USER’S GUIDE
clastics 3 Dominant clay
3.5 Ratios and Estimates Related to Particle-Size Analysis, Bulk Density, and Water Retention Density, and Water Retention
moderately moist or very moist. Test is most useful only if the full range of color value from air-dry to moderately moist exceeds one unit of color value.
• Ball test.—Quantity of soil is squeezed firmly in palm of hand (5 squeezes) to form ball about 3 to 4 cm in diameter. Procedure is consistent for an individual. Ball is dropped from progressively increasing heights (<100 cm) onto nonresilient surface. If ball flattens and does not rupture, the term “deforms” is used; if ball breaks into 5 or less units, the term “pieces”
is used; and if more than 5 pieces, the term “crumbles” is used.
• Rod test.—Soil material is rolled between thumb and first finger or on surface to form rod 3 mm in diameter or less. Rod must remain intact while being held vertically from an end for recognition as a rod. Maximum length required is 2 cm. If maximum length formed is 2 to 5 cm, rod is weak. If maximum length equals or exceed 5 cm, rod is strong.
• Ribbon test.—Soil material is smeared out between thumb and first finger to form flattened body about 2 mm thick. The minimum length of coherent unit required for recognition of ribbon is 2 cm. If maximum length equals or exceeds 4 cm, ribbon is strong.
Refer to Soil Survey Division Staff (1993) for additional information on these tests and their evaluation.
3.5 Ratios and Estimates Related to Particle-Size Analysis, Bulk
gypsiferous soils reported on an oven-dry weight basis should be converted to include the weight of crystal water in gypsum. The AD/OD ratio is used to convert soil properties to an oven-dry basis. For gypsiferous soils, the AD/OD ratio is converted to a crystal water basis (Nelson et al., 1978). The inclusion of weight of crystal water in gypsum allows the properties of gypsiferous soils to be compared with those properties of nongypsiferous soils. This conversion also avoids the possible calculation error of obtaining >100% gypsum when the data are expressed on an oven-dry basis (Nelson, 1982).
The methods described in this manual are intended for use in the field or office setting with little or no sample preparation (e.g., air-drying). Because it might be important for purposes of the reporting base to use a constant sample weight, the method description for sample weight base is included in this manual.
Procedures and calculations described herein are after the Soil Survey Staff (2014b, methods 3D1, 3D2, and 3D3) and ASTM (2008d, ASTM Standard Test Method D-4643-00). Two alternative procedures for oven-drying are presented as follows: Standard laboratory oven (Soil Survey Staff, 2014b) and microwave (ASTM, 2008d). Two alternative procedures for air-drying soils are presented as follows: Standard laboratory oven (Soil Survey Staff, 2014b) and ambient
temperature (Jones, 2001). For other types of sample collection and preparation procedures, refer to the Soil Survey Staff (2014b).
Summary of Method
A sample is weighed, dried to a constant weight in an oven or microwave, and reweighed. The moisture content is expressed as a ratio of the air-dry to the oven-dry weight (AD/OD). Soil properties of gypsiferous soils that are reported on an oven-dry weight basis are converted to include the weight of the crystal water. When the water content of gypsiferous soils is reported, the crystal water content must be subtracted from the total oven-dry water content. The AD/OD ratio is corrected to a crystal water basis when the gypsum content of the soil is
>1%.
Interferences
Traditionally, the most frequently used definition for a dry soil is the soil mass after it has come to a constant weight at a temperature of 100 to 110 °C, after ASTM Standard Practice 2216-05 (ASTM, 2008e). Many laboratory ovens are not capable of maintaining this prescribed temperature range. Temperatures that are >50 °C may promote oxidation or decomposition of some forms of organic matter.
Samples may not reach a constant weight with overnight drying. Do not add moist samples to an oven with drying samples unless the drying samples have been in the oven for at least 12 to 16 hr. Soil samples may adsorb significant amounts of moisture from the atmosphere after cooling. Prompt weighing, i.e.,
<30 min after samples have cooled, helps to eliminate this problem. During the weighing or drying processes, the nonuniform weight of weighing vessels, sample contamination, or sample loss may lead to erroneous results.
Removal of structural water, most commonly in gypsum, can produce a positive error. When the water content of gypsiferous soils is reported, the
crystal water content must be subtracted from the total oven-dry water content.
Gypsum and hydrous oxides may be affected.
In regards to use of a microwave oven, some notes (ASTM, 2008d) are as follows: The initial power setting may need to be higher than “defrost,” and the proper setting with a particular microwave oven can be determined only through use and experience; soils that contain a high amount of moisture and a large portion of clay take a longer time to dry, with initial time around 12 min; care should be taken to reduce cohesive samples to ¼-in particles and thus speed drying and prevent crusting or overheating of surface while drying the interior;
constant weight is defined as the weight at which further drying will cause <0.1%
additional loss in mass when weighed at specified intervals; the specified
weighing interval for microwave drying is 1 min. The principal objection to use of the microwave for water-content determination has been the possibility of
overheating the soil, thereby yielding a water content higher than would be determined by ASTM Test Method D 2216-05 (ASTM, 2008e). The
recommended drying procedure described in ASTM Test Method D 4643-00 will minimize its effects (ASTM, 2008d).
Safety
Use safety glasses, gloves, and tongs when removing weighing containers from a hot oven. Caution is needed when hot items are handled and when the oven or microwave is used. Follow the safety precautions supplied by the manufacturer of the oven or microwave. A calibration check of the oven should be performed annually as a minimum, or whenever damage or repair occurs.
Highly organic soils and soils containing oil or other contaminates may ignite into flames during microwave drying. Means for smothering flames to prevent
operator injury or oven damage should be available during testing. Fumes given off from contaminated soils or wastes may be toxic, and the oven should be vented thoroughly. Do not use metallic containers in a microwave because arcing and oven damage may result. Do not place test specimen directly on the glass liner tray provided with some microwaves as the concentrated heating of the specimen may result in the glass tray shattering, possibly injuring the
operator. Refer to ASTM Test Method D 4643-00 (ASTM, 2008d) for additional discussion of potential hazards associated with microwave use for drying soils.
Equipment
1. Electronic balance, ±1-mg sensitivity. Refer to Appendix 9.7.
2. Oven, 30 ±5 °C, or alternatively, room with circulating air (21 to 27 °C) 3. Oven, 110 ±5 °C, or alternatively, microwave, with vented chamber. Refer
to Appendix 9.7.
4. Thermometer, 0 to 200 °C
5. Tin dishes, 4.5-cm diameter x 3-cm height, with covers, or alternatively, microwave safe dish
6. Gloves, insulated, heat-resistant (e.g., Clavies Biohazard Autoclave Glove)
7. Tongs, metal, long 8. Glass rod, spatula, knife
9. Oven mitts
10. Heat sink, used to enhance heat dissipation from hot surfaces associated with microwave
11. Safety goggles 12. First-aid kit Reagents
None.
Procedure
1. Air-dry the sample in oven at 30 to 35 °C for 3 to 7 days (Soil Survey Staff, 2014b).
2. Alternatively, air-dry at ambient temperature (21 to 27 °C; 70 to 80 °F) (Jones, 2001). Drying process should be done as promptly and rapidly as possible to minimize microbial activity (mineralization). Time required to bring a soil sample to an air-dried condition is determined by its moisture, organic matter content, and texture. Soils high in clay and/or organic matter require a considerably longer time to bring to an air-dried condition than do sandy-textured soils. Drying can be facilitated by exposing as much surface as possible. Do not exceed 38 °C (100 °F) because
significant changes in the physiochemical properties of the soil can occur at elevated drying temperatures (Jones, 2001). Refer to Jones (2001) for additional information on air-drying at ambient temperature.
3. For AD/OD determination, tare dishes. Record each sample number and associated dish number. Add 10 to 20 g air-dry soil to each moisture dish.
Weigh the dish plus the sample and record the weight. For FM/OD determination, tare dishes. Record each sample number and associated dish number. Add enough moist soil to achieve ≈10 to 20 g sample of air- dry soil. Weigh dish plus sample and record weight. Place sample dish in drying oven set at 110 °C. Allow sample to remain in the oven overnight (12 to 16 hr).
4. Alternatively, for AD/OD determination, tare clean, dry, microwave-safe dishes. Place 10 to 20 g air-dry soil in each dish. Weigh the dish plus the sample and record the weight. For FM/OD determination, add enough moist soil to achieve ≈10 to 20 g sample of air-dry soil. Weigh dish plus sample and record weight. Place sample dish in microwave oven with a heat sink, set power to defrost setting, set timer for 3 min, and start. The 3-min initial time is a minimum. When the microwave stops, remove sample dish from the oven and weigh. Use a small spatula, glass rod, or knife and carefully mix the soil, taking care not to lose any soil. Return the container to the microwave and reheat 1 min. Remove, weigh, and again mix. Repeat the process until a constant weight is achieved. Discard sample. The ASTM (2008d) recommendations for determining required sample size are as follows:
Sieve retaining not more than about 10%
of sample
Recommended mass of moist
specimen No. 10 (2.0 mm) 100 to 200 g No. 4 (4.75) 300 to 500 g
¾” (19 mm) 500 to 1000 g
5. Remove sample dish and allow it to cool before reweighing. Record weight.
6. Do not allow sample dish to remain at room temperature for >30 min before reweighing.
7. Discard sample.
8. Refer to the calculations for the correction for crystal water of gypsum in gypsiferous soils.
Calculations
Calculations for AD/OD ratio are as follows:
AD/OD ratio = AD/OD where:
AD = (Air-dry weight) − (Tin tare weight) OD = (Oven-dry weight) − (Tin tare weight) H2O = [(AD − OD) x 100] / OD
where:
H2O = % Water content
AD = (Air-dry weight) − (Tin tare weight) OD = (Oven-dry weight) − (Tin tare weight)
Calculations for FM/OD ratio are as follows:
FM/OD ratio = FD/OD where:
FM = (Field-moist weight) − (Tin tare weight) OD = (Oven-dry weight) − (Tin tare weight)
Calculations for gypsum H2O correction are as follows:
(AD/OD)c = (AD/OD)uc / [1 + (Gypsum x 0.001942)]
where:
AD/ODc = Air-dry/oven-dry ratio, corrected basis, gypsiferous soils AD/ODuc = Air-dry/oven-dry ratio, uncorrected basis
Gypsum = % Gypsum uncorrected
H2Oc = [H2Ouc − (Gypsum x 0.1942)] / [1 + (Gypsum x 0.001942)]
where:
H2Oc = % Water content, corrected basis, gypsiferous soils H2Ouc = % Water content, uncorrected basis
Gypsum= % Gypsum uncorrected AD/OD Data Use
The following equation is used to calculate the weight of air-dry soil needed to provide a given weight of oven-dry soil for other analytical procedures.
AD = (ODr) / [1 − (H2O / 100)]
where:
AD = Required weight of air-dry soil ODr = Desired weight of oven-dry soil
H2O = Percent water determined from AD/OD Report
Report the AD/OD and/or FM/OD ratio as a dimensionless value to the nearest 0.01 unit.