determined by Karl Fischer titrations consists of the following: (1) water present in the original glycol base; (2) water added (for example, inhibitor solutions); (3) water of hydration of inhibitors (for example, Na2B4O7·5H2O); (4) water formed in the chemical reaction between borate and ethylene glycol, producing boratediol condensate and water; and (5) quantitative interference by the reaction of the reagent with inhibitors such as tetraborate or sodium hydroxide.
SCOPE
1.1 These test methods cover the determination of the water present in new or unused glycol-based coolant concentrates using a manual (Test Method A) or an automatic (Test Method B) coulometric titrator procedure.  
1.2 Many carbonyl compounds react slowly with the Fischer reagent, causing a fading end point and leading to high results. A modified Fischer reagent procedure is included that minimizes these undesirable and interfering reactions.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazards statements see Sections 8 and 16.  
1.5 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.

SIGNIFICANCE AND USE
4.1 This test method provides for the qualitative and quantitative determination of denatonium benzoate in engine coolant in milligrams per litre to low percent range and requires approximately 1 mL per test, with results available in less than 10 min. Denatonium benzoate is a compound composed of a quaternary ammonium cation, denatonium and an inert anion, benzoate. In solution the denatonium benzoate exists in equilibrium between the denatonium benzoate compound, the denatonium cation and benzoate anion. By slightly adjusting the pH of the solution to be more acidic (≈ pH 4.6) the equilibrium will be shifted to the direction of forming more denatonium and benzoate ions in the solution.
SCOPE
1.1 This test method covers the chemical analysis of engine coolant for denatonium benzoate (DNB) by high-performance liquid chromatography (HPLC). DNB is added to potentially render engine coolant unpalatable to animals and humans. This analytical method was designed for the analysis of DNB and is not valid for any other bittering agents such as denatonium saccharide.  
1.2 This test method is applicable to both new and used coolants.  
1.3 Coelution of other ions may cause interferences in the detection of the denatonium cation. In the case of unfamiliar formulations, identification verification should be performed by either or both fortification and dilution of the sample matrix with denatonium ion.  
1.4 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.  
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.6 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.

SIGNIFICANCE AND USE
5.1 The presence of acids or glycol esters in the glycol used to produce engine coolant is undesirable. Under conditions in an engine cooling system, the esters can hydrolyze to form glycol and an acid. The acid will react with the corrosion inhibitors, thereby reducing the useful life of the coolant. This method can determine the amount of acid and glycol ester present in the glycol.
SCOPE
1.1 This test method covers the determination of free acids and glycol esters in glycols by titration.  
1.2 This test method is typically used on glycols used for the manufacture of engine coolant. It cannot be used on formulated engine coolant. The inhibitors will interfere with the determination.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
4.1 Knowledge of an approved method is required to establish whether the product meets the requirements of its specifications. The use of glycols in the reference sample is not intended to suggest the presence of glycol (EG, PG and DPG) impurities, but to demonstrate and quantify the separation of commonly used Engine Coolant glycols from PDO.
SCOPE
1.1 This test method describes the gas chromatographic determination of purity for 1,3-propanediol (PDO). This test method was originally developed to determine the purity of 1,3-propanediol used for the application as the freeze point depressant base fluid in formulated PDO engine coolants. Use of the method for purity of PDO for other applications may be viable.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.2.1 Exception—Inch-pound units (psi) are used in Table 1, Pressure Program, Options A and B.  
1.3 Review the current Material Safety Data Sheets (MSDS) for detailed information concerning toxicity, first aid procedures, and safety precautions.  
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
5.1 The presence of acids or glycol esters in the ethylene glycol used to produce engine coolant is undesirable. Under conditions in an engine cooling system, the esters can hydrolyze to form glycol and an acid. The acid will react with the corrosion inhibitors, thereby reducing the useful life of the coolant. This method can determine the amount of acid and glycol ester present in the ethylene glycol.
SCOPE
1.1 This test method covers the determination of free acids and glycol esters in ethylene glycol by titration.  
1.2 Laboratory testing has proved that the test method can also be used on propylene glycol and 1,3-propanediol.  
1.3 This test method is typically used on glycols used for the manufacture of engine coolant. It cannot be used on formulated engine coolant. The inhibitors will interfere with the determination.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.6 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.

SIGNIFICANCE AND USE
5.1 The presence of acids or glycol esters in the ethylene glycol used to produce engine coolant is undesirable. Under conditions in an engine cooling system, the esters can hydrolyze to form glycol and an acid. The acid will react with the corrosion inhibitors, thereby reducing the useful life of the coolant. This method can determine the amount of acid and glycol ester present in the ethylene glycol.
SCOPE
1.1 This test method covers the determination of free acids and glycol esters in ethylene glycol by titration.  
1.2 This test method is for used on ethylene glycol used for the manufacture of engine coolant. It can not be used on formulated engine coolant. The inhibitors will interfere with the determination.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
4.1 This test method provides for the qualitative and quantitative determination of denatonium benzoate in engine coolant in milligrams per litre to low percent range and requires approximately 1 mL per test, with results available in less than 10 min. Denatonium benzoate is a compound composed of a quaternary ammonium cation, denatonium and an inert anion, benzoate. In solution the denatonium benzoate exists in equilibrium between the denatonium benzoate compound, the denatonium cation and benzoate anion. By slightly adjusting the pH of the solution to be more acidic (≈ pH 4.6) the equilibrium will be shifted to the direction of forming more denatonium and benzoate ions in the solution.
SCOPE
1.1 This test method covers the chemical analysis of engine coolant for denatonium benzoate (DNB) by high-performance liquid chromatography (HPLC). DNB is added to potentially render engine coolant unpalatable to animals and humans. This analytical method was designed for the analysis of DNB and is not valid for any other bittering agents such as denatonium saccharide.  
1.2 This test method is applicable to both new and used coolants.  
1.3 Coelution of other ions may cause interferences in the detection of the denatonium cation. In the case of unfamiliar formulations, identification verification should be performed by either or both fortification and dilution of the sample matrix with denatonium ion.  
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
4.1 Any residual fatty acid and esters (FA&E) should be present only at very low levels in purified glycerine.  
4.2 This procedure requires the addition of a measured volume of sodium hydroxide, in excess of the amount actually needed to react with FA&E in the glycerine sample. After boiling, the excess sodium hydroxide is back titrated with standardized hydrochloric acid. The quantity of the substance being titrated is calculated as the difference between the volumes of the sodium hydroxide solution originally added, corrected by means of a blank titration, and that was consumed by the titrant in the back titration.
Note 1: The standardized solutions for sodium hydroxide and hydrochloric acid are commercially available.
SCOPE
1.1 This test method provides the quantitative determination of the fatty acid and ester content in purified glycerin by the titrimetric method.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 This standard may involve hazardous materials, operations and equipment. This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific precautions are listed in Section 8.

SIGNIFICANCE AND USE
4.1 This test method provides for the qualitative and quantitative determination of common anions in engine coolant in the milligrams per litre to low percent range and requires only a few millilitres or microlitres of sample per test, with results available in less than 30 min. Acceptable levels of chloride and other anions vary with manufacturer's blending specifications and applicable ASTM minimum or maximum specifications.
SCOPE
1.1 This test method covers the chemical analysis of engine coolant for chloride ion by high-performance ion chromatography (HPIC). Several other common anions found in engine coolant can be determined in one chromatographic analysis by this test method.  
1.2 This test method is applicable to both new and used engine coolant.  
1.3 Coelution of other ions may cause interferences for any of the listed anions. In the case of unfamiliar formulations, identification verification should be performed by either or both fortification and dilution of the sample matrix with the anions of interest.  
1.4 Analysis can be performed directly by this test method without pretreatment, other than dilution, as required by the linear ranges of the equipment. Table 1 indicates several applicable anions and approximate detection limits. (A) Determined using 100-μL sample volume. Sample diluted 99 + 1 (v/v) with chromatographic eluant 30-μS/cm full scale, suppressed conductivity detection. Dionex AS4ASC column with AG4ASC guard columns. Other systems will require MDL determinations using chosen dilution factors, eluants, columns, and detector.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to its use.

ABSTRACT
This standard test method covers the determination of silicon in engine coolant concentrates by atomic absorption spectroscopy. Apparatus and reagents used for this test method include atomic absorption spectrometer, hollow-cathode lamp, reagent grade chemicals, standard silicon solution, ethylene glycol or propylene glycol, and sodium hydroxide. Silicon content shall be determined from an established standard curve and an atomic absorption spectrometer. A nitrous oxide-acetylene flame shall be used.
SCOPE
1.1 This test method covers the determination of silicon in the range from 200 to 500 ppm in engine coolant concentrates by atomic absorption. This method is as accurate and precise as photometric methods, while requiring considerably less operator time and avoiding problems with reagent instability.  
1.1.1 Coolants with silicon content outside of this range may be analyzed by this method by suitably adjusting the sample size. Care should be taken to ensure that the glycol content of the working standards corresponds to that of the sample solution being analyzed.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
4.1 This test method is based on the cold oxidation of the glycerol by sodium metaperiodate in a strong acidic medium. Formaldehyde and formic acid are produced in this reaction and the latter is used to measure the glycerol content by titration with standard sodium hydroxide solution, to a pH 8.1 ± 0.1. The glycerol content is expressed as a percentage (m/m).
4.2 Interferences—The glycerin sample should be free of organic compounds with more than two hydroxyl groups on adjacent carbon atoms (for example, sugars, glycols). These types of compounds may produce formic acid which interferes with the determination of the glycerol content.
SCOPE
1.1 This test method provides the quantitative determination of glycerin by the titrimetric method. It is applicable to all glycerin or glycerin/water mixtures >75 %.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 This standard may involve hazardous materials, operations and equipment. This standard does not purport to address all of the safety problems associated with its use. It is the responsibility of whoever uses this standard to consult the established and appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific precautions are listed in Section 8.

SIGNIFICANCE AND USE
4.1 This test method permits the determination of very low levels of chloride ion in engine coolants containing the common corrosion inhibitor, mercaptobenzothiazole, or related mercaptans, which would normally interfere with the titration by also forming insoluble silver salts with silver nitrate.
SCOPE
1.1 This test method covers the determination of chloride ion in engine coolants in the range from 5 to 200 ppm in the presence of up to 0.6 weight % mercaptobenzothiazole.  
1.2 Other materials that react with silver ion will interfere.  
1.3 Chloride in engine coolants containing an aryltriazole instead of mercaptobenzothiazole can be determined directly by this test method without pretreatment with hydrogen peroxide.  
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazards statements are given in Section 7.

SIGNIFICANCE AND USE
5.1 The total apparent water in engine coolant concentrate as determined by Karl Fischer titrations consists of the following: (1) water present in the original glycol base; (2) water added (for example, inhibitor solutions); (3) water of hydration of inhibitors (for example, Na2B4O7·5H2O); (4) water formed in the chemical reaction between borate and ethylene glycol, producing boratediol condensate and water; and (5) quantitative interference by the reaction of the reagent with inhibitors such as tetraborate or sodium hydroxide.
SCOPE
1.1 These test methods cover the determination of the water present in new or unused glycol-based coolant concentrates using a manual (Test Method A) or an automatic (Test Method B) coulometric titrator procedure.  
1.2 Many carbonyl compounds react slowly with the Fischer reagent, causing a fading end point and leading to high results. A modified Fischer reagent procedure is included that minimizes these undesirable and interfering reactions.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazards statements see Sections 8 and 16.

SIGNIFICANCE AND USE
5.1 This test method is designed to aid in identifying types of coolants. While the ash is primarily due to the inorganic inhibitors used, it is not a measure of the total inhibitor concentration because of the loss of organic inhibitors.  
5.2 An ash content greater than that stated in Specification D3306 may indicate a salt-based product.
SCOPE
1.1 This test method covers the determination of ash content after ignition of commercial engine coolants and antirusts, as packaged or after use.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific warning statements are given in 7.1 and 7.3.

SIGNIFICANCE AND USE
4.1 This test method provides for the qualitative and quantitative determination of denatonium benzoate in engine coolant in milligrams per litre to low percent range and requires approximately 1 mL per test, with results available in less than 10 min. Denatonium benzoate is a compound composed of a quaternary ammonium cation, denatonium and an inert anion, benzoate. In solution the denatonium benzoate exists in equilibrium between the denatonium benzoate compound, the denatonium cation and benzoate anion. By slightly adjusting the pH of the solution to be more acidic (≈ pH 4.6) the equilibrium will be shifted to the direction of forming more denatonium and benzoate ions in the solution.
SCOPE
1.1 This test method covers the chemical analysis of engine coolant for denatonium benzoate (DNB) by high-performance liquid chromatography (HPLC). DNB is added to potentially render engine coolant unpalatable to animals and humans. This analytical method was designed for the analysis of DNB and is not valid for any other bittering agents such as denatonium saccharide.  
1.2 This test method is applicable to both new and used coolants.  
1.3 Coelution of other ions may cause interferences in the detection of the denatonium cation. In the case of unfamiliar formulations, identification verification should be performed by either or both fortification and dilution of the sample matrix with denatonium ion.  
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
The presence of acids or glycol esters in the ethylene glycol used to produce engine coolant is undesirable. Under conditions in an engine cooling system, the esters can hydrolyze to form glycol and an acid. The acid will react with the corrosion inhibitors, thereby reducing the useful life of the coolant. This method can determine the amount of acid and glycol ester present in the ethylene glycol.
SCOPE
1.1 This test method covers the determination of free acids and glycol esters in ethylene glycol by titration.
1.2 This test method is for used on ethylene glycol used for the manufacture of engine coolant. It can not be used on formulated engine coolant. The inhibitors will interfere with the determination.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
Some engine coolants are formulated with silicon containing additives. This test method provides a means of determining the concentration of dissolved or dispersed elements which give an indication of this additive content in the engine coolant.
SCOPE
1.1 This test method covers the determination of silicon in engine coolant by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). Silicon can be determined as low as the range of 5 ppm by this test method. Other elements also found in engine coolant can be determined by this method. This test method is applicable to the determination of dissolved or dispersed elements.
1.2 This test method is applicable to both new and used engine coolant.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
Methanol content reflects the quality of glycerin for use as an engine coolant. The current specification for the maximum methanol content is 0.1 % weight to weight (w/w).
SCOPE
1.1 This test method provides for the quantitative determination of residual methanol in glycerin by gas chromatography. The range of detection for residual methanol is 0.02 to 0.60 mass %.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
pH is a measure of the hydrogen ion concentration and indicates whether an engine coolant, antirust, or a solution of these compounds is acidic, alkaline, or neutral.
The pH range includes values from 0 to 14. Values from 0 to 7 represent the acidic half of the scale. Values from 7 to 14 represent the alkaline or basic half of the scale. The pH value 7 is considered neutral, as it is neither acidic nor alkaline.
pH is sometimes used for production quality control. It is generally desirable that engine coolants have an alkaline pH.
pH is not significant from the standpoint of predicting service life. The pH of used engine coolants or antirust solutions is not a dependable indication of either existing effectiveness or remaining life of the solution.
SCOPE
1.1 This test method covers the determination of the pH of unused engine coolants and antirusts, and used or unused aqueous dilutions of the concentrated products.
Note 1—Antirusts in solid form are not included in this test method.
Note 2—It is believed that this procedure gives all the information required for determining the pH of samples of engine coolant or antirust likely to be encountered. Should additional information on pH determinations be needed, reference should be made to Test Method E70.  
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
Reserve alkalinity is the number of millilitres, to the nearest 0.1 mL of 0.100 N hydrochloric acid (HCl) required for the titration to a pH of 5.5 of a 10-mL sample of an undiluted, unused coolant, antirust, or coolant additive, and unused or used solutions thereof.
Reserve alkalinity is a term applied to engine coolants and antirusts to indicate the amount of alkaline components present in the product. It is frequently used for quality control during production, and values are often listed in specifications. When applied to used solutions, reserve alkalinity gives an approximate indication of the amount of remaining alkaline components. Unfortunately, the term is sometimes misused in that its numerical value is said to be directly related to coolant quality, the higher the number, the better the coolant. ASTM Committee D15 on Engine Coolants believes there is a need to correct some misconceptions and place the term in its proper perspective.
Reserve alkalinity (R.A.) as defined in Section 3 of this method is the number of millilitres of 0.1-N hydrochloric acid required to titrate 10 mL of concentrated coolant to a pH of 5.5. The term is not a completely accurate description of the property being measured because “alkalinity” usually refers to the pH range above 7.0.
A review of the origin of the term may be helpful in attempting to understand its proper use. When ethylene glycol was first used as an engine coolant, it was uninhibited. The need for inhibition soon became apparent and triethanolamine was incorporated. When solutions of this inhibited glycol were titrated with dilute hydrochloric acid, it was found that the steepest part of the neutralization curve occurred at a pH of about 5.0. Following the introduction of triethanolamine, other buffers, such as borates and phosphates, have been used. Titration to 5.5 was employed with these buffers which have an end point close to 5.5.
Generally, most metals in an automotive cooling system corrode less in ...
SCOPE
1.1 This test method covers the determination of the reserve alkalinity of new, unused engine coolants, and liquid antirusts as received, of used or unused aqueous dilutions of the concentrated materials, and of aqueous dilutions of solid antirusts.
1.2 The values stated in SI units are to be regarded as the standard.
1.3 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
The presence of acids or glycol esters in the ethylene glycol used to produce engine coolant is undesirable. Under conditions in an engine cooling system, the esters can hydrolyze to form glycol and an acid. The acid will react with the corrosion inhibitors, thereby reducing the useful life of the coolant. This method can determine the amount of acid and glycol ester present in the ethylene glycol.
SCOPE
1.1 This test method covers the determination of free acids and glycol esters in ethylene glycol by titration.
1.2 This test method is for used on ethylene glycol used for the manufacture of engine coolant. It can not be used on formulated engine coolant. The inhibitors will interfere with the determination.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
The total apparent water in engine coolant concentrate as determined by Karl Fischer titrations consists of the fol-
lowing: (1) water present in the original glycol base; (2) water added (for example, inhibitor solutions); (3) water of hydration of inhibitors (for example, Na 2B4O7·5H2O); ( 4) water formed in the chemical reaction between borate and ethylene glycol, producing boratediol condensate and water; and ( 5) quantitative interference by the reaction of the reagent with inhibitors such as tetraborate or sodium hydroxide.
SCOPE
1.1 These test methods cover the determination of the water present in new or unused glycol-based coolant concentrates using a manual (Test Method A) or an automatic (Test Method B) coulometric titrator procedure.  
1.2 Many carbonyl compounds react slowly with the Fischer reagent, causing a fading end point and leading to high results. A modified Fischer reagent procedure is included that minimizes these undesirable and interfering reactions.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazards statements see Sections 8 and 16.

SIGNIFICANCE AND USE
Some engine coolants are formulated with silicon containing additives. This test method provides a means of determining the concentration of dissolved or dispersed elements which give an indication of this additive content in the engine coolant.
SCOPE
1.1 This test method covers the determination of silicon in engine coolant by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). Silicon can be determined as low as the range of 5 ppm by this test method. Other elements also found in engine coolant can be determined by this method. This test method is applicable to the determination of dissolved or dispersed elements.
1.2 This test method is applicable to both new and used engine coolant.
1.3 The values stated in SI units are to be regarded as the standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
This test method permits the determination of very low levels of chloride ion in engine coolants containing the common corrosion inhibitor, mercaptobenzothiazole, or related mercaptans, which would normally interfere with the titration by also forming insoluble silver salts with silver nitrate.
SCOPE
1.1 This test method covers the determination of chloride ion in engine coolants in the range from 5 to 200 ppm in the presence of up to 0.6 weight % mercaptobenzothiazole.
1.2 Other materials that react with silver ion will interfere.
1.3 Chloride in engine coolants containing an aryltriazole instead of mercaptobenzothiazole can be determined directly by this test method without pretreatment with hydrogen peroxide.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazards statements are given in Section 7.

SIGNIFICANCE AND USE
pH is a measure of the hydrogen ion concentration and indicates whether an engine coolant, antirust, or a solution of these compounds is acidic, alkaline, or neutral.
The pH range includes values from 0 to 14. Values from 0 to 7 represent the acidic half of the scale. Values from 7 to 14 represent the alkaline or basic half of the scale. The pH value 7 is considered neutral, as it is neither acidic nor alkaline.
pH is sometimes used for production quality control. It is generally desirable that engine coolants have an alkaline pH.
pH is not significant from the standpoint of predicting service life. The pH of used engine coolants or antirust solutions is not a dependable indication of either existing effectiveness or remaining life of the solution.
SCOPE
1.1 This test method covers the determination of the pH of unused engine coolants and antirusts, and used or unused aqueous dilutions of the concentrated products.
Note 1—Antirusts in solid form are not included in this test method.
Note 2—It is believed that this procedure gives all the information required for determining the pH of samples of engine coolant or antirust likely to be encountered. Should additional information on pH determinations be needed, reference should be made to Test Method E70.  
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
This test method is designed to aid in identifying types of coolants. While the ash is primarily due to the inorganic inhibitors used, it is not a measure of the total inhibitor concentration because of the loss of organic inhibitors.
An ash content greater than that stated in Specification D3306 may indicate a salt-based product.
SCOPE
1.1 This test method covers the determination of ash content after ignition of commercial engine coolants and antirusts, as packaged or after use.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific warning statements are given in 7.1 and 7.3.

SIGNIFICANCE AND USE
This test method provides for the qualitative and quantitative determination of common anions in engine coolant in the milligrams per litre to low percent range and requires only a few millilitres or microlitres of sample per test, with results available in less than 30 min. Acceptable levels of chloride and other anions vary with manufacturer's blending specifications and applicable ASTM minimum or maximum specifications.
SCOPE
1.1 This test method covers the chemical analysis of engine coolant for chloride ion by high-performance ion chromatography (HPIC). Several other common anions found in engine coolant can be determined in one chromatographic analysis by this test method.
1.2 This test method is applicable to both new and used engine coolant.
1.3 Coelution of other ions may cause interferences for any of the listed anions. In the case of unfamiliar formulations, identification verification should be performed by either or both fortification and dilution of the sample matrix with the anions of interest.
1.4 Analysis can be performed directly by this test method without pretreatment, other than dilution, as required by the linear ranges of the equipment. Table 1 indicates several applicable anions and approximate detection limits.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to its use.  
TABLE 1 Analytes and Minimum Detection Limits   AnalyteDetection Limit, mg/LA Chloride (Cl−) 2.0 Nitrite (NO2−) 5.0 Bromide (Br) 4.0 Nitrate (NO3−) 7.1 o-Phosphate (HPO4)2−20.0 Sulfate (SO4)2− 8.0 Oxalate (C2O4)2−12.0
A Determined using 100-μL sample volume. Sample diluted 99 + 1 (v/v) with chromatographic eluant 30-μS/cm full scale, suppressed conductivity detection. Dionex AS4ASC column with AG4ASC guard columns. Other systems will require MDL determinations using chosen dilution factors, eluants, columns, and detector.

SIGNIFICANCE AND USE
This test method provides for the qualitative and quantitative determination of common anions in engine coolant in the milligrams per litre to low percent range and requires only a few millilitres or microlitres of sample per test, with results available in less than 30 min. Acceptable levels of chloride and other anions vary with manufacturer's blending specifications and applicable ASTM minimum or maximum specifications.
SCOPE
1.1 This test method covers the chemical analysis of engine coolant for chloride ion by high-performance ion chromatography (HPIC). Several other common anions found in engine coolant can be determined in one chromatographic analysis by this test method.
1.2 This test method is applicable to both new and used engine coolant.
1.3 Coelution of other ions may cause interferences for any of the listed anions. In the case of unfamiliar formulations, identification verification should be performed by either or both fortification and dilution of the sample matrix with the anions of interest.
1.4 Analysis can be performed directly by this test method without pretreatment, other than dilution, as required by the linear ranges of the equipment. Table 1 indicates several applicable anions and approximate detection limits.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to its use.  
TABLE 1 Analytes and Minimum Detection Limits   AnalyteDetection Limit, mg/LA Chloride (Cl−) 2.0 Nitrite (NO2−) 5.0 Bromide (Br) 4.0 Nitrate (NO3−) 7.1 o-Phosphate (HPO4)2−20.0 Sulfate (SO4)2− 8.0 Oxalate (C2O4)2−12.0
A Determined using 100-μL sample volume. Sample diluted 99 + 1 (v/v) with chromatographic eluant 30-μS/cm full scale, suppressed conductivity detection. Dionex AS4ASC column with AG4ASC guard columns. Other systems will require MDL determinations using chosen dilution factors, eluants, columns, and detector.

SCOPE
1.1 This test method covers the determination of the reserve alkalinity of new, unused engine coolants, and liquid antirusts as received, of used or unused aqueous dilutions of the concentrated materials, and of aqueous dilutions of solid antirusts.
1.2 The values stated in SI units are to be regarded as the standard.
1.3 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

ABSTRACT
This standard test method covers the determination of silicon in engine coolant concentrates by atomic absorption spectroscopy. Apparatus and reagents used for this test method include atomic absorption spectrometer, hollow-cathode lamp, reagent grade chemicals, standard silicon solution, ethylene glycol or propylene glycol, and sodium hydroxide. Silicon content shall be determined from an established standard curve and an atomic absorption spectrometer. A nitrous oxide-acetylene flame shall be used.
SCOPE
1.1 This test method covers the determination of silicon in the range from 200 to 500 ppm in engine coolant concentrates by atomic absorption. This method is as accurate and precise as photometric methods, while requiring considerably less operator time and avoiding problems with reagent instability.
1.1.1 Coolants with silicon content outside of this range may be analyzed by this method by suitably adjusting the sample size. Care should be taken to ensure that the glycol content of the working standards corresponds to that of the sample solution being analyzed.
1.2 The values stated in SI units are to be regarded as the standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
The total apparent water in engine coolant concentrate as determined by Karl Fischer titrations consists of the fol-
lowing: (1) water present in the original glycol base; (2) water added (for example, inhibitor solutions); (3) water of hydration of inhibitors (for example, Na 2B4O7·5H2O); ( 4) water formed in the chemical reaction between borate and ethylene glycol, producing boratediol condensate and water; and ( 5) quantitative interference by the reaction of the reagent with inhibitors such as tetraborate or sodium hydroxide.
SCOPE
1.1 These test methods cover the determination of the water present in new or unused glycol-based coolant concentrates using a manual (Test Method A) or an automatic (Test Method B) coulometric titrator procedure.
1.2 Many carbonyl compounds react slowly with the Fischer reagent, causing a fading end point and leading to high results. A modified Fischer reagent procedure is included that minimizes these undesirable and interfering reactions.
1.3 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazards statements see Sections 8 and 16.

SIGNIFICANCE AND USE
This test method provides for the qualitative and quantitative determination of denatonium ion in engine coolant in milligrams per liter to low percent range and requires approximately 100 mL per test, with results available in less than 30 min. Acceptable levels of denatonium vary with manufacturer’s blending specifications and applicable minimum or maximum industry and state specifications. Typically specification ranges from 30 to 50 ppm denatonium ion.
SCOPE
1.1 This test method covers the chemical analysis of engine coolant for denatonium ion by high-performance liquid chromatography (HPLC).
1.2 This test method is applicable to both new and used coolants.
1.3 Coelution of other ions may cause interferences in the detection of the denatonium cation. In the case of unfamiliar formulations, identification verification should be performed by either or both fortification and dilution of the sample matrix with denatonium ion..
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
This test method permits the determination of very low levels of chloride ion in engine coolants containing the common corrosion inhibitor, mercaptobenzothiazole, or related mercaptans, which would normally interfere with the titration by also forming insoluble silver salts with silver nitrate.
SCOPE
1.1 This test method covers the determination of chloride ion in engine coolants in the range from 5 to 200 ppm in the presence of up to 0.6 weight % mercaptobenzothiazole.
1.2 Other materials that react with silver ion will interfere.
1.3 Chloride in engine coolants containing an aryltriazole instead of mercaptobenzothiazole can be determined directly by this test method without pretreatment with hydrogen peroxide.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazards statements are given in Section 7.

SCOPE
1.1 This test method covers the determination of chloride ion in engine coolants in the range from 5 to 200 ppm in the presence of up to 0.6 weight % mercaptobenzothiazole.
1.2 Other materials that react with silver ion will interfere.
1.3 Chloride in engine coolants containing an aryltriazole instead of mercaptobenzothiazole can be determined directly by this test method without pretreatment with hydrogen peroxide.
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazards statements are given in Section .

SIGNIFICANCE AND USE
This test method is designed to aid in identifying types of coolants. While the ash is primarily due to the inorganic inhibitors used, it is not a measure of the total inhibitor concentration because of the loss of organic inhibitors.
An ash content greater than that stated in Specification D 3306 may indicate a salt-based product.
SCOPE
1.1 This test method covers the determination of ash content after ignition of commercial engine coolants and antirusts, as packaged or after use.
1.2 The values stated in SI units are to be regarded as the standard.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific warning statements are given in 7.1 and 7.3.

SCOPE
1.1 This test method covers the determination of ash content after ignition of commercial engine coolants and antirusts, as packaged or after use.
1.2 Some commercial antirusts are solid products. This procedure applies only to liquid products.
1.3 The values stated in SI units are to be regarded as the standard.
This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. A specific precautionary statement is given in Note 1.