Most of the submission form is self-explanatory, but please feel free to email us if you have any questions about the form or your sample submission!
- Your sample should be named with a unique identifier.
- If you are requesting multiple techniques, we would prefer it that a separate vial of your compound is sent per technique. If this is not possible, we understand.
- The Multiple Samples button should only be used if you are submitting multiple samples with the same theoreticals, not if you are submitting multiple vials of the same compound for multiple techniques or submitting multiple samples of vastly different types or theoreticals. If you create your submission form incorrectly, you may be charged extra via our billing system.
- Ex: Compound DVA-165, for S, CHN and Br. Three vials, labelled A, B and C.
Sample name: DVA-165
Checked ICP (element sulfur), CHN and Halide (element Br)
In comment section: “Vial A is for ICP, B for CHN and C for halide.”
- Ex: 10 compounds, 1-10, for ICP (S, Na and Hg)
Sample names: 1, 2, 3, 4, 5, 6, 7, 8, 9, 10 using the Multiple Samples button
Checked ICP, making sure to check for S, Na and Hg analysis.
- Ex: 2 different compounds, KS-1 and KS-2, CHN via the air-sensitive protocol
2 separate submission forms, because the theoreticals are not the same.
Each submission form has CHN checked.
Each submission form has the 2 air-sensitive jar designations (XYZ A) for
that compound listed in the appropriate section.
- Ex: Compound DVA-165, for S, CHN and Br. Three vials, labelled A, B and C.
- A physical description (clear liquid, brown solid, etc) is more helpful than a chemical description for the Description section.
- Theoreticals can be estimated by the submitter. If you use a molecular formula in the correct section, it will automatically calculate the theoretical for the technique you select. If you do not know the boiling/melting points for your sample or do not have an attachable structure, please feel free to leave those sections blank.
- Please note in your sample submission whether your samples have any sensitivities (moisture, light, air, acid), precautions (volatile, toxic, explosive) and/or whether they need to be kept under temperature control or in a desiccator. If we don’t know how to store your sample correctly, we cannot be responsible for out of spec results due to improper storage before analysis.
The determination of the concentration of elements in your sample is based upon the direct weight of the material sampled. Therefore, it is very important that samples be dry of water and/or solvent (if the sample is not already in solution) and free of foreign substances such as dust, rust, hair, aluminum foil, parafilm, and paper filter fibers (the most common solid contaminant). Microscopic inspections have shown that often over half of the samples submitted are obviously contaminated.
Samples should also be as homogenous as possible. A sample vial with 10mg of sample, of which 75% is yellow powder and 25% is clear crystals, will give different results between duplicate CHN runs, simply because the ratio of powder to crystals in the 2mg of sample recovered from the vial per run vary the results seen. A lack of precision between sample runs may be a sign that your sample is not homogenous.
Most journals require a +0.40% for each element to be considered ‘in-spec’. (For comparison, NIST standards are 0.03%.) Typical compounds submitted have errors ranging from 0.05% to 0.45% (if not more!) if the compound has not been purified or is not homogenous (ex: a compound that is part liquid and part goo, different colored crystals, clumps vs needles).
- Ex: Let's say while putting your sample into a vial, a speck of graphite from your pencil fell into the vial and blended in with your black crystals. Let's also say that the speck of graphite weighs 100 µg (that's really a large speck by the way). The nominal sample size for CHN is 2000 µg. If the speck is taken as part of the sample, then there is a 5% error in the weight. It doesn't take much to throw the result off
The actual amount of sample needed depends on the concentration of elements to be detected. To avoid confusion, listed below are the requirements for minimum amount of sample needed per regular analysis. It is in the users' best interest to submit enough sample for duplicate analyses. Occasionally analyses will be repeated to verify results. If you are looking for low or trace amounts of element(s), the theoretical values will greatly determine how much sample is needed; please contact an analyst.
Please note that all elemental analysis techniques for this lab are destructive. Note in the Comment Section on the submission form if you would like your excess sample returned. For users outside of University of Illinois at Urbana-Champaign who wish to have their excess samples returned, you will be billed for shipment.
The laboratory does not have the equipment to break-up or grind large pieces of sample
NOTE: THE WEIGHT LISTED IS THE AMOUNT THAT MUST BE ABLE TO BE REMOVED FROM THE SAMPLE VIAL - NOT NECESSARILY THE AMOUNT YOU PUT INTO THE SAMPLE VIAL!
|SERVICE||MINIMUM AMOUNT NECESSARY|
|CHN (routine, duplicate)||5.0 – 6.0 mg recoverable material, preferably in a flat bottom ½ dram(12x35mm) vial. Trace analysis may need more material; talk to analyst. If only 2.0 – 3.0 mg material is recoverable, only one analysis will be run.|
|CHN (routine, soil, duplicate)||20.0 – 30.0 mg recoverable material
If only 10.0 – 15.0 mg material is recoverable, only one analysis will be run.
|CHN (non-routine, liquid (non-aqueous), goo)||9.0 – 15.0 mg recoverable material, preferably in a flat bottom ½ dram(12x35mm) vial. Trace analysis may need more material; talk to analyst. We will not run aqueous solutions via CHN. If only 3.0 – 5.0 mg material is recoverable, only one analysis will be run.|
|CHN (non-routine air sensitive, very moisture sensitive, unstable)||2.0 – 3.0 mg material per capsule via the air-sensitive protocol. If duplicate or more runs of the same compound are needed, prepare that number of jars. Trace analysis may need more material; talk to analyst.
Please talk with the CHN analyst via email or when you pick up the protocol jars to schedule when your samples will be run. For unstable samples, a specific time can be set up to minimize the time your sample is unanalyzed.
|ICP/METALS (solids)||2 - 10.0 mg recoverable material. Trace analysis may need more material; talk to analyst.|
|ICP/METALS (air sensitive)||10 mg via the air-sensitive protocol. If duplicate or more runs of the same compound are needed, prepare that number of jars. Trace analysis may need more material; talk to analyst.
Please talk with the ICP analyst via email or when you pick up the protocol jars to schedule when your samples will be run.
|ICP/METALS (predissolved, aqueous)||10.0 ml / element recoverable material|
|BIOLOGICAL (samples)||contact Elizabeth Eves|
|HALIDES (solids)||5.0 - 15.0 mg recoverable material, preferably in a flat bottom ½ dram(12x35mm) vial. Trace analysis may need more material; talk to analyst.|
|HALIDES (solutions)||Please talk with an analyst.|
|HALIDES (unstable or air sensitive)||Please talk with the analyst for amount necessary and how to use the air-sensitive protocol.
Please talk with the Halide analyst via email or when you pick up the protocol jars to schedule when your samples will be run.
Containers should be clean and all surfaces inert to your sample. Take into account how the sample will be recovered when planning your submission. If your sample is a film, recovery from a 20ml scintillation vial will be impractical, as all elemental analyses are based on a recorded weight, unless predissolved. Inadequate weights for the technique may affect your results. If you do not submit enough recoverable sample for the technique, you will still be charged for the runs that we attempt.
|Solids, powders, fibers, liquids, goo||flat-bottomed vial||<0.75" diameter|
|Extremely small samples||v-vial||<0.75" diameter|
|Predissolved, aqueous||10-100 ml||any size|
It is important to have sample ID on the sample vial container, not the vial cap. Please make sure your sample id on the vial and the online request match. This will avoid any confusion that may occur.
This protocol is for air-sensitive, especially-moisture-sensitive and unstable compounds. A drawer in 47 Noyes contains the plastic jars for the air-sensitive protocol, each which has its own unique designation. Inside each plastic jar, there is a glass vial with that same designation. Inside each vial, there is a pre-weighed capsule (red jars have tin capsules, blue jars have aluminum capsules). Each capsule should have an amount (dependent on the technique needed) of sample added, then the top of the capsule either crimped shut or cold-welded shut. Make sure that there is no excess compound on the outside of the capsule. The better the capsule is sealed, the less exposure there will be to the compound inside while the capsule is being weighed and then analyzed.
When the jars are procured, the client should talk with the analyst to set up a time for when the samples will be run and to see how much sample will be necessary. If you are an off-campus client, please contact Elizabeth Eves about shipping pre-weighed capsules to you.
Red jars: Tin capsules are for CHN analysis, fluoride analysis and aluminum analysis via ICP.
Blue jars: Aluminum capsules are for all other ICP analyses and all other halide analyses.
Since the lab has no feasible way of extracting excess sample from a capsule, it is important to put in as close to the recommended range as possible. Halide analyses may not completely combust. CHN analyses of overfilled capsules could lead to erroneous results. Analyses for ICP can be diluted, however.
Your results will be sent to you via email to the email address your account is made under. Depending on the status of the previous day’s runs, the sample que and whether instrument maintenance is needed, turnaround time for results is usually:
- CHN analysis: 2-3 business days. If 24-hour turnaround is needed, please talk to Elizabeth Eves (email@example.com).
- ICP analysis: 3-10 business days
- Halide analysis: 3-5 business days
These times will be longer if there are instrumental problems or maintenance or if the staff is reduced due to sickness, vacation or meetings.