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From sediment to sample

Sample sediments are typically sent in a large plastic bag inside a brown paper bag labeled with the company or organization name, drill site name and number, and the depth the sediment was taken (in meters).

The first step in determining a lithology is to prepare a sample from your bulk sediment. To do this, you will need to crush some of the bulk rocks of your sediment into finer grains ( [link] ). You will need a hard surface, a hammer or mallet, and your sediment. An improvised container such as the cardboard one shown in [link] may be useful in containing fragments that try to escape the hard surface during vigorous hammering. Remove the plastic sediment bag from the brown mailer bag. Empty approximately 10-20 g of bulk sediment onto the hard surface. Repeatedly strike the larger rock sized portions of the sediment until the larger units are broken into grains that are approximately the size of a grain of rice.

Crushing
A hammer and hard surface for crushing. The makeshift cardboard shield on the left can be placed around the hard surface to control fragmentation.
Some samples will give off oily or noxious odors when crushed. This is because of trapped hydrocarbons or sulfurous compounds and is normal. The next step in the process, washing, will take care of these impurities and the smell.

Once the sample has been appropriately crushed on the macro scale, a micro uniformity in grain size can be achieved through the use of a pulverizing micro mill machine such as the Planetary Mills Pulverisette 7 in [link] .

milling
A Pullsette micro mill, milling cup removed. The mill is set to 520 rotations per minute and a five minute run time.

To use the mill, load your crushed sample into the milling cup ( [link] ) along with milling stones of 15 mm diameter. Set your rotational speed and time using the machine interface. A speed of 500-600 rpm and mill time of 3-5 minutes is suggested. Using higher speeds or longer times can result in loss of sample as dust. Load the milling cup into the mill and press start; make sure to lower the mill hood. Once the mill has completed its cycle, retrieve the sample and dump it into a plastic cup labelled with the drill site name and depth in order to prepare it for washing. Be sure to wash and dry the mill cup and mill stones between samples if multiple samples are being tested.

cupping
A milling cup with mill stones and the crushed sample before milling.

Washing the sample

If your sample is dirty, as in contaminated with hydrocarbons such as crude oil, it will need to be washed. To wash your sample you will need your sample cup, a washbasin, a spoon, a 150-300 µm sieve, household dish detergent, and a porcelain ramekin if a drying oven is available ( [link] ).

washing
A washbasin, with detergent in a squirt bottle and the sample in a cup for washing (sieve not pictured).

Take your sample cup to the wash basin and fill the cup halfway with water, adding a squirt of dish detergent. Vigorously stir the cup with the spoon for 20 seconds, ensuring each grain is coated with the detergent water. Pour your sample into the sieve and turn on the faucet. Run water over the sample to allow the detergent and dust particles to wash through the sieve. Continue to wash the sample this way until all the detergent is washed from the sample. Once clean, empty the sieve onto a surface to leave to dry overnight, or into a ramekin if a drying oven is available. Place ramekin into drying oven set to at least 100 °C for a minimum of 2 hours to allow thorough drying ( [link] ). Once dry, the sample is ready to be picked.

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Source:  OpenStax, Physical methods in chemistry and nano science. OpenStax CNX. May 05, 2015 Download for free at http://legacy.cnx.org/content/col10699/1.21
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