ASTM D – Free download as PDF File .pdf), Text File .txt) or read online for free. New ASTM Method D With the manufacture of Freon banned by the Montreal Protocol in , the old ASTM method (D ) that used infrared. The FT-IR Environmental Hydrocarbons ASTM D Application Pack contains all of the resources and components necessary to perform efficient analysis of.
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A number in parentheses ashm the year of last reapproval. A superscript epsilon e indicates an editorial change since the last revision or reapproval. Included in this estimation of oil and grease are any other compounds soluble in the solvent. Similarly, this test method de?
It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine D Guide for Good Laboratory Practices2 the applicability of regulatory limitations prior to use. Summary of Test Method 4. The extract is diluted to 50mL and a portion is examined by infrared spectroscopy IR for an oil and grease measurement.
The nonpolar material is measured by infrared spectroscopy. Current edition approved June 1, This test method contains procedures that can assist the analyst in breaking such emulsions. Of those measured, certain ones may be adsorbed by silica gel while others may not.
Those not adsorbed are measured as nonpolar material. Unless otherwise indicated, it is intended that all reagents shall conform to the speci? Other grades may be used, provided it is? Powdered sodium sulfate should not be used because water may cause it to solidify. Mix equal volumes of concentrated HCl and water 8. Wet thoroughly with solvent before using. Prerinse the sample bottle and cap with the solvent prior to sample collection. Do not rinse the sample bottle with the sample to be analyzed.
Fill bottle with minimal headspace to prevent loss of volatile constituants. Do not allow the sample to over? Use the entire sample because removing a portion would not apportion the oil and grease that adheres to the bottle surfaces.
The high probability that extractable matter may adhere to sampling equipment and result in measurements that are biased low precludes the collection of composite samples for determination of oil and grease. Therefore, samples must be collected as grab samples.
If a composite measurement is required, individual grab samples collected at prescribed time intervals may be analyzed separately and the concentrations 7d066. Alternatively, samples can be collected in the?
For example, collect four individual mL samples over the course asgm a day. Do not exceed 50 mL of total solvent during the extraction and rinse procedure. The amount of acid required will be dependent upon the pH and buffer capacity of the sample at the time of collection. If the amount of acid required is not known, make the pH measurement on a separate sample that will not be analyzed. Introduction of pH paper to an actual sample or sample cap may remove some oil from the sample.
To more accurately calculate the?
If the sample is to be shipped by commercial carrier, U. Collect an additional 1 or 2 sample aliquots for the matrix spike and matrix spike duplicate Section Freezing the sample may break the bottle. In a few cases, the composition of the oil and grease in a sample will be known. However, in order to obtain consistent results between sample sets and between laboratories with different wastewater matrices, calibration with the known oil and grease in a sample should not be used in this method.
ASTM D – standard test method by Infrared Determination
Transfer volumes have been rounded for ease of measurement and calculation. It is highly recommended that calibration standards be prepared on a weight basis i. A solution containing equal volumes of isooctane and octanoic acid will have a density of 0. To assure the most accurate concentrations, use the smallest serological pipet or syringe for measurements. The volume should always be greater than 1?
Ideally, a linear calibration curve will be obtained from these standards. As discussed in Section 11, the concentrations of these standards can be adjusted to stay within the linear range of the IR instrument. Cap the bottle and shake well. L for solution density of 0. L of isooctane by the water volume in liters. L of octanoic acid by the water volume in liters. A fresh spiking solution should be prepared weekly or bi-weekly. Calibration NOTE 3—The cell s used for calibration must be initially thoroughly cleaned with solvent and dried prior to beginning the calibration procedure.
To reduce the solvent expense, it may be prudent to use methylene chloride or a solvent other than the solvent used for extraction. However, all traces of methylene chloride or other solvent must be removed so that they do not compromise the measurement. Cool cell to room temperature before use. NOTE 4—For infrared instruments having computer capability, data may be obtained automatically or as described in However, all data must be obtained consistently by one means or the other, not a combination of the two.
The same cell or matched cells should be used throughout the calibration. Take care to avoid insertion of the cell stopper so tightly that the cell could burst from expansion of its contents as it resides in the light beam.
It is desirable to? For double-beam operation, either block the light beam from the reference cell containing solvent or remove the reference cell from the instrument during the intervals between scans in order to protect the solvent from unnecessary warming.
However, place the reference cell in the reference beam during all scans. Rely upon recommendations of the manufacturer for single-beam and infrared?
Also, in relation to infrared? In the procedure below, the IR instrument is calibrated from 0. If the IR instrument cannot be calibrated to 0.
Ideally, the calibration curve obtained will be linear refer to Section If linearity cannot be achieved past a certain concentration, consider that concentration the upper bounds of the calibration and adjust the calibration standards accordingly. If a sample is encountered that exceeds the calibration range, dilute the sample extract to bring the concentration into the calibration range.
A nearly horizontal, straight line should be obtained. If not, check cells for cleanliness, matching, etc. Drain and clean the sample cell. For single-beam and infrared?
After running, drain, and clean the sample cell. Scan as in Obtain the net absorbance for the peak that occurs near cm-1 3. Obtain net values for single-beam and infrared?
Calculate the calibration factor CFx in each of the?
Either the average calibration factor CFm or the calibration curve is used, not both. If calibration is not veri? Weighing will be more accurate. NOTE 5—Use of the sodium sulfate is necessary to prevent water from interfering in the determination. If the sodium sulfate cakes when contacted with the extract,? Remove the solid with a clean spatula, and add about 1 g of fresh sodium sulfate to the? Rewet sodium sulfate with solvent before use. Rinse with a small portion of solvent and discard the rinsate.
NOTE 8—The amount of silica gel needed has been estimated at 3 g for every mg of polar material. However, this amount may be insufficient for some samples.
If there is doubt about whether the amount of silica gel is adequate, the amount needed should be determined by test. Cap with the original cap and shake the sample bottle to rinse all interior surfaces. Pour the solvent into the separatory funnel, rinsing down the sides of the transfer funnel. Vent the funnel slowly to prevent loss of sample.
NOTE 6—Certain types of samples, such as those containing a large amount of detergent, may form an emulsion during the extraction. If emulsion forms between the phases and the emulsion is greater than one-third the volume of the solvent layer, the laboratory should employ emulsion-breaking techniques to complete the phase separation. The optimum technique depends upon the sample, but may include stirring,?
Alternatively, solid-phase extraction SPEcontinuous liquid-liquid extraction, or other extraction techniques may be used to prevent emulsion formation.
If such an emulsion cannot be broken by any attempted means, the test method is not applicable to the problem sample. Do not attempt to proceed since accurate, quantitative results for the test are not obtainable. If the concentration of non-polar material exceeds the calibration range, dilute the extract to bring the concentration within the calibration range.
Keep a record of each dilution for use in Rinse the tip of the separatory funnel, Na2SO4,?