
Snowpack looking fine for upcoming river trip. Check out the handy website if it is new to you.
Nevada Isotope Geochronology Laboratory - Sample Descriptions – House - NBMG
General Comments: Your samples were run as conventional furnace step heating analyses. This type of sample run produces what is referred to as an apparent age spectrum. The "apparent" derives from the fact that ages on an age spectrum plot are calculated assuming that the non-radiogenic argon (often referred to as trapped, or initial argon) is atmospheric in isotopic composition (40Ar/36Ar = 295.5). If there is excess argon in the sample (40Ar/36Ar > 295.5) then these ages will be older than the actual age of the sample. U-shaped age spectra are commonly associated with excess argon, and this is often verified by isochron analysis, which utilizes the analytical data generated during the step heating run, but makes no assumption regarding the composition of the non-radiogenic argon. Thus, isochrons can verify (or rule out) excess argon, and isochron ages are usually preferred if a statistically valid regression is obtained (as evidenced by an acceptably low MSWD value). If such a sample (U-shaped, or more generally discordant) yields no reliable isochron, the most conservative estimate of the age is that the minimum on the age spectrum is a maximum age for the sample (it could be affected by excess argon, the extent depending on the radiogenic yield). 40Ar/39Ar total gas ages are equivalent to K/Ar ages. Plateau ages are sometimes found, these are simply a segment of the age spectrum which consists of 3 or more steps, comprising >50% of the total gas released, which overlap in age at the ±2σ analytical uncertainty level. Such ages are preferred to total gas or maximum ages if obtained. However, in general an isochron age is the best estimate of the age of a sample, even if a plateau age is obtained.
OWY-36 Basalt Groundmass
The age spectrum for this sample is discordant, with both positive and negative ages which overlap 0 within uncertainties, to ages as high as ~660 ka. The total gas age is 194 ± 27 ka, and is equivalent to a conventional K-Ar age. No plateau age or isochron age was defined by these data. This sample had very low, often negative radiogenic argon (%40Ar*) concentrations (i.e. there was no measurable 40Ar* in two of the steps), likely reflecting both low-K contents and young age. In a case such as this there are two possible interpretations. The first is that the sample contains no excess argon and the total gas age is a reasonable estimate. Unfortunately, with no isochron the presence, or absence, of excess argon cannot be confirmed, making this interpretation somewhat tenuous. The most conservative approach is to assume that the discordance is a result of excess argon, and thus the minimum age on the age spectrum is a maximum age for the sample. In this case, since the minimum ages are actually negative, this interpretation would hold that the sample is effectively 0-age. It should be noted that in such as case as this discordance could simply result from there being very little, to no, measurable 40Ar*, which would result in inaccurate and imprecise age determinations. Which interpretation one should choose depends somewhat on geologic relationships. Does the geology and stratigraphy support an age as old as ~194 ka?
OWY-35 Basalt Groundmass
The age spectrum for this sample is mildly discordant and U-shaped. Ages range from an initial age of ~450 ka, to a plateau segment with ages of ~250 ka, and a higher final step age of ~780 ka. The total gas age is 301 ± 24 ka. Steps 2-10 (94% of the total 39Ar released) define a plateau with a younger age of 248 ± 25 ka. Steps 1-4 (49% of the total 39Ar released) yield an isochron age of 179 ± 21 Ma. The isochron indicates the presence of excess argon (initial 40Ar/36Ar = 305 ± 2) in this sample. Thus, ages calculated for the age spectrum, which assume the initial argon has 40Ar/36Ar = 295.5, should be considered anomalously old. The isochron age is the most reliable for this sample. Note that the radiogenic yields are significantly higher for this sample than for the previous OWY-36 sample, thus the ages should be considered significantly more reliable.
OWY-23 Basalt Groundmass
The age spectrum for this sample is also moderately discordant and U-shaped, with ages which fall from an initial step of ~1.5 Ma to a plateau segment with ages of ~180 ka, and followed by older steps (to ~840 ka) in the final ~15% gas released. The total gas age is 292 ± 39 ka. Steps 2-7 (81% of the total 39Ar released) define a plateau with a younger age of 182 ± 42 ka. Steps 2-7 also yield an imprecise isochron age of 120 ± 130 ka. The isochron does not indicate the presence of excess argon (initial 40Ar/36Ar = 298 ± 6) in this sample. Also, note that all the data points defining the isochron fall near the y-axis in a cluster (similar radiogenic yields, ), thus the y-axis intercept (initial 40Ar/36Ar ratio) is fairly well defined, whereas the x-axis intercept (age) is very poorly defined. Thus, this isochron is not useful for age determination, but does provide important information regarding excess argon, i.e. within uncertainty the sample cannot be said to contain excess argon. Other processes, such as recoil of reactor generated 39Ar during irradiation, can also produce discordant age spectra for fine grained basalt groundmass samples, and this may explain this samples age spectrum in particular. Given these considerations, the plateau age should be considered the most reliable for this sample.
OWY-22 Basalt Groundmass
The age spectrum for this sample is nearly ideally flat and concordant, with the exception of higher ages in the final ~10% gas released. The total gas age is 70 ± 19 ka, and steps 1-8 (88% of the total 39Ar released) define a plateau with a younger age of 38 ± 21 ka. Steps 2-5 define a valid isochron age, however, as for OWY-23 above, the data are tightly clustered at the y-axis due to similar, and low, %40Ar* values, making this isochron useful only for confirming the composition of the initial 40Ar/36Ar ratio, which is indistinguishable from atmospheric argon. Thus, the plateau age can be considered reliable and the best estimate of the eruption age for this sample.
OWY-13 Basalt Groundmass
The age spectrum for this sample is discordant, with ages that fall, rise, and fall again with increasing %39Ar released. The total gas age is 8.3 ± 0.6 Ma. Steps 3-7 (62% of the total 39Ar released) define a plateau with a younger age of 7.0 ± 1.0 Ma. There was no isochron defined by these data. The discordance shown by this samples age spectrum must be considered to be potentially caused by the presence of excess argon, although this cannot be confirmed or denied since no isochron was obtained. Thus, in this case the most conservative interpretation is that the youngest age on the age spectrum (step 10, 3.6 Ma) is a maximum age for the sample.
OWY-12 Basalt Groundmass
This sample is similar to OWY-36 described above, and similar interpretations apply. The total gas age is 453 ± 94 ka. Steps 3-5 (50% of the total 39Ar released) define a plateau with a younger, and imprecise, age of 173 ± 145 ka. There was no isochron defined for this sample. Note that overall the age spectrum is distinctly U-shaped. This may indicate excess argon is present in the sample and thus calculated ages may be anomalously old. This cannot be confirmed as no isochron was obtained. As for OWY-36, since several steps yield negative radiogenic yields and 0-age calculations this sample is best interpreted as being effectively 0-age, i.e. it is so young that we cannot accurately measure the accumulated 40Ar* against the background of initial argon. The plateau age should only be used if stratigraphic constraints suggest it is accurate.
As is typical, these comments are made with little knowledge of geologic relationships and are simply interpretations of the laboratory data. Often knowledge of, e.g., stratigraphic relationships can determine which interpretation is most valid for a particular sample. The first sample above, OWY-36 is a good example of this. Feel free to call or email (best way to contact me terry.spell@unlv.edu) if you have further questions that I might assist with.


| Sample | Location | Total Gas | Plateau | Isochron | |
| OWY-12 | Lower Saddle Butte | 452.8 ± 94.1 | 173.0 ± 144.8 | n/a | |
| OWY-13 | Upper Saddle Butte | 8.31 ± 0.62 Ma | 7.03 ± 1.00 | n/a | |
| OWY-22 | Upper West Crater | 69.86 ± 19.15 | 37.60 ± 21.01 | 7.0 ± 8.5 | |
| OWY-23 | Lower West Crater (?) | 292 ± 39 | 182 ± 42 | 120 ± 130 | |
| OWY-35 | Upper AM-PM | 301 ± 24.3 | 247.6 ± 24.9 | 179 ± 21 | |
| OWY-36 | Lower AM-PM | 194 ± 27 | n/a | n/a |
Nevada Isotope Geochronology Laboratory - Sample Descriptions
General Comments:
Isochrons are the most desirable treatment of 40Ar/39Ar data. This is because the isochron actually defines the isotopic composition of the initial argon in the sample (non-radiogenic argon). Ages calculated for an age spectrum are referred to as "apparent ages" because they are calculated assuming the initial argon is atmospheric in composition - thus, if there is excess argon (40Ar/36Ar > 295.5) the age will be overestimated. Isochrons have their measure of reliability, known as the mean square of weighted deviates (MSWD) which is a statistical goodness of fit parameter. If it is greater than a certain value (which changes depending on the number of points, see Wendt and Carl, 1991, the statistical distribution of the mean squared weighted deviation, Chem. Geol., v. 86, p. 275-285) then there is more scatter than can be explained by analytical errors and it is not a statistically valid isochron. If we provide an isochron it means that the statistical test is valid, if not then no valid isochron was obtained. Also, there are issues of number of data points defining the isochron - the more the better. Four points should be considered a bare minimum for statistical reasons, three points is getting to be a real concern. This can be understood simply by considering two points - a perfectly fit straight line can be put through any two points, so completely accidental data can have a perfect line fit. It follows that with three points there is less of a chance of an accidental line fit, but it is still a very real possibility (especially if analytical errors are fairly large), this possibility gets exponentially smaller as the number of points defining the line (isochron) goes up, thus more points = a more reliable isochron.
If there is no isochron, then a plateau age is next in preference. This is because a sample that gives ages which are analytically indistinguishable from step to step is exhibiting what is known as "ideal" behavior, which suggests it has a simple geologic history, e.g., rapid cooling as a basalt lava, followed by no reheating or alteration, both of which may produce disturbed (discordant) age spectra. A reliable plateau is 3 or more consecutive steps which are indistinguishable in age at the 2 sigma level and comprise >50% of the total 39Ar released. The lack of an isochron or a plateau does not mean the sample provides no useful information, but their presence gives greater confidence in the ages obtained and requires less subjective interpretation.
Of course, you must consider that we run samples such as this "blind" in that we do not know the geologic relations of the samples, either when we analyze them, or when we provide these general interpretations. The geologic constraints must always be considered when interpreting isotopic ages; if any discrepancies arise feel free to discuss them with us, as it can in some cases make a difference in how age data are interpreted. All analytical errors are 1σ.
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Surely you read the blog over the Holidays and are busily typing up your GPS coordinates that I asked for, right? In the meantime, take a break from typing and check out the map above and the related photo in the previous post. These are some killer landslides off of Black Mesa in north central New Mexico (I flew over them twice...to and from Okla-coma). Is anyone aware of these being described in the literature? I have not looked yet. Certainly an interesting contrast to the Owyhee given the very different valley bottom morphology. However, as you go upstream the scene begins to look more familiar as you may discern below.
Today, I noticed an announcement that Google Earth had again updated some imagery in Oregon. Now, the Bend and Lava Butte areas are looking good (see screen snag above). The rapids formed at each lava-river interface are easily detected.Mineral Separate Preparation for 3He Cosmogenic samples:
STEP 1: Remove only top 4 cm of the rock (for cosmogenic samples). (If you only use the top 3 cm or top 1 cm, etc., make a note of this. It affects correction of the 3He content in the rocks.) Break the top 4 cm of the rock sample into pieces small enough to fit the crusher (generally the size of a golfball, no bigger). I use a rock hammer and chisel for this process. In some cases, for harder samples, a rock saw is needed, but rarely.
STEP 2: Make sure you clean the crusher in between samples to avoid any contamination. This includes using a dry paintbrush, a vacuum, and/or compressed air to get any/all of the previous sample out of the crusher and out of containers used to catch/transport the sample.
Always save at least one golf-ball sized hand sample of your whole rock for an archive sample. You might need this for chemical analyses etc. in the future. Start with the crusher at its widest position and throw the rock pieces in, reducing the width of the crushing gap each time until you have a variety of grain sizes. You want the majority of your sample to fall in the [250-500 μm] and [500-1000 μm] mesh range (sieve sizes in the US are labeled differently – I used to use US sizes [20-60] or so), so you just have to eye it. Grains in the [125-250] range are okay for analyses too, but makes things a bit more complicated because the grains are much smaller (i.e. handpicking this grain size is slow and tedious). There will still be pieces larger than that, up to 1 cm or so, that’s okay. You want to keep some bigger pieces in case you need to crush more in order to obtain the amount of the mineral you’re looking for. Just don’t overcrush, or you’ll end up with a lot of powder (too small!!) and not mineral grains of desirable size.
STEP 3: Sieving. Here’s a short list of sieve sizes we use:
(From Comparison Table of U.S., Tyler, Canadian, British, French, and German Standard Sieve Series)
| U.S. Standard | U.S. Alternate | Tyler mesh designation |
| 2.00 mm | 10 | 9 |
| 1.68 mm | 12 | 10 |
| 841 micron | 20 | 20 |
| 420 micron | 40 | 35 |
| 250 micron | 60 | 60 |
The sieves we use are the U.S. alternate 10, 20, 40, and 60.
Set the sieves up descending in mesh size from top to bottom. (i.e. the 10 should be on the top, followed by the 20, 40 and 60, with a screen-free container (fitting the stack) at the bottom) to catch the finest part of the sample. You can either dry-sieve or wet-sieve. Both have their benefits. With dry-sieving, you don’t have to wait for the samples to dry, before moving onto the next step. Wet-sieving tends to clean the samples up, so the smaller grain sizes (<>
Either way, place your crushed sample in the top sieve and shake until you have a decent separation (Usually takes ~5 minutes). Take each container and empty it into a properly labelled bag. The labels are as follows (sample # followed by sieve size range; ex: 040609-01 [10-20]):
Clean sieves between samples, using a toothbrush and a thin tool to remove grains lodged in the screen/mesh.
STEP 4: Cleaning: Rinse the sample in a beaker and slowly pour off the dirty water until it runs fairly clear (don’t lose any sample!). Allow to dry. Oven should not be above 55º C (to minimize loss of He from crystals).
STEP 5: Magnetic Separation: I start with a hand magnet and mesh sizes [20–40] and [40-60], unless there are olivines large enough to fall in the [10-20] range, then I use that fraction as well. Often, in my basalt samples, the matrix is very iron-rich and comes off easily with a fairly strong hand magnet. If the hand magnet provides a good separate, put the magnetic material back in the sample bag and save it. Save the non-magnetic part of the sample (olivine, pyroxene, probably some plag and calcite).
Details:
1) Hand magnet: Obtain a typical hand magnet (they’re fairly weak, but work well). Dump your minerals grains on a piece of 8X11.5 paper with a clean piece of paper adjacent to it. Place a plastic baggie or weighing paper over your magnet to keep magnetic grains from sticking to the magnet, thereby decreasing contamination between samples. Run the magnet over the mineral grains, placng the magnetic grains on the empty paper, leaving the nonmagnetic grains behind. In our case, we are generally interested in olivines, pyroxenes, and feldspar. These generally stay on the nonmagnetic side, unless they have lots of inclusions or are coated with magnetic material.
If for whatever reason, the hand magnet doesn’t yield a very good separation, move on to the Frantz magnetic separator.
You can also use a Frantz if the hand magnet doesn’t work. Make sure your sample is washed before using the Frantz.
2) Frantz Magnetic separator: It is best to work with a [40-60] range on this machine, but the [20-40] range is feasible. The larger grains just tend to clog up the sample cup every now and again.
Adjust the desired angle on the ramp by turning the proper knob/wheel. I usually use an angle between 15-20 degrees tilting away from me (15 degree works best). A shallow angle tilting down to the sample collection cups also seems most productive. It allows the grains to interact with the magnet for a longer period of time, allowing for a cleaner separate. Take your clean sample fraction and pour a small amount of it into the sample cup. Turn on all appropriate switches, adjusting the strength of the magnet by increasing or decreasing the amps. I usually start with 0.25 amps, run the sample through 2-3 times. This will separate out the very magnetic material from the less magnetic material. I then switch to a higher amp (somewhere between 1.0 and 1.5) and run the magnetic fraction (when run at 0.25) through (2-3 times). This will separate off the very nonmagnetic. Then I just play around with values in between until I get a nice separate of my mineral of interest. Before changing the amps, I check each collection cup under a microscope to see which has the largest amount of my mineral of interest. These values will vary with different samples. You just have to pick and choose, use what best suits your sample.
STEP 6: Heavy liquid separation: We use lithium metatungstate with a density of 3.0 g/cc. At this density, olivines and pyroxenes (“heavies”) sink and everything you don’t want (“lights”) floats to the surface.
Here’s the address for the company we order from. We use litium metatungstate (density = 3.0). It’s water soluble, allowing for a density variation and recycling.
GEOLIQUIDS
15 E. Palatine Rd., Suite 109
Prospects Heights, Illinois 60070
1-800-827-2411
We recently ordered 3 lbs at a cost of $144/lb, I think.
Here’s a list of equipment we use to
CRU-5000 Centrifuge
50 ml polypropylene, graduated, conical centrifuge tubes with caps
3-piece Whatman filter funnel (9 cm in diameter, 200 ml volume, 17.9 cm height, Whatman no. 1950-009)
Whatman filter papers (medium-fast (1), 9 cm in diameter)
- fill the bottom of centrifuge tubes with sample grains. (Don’t fill it past the 5 ml mark). Label clearly.
- add lithium metatungstate (at a density of at least 2.95, preferably 3.0 or greater) to the 25 or 30 ml line (depends on how much sample you use and how much heavy liquid you have to work with).
- Cap and shake all the tubes
- place in centrifuge at 1.5X1000 rpm for at least 10 minutes.
- have a doer of liquid nitrogen set aside and set up funnel/filtration apparatus.
- remove tubes from centrifuge,
STEP 7: Acids: I usually use HNO3, HCl , and HF to clean up the “heavies” samples. To get rid of any secondary calcite, start with dilute (5-10%) HNO3 and your “heavies” in a beaker placed in a sonicator for 15 to 20 minutes. Then use dilute (5-10%) HCl (in sonicator 15-20 minutes). Sometimes the minerals are well-oxidized. For example, oxidized olivines tend to have an iddingsite “rind” (a red coating) around them. Sometimes HCL will get rid of this. If it doesn’t, move onto a 5% HF solution.
HF treatment: WEAR HEAVY GLOVES, A LAB COAT, AND A FACE MASK. HF is very nasty stuff. Pour your minerals into a small glass or Nalgene beaker (HF etches glass, so if you use glass beakers, set them aside after that for HF use only) and add a 5% HF solution until it submerges your minerals. Don’t use too much. It isn’t necessary to fill the beaker, just top your minerals with the solution. Place in an ultrasound for 15-20 minutes, depending on how oxidized your sample is. Check your sample regularly to make sure you don’t dissolve you minerals completely. Pour off HF into waste container, rinse your sample, and dry. Repeat as necessary, until the majority of your sample is clean (iddingsite-free).
STEP 8: Microscope check. After isolating the olivine/pyroxene, and cleaning them up with acids etc, you should have a good separate. I always check under a microscope and handpick out what looks like crappy mineral grains (grains that are still dirty, or that are obviously not oliv/pyroxene). You want the purest separate of olivine or pyroxene possible.

Thus far, I have spent 10s of hours on the map. As a consequence, the correlation diagram has evolved significantly. The colors in the snippet do not match the map yet, and some of the unit labels have changed. Also, it is likely that some units will be added and some will be dropped as the project continues. All part of my mapping process, and is often maddening to my colleagues. Nonetheless, check it out and go with the flow.

