The IV Line courtesy of inorganicventures.com
Inorganic Ventures' E-newsletter · Spring Ed. 2006 · Volume 17
 
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In this issue:
 News from the Lab  Articles Online
 Analytical Quick Tip  IV Line Humor
 Microwave Digestion Procedure for Steel

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News from the Lab
Sample Preparation Guide

Sample Preparation Guide
We're excited to lauch our most ambitious series to date, Sample Preparation: Considerations In the Preparation of Elemental Chemical Solutions. The first two chapters are complete. New chapters will be added bimonthly through 2010. Take a look »

Improved Online Catalog
Our online catalog now includes detailed analyte tables for all products. Plus, we've added a new component search option to our search page, making your inorganic standards even easier to find.

Analytical Quick Tip

Don't trust volumetric pipette standard solution transfer. Weigh the aliquot of the standard taken. This can be easily calculated provided the density of the standard solution is known. There are too many possible pipetting errors to risk a volumetric transfer without checking the accuracy by weighing the aliquot.

Microwave Digestion Procedure for Steel

Weigh 0.1 to 0.2 grams of sample into a Teflon digestion vessel. A closed Teflon vessel with a pressure relief valve is suggested.

Add 6 mL HCl and 2 mL Nitric acid and allow to sit for the few minutes it takes for the mixture to become active, as indicated by a brown color and evidence of chlorine gas.

steel

Digest in microwave for 30 seconds at 50% power. Afterward, wait a minute or so. If necessary, add more acid as directed above and microwave an additional 30 seconds at 50% power -- repeat as necessary until complete. Note that many steels will go in during the first acid treatment.

Remove from the oven and add 1 mL of HF before diluting with water. Keep acid content in 5 to 10 % v/v range with either HCl or nitric acid. For steels, HCl is usually preferred. Please note that the acid used in the digestion works either on the sample or 'on itself' and is essentially used up. So please use fresh HCl or Nitric for dilution and add your acid before water when diluting.

The above procedure uses Aqua Regia, which does work for Fe, Al, V, as well as many other elements found in steel. HF is needed for Si and other refractories if present.

Articles Online  more articles »

Lithium, Sodium, Potassium, Rubidium and Cesium
This, the second installment of our Sample Preparation Guide, highlights preparation techniques for samples containing the alkali metals.

ICP Operations Guide (complete)
A clear 16-part online guide intended for anyone preparing samples and standards for measurement using ICP. Topics cover many day-to-day tasks required by all operators.

Reliable Measurements: A Guidebook for Trace Analysts (complete)
An essential 17-part online guide for chemical analysts. Topics cover all phases of sample collection, preparation, measurement, and data analysis.

IV Line Humor  more humor »

Q: What emotional disorder does a gas chomatograph suffer from?

A: Separation anxiety.
Elemental Spotlight
Zirconium

Analytical Periodic Table

Storage & Handling:  Keep tightly sealed when not in use. Store and use at 20 ± 4°C. Do not pipet from container. Do not return portions removed for pipetting to container.

Chemical Compatibility:  Soluble in concentrated HCl, HF, H2SO4 (very hot) and HNO3. Avoid H3PO4 and neutral to basic media. Unstable at ppm levels with metals that would pull F- away (i.e. - do not mix with Alkaline or Rare Earths or high levels of transition elements unless they are fluorinated). Stable with most inorganic anions but precipitation with phosphate, oxalate, and tartrate with a tendency to hydrolyze forming the hydrated oxide in all dilute acids except HF.

Stability:  2-100 ppb levels stable (alone or mixed with all other metals that are at comparable levels) as the Zr(F)6-2 + Zr(OH)4F2-2 for months in 1% HNO3 / LDPE container. 1-10,000 ppm single element solutions as the Zr(F)6-2 chemically stable for years in 2-5% HNO3 / trace HF in an LDPE container.

Zr Containing Samples (Preparation & Solution):  Metal (soluble in H2O / HF / HNO3); Oxide unlike TiO2, the ZrO2 is best fused in one of the following ways (Na2O2 in Ni0, Na2CO3 in Pt0 or Borax in Pt0); Organic Matrices (dry ash at 450°C in Pt0 and dissolve by fusing with Na2CO3 and dissolving in HF / HNO3 / H2O).

Excerpt from Inorganic Ventures' Analytical Periodic Table: Includes detailed analytical data for more than 70 elements.
 
Elemental Wordplay
Rearrange the elemental symbols to solve the riddle. Clues appear in quotes.

A "small striped mammal", this creature is born of...

    - Yttrium
    - Carbon
    - 2 parts Boron
    - Tantalum
    - and Astatine.

(answer at bottom of page)
**********************************************************************************************************
 Wordplay answer:  Tabby Cat (Ta,B,B,Y,C,At)
 The IV Line · News from the Lab  · Spring Edition 2006 (Volume 17)
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