NDLI: A novel approach to high pressure flow digestion

Content Provider	Royal Society of Chemistry (RSC)
Author	Tirk, Paul Wiltsche, Helmar Winkler, Monika Motter, Herbert Knapp, Günter
Copyright Year	2014
Abstract	A new high pressure flow digestion system has been developed for sample digestion at a pressure of up to 40 bar and a temperature of about 230 °C. The reaction with acids takes place in a PFA tube and is heated by microwave radiation in a multimode cavity. As the PFA tube cannot withstand the harsh digestion conditions without support, it is placed inside a coiled glass tube pressurized by 40 bar nitrogen thus forming an autoclave. Corrosion of system components by acid fumes and related sample contamination is circumvented by establishing a slow but steady flow of the high pressure nitrogen countercurrent to the sample flow. The presented system does not constrain the selection of the digestion reagent. Acid cocktails of nitric acid with hydrochloric and/or hydrofluoric acid as well as hydrogen peroxide were successfully used for the digestion of various samples. The method accuracy was validated with five certified reference materials (BCR 62, DORM-2, NIST SRM 1515, NIST SRM 1567, NIST SRM 1568) and good agreement between the determined and the certified values was obtained for Al, Ca, Cr, Cu, Fe, Mg, Mn, Ni, Pb, and Zn using inductively coupled plasma optical emission spectrometry (ICP-OES) for analyte quantification. The flow digestion of the CRMs resulted in clear solutions with residual carbon concentrations (RCC) between 11 and 40%. Spike recoveries of Al, As, Ba, Be, Bi, Cd, Co, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Pb, Sb, Se, Sr, Ti, V, and Zn were between 94 and 105%. For Hg the spike recovery was 89%. The fully automated high pressure flow digestion system is capable of digesting up to 6 samples per hour.
Starting Page	272
Ending Page	279
Page Count	8
File Format	HTM / HTML PDF
ISSN	02679477
Volume Number	29
Issue Number	2
Journal	Journal of Analytical Atomic Spectrometry
DOI	10.1039/c3ja50290b
Language	English
Publisher	Royal Society of Chemistry
Access Restriction	Subscribed
Subject Keyword	PFA NIST Cu RCC Ba Spike Mo Microwave Nitrogen Autoclave Acid Countercurrent exchange Reagent Hydrogen peroxide National Institute of Standards and Technology Lead Inductively coupled plasma Inductively coupled plasma atomic emission spectroscopy Analyte Carbon Paramount Network
Content Type	Text
Resource Type	Article
Subject	Spectroscopy Analytical Chemistry

Sl.	Authority	Responsibilities	Communication Details
1	Ministry of Education (GoI), Department of Higher Education	Sanctioning Authority	https://www.education.gov.in/ict-initiatives
2	Indian Institute of Technology Kharagpur	Host Institute of the Project: The host institute of the project is responsible for providing infrastructure support and hosting the project	https://www.iitkgp.ac.in
3	National Digital Library of India Office, Indian Institute of Technology Kharagpur	The administrative and infrastructural headquarters of the project	Dr. B. Sutradhar bsutra@ndl.gov.in
4	Project PI / Joint PI	Principal Investigator and Joint Principal Investigators of the project	Dr. B. Sutradhar bsutra@ndl.gov.in Prof. Saswat Chakrabarti will be added soon
5	Website/Portal (Helpdesk)	Queries regarding NDLI and its services	support@ndl.gov.in
6	Contents and Copyright Issues	Queries related to content curation and copyright issues	content@ndl.gov.in
7	National Digital Library of India Club (NDLI Club)	Queries related to NDLI Club formation, support, user awareness program, seminar/symposium, collaboration, social media, promotion, and outreach	clubsupport@ndl.gov.in
8	Digital Preservation Centre (DPC)	Assistance with digitizing and archiving copyright-free printed books	dpc@ndl.gov.in
9	IDR Setup or Support	Queries related to establishment and support of Institutional Digital Repository (IDR) and IDR workshops	idr@ndl.gov.in

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