abstract results methods second€¦ · zircon and apatite separation using a spiral panning table:...

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Zircon and Apatite Separation Using a Spiral Panning Table: Evaluation of Time and Yield Efficiency Student Researchers: Brittany Fagin and Ashley Edwards Research Advisor: Dr. Chris Mattinson Affiliation: Central Washington University, Ellensburg, WA ABSTRACT RESULTS Mineral separations concentrate the heavy minerals apatite and zircon necessary to accurately date rock samples, but current methods are time-consuming, toxic, expensive, and have unknown yield efficiencies. To evaluate and improve separation methods, I processed five, ~1.4 kg samples (hornblende-biotite tonalite, 65.47 wt % SiO 2 , 137 ppm Zr, 0.138 wt % P 2 O 5 , collected from the Mt. Stuart Batholith near Leavenworth, WA; expected yields per kg, calculated from CIPW-norm: 300 mg zircon; 3200 mg apatite) with a new procedure using a spiral panning table (panner) to wash and pre-concentrate heavy minerals before magnetic, lithium polytungstate (LST) and methylene iodide (MEI) heavy liquid separations. The control sample (#3) was hand washed, separated magnetically, and processed with LST and MEI, resulting in 33.5 mg zircon and 308.9 mg apatite. Panner trial #1 used a fast sample feed rate (58.4 g/min) and slow rotation speed (13.7 rpm), resulting in 3.7 mg zircon and 1.0 mg apatite. Panner trial #2 used a slow sample feed rate (11.5 g/min), the same slow rotation speed as trial #1, and yielded 6.1 mg zircon and 6.0 mg apatite. Surfactant was used in panner trial #4 to cut surface tension along with a slow feed rate of 9.1 g/min and the same slow rotation speed as trial #1, yielding 6.9 mg zircon and 3.4 mg apatite. Last, panner trial #5 used a faster rotation speed (24.7 rpm) and a fast feed rate (36.2 g/min), which produced the highest yields: 13.2 mg zircon, 12.9 mg apatite. Compared with the expected yields (above), the yields from both control (~50% purity separates containing 33.5 mg zircon, 308.9 mg apatite) and panner trials (high-purity separates containing 3.7-13.2 mg zircon, 1.0-12.9 mg apatite) were much less, likely due to the loss of small grains and inclusions. The panner technique yielded 10x the concentration of zircon than the control, so toxic MEI would ideally not be needed to separate apatite from zircon in future projects, making this project’s protocol safer than current methods. The experimental process took ~7 hours per sample, compared to ~38 hours for the control. The greater speed, improved zircon concentration, and avoidance of toxic heavy liquids are significant advantages of the methods in this project similar to the larger, more expensive Gemeni table, and further development will improve recovery efficiency. 1) 12) 7) 6) 5) 4) 3) 2) 16) 17) 18) 15) 14) 9) 19) 11) 8) METHODS FIRST - All sample fractions received the same treatment before picking a control. 7) The control (Bag #3), after handwashing, was magnetically separated with a Frantz Isodynamic Magnetic Separator. 8) The non-magnetic portion was directed by gravity into the Dixie cup on the left and the magnetic portion was directed by electromagnetism into the Dixie cup on the right. 9) This rock sample fortuitously showed a color difference between the non-magnetic minerals (beaker on the left) and the magnetic minerals (Dixie cup on the right). Also, the difference of amounts between the non-magnetic and the magnetic portions is shown in this image. 1) Chunks of sample fresh from the outcrop. 2) Sledge hammer, to break sample into ~1 in. diameter pieces (sieve at bottom of image). 3) Sample pieces were then ground into >500 micron bits. 4) Then sieved to 250 microns. 5) Example of sample divided into fractions ~1.4 kg. Bag #3 was used as the control. MEANWHILE - Thin section preparation + Whole-rock geochemistry 6) Researcher Brittany cutting a billet for thin section preparation. SECOND - The control sample bag is processed with a Frantz Isodynamic Magnetic Separator. THIRD - SPIRAL PANNING - How does it work? 11) Pro-Camel 24 by Camel Mining Products. Samples are fed through the yellow funnel and the rotation is clock-wise. “Lighter” minerals are washed away and collected in the blue bucket. Copper bar has water nozzles wetting the panner during processing. 12) Fortunately, our rock sample showed a prominent color difference between the “light” minerals and the “heavy” minerals. 13) Heavies are transported up the grooves to the center hole and depositied in a beaker. 10) Inner processes of the Frantz magnet. Sample flows from right to left. 13) 14) Panner trials resulted in smaller concentrated portions of heavy minerals to be processed later by the Frantz magnet. 15) Microscopic view of heavy yield straight from the panner after drying. Zircon grain present in the center. ZRC FINALLY - Heavy Liquid Separations 17) Researcher Ashley is excited to see zircons sinking through the next heavy liquid. “It’s raining zircons!” 16) Set up for lithium polytungstate (LST) separation. Image shows control sample; note high quantity of sample remaining at this step. 19) Pipetting the final batch of heavy minerals from the MEI into the filter of a flask for collection. 18) Methylene iodide separation. Amount of samples and liquid are small. 10) CONCLUSIONS All values in graphs are normalized to 1 kg sample. Common Beginning Steps -Hammering, crushing, grinding, sieving (500 μm) -De-magging (remove metal from sample after grinding) -Divide sample into ~1.4 kg bags THE PROCESS Control -250 μm sieve -Ultrasonic wash (DI water); large volume -Frantz Isodynamic Magnetic Separator -Ultrasonic wash (DI water) -Lithium Polytungstate (LST) heavy liquid separation -Ultrasonic wash (Ultra-Pure water) -Methylene Iodide (MEI) heavy liquid separation -Ultrasonic wash (Acetone) -Weigh zircon and apatite yields Panner Trials -Sample processed on panner (each trial varied parameters; feed-rate, rotation-speed, water-nozzle flow -rate/direction, surfactant) -Ultrasonic wash (DI water); small volume -250 μm sieve -Frantz Isodynamic Magnetic Separator -Ultrasonic wash (DI water) -Lithium Polytungstate (LST) heavy liquid separation -Ultrasonic wash (Ultra-Pure water) -Methylene Iodide (MEI) heavy liquid separation -Ultrasonic wash (Acetone) -Weigh zircon and apatite yields May 21, 2013 Abstract No: 219530 Type of Session: Poster Session Number 27: T6. Using Detrital Zircon Age Data to Reassemble the Cordilleran Jigsaw PuzzleSession Start Time: 1:30 PM Location: Radisson Hotel and Conference Center, Salon B/C Poster Booth Number: 15 In conclusion: 1) We were able to improve yield quantity and purity with the use of the spiral panning table. 2) We were able to modify the panner process to significantly improve efficiency and yield with each progressive step. 3) The control method yielded the largest amount of zircon, but the quantity was less pure and the process required more time. 4) For the majority of the samples, the spiral panning table is preferred for its quicker time, higher yield purity, and the added bonus of possibly skipping the MEI step (this would improve safety because MEI is highly toxic). 5) Note that the times displayed in the results section do not include the time needed to recover the LST and MEI heavy liquids, contributing to the conclusion that the panner method is better (very large quantities of LST were needed to process the control sample; the same amount of liquid was used to process all of the panner samples). Times per Step per Trial - This graph shows the individual times for each step of each method tested (shows only run-time; set-up and clean-up are assumed to be the same for each process). 126 46 46 46 46 38 87 125 44 4 15 22 21 9 10 1099 15 21 8 8 16 6 6 6 6 113 37 37 37 37 37 156 min 165 min 251 min 1388 min 207 min Significant Zircon Purity Difference Control #3 Zrc Yield Control trial MEI heavy mineral yield. Fewer discernible zircons alongside many unidentified clear-to-white minerals. (Lower purity, ~50%). Panner trials MEI heavy mineral yield. Much higher proportion of zircons to other heavy minerals. (Higher purity, near ~100%). Note: zircon grain size is larger, possibly due to preferential loss of smaller grains during panning. Ttn? Zrc Panner #5 Zrc Yield Zrc Ttn? Zircon and Apatite Yield / Total Time for Each Trial - This graph shows the relationship between the zircon and apatite yields for each trial, cross-referenced with the amount of time for each step. 4.79 0.81 1.65 13.34 2.98 1.74 1.77 0.39 1.43 4.68 Total Zircon and Apatite Yields (mg) - This graph shows the amount of zircon and apatite yielded from each method. Control apatite yield is too large to fit the graph. 308.9 13.2 12.9 6.9 3.4 33.5 6.1 6.0 3.7 1.0

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Page 1: ABSTRACT RESULTS METHODS SECOND€¦ · Zircon and Apatite Separation Using a Spiral Panning Table: Evaluation of Time and Yield E˜ciency Student Researchers: Brittany Fagin and

Zircon and Apatite Separation Using a Spiral Panning Table: Evaluation of Time and Yield E�ciencyStudent Researchers: Brittany Fagin and Ashley Edwards

Research Advisor: Dr. Chris MattinsonA�liation: Central Washington University, Ellensburg, WA

ABSTRACT RESULTS

Mineral separations concentrate the heavy minerals apatite and zircon necessary to accurately date rock samples, but current methods are time-consuming, toxic, expensive, and have unknown yield e�ciencies. To evaluate and improve separation methods, I processed �ve, ~1.4 kg samples (hornblende-biotite tonalite, 65.47 wt % SiO2, 137 ppm Zr, 0.138 wt % P2O5, collected from the Mt. Stuart Batholith near Leavenworth, WA; expected yields per kg, calculated from CIPW-norm: 300 mg zircon; 3200 mg apatite) with a new procedure using a spiral panning table (panner) to wash and pre-concentrate heavy minerals before magnetic, lithium polytungstate (LST) and methylene iodide (MEI) heavy liquid separations. The control sample (#3) was hand washed, separated magnetically, and processed with LST and MEI, resulting in 33.5 mg zircon and 308.9 mg apatite. Panner trial #1 used a fast sample feed rate (58.4 g/min) and slow rotation speed (13.7 rpm), resulting in 3.7 mg zircon and 1.0 mg apatite. Panner trial #2 used a slow sample feed rate (11.5 g/min), the same slow rotation speed as trial #1, and yielded 6.1 mg zircon and 6.0 mg apatite. Surfactant was used in panner trial #4 to cut surface tension along with a slow feed rate of 9.1 g/min and the same slow rotation speed as trial #1, yielding 6.9 mg zircon and 3.4 mg apatite. Last, panner trial #5 used a faster rotation speed (24.7 rpm) and a fast feed rate (36.2 g/min), which produced the highest yields: 13.2 mg zircon, 12.9 mg apatite. Compared with the expected yields (above), the yields from both control (~50% purity separates containing 33.5 mg zircon, 308.9 mg apatite) and panner trials (high-purity separates containing 3.7-13.2 mg zircon, 1.0-12.9 mg apatite) were much less, likely due to the loss of small grains and inclusions. The panner technique yielded 10x the concentration of zircon than the control, so toxic MEI would ideally not be needed to separate apatite from zircon in future projects, making this project’s protocol safer than current methods. The experimental process took ~7 hours per sample, compared to ~38 hours for the control. The greater speed, improved zircon concentration, and avoidance of toxic heavy liquids are signi�cant advantages of the methods in this project similar to the larger, more expensive Gemeni table, and further development will improve recovery e�ciency.

1)

12)

7)

6)

5)4)

3)2)

16)

17)

18)

15)

14)

9)

19)

11)

8)

METHODS

FIRST - All sample fractions received the same treatment before picking a control.

7) The control (Bag #3), after handwashing, was magnetically separated with a Frantz Isodynamic Magnetic Separator.

8) The non-magnetic portion was directed by gravity into the Dixie cup on the left and the magnetic portion was directed by electromagnetism into the Dixie cup on the right.

9) This rock sample fortuitously showed a color di�erence between the non-magnetic minerals (beaker on the left) and the magnetic minerals (Dixie cup on the right). Also, the di�erence of amounts between the non-magnetic and the magnetic portions is shown in this image.

1) Chunks of sample fresh from the outcrop.

2) Sledge hammer, to break sample into ~1 in. diameter pieces (sieve at bottom of image).

3) Sample pieces were then ground into >500 micron bits.

4) Then sieved to 250 microns. 5) Example of sample divided into fractions ~1.4 kg. Bag #3 was used as the control.

MEANWHILE - Thin section preparation + Whole-rock geochemistry

6) Researcher Brittany cutting a billet for thin section preparation.

SECOND - The control sample bag is processed with a Frantz Isodynamic Magnetic Separator.

THIRD - SPIRAL PANNING - How does it work?

11) Pro-Camel 24 by Camel Mining Products. Samples are fed through the yellow funnel and the rotation is clock-wise. “Lighter” minerals are washed away and collected in the blue bucket. Copper bar has water nozzles wetting the panner during processing.

12) Fortunately, our rock sample showed a prominent color di�erence between the “light” minerals and the “heavy” minerals.

13) Heavies are transported up the grooves to the center hole and depositied in a beaker.

10) Inner processes of the Frantz magnet. Sample �ows from right to left.

13) 14) Panner trials resulted in smaller concentrated portions of heavy minerals to be processed later by the Frantz magnet.

15) Microscopic view of heavy yield straight from the panner after drying. Zircon grain present in the center.

ZRC

FINALLY -Heavy Liquid Separations

17) Researcher Ashley is excited to see zircons sinking through the next heavy liquid. “It’s raining zircons!”

16) Set up for lithium polytungstate (LST) separation. Image shows control sample; note high quantity of sample remaining at this step.

19) Pipetting the �nal batch of heavy minerals from the MEI into the �lter

of a �ask for collection.

18) Methylene iodide separation. Amount of samples and liquid are small.

10)

CONCLUSIONS

All values in graphs are normalized to 1 kg sample.

Common Beginning Steps-Hammering, crushing, grinding, sieving (500 µm)

-De-magging (remove metal from sample after grinding)-Divide sample into ~1.4 kg bags

THE PROCESS

Control

-250 µm sieve-Ultrasonic wash (DI water); large volume-Frantz Isodynamic Magnetic Separator-Ultrasonic wash (DI water)-Lithium Polytungstate (LST) heavy liquid separation-Ultrasonic wash (Ultra-Pure water)-Methylene Iodide (MEI) heavy liquid separation-Ultrasonic wash (Acetone)-Weigh zircon and apatite yields

Panner Trials

-Sample processed on panner (each trial varied parameters; feed-rate, rotation-speed, water-nozzle �ow -rate/direction, surfactant)-Ultrasonic wash (DI water); small volume-250 µm sieve-Frantz Isodynamic Magnetic Separator-Ultrasonic wash (DI water)-Lithium Polytungstate (LST) heavy liquid separation-Ultrasonic wash (Ultra-Pure water)-Methylene Iodide (MEI) heavy liquid separation-Ultrasonic wash (Acetone)-Weigh zircon and apatite yields

May 21, 2013Abstract No: 219530Type of Session: PosterSession Number 27: “T6. Using Detrital Zircon Age Data to Reassemble the Cordilleran Jigsaw Puzzle”Session Start Time: 1:30 PMLocation: Radisson Hotel and Conference Center, Salon B/CPoster Booth Number: 15

In conclusion:1) We were able to improve yield quantity and purity with the use of the spiral panning table.2) We were able to modify the panner process to signi�cantly improve e�ciency and yield with each progressive step.3) The control method yielded the largest amount of zircon, but the quantity was less pure and the process required more time.4) For the majority of the samples, the spiral panning table is preferred for its quicker time, higher yield purity, and the added bonus of possibly skipping the MEI step (this would improve safety because MEI is highly toxic).5) Note that the times displayed in the results section do not include the time needed to recover the LST and MEI heavy liquids, contributing to the conclusion that the panner method is better (very large quantities of LST were needed to process the control sample; the same amount of liquid was used to process all of the panner samples).

Times per Step per Trial - This graph shows the individual times for each step of each method tested (shows only run-time; set-up and clean-up are assumed to be the same for each process).

12646 464646

38 87 12544

4

1522

21910

1099

15

218

8

16

6

66

6

11337

37

3737

37156 min 165 min

251 min

1388 min

207 min

Signi�cant Zircon Purity Di�erence

Control #3 Zrc Yield

Control trial MEI heavy mineral yield. Fewer discernible zircons alongside many unidenti�ed clear-to-white minerals. (Lower purity, ~50%).

Panner trials MEI heavy mineral yield. Much higher proportion of zircons to other heavy minerals. (Higher purity, near ~100%). Note: zircon grain size is larger, possibly due to preferential loss of smaller grains during panning.

Ttn?

Zrc

Panner #5 Zrc Yield

Zrc

Ttn?

Zircon and Apatite Yield / Total Time for Each Trial - This graph shows the relationship between the zircon and apatite yields for each trial, cross-referenced with the amount of time for each step.

4.79

0.811.65

13.34

2.98

1.741.77

0.39

1.43

4.68

Total Zircon and Apatite Yields (mg) - This graph shows the amount of zircon and apatite yielded from each method. Control apatite yield is too large to �t the graph.

308.9

13.212.9

6.9

3.4

33.5

6.16.03.7

1.0