v.378P

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Manual Information

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Author(s):

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N. Lawler & A. Armstrong

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Reviewer(s):

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C. Bennight, E. Jackson, H. Barnes

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Management Approval:

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D. Houpt

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Current Version:

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V371T | July 2017 | Reviewed X374 | March 2018

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Previous Versions:

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V1.2 | 6/10/2017, V1.1 |  1/6/2014 (IODP-II)

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Domain:

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Chemistry; XRD lab

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System:

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ICP-AES Elemental Analysis

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Keywords:

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Element oxide, ICP, solids

In This User Guide

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Introduction

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Laboratory Apparatus

General Laboratory Equipment

• Compensated Dual Analytical Balance System 
• Drying ovens at 110°C and 60°C

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• Quartz crucibles
• Tongs
• Vials containing 400 mg lithium metaborate flux (preweighed on shore) (Figure 9)
• Milligram calibration weighing set
• Weighing paper, 2 x 2
• Acid-washed vials for excess ignited powder
• Agate mortar and pestle
• Pt-Ag crucibles

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Each sample will correspond to one beaker; collect as many as needed. Beakers need to be cleaned (DI water and isopropyl alcohol) and labeled ( ex. 1, A, or sample label).
Next start the grinding process using the Buehler grinder located in the Xray prep area of the thing section lab (Fig. Figure 1).
Note: Make sure that the correct diamond disc is attached to the wheel. The diamond disc is attached to a magnetic disc which is then placed on the wheel plate. Attach the diamond disc using either the adhesive on the back or an aluminum ring.

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To start the polisher flip the 'On' switch in the back. The power indicator light (Fig. Figure 1A) should illuminate. Press the timer button (Fig. Figure 1B) to get continuous disc rotation. Turn the water on by flipping the 'Water' switch to the 'On' position (Fig. Figure 1C). The water flow can be adjusted by turning the knob shown in Fig Figure 1D.
The rotation speed is controlled by the dial shown in Fig. Figure 1E. The range is 0 rpm to 500 rpm. 150 rpm is a good starting position. Adjust the speed if needed: faster for hard rocks and slower for softer rocks.
With the water on and the RPM adjusted press the 'Run' button (Fig Figure 1F). Move the sample back and forth across the disc to prevent making a groove. If there is an emergency press the 'Emergency Stop' button (Fig. Figure 1H) to stop rotation and cut off the water. To enable the wheel again twist the knob until it pops back out.
Polish the rocks until they're completely smooth and round on all edges. There should no pits or jagged corners. Put the rock into a labeled beaker and polish the next sample. Do this for all samples and then move on to 'Cleaning Samples'.

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Pour either DI water or isopropyl alcohol (70%) into the beaker to cover the sample. Check with the scientists for their preference in solution. There should be enough liquid to keep the sample from floating in the sonic bath (Fig.3).

Figure 3. Sonic Bath 

Fill the sonic bath with a little bit of water and place beakers inside. Sonicate for 15 minutes. You should notice the water becoming cloudy from residue being shaken off the samples. Then follow the wash sequence below:

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Place the beakers into the ICP Oven at 110°C for 12 hours (Fig. Figure 5). Turn on the power button and adjust the knob to 110°C, which is marked on the oven. A thermostat is located inside to double check temperature.

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After 12 hours remove the beakers from the oven and place them inside the desiccator (Fig. Figure 6) while you prepare the X-press station.
Note: The ICP oven should be kept clean at all times, as samples are left open and are susceptible to contamination. The ICP oven should only be used for ICP samples.
 

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The X-Press is a motorized hydraulic press that crushes samples into smaller pieces.
First clean the X-press with simple green and isopropyl alcohol. Clean the work area and materials with isopropyl alcohol for each sample.
Place a large KimWipe on your working surfaces for your clean materials. Next collect the following supplies that make up the 'crushing unit' of the X-press (Fig. Figure 7). Materials are located in the drawer labeled 'X-PRESS SUPPLIES' in the X-Ray Prep Area.

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• Grab the stainless steel dish. This is the base for the crushing unit (Fig. Figure 8).

Figure 8. Stainless stell dish

• Place a piece of Weigh Paper on the Base (Fig. Figure 9).

Figure 9. Dish with Weigh paper

•  Put one Derlin disc on top of the weigh paper (Fig. Figure 10).

Figure 10. Derlin Disk Added

• Place the sample on top of the Derlin Disc (Fig. Figure 11). These discs can fracture leaving Teflon flakes in the sample so arrange the sample such that the two flattest surfaces are the top and bottom.

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• Now place the second derlin disc on top of the sample (Fig. Figure 12). Again make sure the disc rests flat against sample.

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•  Put the aluminum die on top of the derlin disk, holding it until you slip the core liner over the unit (Fig. Figure 13).

Figure 13. Aluminum Die added

• Now slip the piece of core liner over all the pieces and resting inside the stainless steel base (Fig. Figure 14). This contains the sample pieces inside the unit.

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Place the crushing unit inside the X-Press in the middle of the metal platform (Fig. Figure 15 A). Put in the sliding polycarbonate door. Tighten the jackscrew (Fig. Figure 15 B) until it rests firmly against the aluminum die. Tighten the 'pressure relief handle' with a clockwise turn (Fig. Figure 15 C).

Note: The polycarbonate door sits on two interlock switches that enable operation. If the door is not fully closed or pressing down on these switches the machine will not work.
Crush the sample by continuously holding down the toggle switch (Fig Figure 15 D). The motor and pump can be heard and the pressure will rise (Fig 15EFigure 15 E). Once the desired pressure is reached the toggle can be released and the sample will sit under that pressure. For most samples ~5 tons of pressure is enough force to crack it. If you find the need to go past 10 tons, try rotating the sample onto another side and apply pressure again.

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Turn on the Shatterbox by flipping the 'On' switch located on the back panel (Fig. Figure 16A). The control panel is located on the front of the lid next to the handle (Fig. Figure 16C).

Figure 16. Shatterbox. A. Power switch. B. Cover. C. Control panel

There are two sizes of grinding vessels: small and large. Each size has different components and requires a different setup inside the Shatterbox. The small vessel holds between 5-20 mLs of material and has three components: a container, puck, and lid (Fig. Figure 17).

Figure 17. Small vessel components. A. Container B. Puck. C. LidFigure 16. Shatterbox. A. Power switch. B. Cover. C. Control panel

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The large grinding vessel holds between 20 – 60mLs of material and has five components: a container, puck, inner ring, O-Ring, and lid (Fig. Figure 18).

Figure 18. Large Vessel components. A. Container B. Inner Ring C. Puck D. O-Ring E. Lid

The small vessels have a small indent in the bottom of the container and they will sit in the shatterbox resting on either a three pinned plate (Fig. Figure 19) or a one pinned plate (Fig. Figure 20).

Figure 19. Three pinned rack plate to hold three small vessels in Shatterbox

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Transfer the sample pieces into the grinding vessel. Pour sample pieces between the puck and the wall of the vessel (Fig. Figure 21). There can't be any material on top of the puck or inside the sealing ring; otherwise the vessel will not seal properly and the sample can spill inside the Shatterbox. If any pieces are on top of the puck or ring, use gloves, tongs, or a KimWipe to move the sample into the vessel. Put on the lid and start assembling the shatterbox.

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Open the lid, pull out the lever arm (Fig. Figure 22A), and pull up the clamp arm (Fig. Figure 22B). This will reveal full access to the inner capsule (Fig. Figure 22C).

Figure 22. The inside of the Shatterbox. A. The lever arm B. The clamp arm C. The inner capsule 

 Depending on vessel size, you will either put in the pinned plate (small vessels) or the large vessel directly. The shatterbox setup will also vary depending on sample number. If you are crushing one sample use the one pinned plate, whereas for two or three samples use the three pinned plate (Fig. Figure 23). For crushing two samples, two vessels will be full, whereas the third will be empty without a puck. It is important to maintain balance within the machine to prevent damage.

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Now load vessels onto the plate (Fig. Figure 24). The divet in the bottom of the vessels will settle onto the pins and fit firmly in place.

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Put the top rack plate over the vessels. Bring down the clamp arm (Fig. Figure 25A). The guide on the clamp arm will settle into the boss (Fig. Figure 25B) when centered properly.

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Bring the lever arm down and push it into the end of the clamp arm (Fig. Figure 26B). Then push the lever arm down over the clamp arm (Fig. Figure 26A).

Figure 26. A. The lever arm inserted into the end of the clamp arm. B. The clamp arm pushed over the lever arm.

The resistance in the lever arm is very important and must be adjusted before use. There should be moderate resistance in the arm while pushing it down. If the resistance is too low the containers can shake free; whereas, if it's too strong the clamp can break. Ideal tightness is just past the point where the vessels can be rotated while the clamp is down. Adjust the resistance by raising the clamp arm and pushing on the 'locking pin.' Hold the locking pin and turn the guide (Fig. Figure 27A). Rotating the guide clockwise decreases resistance; whereas counterclockwise increases resistance.

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Now close the lid and turn the emergency stop switch to 'On'. This does not start the Shatterbox but does enable operation. If an emergency shutdown is needed, flip this switch to 'Off' and all shaking will stop even though the timer will continue to count down.
Set the grinding time. The LCD screen displays the current operating time (Fig. Figure 28A). Adjust the time by pressing on the 'Minute' (Fig. Figure 28B) and 'Second' (Fig. Figure 28C) buttons. The timer maximum is 9:59.

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When the time is set press the 'Start' button (Fig. Figure 28D). To temporarily pause the operation press the 'Pause/Stop' button once (Fig. Figure 28E).To stop the machine press 'Pause/Stop' twice.

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• In a vial, mix 400 mg lithium metaborate flux (pre-weighed onshore) with non-ignited, or raw, powdered sample. This step is typically completed by the chemistry technicians.
• Fuse both sample powder and flux into a glass bead (Fig. Figure 29). Dissolve the bead in nitric acid. This solution will be further diluted and analyzed by the ICP.

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Collect platinum crucibles, platinum tipped tongs, 0.172 LiBr, and pipette tips from the safe above the Bead Maker (Figure 30). Get the 10-100ul pipette and teflon spatula from the drawer and clean with isopropyl alcohol. Have a tray of samples that need to be fused and an empty tray for finished beads.

 

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Turn 'On' the Bead Maker (Fig. Figure 31; switch on the right side of the instrument). 

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Next, turn on the water (Fig. Figure 32; 33). The handle is to the left of the machine on the wall. Raise the handle slightly to turn it on. You will hear a small click once it is in the 'on' position. Now the 'Water' and 'Ready' indicator lights should be on. Do not run any samples unless these lights are on.

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 Place a large sheet of paper in front of the balances and place supplies here. For each sample you need weigh paper (Fig. Figure 34A), a scoopula (Fig. Figure 34C), and a quartz crucible set (Fig. Figure 34B). Clean the scoopula with isopropyl alcohol in between each sample as it has direct contact with the sample powder.



Figure 34. Materials needed for weighing LOI. A. Clean paper or kim wipe. B. Crucible set. C. Scoopula. D. Samples

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Samples are weighed on the Mettler-Toledo Dual Balance. The Dual balance uses two weighing stations to compensate for shipboard motion: one a 'known' reference weight (Fig. Figure 35A) and the other an 'unknown' sample weight (Fig. Figure 35B). The balance takes a series of measurements and uses the average value as the final weight (for a more in-depth guide refer to the Balance User Guide on Cumulus). Each balance has a control panel plate, which constantly record weight. These plates communicate with the "Mettler Balances" program.

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 Open the Mettler Balances program (Figure 36). There are multiple panes and parameters that are set before we start measuring.

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Graphical Measurement Window: Shows a line graph of the live-time measurement weight and the running average weight.
Final Weight Panel: Displays the Final Weight after all measurement counts have been made
Statistics Panel: Shows the average weight adjusting with time.
Counter Weight: Enter in the reference weight Counts: The elapsed amount of measurements
Tare: Shows and applies the tare or 'zero' value
Sample ID: Name the sample being measured
Commands Panel: Executable commands
Weigh: Starts measurement
Tare: Determines the 'zero' weight. This value is applied to the final weight.
Halt: Stops a measurement before it has gone through all counts
History Panel: Shows statistics on all measurements taken. This file can be exported into an excel file by using the 'Export' button. Note: The 'Export CSV' file does not work.
Options Panel: Editable measurement parameters. We measure using the 'Counts' feature. 'Counts' is active when the dot is blue. Change the number of counts or measurements the balance takes here.
At the beginning of a series of measurements, tare the balances. To do this first make sure that the 'Counter Weight' field is set to '0' and then set the 'Count' value. The 'Count' is dependent of the sea state: 600 for calm waters and 1000 counts for rough waters. If seas are too rough than wait until the weather settles before continuing to measure.
A rule of thumb is that the measurement of a known reference mass shouldn't have a larger deviation than the accuracy desired. For example, our accuracy is +/- 0.05 grams; weigh a reference mass in the unknown balance that is close to the masses you are measuring (e.g., 25 grams) and perform the measurement with the appropriate counterbalance mass in the reference balance pan. You should get a final mass of 24.95—25.05 grams.
Once parameters are set, select the 'Tare' button. When the tare is complete the 'Final Weight' Section turns orange and the 'History' Section updates (Fig. Figure 37).

Figure 37. Mettler Balance program window showing a tare calculation.

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 The quartz crucibles have three sections: an outer (or large) crucible, an inner (or small) crucible, and a lid (Fig. Figure 39).

Figure 39. Crucible components. A. Outer (large) crucible. B. Inner (small) crucible. C. Lid.

The inner crucible holds the sample material and is the only piece that is weighed. They are assembled as seen below with the inner crucible inside of the outer crucible and the lid sitting over the entire unit (Fig. Figure 40). Crucible sets (large, small and lid) are engraved and lettered and should be kept as a set. For example, Crucible lid 'A' should always be run with large and small crucible 'A'. If a crucible is unlabeled use a diamond-tipped pen to etch in an unused lid.

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Weight measurements are recorded in an excel spreadsheet which will be uploaded to LIMS at the end of an expedition (Fig Figure 41). Open the excel spreadsheet titled 'LOI Template' found in Local Disk > DATA and save the spreadsheet in Local Disk > DATA > IN as 'EXP # LOI'.

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The spreadsheet has multiple columns to fill in.'SITE', TEXT ID', 'CORE/SECT/INTERVAL', 'CRUCIBLE ID', 'CRUCIBLE WT', 'CRU+FRESH SAMPLE WT', and 'CRU+IGN SAMPLE WEIGHT'. 'SAMPLE WEIGHT', POST IGNITION LOSS', and '%LOI' are calculated values based on the weights entered in columns E – G.
The first measurement taken will be the initial weight of an empty crucible. To complete this measurement, open the side door and place an empty inner crucible in the center of the 'Unknown' balance (Fig. Figure 42). Record the number or letter etched onto the crucible in the excel spreadsheet under 'Crucible ID.'

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Weigh out 5 grams of sample powder into the quartz crucible within +/- 0.05g (Fig. Figure 43). The total weight should be the crucible weight + 5 grams within +/- 0.05 grams. For example, a crucible weighs 14.32g, thus the total weight plus the sample will be between 19.27 – 19.37g.

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When the sample is close to this range click 'Weigh.' Press 'Halt' to stop the measurement and either add or remove sample if needed, and then click on 'Weigh' again to take a new measurement. 
When a sample's final weight is within the allowable range, record the 'final weight' value into the spreadsheet under 'CRU + FRESH SAMPLE WT'.
Carefully remove your sample from the balance. Place your crucible into the larger quartz holder and cover with a lid (Fig. Figure 44). Repeat this process for all samples. After all samples have been weighed and recorded, take samples from the desiccator and bring over to the muffle furnace in the Chemistry Lab.

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Bring crucibles over to the Muffle Furnace (Fig. Figure 45). Turn the power switch on and the control panel will illuminate.

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Open the Excel File 'LOI Spreadsheet Upload Template' in Local Disk > DATA (Fig. Figure 47). Put your LOI information into the spreadsheet following the example format. Fill in the Text ID, Analysis, Replicate, Crucible number, and all weights and units including the %LOI.

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Open up the program ‘Spreadsheet Uploader’ Pinned to the Taskbar (Fig. Figure 48). 

Figure. 48. Spreadsheet Uploader Icon.

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