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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.Figure 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 (Figure 54). 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.

Figure 54. The ICP Prep Oven located in the X-Ray lab. A. ‘On/Off’ Switch B. Temperature Setting C. Heating Indicator

After 12 hours remove the beakers from the oven and place them inside the desiccator (Figure 65) 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.
 

Figure 65. Desiccators located in the X-ray lab

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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 (Figure 76). Materials are located in the drawer labeled 'X-PRESS SUPPLIES' in the X-Ray Prep Area.

•  Weigh Paper 6" x 6"
• Core liner
• Two derlin discs
• Stainless steel base
• Figure 76: Materials needed for assembly of 'crushing unit'. A. Weigh Paper 6"x6". B. Core Liner C. Two Derlin Discs D. Stainless Steel Base E. Aluminum DieAluminum die.

Figure 76: Materials needed for assembly of ‘crushing unit’. A. Weigh Paper 6”x6”. B. Core Liner C. Two Derlin Discs D. Stainless Steel Base E. Aluminum Die

Put on gloves and 'wash' them with isopropyl alcohol. Clean the crushing supplies with isopropyl alcohol and set them down on the clean surface.
Collect sample beakers from the dessicator. Put a piece of parafilm over each beaker and bring them over to the X-press.
Now that the X-press area is clean and the samples are in the lab, assemble the crushing unit as follows:

• Grab the stainless steel dish. This is the base for the crushing unit (Figure 87).

Figure 87. Stainless stell dish

• Place a piece of Weigh Paper on the Base (Figure 98).

Figure 98. Dish with Weigh paper

•  Put one Derlin disc on top of the weigh paper (Figure 109).

Figure 109. Derlin Disk Added

• Place the sample on top of the Derlin Disc (Figure 1110). 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.

Figure 1110. Sample Added

• Now place the second derlin disc on top of the sample (Figure 1211). Again make sure the disc rests flat against sample.

Figure 1211. Second Derlin Disk added

•  Put the aluminum die on top of the derlin disk, holding it until you slip the core liner over the unit (Figure 1312).

Figure 1312. Aluminum Die added

• Now slip the piece of core liner over all the pieces and resting inside the stainless steel base (Figure 1413). This contains the sample pieces inside the unit.

Figure 1413. Core Liner added

• The crushing unit is now assembled and we can start crushing samples (Figure 14).

Figure 1514: Overview of the X-Press. A. Metal platform sample rests on B. Jacksrew C. Pressure Relief Handle. D. ‘On’ toggle E. Pressure Gauge.

Place the crushing unit inside the X-Press in the middle of the metal platform (Figure 15 14 A). Put in the sliding polycarbonate door. Tighten the jackscrew (Figure 15 14 B) until it rests firmly against the aluminum die. Tighten the 'pressure relief handle' with a clockwise turn (Figure 15 14 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 (Figure 15 14 D). The motor and pump can be heard and the pressure will rise (Figure 15 14 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 (Figure 16A15A). The control panel is located on the front of the lid next to the handle (Figure 16C15C).

Figure 1615. 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 (Figure 1716).

Figure 1716. 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 (Figure 1817).

Figure 1817. 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 (Figure 1918) or a one pinned plate (Figure 2019).

Figure 1918. Three pinned rack plate to hold three small vessels in Shatterbox

Figure 2019. Single pinned rack plate to hold one small vessel 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 (Figure 2120). 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.

Figure 2120. Small vessel filled with sample pieces. No sample material is on the top the puck or in the lid ring.  

Open the lid, pull out the lever arm (Figure 22A21A), and pull up the clamp arm (Figure 22B21B). This will reveal full access to the inner capsule (Figure 22C21C).

Figure 2221. 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 (Figure 2322). 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.

Figure 2322. Inside the Shatterbox with the bottom three pinned rack plate resting inside the inner capsule.

Now load vessels onto the plate (Figure 2423). The divet in the bottom of the vessels will settle onto the pins and fit firmly in place.

Figure 2423. Three samples loaded into the Shatterbox.

Put the top rack plate over the vessels. Bring down the clamp arm (Figure 25A24A). The guide on the clamp arm will settle into the boss (Figure 25B24B) when centered properly.

Figure 2524. The top rack plate sitting on top of the three samples. A. Clamp arm. B. the “boss” of the rack plate, where the clamp arm will attach.

Bring the lever arm down and push it into the end of the clamp arm (Figure 26B25B). Then push the lever arm down over the clamp arm (Figure 26A25A).

Figure 2625. 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 (Figure 27A26A). Rotating the guide clockwise decreases resistance; whereas counterclockwise increases resistance.

Figure 2726. The lever arm and the guide. A. Retractable locking pin being pushed to allow adjustment of the 'guide' length.

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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 (Figure 28A27A). Adjust the time by pressing on the 'Minute' (Figure 28B27B) and 'Second' (Figure 28C27C) buttons. The timer maximum is 9:59.

Figure 2827. A. Current operating time. B. Minute button. C. Second button. D. Start button. E. Pause/Stop button.

When the time is set press the 'Start' button (Figure 28D27D). To temporarily pause the operation press the 'Pause/Stop' button once (Figure 28E27E).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 (Figure 2928). Dissolve the bead in nitric acid. This solution will be further diluted and analyzed by the ICP.

Figure 2928. Fused glass bead. 

Weighing the Sample

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Collect platinum crucibles, platinum tipped tongs, 0.172 LiBr, and pipette tips from the safe above the Bead Maker (Figure 3029). 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.

 

Figure 3029. Bead making supplies. A. Platinum tipped tongs. B. Platinum crucibles. C. 0.172 Libr wetting agent. D. Pipette. E. Teflon spatula. F. Pipette tips. 

Turn 'On' the Bead Maker (Figure 3130; switch on the right side of the instrument). 

Figure 3130. Beadmaker. A. control panel. B. Site of platinum crucible. C. View port window. D. Fan to cool platinum crucible. E. Ceramic plate used for dislodging the fused bead.

Next, turn on the water (Figure 31; 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.

Figure 3231. Water in off position.

Figure 3332. Water in on position.

1. Lay a large Kim wipe and a piece of weigh paper down next to the Bead Maker. Unwrap a platinum crucible and place it on the weigh paper. Pour the powder mix into the crucible. The sample should evenly cover the bottom.
2. Pipette 10 µL of 0.172 mM LiBr wetting agent into the center of the sample powder.
3. Open the Bead Maker lid and place sample inside the sample holder. The short wide crucible will fit directly; whereas, the tall narrow crucible will need an additional ceramic ring.
4. Close the lid. Double check both indicator lights are on. Press 'On' to start the program. The process will take 12 minutes and the sample is heated in three stages:
   • Stage 1:700°C for 2 min
   • Stage 2:1050°C for 5 min,
   • Stage 3: 1050°C in agitation for 5 min.
5. Be prepared to remove the crucible as soon as the timer is done. The material hardens very quickly so be ready with safety glasses, gloves, and the platinum tipped tongs before the final stage has finished.
6. With the Pt-tipped tongs, lift out the crucible and swirl the contents around to get the entire sample into one bead. Wear eye protection! The bead is very hot and rapid cooling can cause it to shatter and fly out.
7. Place the crucible on its cooling rack. When seated properly the red light behind it will start flashing. When the flashing stops the bead and crucible have finished cooling down.
8. Place a sheet of 6x6 weigh paper on the ceramic plate. Take crucible from the cooling rack and prepare to flip it upside down on the paper to extract the bead.
9. With crucible in hand flip over and give it a firm whack on the weigh paper. The bead should pop off without much resistance. Put the bead back into the vial that contained the flux.
10. If there are small pieces of bead left behind you can use your Teflon spatula to try pry it off. Do not use too much force. The platinum is malleable and will get scratched and damaged if put under too much force. If it still remains, make a note of the sample number and inform the chemistry technician. The residue (if any) should come off during the cleaning process.
11. Repeat process for all samples.
12. Hand off all beads to the chemistry technicians to continue on with the ICP analysis.

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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 (Figure 34A33A), a scoopula (Figure 34C33C), and a quartz crucible set (Figure 34B33B). Clean the scoopula with isopropyl alcohol in between each sample as it has direct contact with the sample powder.



Figure 3433. 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 (Figure 35A34A) and the other an 'unknown' sample weight (Figure 35B34B). 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.

Figure 3534. Mettler Balance Station located in the XRay lab. A. Reference balance. B. Unknown balance. C. Sliding door. D. Reference power module. E. Unknown power module
 

 Open the Mettler Balances program (Figure 3635). There are multiple panes and parameters that are set before we start measuring.

Figure 3635. Mettler Balance program window. A. Graphical measurement window. B. Final weight panel. C. Statistics panel. D. Weigh. E. Tare. F. Halt. G. Options panel. H. History panel.

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 (Figure 3736).

Figure 3736. Mettler Balance program window showing a tare calculation.

Put in a reference weight into the "Reference' balance. With the tweezers, select the 20g weight and place it in the center of the 'Reference' balance (Figure 37). To have a more accurate measurement, the reference weight should be close to the expected 'Unknown' sample weight (roughly ~20g).

Figure 3837. Reference weights. A. Weights. B. Tweezers.

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 The quartz crucibles have three sections: an outer (or large) crucible, an inner (or small) crucible, and a lid (Figure 3938).

Figure 3938. 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 (Figure 4039). 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.

Figure 4039. Complete and assembled crucible unit.

Weight measurements are recorded in an excel spreadsheet which will be uploaded to LIMS at the end of an expedition (Figure 4140). Open the excel spreadsheet titled 'LOI Template' found in Local Disk > DATA and save the spreadsheet in Local Disk > DATA > IN as 'EXP # LOI'.

Figure 4140. LOI spreadsheet.

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 (Figure 4241). Record the number or letter etched onto the crucible in the excel spreadsheet under 'Crucible ID.'

Figure 4241. Weighing an empty inner crucible.
 

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Weigh out 5 grams of sample powder into the quartz crucible within +/- 0.05g (Figure 4342). 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.

 Note: If there is only a small amount of material, you can use less but the %LOI error will be larger. 

Figure 4342. Crucible with approximately 5g of sample. Pre-ignition measurement

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 (Figure 4443). 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.

Figure 4443. Complete crucible unit with sample, ready for ignition.

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Bring crucibles over to the Muffle Furnace (Figure 4544). Turn the power switch on and the control panel will illuminate.

Figure 4544. The Thermolyne Muffle Furnace. A. Power Switch B. Control Panel C. Door handle.
 

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A common program is an increase in temperature of 3°C/min to a target temperature of 900°C and a hold of one hour. Then ramp up at a rate of 3°C/min to a target temperature of 1025°C and hold for four hours. This ramp cycle is already programmed into the furnace and corresponds to 'Program 1'. To check or edit a program see additional guides attached to the furnace itself. It is also possible to run the furnace manually without a ramp up cycle. Discuss with scientists their preference

Either enter the desired temperature manually or select your program. If you are running the furnace manually, enter the desired temperature; no other buttons or steps are needed. If selecting a program, press and hold 'Run' (Fig. 46Figure 45).

Figure 4645. Control Panel on Thermolyne Muffle Furnace. A. Actual temperature. B. Desired/ Set temperature. C. Run/ stop button. D. Auto run button. E. Page button. F. Scroll button. G. Down button. H. Up button. 

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Uploading LOI Data To LIMS

Open the Excel File 'LOI Spreadsheet Upload Template' in Local Disk > DATA (Figure

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46). 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.

Figure 4746. LOI Spreadsheet Upload Template.

Open up the program ‘Spreadsheet Uploader’ Pinned to the Taskbar (Figure 4847). 

Figure 47. 48. Spreadsheet Uploader Icon.

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This document originated from Word document ICP_HR_Prep_UG_376.doc (see Archived Versions below for a pdf copy) that was written by H. Barnes & K. Bronk; later edited by N. Lawler & A. Armstrong. Credits for subsequent changes to this document are given in the page history.

Archived Versions