12 PROPOSED ADMINISTRATIVE RULES

 

 

ORR # 2002-054 DEPARTMENT OF AGRICULTURE

LABORATORY DIVISION

 

REGULATION NO. 564. AUTOMOTIVE GASOLINE PURITY, ADDITIVES, AND GRADING

 

Filed with the Secretary of State on

These rules take effect 7 days after filing with the Secretary of State

 

(By authority conferred on the director of the department of agriculture by section 3 of Act No. 44 of the Public Acts of 1984, being '290.643 of the Michigan Compiled Laws)

 

R  285.564.1,  R  285.564.2,  R  285.564.3,  R  285.564.4,  R  285.564.5,  R  285.564.6,  R  285.564.7,  R

285.564.8,  R  285.564.10,  R  285.564.11  and  R  285.564.13  of  the  Michigan  Administrative  Code  are amended and R 285.564.9 is rescinded as follows:

 

R 285.564.1 Definitions.

Rule 1. (1) As used in these rules:

(a)    "Act" means Act No. 44 of the Public Acts of 1984, being §290.641 et seq. of the Michigan Compiled Laws.

(b)   "Antiknock index (AKI)" means (RON + MON)/2.

(c)    "ASTM" means the scientific and technical organization founded for the development of standards and located at 1916 Race Street, Philadelphia, PA 19103 100 BARR HARBOR DRIVE, W. CONSHOHOCKEN, PA 19428-2959.

(d)   "Maximum phase separation temperature" means the temperature of a gasoline containing  alcohol which retains water in solution or in a stable suspension.

(e)    "Motor octane number (MON)" means a knock characteristic of automotive gasoline determined by use of standard procedures on a motor engine.

(f)    "Research octane number (RON)" means a knock characteristic of automotive gasoline determined by use of standard procedures on a research engine.

(2)      The terms defined in the act have the same meanings when used in these rules.

 

R 285.564.2 Permissible oxygen content in gasoline; gasoline clarity.

Rule 2. (1) The calculated oxygen content permitted in any gasoline sample shall not exceed 3.7% by weight. The percentage of oxygen by weight shall be calculated on the basis of the oxygenate added per 1% volume, without regard to the actual gravity of the finished gasoline, as listed in the following table:

Table 1

 

 

Oxygenate added	Percentage by Weight of oxygen per         1% Volume oxygenate
Methanol	.53%
Ethanol	.37%
Tertiary butyl alcohol	.23%
Methyl-tertiary butyl ether	.18%

 

The following are examples of calculated oxygen equivalents:

(a)    Gasoline having 10% by volume ethanol. Oxygen by weight: 10 x .37 =3.7%.

(b)   Gasoline having 4 1/2% by volume methanol and 4 1/2% by volume tertiary butyl alcohol. Oxygen by weight: 4.5 x .53 + 4.5 x .23 = 3.4%.

(c)    Gasoline having 11% by volume methyl-tertiary butyl ether and 3% by volume methanol. Oxygen by weight: 11 x .18 + 3 x .53 = 3.6%

The department shall provide oxygen equivalents for oxygenates not listed in table 1 upon request, which shall be based upon gasoline with a specific gravity of .7412 (6.17 pounds per gallon) at 60 degrees Fahrenheit.

BEGINNING JUNE 1, 2003, THERE SHALL NOT  BE INTENTIONAL ADDITION OF METHYL TERTIARY BUTYL ETHER (MTBE) TO THE GASOLINE.

(2)       Gasoline shall be visually free of undissolved water, sediment, and suspended matter; and IT shall be clear and bright at the ambient temperature of OR 70 degrees Fahrenheit (21 DEGREES CELSIUS), WHICHEVER IS HIGHER.

(3)         THE FINISHED FUEL SHALL BE FREE OF ANY ADULTERANT OR CONTAMINANT THAT MAY RENDER THE FUEL UNACCEPTABLE FOR ITS COMMONLY USED APPLICATIONS.

 

R 285.564.3 Gasoline grades.

Rule 3. (1) There shall be 6 uniform grades of gasoline as follows:

(a)    Unleaded “SUBREGULAR” WITH AN AKI OF 85 OR ABOVE.

(b)   Unleaded “REGULAR” WITH AN AKI OF 87 OR ABOVE.

(c)    Unleaded premium “MIDGRADE 88” WITH AN AKI OF 88 OR ABOVE.

(d)  Leaded subregular “MIDGRADE 89” WITH AN AKI OF 89 OR ABOVE.

(e)  Leaded regular “PREMIUM” WITH AN AKI OF 90 OR ABOVE.

(f) Leaded premium “PREMIUM 91” WITH AN AKI OF 91 OR ABOVE

(g)  “PREMIUM 92” WITH AN AKI OF 92 OR ABOVE

(h)  “PREMIUM 93” WITH AN AKI OF 93 OR ABOVE

(i)  “PREMIUM 94” WITH AN AKI OF 94 OR ABOVE

(2)  The following are 2 special grades of gasoline which shall meet the specifications of R 285.564.7(2): Unleaded special.

Leaded special.

(3)   The special grades of gasoline may be offered for sale if listed with and approved by the department. To apply for listing, the refiner or blender shall provide the department with the gasoline brand name, the grade specifications, and a copy of the complete test results for all applicable standards specified in these rules and other tests as required by the department.

 

R 285.564.4 Grades of gasoline; specifications.

Rule 4. All uniform and special grades of gasoline shall meet the following specifications:

 

 

(a)  The test method for alcohols OXYGENATES shall be gas chromatography ASTM STANDARD D5599-

95. If the total amount of any alcohol contained is 1% by volume or greater, the pump shall be required to be posted with an alcohol notice. Gasoline containing alcohol shall meet all other specifications contained in these rules. BEGINNING JUNE 1, 2003, THERE SHALL NOT BE INTENTIONAL ADDITION OF METHYL TERTIARY BUTYL ETHER (MTBE) TO THE GASOLINE.

(b)   The test method for corrosion shall be ASTM standard D 130-83 94. Copper strip corrosion shall not exceed No. 1 on the test scale specified in test method ASTM standard D 130-83 94.

(c)  The test method for distillation range shall be ASTM standard D86-82 00. In addition, all of the following provisions apply to the distillation range:

(i).       The 10% evaporated temperature shall not exceed any of the following:

(A)             One hundred and twenty-two degrees Fahrenheit during the months of January, February, March, November, and December.

(B)              One hundred and thirty-one degrees Fahrenheit during the months of April, May, September, and October.

(C)              One hundred and forty FIFTY EIGHT degrees Fahrenheit during the months of June, July, and August.

(D)             During the transition months of March, APRIL, May, September, and November, it shall be permissive to use the next higher evaporated temperature specification.

(i).       The 50% evaporated temperature shall BE:

(A)  not be less than 170 ONE HUNDRED AND FIFTY SEVENTY degrees fahrenheit and shall not exceed any of the following (A) two hundred and thirty degrees fahrenheit during the months of January, February, March, November, and December.

(C)   NOT LESS THAN ONE HUNDRED AND SEVENTY DEGREES FAHRENHEIT AND SHALL NOT EXCEED Two hundred and forty FIFTY degrees Fahrenheit during the months of June, July, and August During the transition months of March, May, September, and November, it shall be permissive to use the next higher evaporated temperature specification.

(ii).      The 90% evaporated temperature shall not exceed:

(A)    365 THREE HUNDRED AND SIXTY FIVE degrees fahrenheit DURING THE MONTHS OF JANUARY, FEBRUARY, MARCH, OCTOBER, NOVEMBER, AND DECEMBER.

(B)   THREE HUNDRED AND SEVENTY FOUR DEGREES FAHRENHEIT DURING THE MONTHS OF APRIL, MAY, JUNE, JULY, AUGUST, SEPTEMBER.

(iii).         The end point shall not exceed 437 FOUR HUNDRED AND THIRTY SEVEN degrees fahrenheit. (iv).         The residue shall not exceed 2%.

(v)   THE DRIVEABILITY INDEX SHALL BE DERIVED USING ASTM D4814-01a (ALL DIGITS IN THE VALUES ARE SIGNIFICANT DIGITS). THE DRIVEABILITY INDEX AT THE REFINERY AND TERMINALS SHALL NOT:

(A)             EXCEED 1200 DEGREES FAHRENHEIT DURING THE MONTHS OF JUNE, JULY AND AUGUST.

(B)              EXCEED 1220 DEGREES FAHRENHEIT DURING THE MONTHS OF APRIL, MAY, SEPTEMBER, AND OCTOBER.

(C)              (C) EXCEED 1250 DEGREES FAHRENHEIT DURING THE MONTHS OF JANUARY, FEBRUARY, MARCH, NOVEMBER, AND DECEMBER.

 

 

 

 

 

 

 

Table 2

(D)             (D) The test method for existent gum shall be ASTM standard D 381-80 99.The existent gum shall not exceed 5.0 mg per 100.0 ml.

(E)              (E) For the test method for maximum phase separation temperature SHALL BE ASTM D6422 see R 285.564.8. The maximum temperature for phase separation of gasoline containing alcohol shall be 1 of the following temperatures listed in table 2.

 

Lower Peninsula
Month	Maximum   temperature       for   phase   separation degrees Fahrenheit (CELSIUS)
January	0 (-18)
February	1 (-17)
March	10 (-12)
April	27 (-3)
May	34 (1)
June	45 (7)
July	50 (10)
August	48 (9)
September	41 (5)
October	32 (0)
November	21 (-6)
December	7 (-14)

 

Upper Peninsula
Month	Maximum   temperature       for   phase   separation degrees Fahrenheit (CELSIUS)
January	-6 (-21)
February	-4 (-20)
March	5 (-15)
April	21 (-6)
May	30 (-1)
June	43 (6)
July	48 (9)
August	48 (9)
September	39 (4)
October	30 (-1)
November	16 (-9)
December	0 (-18)

 

(g)(F) The test method for Reid vapor pressure for gasoline AND GASOLINE OXYGENATE BLENDS SHALL BE ASTM D6378-99e1 not containing alcohol shall be ASTM standard D 323-82.

For gasoline containing alcohol, see R 285.564.9. The Reid THE vapor pressure shall not exceed any of the following:

 

 

(i). Sixteen and one-half pounds per square inch during the months of  January,  February,  March, November, and December.

(iii).  Eleven and one-half TEN pounds per square inch during the months of June, July, and August EXCEPT AS PROVIDED FOR IN SECTION 3 OF P.A. 44 AND REGULATION 561, DISPENSING FACILITY REID VAPOR PRESSURE.

FOR GASOLINE NOT CONTAINING 9-10 % ALCOHOL, THE VAPOR PRESSURE SHALL NOT EXCEED ANY OF THE FOLLOWING:

(i). FIFTEEN AND ONE-HALF POUNDS PER SQUARE INCH DURING THE MONTHS OF JANUARY, FEBRUARY, MARCH, NOVEMBER, AND DECEMBER.

(ii). THIRTEEN AND ONE-HALF POUNDS PER SQUARE INCH DURING THE MONTHS OF APRIL, MAY, SEPTEMBER, AND OCTOBER.

(iii). NINE POUNDS PER SQUARE INCH DURING THE MONTHS OF JUNE,  JULY,  AND AUGUST EXCEPT AS PROVIDED FOR IN SECTION 3 OF P.A. 44 AND REGULATION 561, DISPENSING FACILITY REID VAPOR PRESSURE.

(j) (G) The test method for the vapor-liquid ratio for gasoline which does not contain alcohol or ether shall be ASTM standard D 2533-82 5188-99.

For gasoline containing alcohol or ether, or both, see R 285.564.10 for a reference only. A proven test method which does not require complex health safeguards is not currently available. R 285.564.10 will be replaced by a standard when a proven test method is approved by ASTM. For gasoline not containing alcohol or ether or alcohol and ether, the test temperature at which the vapor-liquid ratio is a maximum of 20 to 1 shall be 1 of the following:

(i).    One hundred and five degrees Fahrenheit during the months of January, February, March, November, and December.

(ii). One hundred and sixteen degrees Fahrenheit during the months of April, May, September, and October.

(iii). One hundred and twenty-four degrees Fahrenheit during the months of June, July, and August, AND SEPTEMBER.

(iv).  During the transition months of March, May, September and November, it shall be permissive to use the next higher temperature specifications.

 

R 285.564.5 Grades of leaded gasoline; additional specifications.

Rule 5. In addition to the specifications listed in R 285.564.4, all uniform and special grades of leaded gasoline shall meet the following specifications:

(a) The test method for lead content shall be ASTM standard D 3237-79 5185-97,atomic absorption spectrometry. Leaded gasoline may contain lead compounds not to exceed 4.2 grams of lead per gallon in any sample .

(b) The test method for sulfur shall be ASTM standard D 2622-82 5453-00, x-ray spectrography. The sulfur content shall not exceed 0.15% by weight.

 

R 285.564.6 Grades of unleaded gasoline; additional specifications.

Rule 6. In addition to the specifications listed in R 285.564.4, all uniform and special grades of unleaded gasoline shall meet the following specifications:

 

 

(a)    The test method for lead content shall be ASTM standard D 3237-79 5185-97, atomic absorption spectrometry. There shall be no intentional addition of lead compounds to unleaded ANY UNIFORM GRADE OF gasoline. Any single sample shall contain not more than 0.05 gram (50 milligrams) of lead per gallon.

(b)   The test method for sulfur content shall be ASTM standard D  2622-82 5453-00,x-ray spectrography. Sulfur shall not exceed 0.10% by weight.

 

R 285.564.7 Antiknock index standard.

Rule 7. (1) All uniform grades of gasoline shall meet the specified standard for antiknock index (octane) as follows:

(a)  For leaded automotive gasolines, the following standards apply: (i).       Subregular: not less than 87 AKI.

(ii).          (ii) Regular: not less than 89 AKI. (iii).                (iii) Premium: not less than 93 AKI.

(b)  For unleaded automotive gasoline, the following standards apply: (i).      Subregular: not less than 85.0 85 AKI.

(ii)                                  Regular: not less than 87.0 87 AKI and not less than 82.0 82 MON.

(iii)         MIDGRADE 88: NOT LESS THAN 88.0 AKI.

(iv)        MIDGRADE 89: NOT LESS THAN 89.0 AKI.

(iii) (v) Premium: not less than 90.0 90 AKI.

(vi)                              PREMIUM 91: NOT LESS THAN 91.0 AKI

(vii)                           PREMIUM 92: NOT LESS THEN 92.0 AKI

(viii)                        PREMIUM 93: NOT LESS THEN 93.0 AKI

(ix)                              PREMIUM 94: NOT LESS THEN 94.0 AKI

(2) All special grades of gasoline shall meet the specified standard for antiknock index as follows: For leaded gasoline: not less than 95 AKI.

For unleaded gasoline: not less than 92 AKI.

(3)  The test method for antiknock index shall be ASTM standard D 2700-84 99 for a motor engine and ASTM standard D 2699-84 99 for a research engine.

(4)  (3) The formula for determination of the antiknock index shall be AKI =(RON + MON) ¸ 2.

 

285.564.8 Maximum phase separation temperature ; test method.

Rule 8. (1) The test method for maximum phase separation temperature shall be  as follows: ASTM TEST METHOD D6422.

(a)Rinse out the sample container with some of the fuel to be tested. Drain.

(b)Pour about 40 ml of the fuel into the sample container. The precise amount is not critical, but it must be enough to submerge the thermometer bulb adequately, without being so much as to require an excessive amount of cooling time.

(c)Seal the sample container. Locate a thermometer of the appropriate temperature range with the bulb approximately at the center of the fuel sample.

(d)   Cool the sample by intermittent immersion in or circulation of the coolant. The fuel is either stirred continuously or vigorously shaken. Starting at a temperature about 30 degrees Fahrenheit above the test temperature, cool the sample at a maximum rate of 4 degrees Fahrenheit per minute to the temperature given in table 2 for the water tolerance required. If phase separation is observed before reaching the test temperature, the cooling haze point temperature is recorded. Then the sample is allowed to warm while

 

 

being shaken frequently or stirred and a warming haze point temperature is recorded. The cooling and warming temperatures are averaged to determine the actual haze point. The cooling and warming haze point temperatures may be repeated for improved accuracy.

(e)Report "Pass" if no separation occurs at the specified temperature for the water tolerance class required; otherwise, note the temperature for phase separation and report "Fail."

(2)  The apparatus for testing maximum phase separation temperature shall be as follows:

(a)The sample container shall be any glass container of about 100 ml capacity capable of accommodating a thermometer.

(b)The thermometers shall meet the requirements of ASTM specification E1, with a range appropriate to the test requirement.

(c)The cooling bath may be of similar dimensions to those specified in ASTM standard D 2500, section 4.7, and shall be provided with a jacket, disc, and gasket as specified by sections 4.4 to 4.6 of ASTM standard D2500, filled with an equal volume mixture of water and permanent antifreeze, and provided with refrigeration coils capable of reducing its temperature to minus 40 degrees Fahrenheit. Any bath of adequate size maybe used.

(3)   In this test, the sample of fuel is cooled slowly to its expected use temperature and is observed for phase separation. The apparatus of ASTM standard D 2500 or a dry ice/isopropyl alcohol bath may be used. The procedure of ASTM standard D 2500, in which the sample is cooled rapidly to the test temperature by immersion in a bath that is maintained at a considerably lower temperature, shall not be used due to the large temperature gradient employed and because phase separation in gasoline containing alcohol has a relatively long but unpredictable induction period.

(4)  Some gasoline containing alcohol has a very limited ability to retain water in solution or in stable suspension. If the amount of water in the blend exceeds this limit, the fuel will separate into a lower oxygenate-rich aqueous phase and an upper oxygenate-lean hydrocarbon phase. The most important factor governing the ability of a specific fuel to retain water without such separation is its temperature. This test method is intended to determine the maximum temperature at which the fuel will separate. The tenth percentile 6-hour minimum temperatures or 50degrees Fahrenheit, whichever is lower, for the time of year and geographic area of the state in which the fuel may be used are specified in this rule. These temperatures represent the maximum temperatures above which the fuel blend shall not separate into 2 distinct phases. In this test, actual separation of the sample into 2 distinct phases separated by a single common boundary, which may consist of a layer of emulsion, is the criterion for failure. Formation of a haze without such separation into distinct phases shall not be cause for rejection.

 

285.564.9  Reid vapor pressure test method for gasoline containing alcohol. RESCINDED.

Rule 9. (1) The test method for Reid vapor pressure for gasoline containing alcohol shall be as follows:

(a)With everything in readiness, remove the chilled sample container from the bath, dry it with absorbent material, uncap it, and dry and insert the chilled transfer apparatus as shown in Figure 1. Quickly place the chilled fuel chamber, in an inverted position, over the sample delivery tube of the transfer apparatus. Invert the entire system rapidly so that the fuel chamber is upright, with the end of the delivery tube touching the bottom of the fuel chamber. Fill the fuel chamber to overflowing. Withdraw the delivery tube from the fuel chamber while allowing the sample to continue flowing up to the moment of complete withdrawal.

(b)Make provision for suitable collection and disposal of the overflowing fuel to avoid a fire hazard.

(c)Immediately remove the air chamber from the water bath and immediately dry the exterior of the chamber with absorbent material, giving particular care to the connection between the air chamber and the fuel chamber. Remove the stopper after drying and immediately couple the 2 chambers. Not more than 10 seconds shall elapse in coupling the 2 two chambers.

 

 

(d)   When the air chamber is removed from the water bath, is dried, and the stopper is removed, connect it to the fuel chamber without undue movements through the air which could promote the exchange of room temperature air with the 100-degree Fahrenheit air in the chamber.

(e)Turn the assembled vapor pressure apparatus upside down to allow the sample in the fuel chamber to run into the air chamber. With the apparatus still inverted, shake it vigorously 8 times in a direction parallel to the ength of the apparatus. With the gauge end up, immerse the assembled apparatus in the bath, maintained at 100 degrees Fahrenheit, plus or minus0.2 degrees Fahrenheit, in an inclined position so that the connection of the fuel and air chambers is below the water level and may be carefully examined for leaks. If no leaks are observed, further immerse the apparatus to at least 1 inch above the top of the air chamber. Observe the apparatus for leakage throughout the test. Discard the test at any time a leak is detected.

(f)    Liquid leaks are more difficult to detect than vapor leaks. Because the coupling between the chambers is normally in the liquid section of the apparatus, give the coupling particular attention.

(g)   After the apparatus has been immersed in the bath, check the remaining sample for phase separation. If the sample is contained in a glass container, this observation can be made before sample transfer. If the sample is contained in a nontransparent container, shake the sample vigorously for 5 seconds and then immediately pour a portion of the remaining sample into a clear glass container. Immediately after shaking this sample again for 5 seconds, observe the sample for phase separation. If this sample is not clear and bright and free of a second phase, discard the test and the sample.

(h)   After the assembled vapor pressure apparatus has been immersed in the bath for not less than 5 minutes, tap the pressure gauge lightly and observe the reading. Withdraw the apparatus from the bath and repeat the procedure specified in subdivision (e) of this subrule. At intervals of not less than 2 minutes, perform the procedure specified in subdivision (e) of this subrule until a total of not less than 5 shakings and gauge readings has been made; continue thereafter, if necessary, until the last 2 consecutive gauge readings are constant, indicating equilibrium attainment. These operations normally require 20 to 30 minutes. Read the final gauge pressure to the nearest 0.05 pounds per square inch for gauges with intermediate graduations of 0.1 pounds per square inch or less and to the nearest 0.1 pounds per square inch for gauges with graduations of 0.2to 0.5 pounds per square inch, and record the value as the uncorrected vapor pressure of the sample. Without undue delay, remove the pressure gauge and, without attempting to remove any liquid which may be trapped in the gauge, check its reading against that of the manometer while both are subjected to a common steady pressure which is not more than 0.2 pounds per square inch different from the recorded uncorrected vapor pressure. If a difference is observed between the gauge and manometer readings, the difference shall be added to or subtracted from the uncorrected vapor pressure recorded for the sample being tested, and the resulting value shall be recorded as the vapor pressure of the sample.

(i)     Cooling the assembly before disconnecting the gauge will facilitate disassembly and reduce the amount of hydrocarbon vapors released into the room.

(j)Disconnect the air chamber from the fuel chamber. Drain the sample from the air and fuel chambers as completely as possible into a dry 8-ounce clear glass bottle. Seal the bottle and shake it vigorously for 5 seconds. If the sample is clear and bright and free of a second phase, note this observation and record that the test is valid. If the sample is not clear and bright and free of a second phase, immerse the bottle in the100-degree Fahrenheit water bath up to about 1 inch above the top of the sample level for 15 minutes in order to heat the sample to the test temperature. Remove the sample from the water bath and immediately shake it vigorously for 5 seconds and observe the sample. If the sample is not clear and bright and free of a second phase, note this observation and record that the test is not valid because of phase separation. A fuel that is not clear and bright and free of a second phase at this point of the test indicates that the fuel was contacted with sufficient water to exceed the water tolerance of the fuel during the test procedure. Water

 

 

can most likely get into the test chambers during preparation of the fuel and air chambers or assembly of the air and fuel chambers, especially if water baths are used for these procedures.

(k)Thoroughly purge the air chamber of residual sample by filling it with warm water above 90 degrees Fahrenheit and allowing it to drain. Repeat this purging not less than 5 times. After disconnecting the pressure gauge from its manifold connection with the manometer, remove trapped fluid in the Bourdon tube of the gauge by repeated centrifugal thrusts. This may be accomplished in the following manner: hold the gauge between the palms of the hands with the right hand on the face side and the threaded connection of the gauge forward. Extend the arms forward and upward at an angle of 45 degrees with the coupling of the gauge pointing in the same direction. Swing the arms downward through an arc of about 135degrees so that the centrifugal force aids gravity in removing the trapped liquid. Repeat this operation 3 times to expel all liquid. Purge the pressure gauge by directing a small jet of air into its Bourdon tube for not less than 5 minutes. Rinse both chambers and sample transfer connection several times with petroleum naphtha, then several times with acetone, then blow dry using dried air. Stopper the fuel chamber and place it in the refrigerator or an ice water bath for the next test.

(l)     If the purging of the air chamber is done in a bath, be sure to avoid small and unnoticeable films of floating sample by keeping the bottom and top openings of the chamber closed as they pass through the water surface.

(2)Gross errors can be obtained in vapor pressure measurements if the prescribed procedure is not followed carefully. The following precautions shall be followed:

(a)Check all gauges against a manometer after each test in order to ensure high precision of results. Read all gauges while the gauges are in a vertical position and after tapping them lightly.

(b)Shake the container vigorously to ensure equilibrium of the sample with the air in the container. (c) Check the apparatus before and during each test for both liquid and vapor leaks.

(d)   Because initial sampling and the handling of samples will greatly affect the final results, employ the utmost precaution and the most meticulous care to avoid losses through evaporation and even slight changes in composition. In no case shall any part of the apparatus itself be used as the sample container previous to actually conducting the test.

(e)Thoroughly purge the pressure gauge, the fuel chamber, and the air chamber to be sure they are free of residual sample. This is most conveniently done at the end of the previous test. It is important to remove all water from the apparatus before cooling the gasoline chambers and heating the air chamber. In high humidity conditions, be alert for and avoid condensation on the transfer connection and interior walls of  the apparatus.

(f)            Carefully observe the requirements of subrule (1)(c) of this rule.

(g)           Shake the apparatus vigorously as directed in subrule (1)(e) of this rule in order to insure equilibrium.

(3)The vapor pressure shall be reported in pounds-force per square inch without references to temperature to the nearest 0.05 pounds per square inch for gauges with intermediate graduations of 0.1 pounds per square inch or less or to the nearest 0.1 pounds per square inch for gauges with graduations of 0.2 to 0.5 pounds per square inch after correcting for any difference between the gauge and manometer.

(4)           Figure 1 reads as follows:

**** For Figure 1 see attached file labeled "Figures" ****

(5)The apparatus for testing the Reid vapor pressure shall be as described in annex Al of ASTM standard D 323-82.

(6)           Reagent grade chemicals shall be used in all tests. Other grades maybe used if it is first ascertained that the reagent is of a sufficiently high purity to permit its use without lessening the accuracy of the determination. Acetone and naphtha are extremely flammable. Use with extreme caution.

 

 

(7)   The extreme sensitivity of vapor pressure measurements to losses through evaporation and the resulting changes in composition is such as to require the utmost precaution and the most meticulous care in the handling of samples. All of the following provisions apply to all samples for vapor pressure determinations:

(a)The size of the sample container from which the vapor pressure sample is taken shall be 1 liter (1 qt.). It will be 70 to 80% filled with the sample.

(b)Determine vapor pressure as the first test run on a sample. Do not withdraw more than 1 sample from the sample container for this test.

(c)Protect samples from excessive heat before testing.

(d)           Do not test samples in leaky containers. Discard them and obtain new samples. (e) Discard samples that have separated into 2 phases and obtain new samples.

(f) In all cases, cool the sample container and contents to 32 to 34degrees Fahrenheit before the container is opened. To insure sufficient time to reach this temperature, directly measure the temperature of a similar liquid in a like container placed in the cooling bath at the same time as the sample.

(8)           To prepare for the test, all of the following provisions shall be complied with:

(a)With the sample at a temperature of 32 to 34 degrees Fahrenheit, take the container from the cooling bath, wipe dry with an absorbent material, unseal it, and examine its ullage. The sample content, as determined by use of a suitable gauge, shall be equal to 70 to 80% of the container capacity. Discard the sample if its volume is less than 70% of the container capacity. If the container is more than 80% full, pour out enough sample to bring the container contents within the 70 to 80% range. Any sample which is poured out shall not be returned to the container.

(b)With the sample again at a temperature of 32 to 34 degrees Fahrenheit, take the container from the cooling bath; wipe it dry with an absorbent material; unseal it momentarily, taking care to prevent water entry; reseal it; and shake it vigorously. Return it to the bath for a minimum of 2 minutes. Repeat the procedure 2 additional times. Return the sample to the bath and keep it there until the beginning of the procedure.

(c)Observe the apparatus preparation procedure of subrule (1)(k) of this rule, then store the stoppered fuel chamber and the sample transfer connection in a refrigerator or ice water bath for a sufficient time to allow the chamber and the connection to reach a temperature of 32 to 34degrees Fahrenheit. If an ice water bath is used, keep the chamber upright and not immersed over the top of the coupling threads. The transfer connection is inserted into a plastic bag to keep it completely dry during cooling.

(d)   Observe the apparatus preparation procedure of subrule (1)(k) of this rule. Connect the gauge to the air chamber and close the lower opening securely with a dry no. 6 1/2 rubber stopper. Make sure the stopper is inserted far enough to securely close the vent hole in the air chamber connection. Immerse the air chamber to at least 1 inch above it stop in the water bath maintained at 100 degrees Fahrenheit, plus or minus0.02 degrees Fahrenheit, for not less than 20 minutes. Do not remove the air chamber from the water bath until the fuel chamber has been filled with the sample as described in subrule (1)(a) of this rule.

(9)           This method covers the determination of the absolute vapor pressure of gasolines containing alcohol. Because the external atmospheric pressure is counteracted by the atmospheric pressure initially present in the air chamber, the vapor pressure is an absolute pressure at 100 degrees Fahrenheit in pounds-force per square inch. This vapor pressure differs from the true vapor pressure of the sample due to some small sample vaporization and the presence of air in the confined space. The fuel chamber of the vapor pressure apparatus is filled with the chilled sample and connected to the air chamber at 100 degrees Fahrenheit. The apparatus is immersed in a bath at 100 degrees Fahrenheit and is shaken periodically until a constant pressure is observed on the gauge attached to the apparatus. The gauge reading, suitably corrected, is reported as the vapor pressure.

 

285.564.10 Vapor/liquid test method for gasoline containing alcohol or ether.

 

 

Rule 10. (1) The test method for vapor/liquid for gasoline containing alcohol or ether, or both, shall be D 5188- 99 as follows: .

(a)Read and record the barometric pressure.

(b)With the vapor/liquid buret at room temperature or somewhat above and everything in readiness, carry out the following steps as quickly as possible. Take the container from the water cooling bath, wipe dry with an absorbent material, open it, tip it so as to reach the liquid with the hypodermic syringe needle, and partially fill the syringe. Point the needle upward and dispel the contents to eliminate all air bubbles. Immediately refill the syringe from the sample container and check for air or vapor in the syringe.

(c)Mercury in the buret may be somewhat above room temperature due to warming in the previous test, but shall not be so warm as to cause the sample to vaporize when injected. Mercury may be harmful or fatal if inhaled or swallowed.

(d)   Vapor may form if the sample is drawn in too rapidly. If this happens, repeat the sampling with a clean, chilled syringe.

(e)Depress the plunger exactly to the mark for the sample size desired, then, taking care not to disturb the plunger position, insert the needle through the rubber septum full length into the vapor/liquid buret. Depress the plunger all the way to inject the sample and withdraw the needle. Use a 1-ml sample if the highest vapor/liquid ratio expected for the sample is less than 35. For higher vapor/liquid ratios, use a smaller sample sufficient to give 20 to 35 ml of vapor at the highest temperature to be tested.

(f)    Record the volume of sample charged, corrected by means of the calibration specified in subrule (8)(a) and (b) of this rule.

(g)   Transfer the charged buret to the water bath set at the desired temperature and position the buret so that the water level comes above the stopcock barrel.

(h)   As vapor forms in the buret, adjust the height of the leveling bulb to give the desired pressure, normally 760 mm mercury, on the sample. Raise the level of mercury in the reservoir 1.0 mm above the level in the buret for every millimeter of mercury that the barometric pressure is below the desired pressure or lower it by a like amount for every millimeter that the barometric pressure is above the desired pressure.

(i)     With some narrow boiling gasoline fractions, super heating may occur and no vapors are formed in the buret, even after immersion for as long as 15 minutes or more. When vaporization takes place, it does so rapidly and sometimes explosively. With these samples, it is recommended that injection be carried out with warm mercury in the buret so that a few milliliters of vapor are formed immediately after injection. The temperature of the mercury is dependent on the sample composition, but in general shall not be more than 50 degrees Fahrenheit above ambient.

(j)If the difference between the atmospheric pressure in the laboratory and the pressure for which the vapor/liquid measurement is desired is too great for convenient correction by means of the leveling bulb alone, use the mercury-filled manometer described in subrule (6)(e) of this rule to set the pressure. Keep the level of mercury in the leveling bulb the same as that in the buret and apply pressure or vacuum gently to the air space in the leveling bulb as needed to obtain the desired pressure on the manometer.

(k)Without removing the buret from the water bath, shake it sufficiently to agitate the liquid sample, but not so vigorously as to disperse droplets of sample into the mercury. Readjust the height of the leveling bulb, if necessary, to give the desired pressure in the sample. Because of mercury's high density, the use of a cathetometer or similar optical leveling device has been found necessary to minimize pressure errors.

(l)     Read the volume of vapor to the nearest 0.1 ml. Repeat until the volume remains constant for not less than 2 minutes. Record the volume, corrected by means of the calibration specified in subrule (8)(a) and (b)of this rule, the bath temperature, and the pressure.

 

 

(m) Any spilled mercury, and any that may be purged from the equipment, shall be placed in an airtight closed vessel. This recovered mercury maybe sent to a reprocessor, who can provide shipping instructions. Names of mercury reprocessors are available from ASTM headquarters. To minimize spillage, a catch pan that is large enough to contain all the mercury incase of failure shall be placed under the apparatus.

(n)   If the vapor/liquid ratio is also desired at another temperature, either adjust the temperature of the bath accordingly or transfer the buret to another bath at the desired temperature. Repeat the operations described in subdivisions (h) and (k) of this subrule.

(2)  For each determination, calculate the vapor/liquid ratio as follows: Vapor/liquid ratio = A/B where:

A = volume of vapor, ml, and

B = volume of sample charged, ml

(3)  Report the vapor/liquid ratio to the nearest 0.1 unit and the corresponding temperature in degrees Fahrenheit to 0.1 degrees. Also report the pressure in millimeters of mercury if other than 760. If not reported, the pressure is understood to be 760 mm mercury.

(4)  If vapor/liquid ratios have been determined at a series of not less than 3 temperatures, and if values at intermediate temperature or temperatures for intermediate vapor/liquid ratios are desired, proceed as follows: Plot the experimental results in the form of a curve of vapor/liquid ratio versus temperature, smoothing if necessary, on graph paper which can be read easily to 0.1 vapor/liquid and 0.2 degrees Fahrenheit. Read from this curve the desired intermediate vapor/liquid and temperature values. Report vapor/liquid, temperature, and pressure as prescribed in subrule (3) of this rule, but accompany the result with the word "interpolated." Thus, for example, report "vapor/liquid = 15.0interpolated at 127.6 degrees Fahrenheit" or "vapor/liquid = 12.3interpolated at 125.0 degrees Fahrenheit and 665 mm mercury."

(5)  Figures 2 and 3 are as follows:

*** For Figures 2 and 3 see attached file labeled "Figures" **** (6) The apparatus for testing vapor/liquid ratio shall be as follows:

(a)The vapor/liquid buret shall be constructed of borosilicate glass according to the dimensions shown in figure 2. The short bottom arm is closed with a rubber serum bottle stopper, United States Army medical corps type.

(b)There shall be a 250-ml leveling bulb which contains mercury and which is attached to the vapor/liquid buret by rubber tubing as shown in figure 3. The top of the leveling bulb shall be fitted with a drying tube containing mercury vapor absorbent packed between balls of glass wool. This drying tube is used to minimize the escape of mercury vapor.

(c)A cathetometer or similar optical leveling device is suitable for measuring the difference in liquid level between the vapor/liquid buret and the leveling bulb. A millimeter scale may be used to provide a rough estimate.

(d)           The barometer shall be accurate to 0.5 mm mercury.

(e)A mercury manometer with 1-mm divisions is required only for measurements at pressures appreciably above or below the prevailing atmospheric pressure. The manometer shall be connected with rubber tubing to 1 arm of a glass T-tube, the other arms of which shall be connected to the top of the mercury leveling bulb and to a stopcock or pinch clamp.

(f)    The water bath shall be glass, not less than 10.5 inches deep, stirred and thermostatically controlled, capable of being adjusted to any temperature between 100 degrees Fahrenheit and 180 degrees Fahrenheit, and shall maintain the water temperature within plus or minus 0.2 degrees Fahrenheit of the desired temperature.

 

 

(g)   The thermometers shall be precision thermometers having ranges from77 to 131 degrees Fahrenheit and 122 to 176 degrees Fahrenheit.

(h)           The cooling bath shall contain ice and water at 32 to 36 degrees Fahrenheit.

(i)             The hypodermic syringe shall be 0.5 and 1.0-ml Hamilton syringes with Chaney adaptors, fitted with a no.

20 gauge, 2-inch needle.

(j)The calibration accessories shall include an analytical balance accurate to at least  1 mg,  a capillary stopcock, and weighing vials. A calibration stopper for the vapor/liquid buret stopcock, that is, an extra 3- way solid stopcock stopper with an outlet through the end of the stopper, is convenient during calibration.

(7)  Take precautions against loss of volatile material in the sample. The extreme sensitivity of the vapor/liquid ratio to losses through evaporation and to slight changes in composition is such as to require the utmost precaution and the most meticulous care in the handling of samples. Except for the vapor pressure, the vapor/liquid ratio shall be the first test to be run on a sample.

(8)  All of the following provisions apply to the test method for vapor/liquid ratio determination:

(a)The vapor/liquid buret and the hypodermic syringe shall be calibrated and the subsequent experimental readings shall be corrected from the calibration curves obtained.

(b)Fill the hypodermic syringe with air-free distilled water at 77degrees Fahrenheit, expel any air bubbles, and depress the plunger exactly to a calibration mark. Discharge the contents, to the bottom of plunger travel, into a weighing vial and weigh. Repeat at 0.2 ml intervals from0.2 to 1.0 ml and average the results from 2 or more determinations. Calculate the volumes at 32 degrees Fahrenheit from the average weights of water and prepare a calibration curve.

(c)One gram of water at 77 degrees Fahrenheit equals 1.0036 ml volume at 32 degrees Fahrenheit in resistance glass or 1.0038 ml volume at 32degrees Fahrenheit in borosilicate glass.

(d)   Clean the vapor/liquid buret thoroughly, rinse with distilled water, attach a capillary stopcock with rubber tubing snug to the side arm, and fill the system completely with air-free distilled water at 77 degrees Fahrenheit. Calibrate at 5-ml intervals starting from the bottom of the buret stopcock by weighing water drained through the capillary stopcock into weighing vials. Repeat and average for 2 or more determinations. Calculate the volumes at 122 degrees Fahrenheit from the weights of water and prepare a calibration curve.

(e)Use of the calibration stopper described in subrule (6)(j) of this rule, facilitates setting the water level at the bottom of the stopcock.

(f)    One gram of water at 77 degrees Fahrenheit equals 1.0042 ml volume at 122 degrees Fahrenheit in borosilicate glass.

(9)        To summarize this method, a measured volume of liquid fuel at 32 to 40 degrees Fahrenheit is introduced through a rubber septum into a mercury-filled buret. The charged buret is placed in a temperature-controlled water bath. The volume of vapor in equilibrium with liquid fuel is measured at the desired temperature or temperatures and the specified pressure, usually 760 mm mercury. The vapor/liquid ratio is then calculated. If it is desired to know the temperature corresponding to a given vapor/liquid, the vapor/liquid ratio is determined at several temperatures and the selected pressure. The results are plotted and the temperature read at the given vapor/liquid. The tendency of a fuel to vaporize in common automobile fuel systems is indicated by the vapor/liquid ratio of that fuel at conditions approximating those in critical parts of the fuel systems. ASTM standard D 2533-82 is not applicable to fuels containing alcohol, ethers, or other compounds soluble in glycerine. This test method substitutes mercury for glycerine as the confining fluid. A relationship between the vapor/liquid ratio of gasoline containing alcohol or ether and vehicle performance has not been determined.

(10)  To prepare for the test, all of the following provisions shall be complied with:

 

 

(a)Before assembly, thoroughly clean and dry all the equipment, including burets, hypodermic syringes, leveling bulbs, and connecting tubing. Lubricate the buret stopcock with high-vacuum silicone stopcock grease and attach a spring or rubber band to hold securely in place. Thereafter, to clean the buret between tests, rinse thoroughly by flushing with water, then with acetone, and dry with air. Clean the hypodermic syringe and needle with acetone and dry in an air stream. Acetone is extremely flammable. Use with extreme caution.

(b)If a film is noted in the buret, clean it further with chromic acid solution. Chromic acid is a strong oxidizer and a recognized carcinogen. It causes severe burns and in contact with organic material may cause fire.

(c)Connect the leveling bulb to the buret with rubber tubing, fill the bulb with mercury at room temperature, and attach the drying tube containing the mercury vapor absorbent. Fill the buret by raising the leveling bulb. Move the buret up and down to work all air bubbles from the tubing and rubber septum attachment. Raise the mercury level in the buret up through the stopcock and close the stopcock. It is not necessary to completely recharge the apparatus with mercury for subsequent tests. After each test, open the stopcock, lower the leveling bulb, and allow all but a few milliliters of the mercury to flow back into it. Apply a pinch clamp to the rubber tubing as near the buret as possible and remove the buret, to be cleaned for another test. Remove the pinch clamp and dispel a small portion of mercury from the end of the tubing before attaching it to a clean buret. Fill the buret and dispel air bubbles as before. Add mercury to the leveling bulb as needed.

(d)   Assemble the syringe and needle and insert the needle tip in a small rubber stopper. Cover with drained chipped ice or chill by other means to32 to 36 degrees Fahrenheit.

(e)With the sample at a temperature of 32 to 40 degrees Fahrenheit, take the container from the water cooling bath, wipe dry with an absorbent material, unseal it, and examine it for its liquid content, which shall be between 70 and 80% of the container capacity. After the correct liquid content has been assured, reseal the container, shake it vigorously, and return it to the water cooling bath.

(f)    Adjust the water bath to the desired test temperature and maintain at that temperature plus or minus 0.2 degrees Fahrenheit.

 

285.564.11  ASTM standards; adoption by reference.

Rule 11. (1) The department adopts the following standards of the ASTM for gasoline (OR AN ASTM METHOD APPROVED BY THE DEPARTMENT):

(a) D 86 – 82 00.

(b) D 130 – 83 94.

(c) D 323 – 82 6378-99-1. (d) D 381 – 80 99.

(e) D 2533 - 82 5188-99. (f) D 2622 – 82 5453-00. (g) D 2699 – 84 99.

(h) D 2700 – 84 99.

(i)  D 3237 – 79 5599-95.

(2) Copies of these standards may be obtained, at actual printing and mailing cost, by writing to the Department of Agriculture, Food Division ,P.O. Box 30017, Lansing, Michigan 48909 Laboratory Division, 940 Venture Lane, Williamston, Michigan 48895, or, for a fee as specified in this subrule, from the ASTM, 1916 Race Street, Philadelphia, Pennsylvania19103 100 Barr Harbor Drive, W. Conshohocken, PA 19428-2959. The ASTM standards are composed of volumes priced as follows:

Volume 05.01: D 56 to D 1660.....................................$69.00 $186.00.

Volume 05.02: D 1661 to D 2896...................................$69.00 $207.00.

 

 

Volume 05.03: D 2981 to latest...................................$79.00 $196.00.

Most ASTM standards are available as separate copies as follows: 1 to 32 pages....................................................$ 8.00.

33 to 64 pages...................................................$10.00.

65 or more pages.................................................$12.00.

 

R 285.564.13 Waivers granted by United States environmental protection agency; listing.

Rule 13. Gasoline which does not meet the specifications established in R 285.564.4 (c) and (f), but which is permitted by the United States environmental protection agency by regulatory citation at 44 F.R. p. 20777(April 6, 1979) or 47 F.R. p. 14596 (April 5, 1982) pursuant to section 211(f)(4) of the clean air act, 42 U.S.C. S7545, and leaded gasoline made under the same formula with leaded gasoline substituted for unleaded gasoline may be marketed and graded as 1 of the 6 uniform or 2 special grades based upon the AKI. Gasoline marketed under such a valid waiver shall be listed with the department. The listing shall state the gasoline brand name and the grade specification and shall include proof of a valid waiver, a copy of the complete fuel specification, and a copy of the complete test results indicating the fuel meets the specifications.