Sample preparation for ICP analysis of biochar typically involves the following steps:
1. Homogenization: The biochar sample is first ground and homogenized to ensure that the sample is representative and that any heterogeneous material is evenly distributed.
2. Acid digestion: The homogenized sample is then digested in acid to dissolve the metals and other elements of interest. A mixture of hydrochloric acid (HCl) and nitric acid (HNO3) is commonly used for this purpose. The exact acid mixture and digestion conditions will depend on the specific elements being analyzed and the analytical method used.
3. Filtration: After digestion, the sample is filtered to remove any remaining solids that could interfere with the analysis.
4. Dilution: The filtered solution is then diluted with deionized water to bring the metal concentration within the working range of the ICP instrument.
5. Analysis: The diluted sample is then analyzed by ICP, which measures the concentrations of various metals and elements.
It's important to note that the sample preparation procedure may need to be optimized based on the specific biochar matrix and the metals of interest. The choice of acid mixture, digestion conditions, and dilution factor may need to be adjusted to ensure accurate and precise analysis.
Reference:
Mohan D, Pittman CU. Activated carbons and low cost adsorbents for remediation of tri- and hexavalent chromium from water. Journal of hazardous materials. 2006 Aug 25;137(2):762-811.
This paper might be helpful: Wathudura et al 2020.
Article Microwave and open vessel digestion methods for biochar
A couple of points to add to Lamia Fatima 's answer:
Homogenization needs to be done with a non-contaminating grinder. Steel toothed grinders can and do wear down, leaving quite noticeable amounts of their compostion in the sample. Often quite at random, which gets annoying. Use a known "clean" sample to check - 10 or 20 sequential samples should show up if any wear is occurring. We used to use rice as it had a low element density. You might need something a bit more substantial for biochar.
It depends on which elements you are interested in. Biochar may require some stronger acids than nitric and hydrochloric. PLEASE make sure you have the appropriate safety equipment if you use stronger acids, they can be very hazardous. Also, check the acid for contaminating elements. Glass is not as inert as you expect, and will leach elements (usually the ones you are interested in) into the acid during storage. This also goes for the test tubes you may be using to digest the samples, do a blank digest on all of them before starting, if you are unsure of their previous history (including brand new ones).
Filtration - like 1 and 2 above, can add contaminating elements to your samples. Centrifuging and careful decanting may be a better option. Test any hardware that comes in contact with samples and solutions for potential contamination.
Dilution, again, potential for contamination (1, 2 & 3 above), and errors in pipetting are also common at this stage. Note that some elements are not fully removed by ion-exchange units (Boron particularly).
Make sure your calibration standards match the composition of your digested samples, otherwise you will get erroneous results.
To supplement the suggestions of the above two experts: Complete digestion should be necessary, right? Digested samples should be clarified. If sedimentation occurs, and u centrifuge it, indicating incomplete digestion and get unreliable data.
Junhang Dong : It depends if "complete extraction" extracts "all" the metal constituents of interest. A complete digestion won't have any particulates, so won't need filtering (operator induced contamination). If there is Si or Ti (for example) still present in solid form, but it is not of interest to the study, then I would suggest it is not an efficient use of time and resources to attempt to dissolve these elements.
On the other hand, there is always the possibility of an insoluble component of Mn or Zn (for example) that requires that extra effort to solubilise.
Vivian Chimezie Usha , I forgot to mention: use of a reference material with known elemental composition (biochar, charcoal, coke, something along those lines) that you treat the same as your samples will give you an indication of how well your process works.