An American National StandardDesignation: D – 96 (Reapproved ) Designation: Manual of Fuels for Volatility Measurement (ASTM Practice. Products (ASTM Practice D). MPMS Chapter Standard Practice for the Sampling and. Handling of Fuels for Volatility Measurements (ASTM. Practice. Last previous edition approved in as D –96(20 –96(). 00). 2 For referenced ASTM standards, visit the ASTM website.

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ASTM D – Free Download PDF

Sco Scope pe 1. Currentt editio Curren edition n approv approved ed June 1, Publis Published hed October Origin Originally ally e5854 approv ed in Last previous edition approved in as D —96 20 —96 D — 96 3. The treatment of samples from the time of collection until they are analyzed requires care and effort to maintain their compositional integrity.

Safety and Health Precautions 5. All equipment should be installed, operated, and maintained in a manner to minimize potential health and safety hazards. The following are general design and construction considerations for sample containers. A means of installing security seals should be e5854. A pressure gage should also be provided. As a minimum there should be one suction port at the lowest point in the container.

Exercise care in the selection of container material as it could affect the test results obtained from the sample.

ASTM D5854 – 96(2015)

Containers acceptable for samples to be tested immediately may not be acceptable for storage of sample. Clear glass bottles may be examined visually for cleanliness and allow for visual inspection of the sample for free water or solid impurities. Some petroleum samples are affected by exposure to sunlight if clear glass is used. In these cases, brown glass bottles may afford the necessary protection.

Exercise care also to ensure that samples containing free or entrained water are not corrosive to the metal. Internally epoxy-lined tin cans may have residual contamination and precaution should be taken to ensure its removal. Other than ensuring the cleanliness, d5845 of these containers presents no unusual concerns.

This is especially a consideration when using plastic for long term storage of certain petroleum products. Clear plastic bottles are unsuitable for samples sensitive to light.

D — 96 6. This practice gives information on the types of containers that have been d5584 satisfactory for tests to determine water separation, copper corrosion, electrical conductivity, thermal stability, lubricity, and trace metal content.

Care must be used when using cork stoppers. Rubber stoppers should never be used. Caps should provide a vapor tight seal. Consideration of closure type is important for samples where vapor loss will affect the test results.

Samples should be protected during storage to prevent weathering or degradation from light, heat, or other potential detrimental conditions. Prior to further use, reusable containers such as cans and bottles should be rinsed with a suitable solvent.

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Use of sludge solvents to remove all traces of sediments and sludge may asmt necessary. When dry, stopper or cap the container immediately.

Normally, it is not necessary to wash new containers. In most applications, it is not desirable f5854 practical to wash these receivers using soap and water as FIG. Those who handle petroleum samples must be familiar with these regulations in addition to their own company ast and procedures.

Handling and Mixing Samples 7.

However, it is recognized that all sampling methods do not permit this nor do requirements to transport and store samples. The number of transfers using intermediate containers between the initial sampling operation and the analytical test should be minimized.

Each use of intermediate containers increases the potential for loss of light hydrocarbons, loss of water due to clingage, or inefficient mixing and contamination of the sample from external sources including weather.

When analytical tests are performed on individual samples, which is the recommended procedure, the test results are generally averaged. Depending on the particular application, the results may be averaged arithmetically or on a volumetrically proportional basis according to the proportion of the total petroleum which the sample represents.

When a composite is required, it must consist of proportional parts from each zone if it is for a single tank. If the composite is for multiple tanks, it must consist of proportional parts from each tank sampled. Therefore, samples to be composited should be submitted to the laboratory along with a list of each tank and the volume represented by each sample.

The method of compositing should be documented and care taken to preserve the integrity and representativeness of the composite sample. Sample Mixing Methods 8. These categories vary greatly in severity depending on the type of analytical test to be conducted and the characteristics of the sample.

The following is a brief discussion of each category: Power mixers may entrain air into the sample that could affect certain analytical tests. Loss of vapor normally associated with rise in temperature may also occur which could affect tests results for water, RVP, and density.

These mixers can be used on a variety of different types and sizes of sample containers. Non-aerating or highspeed shear mixers are examples of insertion mixers. Insertion mixers may also be of a circulating loop design where a suction port is inserted into the sample container and the sample is circulated externally by means of a pump through a static mixer and discharged back into the sample container through a dispersal system.

The mixer may be an integral part of a stationary sample receiver or a stand-alone unit used for portable sample receivers.

ASTM D5854

Samples should not be mixed where the analytical tests to be conducted may be affected by air which could be induced by power mixing or shaking. Selection of Sample Mixing Method 9.

The degree of mixing depends on the type of transfer being made, the analytical test to be conducted and the characteristics of the sample.

Power mixing is also required when the sample has been transported or stored in either a primary or intermediate container. Static sample removed from a storage tank; that is, thief to analytical glassware, at time of sampling. However, when such a sample is stored or transported in the extracting device, mixing is required. Before its use, each power mixer design and sample container combination must be tested and proven to be effective.


This annex presents the calculation of sample preparation precision, together with a sample calculation. The following annexes outline mixing procedure acceptance testing and present recommended forms for recording the results of such testing. Tests are then conducted to see if analytical water test results agree with the known baseline water plus the known water added without affecting density of the total mixture by loss of light ends.

First, there must be repeatability between the three test specimens. Second, the system must be shown to be effective or free of bias. If repeatability or system bias is not acceptable, identify and correct the problem and then proceed with re-testing. Values in Column B are calculated from the larger of 0. It is felt that the data is sufficient to provide a reasonable guideline for the industry at this time. In the case of insertion mixers, each mixer must be reevaluated for any change in type of petroleum liquid, volume in the sample container, type of sample container, change in mixing conditions such as mixing speed or mixing time and increase in free water level.

Other water test methods are acceptable. The volume of test specimen D — 96 will therefore need to be adjusted accordingly, if the centrifuge or distillation methods are used. Regardless of the test method used for water in the acceptance test, it is recommended that the acceptance test results be validated using the water test method normally used to determine water content.

Fill the container to the selected level with petroleum liquid. The petroleum liquid used in the acceptance tests should contain no free water. The suggested mixing time for constant speed circulation mixers is 5 min.

For analytical tests using volumetrics, non-aerating shear mixers should be used. Calculate the average water content to the nearest 0. To add water to sample volumes less than 1 L, use a syringe. It is preferable to use a needle that will reach to the bottom of the container. A beaker may be used to add water to sample containers larger than 1 qt. Exercise care to prevent a rise in temperature that would cause liquid or foam to boil from the sample container.

To prevent a boil-over, it may be necessary to place the sample container in an ice bath. A change in one of the other conditions is then necessary. D — 96 FIG. These systems need to be evaluated at installation and reevaluated with changes in petroleum liquid, increase in free water concentration, or minimum and maximum sample volume. The test liquid should contain no free water. After 5 min and while the mixer is running, draw three test specimens.

Calculate the average baseline water content to the nearest 0.

If formation water is used, the sediment and salt content must be determined. At intervals of 5 min, continue to draw sets of three test specimens for a total of 15 min mixing time.