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prof_genius
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sad.gif posted on 1-7-2014 at 14:57
Discontinued reagents


I have recently seen that many chemical suppliers are discontinuing chemicals. I can no longer purchase picric acid from Merck, and thorium and uranium compounds are becoming scarce. I find this very annoying, why would they discontinue all these reagents? I have also seen sigma aldrich turn the riedel de haen product line into aldrich products, this also drove up the price. They are currently discontinuing a lot of Fluka Reagents. :( What are your thoughts about this?
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[*] posted on 1-7-2014 at 15:28


When I was working professionally this was rarely an issue. You sent the request to the purchasing department and they took care of all of the legwork. ;)

Now that I am retired and I am attempting to procure the common reagents and intermediates that I long took for granted I am realizing how difficult life has become for amateurs. With the help of the mountain of wisdom that is available on this site I am re-learning the basic preparative lab skills that I first learned over 50 years ago and I have again become "fluent" in the preparation of many basic reagents and starting materials, as well as finding alternative means to accomplish my desired synthetic tasks.

I am now coming to the realization that while something may have been lost, that possibly some more important has been gained. ;)
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[*] posted on 1-7-2014 at 15:39


It would be great if there could be a company that specialized in making reagents for amateurs. Or home chemist co-ops, in which multiple amateurs who live near each other pool resources to have a lab for preparing needed reagents in a semi-industrial manner to share.



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[*] posted on 1-7-2014 at 15:56


You make a good point. I have found that some reagent preps are difficult to scale down. I had considered trading but I have found that DoT regulations make this highly impractical, plus there is a potential legal liability if they are supplied to people who lack the necessary skills to handle them properly. :(

[Edited on 1-7-2014 by Burner]
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[*] posted on 1-7-2014 at 18:12


I have the same problem. I was set to acquire a whole bunch of hydrazine sulfate and redistribute it to SM, etc., until I learned about the insane shipping regulations regarding the chemical. Sadly the best method for amateurs to get exotic reagents is simply to order out of the country and have it shipped illegally.

On the other hand, if we all work together to make pictographic writeups concerning preparations of some intermediate reagents, we could all benefit SM and the chemistry community as a whole.

[Edited on 2-7-2014 by Praxichys]




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[*] posted on 1-7-2014 at 18:23


I have seen the same thing. Chemicals such as HOBT, Dess-Martin reagent, and a few others are hard to get, due to DOT issues, synthesis risks, and the like. But in many cases there are ways around, like buying a solution or diluted material, altering the reagent to make it less unstable, etc.

It is like a cat and mouse game or wack-a-mole, where you try to work round the latest problem with a new solution. Some of it is stupid, like picric acid and HOBT being put in the same shipping category as TNT or nitroglycerine, but other things like the Dess-Martin can be solved with a better synthesis.
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[*] posted on 1-7-2014 at 18:59


Quote: Originally posted by Praxichys  
Sadly the best method for amateurs to get exotic reagents is simply to order out of the country and have it shipped illegally.


With some trepidation I have considered this method for 2 reagents. I must say that in both cases I would be quite pleased with the price and likely the quality too.

I was concerned that US Customs would wrongly assume that the reagents were for making drugs or explosives. But as you rightly point out, improper shipping could also bring trouble with the DOT.




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[*] posted on 1-7-2014 at 19:37


I'd seriously consider trying to start an amateur chemist's co-op, except there aren't enough others near me, as far as I know.



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[*] posted on 2-7-2014 at 00:56


A chemist's co-op would be great because you could register it as a business and order from aldrich and merck. One of the main reasons i'm so mad about this is because I can no longer find thorium and uranium compounds from truste suppliers like BDH(now part of merck).

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[*] posted on 2-7-2014 at 05:13
Another trial by fire of professionalism


== Content removed ==

I'm going to apologize for this post by saying that I suggested doing something illegal and potentially life threatening to unsuspecting people for the purposes of profit. It is easy to forget about ethics when you take to heart the feeling of being wronged by years of the inability to acquire certain things because of restrictions designed to prevent people from getting hurt.

The reality of the situation is that there really is no good way to ship hazardous things cheaply anymore in the USA.

I guess instead of shipping chemicals, the best way might be to create some sort of collaborative space full of detailed syntheses of these intermediates.


[Edited on 2-7-2014 by Praxichys]




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[*] posted on 2-7-2014 at 05:57


Quote: Originally posted by Praxichys  

If the customers agree to waivers, pay dues, and are accepted into "the society" by application only, the only real risk is if a shipment somehow breaks open or is inspected, the odds of which during a domestic shipment are basically nothing.



That's what I thought too. Maybe I just got unlucky, but when I got some used glassware, the package was inspected even though it was domestic in the US. Three beakers were shattered from being dropped, I assume the inspector did it, because they were extremely padded in the middle of the box.
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[*] posted on 2-7-2014 at 06:00


Despite how nice it would be to have access to the big suppliers, deliberately mislabeling packages is dangerous and irresponsible. Consider this: you ship some lead nitrate in a box labeled "table salt." Something happens in the warehouse and everything breaks and spills (no matter how careful you are on your end, it can happen), and a worker cleaning it up gets the chemical all over themself. They say"oh don't worry it's just table salt," don't bother washing their hands, and now they have lead poisoning. It's not just foiling the government's rules - people handle your chemical shipments and could be seriously hurt if they aren't informed of what they are. I don't know; you might think you have an ironclad bulleted list there, but please consider the safety of everyone involved.

And deleteing your post after a few days is pointless. I saw it, others have seen it, and if something bad happens in one of your shipments investigators will find it. You don't think it's already been archived somewhere?



Edit: Case in point: gdflp's story about broken glass, despite being well-packaged. What if those were bottles filled with hazardous chemicals labeled as something innocuous? The inspector's health is now at risk.

[Edited on 7-2-2014 by MrHomeScientist]
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[*] posted on 2-7-2014 at 06:54


It's not all bad either. Turns out Lead Nitrate is easily shipped legally - up to 10lbs may be shipped FedEx without special labeling if packed under 49CFR 173.13.

I think a simple elimination of the unscrupulous side (namely, the mislabeling) of the model would actually make it work rather well. So:


Quote:

I have recently acquired the ability to order chemicals from name-brand companies (Acros, Sigma, etc) through my employer who has graciously let me use their accounts. My first order has finally cleared and I am receiving 100g cyanuric trichloride, 100g NaN3, and 500g KCN sometime next week.

I too am very interested in synthesizing some specialty chemicals, with the goal to supply the small industry this hobby creates. As long as the product is legally shipped (Which, for small amounts, is surprisingly lenient for most things), there shouldn't really be a problem.

If the customers agree to waivers, pay dues, and are accepted into "the society" by application only, we can control what goes where, and to whom.

And did I mention this is insanely profitable? My 500g KCN from Millipore was $18 plus shipping. This could easily be resold in the amateur market for something like $10/25g. The potential profit for that tiny bottle is something like $182, minus containers and the time spent weighing, packing, labeling, etc. The idea is to dump that profit into buying a great variety of stock, supplying very affordable amounts of hard to get chemicals to the amateur sector.

If some of the bigger people on this forum team up, we could form an unstoppable supply network with chemical stock spread across the country, getting the best deals on chemicals based on regional availability to maximize both economy to the customer as well as profit.





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[*] posted on 2-7-2014 at 07:26


There are DOT exceptions for small amounts of materials, typically under 35g, which can be used to ship small samples as such, without the normal labeling requirements. But the rules state that you must be trained to know which materials can be shipped that way and which cannot.

They still have to be in proper containers, sealed well, packaged well, bagged, and done in a manner that prevents leaks in any scenario. I used to put the material in a bottle, parafilm it, wrap in paper towels or similar material, put that in a bag, and then put that bag in a plastic container or metal can. That can then be shipped packed in side a cardboard box with some padding material. But my training is out of date, and the rules change often.
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[*] posted on 2-7-2014 at 07:42


Quote: Originally posted by Dr.Bob  
I used to put the material in a bottle, parafilm it, wrap in paper towels or similar material, put that in a bag, and then put that bag in a plastic container or metal can. That can then be shipped packed in side a cardboard box with some padding material. But my training is out of date, and the rules change often.

If they're requiring more safety measures than that now, that would be rather depressing…




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[*] posted on 2-7-2014 at 08:39


I think that another good approach to this problem would be to convince tomholm at Elemental Scientific to stock some of the more difficult to attain reagents. It's encouraging that he is maintaining good communication with us and seems open to this idea.

I believe he just has to be convinced that 1) there is sufficient profit, and 2) his liability for any problems resulting from our use of these more reactive, hazardous, etc, reagents is sufficiently low.




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[*] posted on 2-7-2014 at 08:56


Quote: Originally posted by Magpie  
2) his liability for any problems resulting from our use of these more reactive, hazardous, etc, reagents is sufficiently low.


I suspect that this will be partuicularly problematical. We are a highly diverse group with varying levels of skill and laboratory training, operating in facilities ranging from primitive to sophisticated, pursuing experiments that can be cookbook to bleeding edge. Let's face it - we are risky in this regard, and there is little I feel that we can do to alter that perception when significant legal liability may be attached to these decisions.
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[*] posted on 2-7-2014 at 08:58


@ DrBob

Correct me if I'm wrong, but let us use something reasonable, like 100g sodium azide through FedEx as an example.

http://images.fedex.com/us/services/pdf/HazmatShippingGuide....

This says it is a class 6.1 and is "Accepted only when packaged under applicable special permit or 49CFR 173.13"

So we look here at 49CFR 173.13:

http://www.gpo.gov/fdsys/pkg/CFR-2007-title49-vol2/xml/CFR-2...

And find that:

- The package need not be labeled externally and can travel on passenger aircraft if it meets § 173.27 (Not an issue)
- You can ship up to 6.25 pounds at a time, including innner packaging weight
- A bottle in a bag inside a padded cardboard box will suffice.

Pretty easy. It's exactly the same way I ship Hg metal. I think I'm missing something though... when do you need to take a class?

@ Magpie

And yes, getting Mr. Holm to do it would be nice, but I think a lot of us are capable of it ourselves and just don't realize it, unless I'm missing something big from the shipping perspective.

[Edited on 2-7-2014 by Praxichys]

[Edited on 2-7-2014 by Praxichys]




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[*] posted on 2-7-2014 at 09:57


I am saying that the government (DOT) says that you have to be trained in order to ship under the exception rule, meaning, "No placards", for smaller samples, which can be hazardous, and would otherwise need to be labels with diamonds, and other paperwork.

What FedEx says is just their rules, and is dated 2009, I am certain that things have changed since then. If you miss a DOT rule, FedEx may not care, but the DOT can still arrest you. Their rules are a nightmare, and the DOT regs span several hundred pages, so they are not that easy, as well they often conflict each other (eg black powder can be shipped in some cases without paperwork, but in other cases it needs to be placarded). I ship certain hazardous items often (just not current in the small sample rules) and I can tell you it is not as easy as many people think or some Chinese companies act.

See FedEx's disclaimer below and the training info below that.

For instance, Sodium Azide is considered to be an explosive in some cases, and is thus has extra rules, like in car airbags, which have to be shipped specially. Also, the post office has additional rules, which mean chemicals are best shipped Fed Ex. Another example. certain fireworks can be shipped via FedEx, other cannot, but all are 1.4 items. Even odder if that there are a few 1.4 items that cannot be shipped FedEx, but CAN be shipped by the post office. It is safe to say that the rules are very complex.

----
here is their disclaimer, read it carefully:

"FedEx Ground Package Systems Inc. is committed to the safe transportation of hazardous materials. It is very important that each
person engaged in the transportation of hazardous materials become
thoroughly familiar with the Title 49CFR (Code of Federal
Regulations). This guide is intended only to assist you in your
preparation of hazardous materials shipped via FedEx Ground
Package Systems Inc. It is the shipper’s responsibility to ensure
each hazardous material package is in compliance with applicable
Department of Transportation (D.O.T.) regulations and FedEx Ground
Package Systems Inc. requirements. Failure to comply with these
regulations and requirements may subject the shipper and carrier to
fines and penalties.
Due to the changing nature of D.O.T. regulations and other information, it is impossible to guarantee absolute accuracy of the material contained in this guide. FedEx Ground Package Systems Inc., therefore, cannot
assume any responsibility for omissions, errors, misprinting, or ambiguity contained within this guide and shall not be held liable in any degree for any loss or injury caused by such omission or error presented in this publication.
The FedEx Ground Hazardous Materials Shipping Guide is intended to simplify Title 49 CFR. FedEx Ground Package Systems Inc. reserves the right to be more restrictive than the federal regulations (49 CFR). Customers should be thoroughly familiar with the applicable sections of this guide when shipping hazardous materials via FedEx Ground Package Systems In c. This guide reflects current dockets under final rule published on or before March 1, 2009."
-----

Training
Hazardous material training is required for all employees who perform a hazardous material function. It is the duty of each hazmat employer to comply with the training requirements listed in 49 CFR 172.704.
FedEx Ground offers hazardous materials training via the online
ShipSafe.ShipSmart. Hazardous Materials Training Program. The training
curriculum includes the following:
•Rules and Regulations (Ground Shipping only)
•Hazard Classes and Divisions
•Shipping Papers
•Packaging (Non-Bulk Only)
•Marking and Labeling
•ORM-D Classification
•Security Awareness
The course is available at www.shipsafeshipsmart.com and is payable by credit card only. The cost for the class is $150.00. A discount is available for groups of more than three students. To obtain a discount please call 1-800-762-3744, ext. 6753 or ext 5059
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[*] posted on 2-7-2014 at 10:14


I appreciate you not getting defensive or anything regarding my post - I'm just trying to keep the safety of everyone involved in mind! Also any kind of 'shady dealings' like that only contributes to the bad press our hobby gets.

I also meant to mention the minimum quantity exceptions. Here's an excerpt from the CFR, section 173.4a, concerning quantities: (source: http://www.ecfr.gov/cgi-bin/text-idx?SID=165841281d11db03c72... )

Quote:
(c) Inner packaging limits. The maximum quantity of hazardous materials in each inner packaging is limited to:

(1) For toxic material with a Division 6.1 primary or subsidiary hazard, PG I or II—

(i) 1 g (0.04 ounce) for solids; or

(ii) 1 mL (0.03 ounce) for liquids;

(2) 30 g (1 ounce) or 30 mL (1 ounce) for solids or liquids other than those covered in paragraph (c)(1) of this section; and

(3) For gases a water capacity of 30 mL (1.8 cubic inches) or less.

(d) Outer packaging aggregate quantity limits. The maximum aggregate quantity of hazardous material contained in each outer packaging must not exceed the limits provided in the following paragraphs. For outer packagings containing more than one hazardous material, the aggregate quantity of hazardous material must not exceed the lowest permitted maximum aggregate quantity. The limits are as follows:

(1) For other than a Division 2.2 or Division 5.2 material:

(i) Packing Group I—300 g (0.66 pounds) for solids or 300 mL (0.08 gallons) for liquids;

(ii) Packing Group II—500 g (1.1 pounds) for solids or 500 mL (0.1 gallons) for liquids;

(iii) Packing Group III—1 kg (2.2 pounds) for solids or 1 L (0.2 gallons) for liquids;

(2) For Division 2.2 material, 1 L (61 cubic inches); or

(3) For Division 5.2 material, 500 g (1.1 pounds) for solids or 500 mL (0.1 gallons) for liquids.


And this is the overall section for transportation regulations: http://www.ecfr.gov/cgi-bin/text-idx?c=ecfr&tpl=/ecfrbro...

I had other links to the definitions of the different Classes and Packing groups, but they no longer work. I guess they've been updating the site and broke a lot of the links :/
You can see, though, that transporting and shipping HAZMAT is no easy task. I work with HAZMAT for my job with the government, so I deal with regulations for ordering, storing, and transporting this stuff on a regular basis. Even so, I feel like I know next to nothing about them.

[Edited on 7-2-2014 by MrHomeScientist]
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[*] posted on 2-7-2014 at 12:39


Quote: Originally posted by MrHomeScientist  
I appreciate you not getting defensive or anything regarding my post - I'm just trying to keep the safety of everyone involved in mind! Also any kind of 'shady dealings' like that only contributes to the bad press our hobby gets.

I also meant to mention the minimum quantity exceptions. Here's an excerpt from the CFR, section 173.4a, concerning quantities: (source: http://www.ecfr.gov/cgi-bin/text-idx?SID=165841281d11db03c72... )

[snip]


I think the lesson here is that both naïveté and 'red tape' are often discovered to be much more extensive than expected.

It just so happens that I also work for a company that handles hazardous materials on a daily basis. I handle them daily but I am not involved with the shipping side of things; however, I think I can weasel my way into a FedEx hazmat shipping class just to get a handle on the situation. I need to talk to someone in the shipping department. It would probably be an eye-opener.

So really it would appear that the easiest method is to do what was suggested above and make your materials in-house, necessitating some sort of "compendium of common lab preparations" as a substitute for simply ordering stuff.




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[*] posted on 2-7-2014 at 13:15


Quote: Originally posted by Praxichys  


So really it would appear that the easiest method is to do what was suggested above and make your materials in-house, necessitating some sort of "compendium of common lab preparations" as a substitute for simply ordering stuff.


Isn't this what we already have in "member publications" and Prepublication? Also we have a lot of good write-ups for syntheses that just haven't been formalized as such. Also there is Len1's book, which takes on some pretty hairy reagents IMO.




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[*] posted on 2-7-2014 at 14:24


Another trick is to make salts of liquids like triethylamine or pyridine, often they are lower hazards, as liquids are almost always harder to ship. It is easy to free base the material then with NaOH, which is still easy to get. I don't mean to be a pain, I ship a lot of non-hazardous items and some special hazardous ones, but not often via FedEx, so the rules are different. No two places have the same rules or even the same interpretation of the DOT rules.

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[*] posted on 4-7-2014 at 07:14
Discontinued Reagents


Hi All,

Very interesting topic. Thanks for thinking of me.

Many interesting points mentioned. No question that obtaining and shipping some of these chemicals has gotten more difficult. I certainly concur that mislabeling packages or bringing in product illegally from another country is not a good idea. A quick list of consequences might be:

  1. Personal liability for injury caused to innocent people - drivers, first responders, warehouse staff, etc.,
  2. Possible jail time,
  3. Serious fines,
  4. Loss of shipping privileges,
  5. Harmed reputation for all chemistry hobbyists,
  6. Even tougher laws in the future.

(Sorry, but I’m also a lawyer and can’t help myself.)

Shipping chemicals properly is not easy. I’ve found that most of the big players have resorted to shipping any chemical that can possibly be regulated as a hazardous material as hazardous and do not attempt to apply the exceptions. It’s not worth it to them to do the time-consuming research to determine if there is an exemption and take the risk associated with getting it wrong. Thus, they charge hazmat shipping charges for all regulated chemicals, regardless of amount.

If you do want to ship hazardous materials using the commercial carriers, e.g. UPS, FedEx, etc., (USPS will not accept any hazardous materials), you are required to show proof of training and state that you understand and will comply with both the shipper’s and DOT regulations. This requires you to be able to follow and apply the regulations as presented in Title 49 of the Code of Federal Regulations (CFR). (Even with my legal training, I do not find this easy and sometimes think that they’ve made it difficult on purpose to discourage the shipment of hazardous material.) Additionally, you need to keep your training up-to-date with regular, certified, training courses.

Hazardous materials shipping charges can have a big effect on the total cost of delivering a product. We have to pay hazmat charges ($20-$30) on most inbound regulated chemicals. Some of these chemicals also have additional “poison pack” packaging fee ($15-$25). For chemicals that we stock, we purchase larger quantities and distribute these added shipping charges over multiple sales transactions. For special orders, we need to recover these hazmat and poison pack charges from the one sales transaction. Often, we need to pay these same hazmat and poison pack charges on outbound shipments to the customer, unless we are able to apply a hazmat shipping exemption. These additional shipping charges can add $15-$55 on each shipping transaction or a total of $30-$110 in additional shipping charges (in addition to standard shipping charges). Add in the cost of the product, often greater than $100 for small quantities of these hard-to-get chemicals, and it’s not uncommon for the cost of the product to exceed $225, even before Elemental’s profit margins are included.

Some of these chemicals are sufficiently dangerous or toxic, and require a higher level of training in order to safely handle the chemicals. For these chemicals, I do not want my employees handling them or re-packaging them in smaller quantities, so we would need to sell them in the same quantities in which we are able to purchase them.

Elemental Scientific is open to looking into some of these more difficult or discontinued reagents to see what is possible. That is, after all, what we are here for. We are willing to do things that the larger chemical distributors are not, in order to build customer loyalty. That said, I want to make it clear that we are not willing to break the law or risk our shipping privileges to make a sale. We also need to be compensated for our time and these types of transactions can be very time consuming, so we have to weigh the number of potential sales of each chemical.

If someone could take the lead and put together a list of these “hard to get” chemicals, I would be willing to look into the availability and shipping costs associated with these chemicals and post a reply on this site. I suggest that the list be limited to those chemicals where there is at least sufficient volume of potential customers to make it worthwhile (I understand that shipping costs may have an impact on this). A “popularity” ranking, indicating the potential number of customers for the product, would be helpful.

Look forward to all comments and Happy 4th of July to everyone!




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[*] posted on 4-7-2014 at 12:04


Thank you Tom for that informative and encouraging post!

To follow up on your suggestion I feel that we should each post the 5 chemicals that we would most like to buy. Then at some time in the future, say 2 weeks from now I could assemble a combined list and the number of individual requests for each reagent. I suggest that for each chemical a volume in ml or a weight in g be included.

I would hope that we each would use good judgement in our submittals. There is no sense in asking for something that Tom is obviously are not going to want to handle.




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