Evaluation of calibration approaches for quantitative analysis of sludge by laser induced breakdown spectrometry
Sludge is a semi-solid organic waste from sewage treatment stations, whose disposal is a serious environmental issue. Application as a soil fertilizer is feasible due to its high organic matter and nutrient ( e.g. Ca, Fe, Zn, and Cu) contents, but it critically depends on a previous chemical analysi...
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| Veröffentlicht in: | Journal of analytical atomic spectrometry 2023-01, Vol.38 (1), p.131-141 |
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| creator | Thiengo, Fernanda Ferreira de Carvalho Elias, Aline Luz, Maciel Santos Intima, Danielle Polidrio Gaubeur, Ivanise Naozuka, Juliana Piovezani Rocha, Fbio Rodrigo Nomura, Cassiana Seimi |
| description | Sludge is a semi-solid organic waste from sewage treatment stations, whose disposal is a serious environmental issue. Application as a soil fertilizer is feasible due to its high organic matter and nutrient (
e.g.
Ca, Fe, Zn, and Cu) contents, but it critically depends on a previous chemical analysis. In this sense, laser-induced breakdown spectrometry (LIBS) deserves attention for skipping sample decomposition and due to the multi-elementary capacity. LIBS quantitative analysis requires proper calibration approaches to overcome matrix effects, mainly for complex samples as sludge. This work aims to propose an analytical method to directly determine Ca, Fe, Zn, and Cu in sludge by LIBS, after the evaluation of different calibration approaches: external calibration (EC), internal standard calibration (ISC), multi-energy calibration (MEC) and slope ratio calibration (SRC). EC, carried out using four certified reference materials (CRMs) with a similar composition to sludge samples, did not yield accurate analytical results. The differences between sample and standard ablated masses were successfully compensated for using carbon as the internal standard, except for Cu. MEC yielded accurate results for all analytes (relative errors |
| doi_str_mv | 10.1039/d2ja00292b |
| format | Article |
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e.g.
Ca, Fe, Zn, and Cu) contents, but it critically depends on a previous chemical analysis. In this sense, laser-induced breakdown spectrometry (LIBS) deserves attention for skipping sample decomposition and due to the multi-elementary capacity. LIBS quantitative analysis requires proper calibration approaches to overcome matrix effects, mainly for complex samples as sludge. This work aims to propose an analytical method to directly determine Ca, Fe, Zn, and Cu in sludge by LIBS, after the evaluation of different calibration approaches: external calibration (EC), internal standard calibration (ISC), multi-energy calibration (MEC) and slope ratio calibration (SRC). EC, carried out using four certified reference materials (CRMs) with a similar composition to sludge samples, did not yield accurate analytical results. The differences between sample and standard ablated masses were successfully compensated for using carbon as the internal standard, except for Cu. MEC yielded accurate results for all analytes (relative errors <5%), requiring only a single standard for calibration. Its main drawback is the need for at least 3 interference-free emission lines. The simplest and more practical calibration approach, also applicable with a single standard, but requiring only the response monitored at a single emission wavelength, was SRC, which yielded accurate results, as demonstrated by agreement with certified values at the 95% confidence level and relative errors <21%.
Sludge disposal is a serious environmental issue and its use in agriculture depends on chemical analysis.</description><identifier>ISSN: 0267-9477</identifier><identifier>EISSN: 1364-5544</identifier><identifier>DOI: 10.1039/d2ja00292b</identifier><language>eng</language><publisher>London: Royal Society of Chemistry</publisher><subject>Ablation ; Calcium ; Calibration ; Chemical analysis ; Confidence intervals ; Copper ; Emission ; Errors ; Laser induced breakdown ; Organic matter ; Pollution monitoring ; Quantitative analysis ; Scientific imaging ; Semisolids ; Sludge ; Spectrometry ; Spectroscopy ; Zinc</subject><ispartof>Journal of analytical atomic spectrometry, 2023-01, Vol.38 (1), p.131-141</ispartof><rights>Copyright Royal Society of Chemistry 2023</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c211t-9e8380dff218a1c717ee91fdb4b5724a0578033ca15327588fa4d2bff2ac14123</citedby><cites>FETCH-LOGICAL-c211t-9e8380dff218a1c717ee91fdb4b5724a0578033ca15327588fa4d2bff2ac14123</cites><orcidid>0000-0003-2517-6347 ; 0000-0003-1504-0323</orcidid></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><link.rule.ids>314,780,784,27924,27925</link.rule.ids></links><search><creatorcontrib>Thiengo, Fernanda Ferreira</creatorcontrib><creatorcontrib>de Carvalho Elias, Aline</creatorcontrib><creatorcontrib>Luz, Maciel Santos</creatorcontrib><creatorcontrib>Intima, Danielle Polidrio</creatorcontrib><creatorcontrib>Gaubeur, Ivanise</creatorcontrib><creatorcontrib>Naozuka, Juliana</creatorcontrib><creatorcontrib>Piovezani Rocha, Fbio Rodrigo</creatorcontrib><creatorcontrib>Nomura, Cassiana Seimi</creatorcontrib><title>Evaluation of calibration approaches for quantitative analysis of sludge by laser induced breakdown spectrometry</title><title>Journal of analytical atomic spectrometry</title><description>Sludge is a semi-solid organic waste from sewage treatment stations, whose disposal is a serious environmental issue. Application as a soil fertilizer is feasible due to its high organic matter and nutrient (
e.g.
Ca, Fe, Zn, and Cu) contents, but it critically depends on a previous chemical analysis. In this sense, laser-induced breakdown spectrometry (LIBS) deserves attention for skipping sample decomposition and due to the multi-elementary capacity. LIBS quantitative analysis requires proper calibration approaches to overcome matrix effects, mainly for complex samples as sludge. This work aims to propose an analytical method to directly determine Ca, Fe, Zn, and Cu in sludge by LIBS, after the evaluation of different calibration approaches: external calibration (EC), internal standard calibration (ISC), multi-energy calibration (MEC) and slope ratio calibration (SRC). EC, carried out using four certified reference materials (CRMs) with a similar composition to sludge samples, did not yield accurate analytical results. The differences between sample and standard ablated masses were successfully compensated for using carbon as the internal standard, except for Cu. MEC yielded accurate results for all analytes (relative errors <5%), requiring only a single standard for calibration. Its main drawback is the need for at least 3 interference-free emission lines. The simplest and more practical calibration approach, also applicable with a single standard, but requiring only the response monitored at a single emission wavelength, was SRC, which yielded accurate results, as demonstrated by agreement with certified values at the 95% confidence level and relative errors <21%.
Sludge disposal is a serious environmental issue and its use in agriculture depends on chemical analysis.</description><subject>Ablation</subject><subject>Calcium</subject><subject>Calibration</subject><subject>Chemical analysis</subject><subject>Confidence intervals</subject><subject>Copper</subject><subject>Emission</subject><subject>Errors</subject><subject>Laser induced breakdown</subject><subject>Organic matter</subject><subject>Pollution monitoring</subject><subject>Quantitative analysis</subject><subject>Scientific imaging</subject><subject>Semisolids</subject><subject>Sludge</subject><subject>Spectrometry</subject><subject>Spectroscopy</subject><subject>Zinc</subject><issn>0267-9477</issn><issn>1364-5544</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2023</creationdate><recordtype>article</recordtype><recordid>eNpFkEtLw0AQgBdRsFYv3oUFb0J0n93kWGt9UfCi5zDZh6am2XQ3qeTfmxrRywzDfDPMfAidU3JNCc9uDFsDISxjxQGaUD4TiZRCHKIJYTOVZEKpY3QS45oQIiSTE9Qsd1B10Ja-xt5hDVVZhLGEpgke9IeN2PmAtx3UbdkOvZ3FUEPVxzLuZ2LVmXeLix5XEG3AZW06bQ0ugoVP479qHBur2-A3tg39KTpyUEV79pun6O1--bp4TFYvD0-L-SrRjNI2yWzKU2KcYzQFqhVV1mbUmUIUUjEBRKqUcK6BSs6UTFMHwrBi4EFTQRmfostx7_DEtrOxzde-C8PZMWdqRgTnaghTdDVSOvgYg3V5E8oNhD6nJN8bze_Y8_zH6O0AX4xwiPqP-zfOvwEe9HSY</recordid><startdate>20230104</startdate><enddate>20230104</enddate><creator>Thiengo, Fernanda Ferreira</creator><creator>de Carvalho Elias, Aline</creator><creator>Luz, Maciel Santos</creator><creator>Intima, Danielle Polidrio</creator><creator>Gaubeur, Ivanise</creator><creator>Naozuka, Juliana</creator><creator>Piovezani Rocha, Fbio Rodrigo</creator><creator>Nomura, Cassiana Seimi</creator><general>Royal Society of Chemistry</general><scope>AAYXX</scope><scope>CITATION</scope><scope>7SR</scope><scope>7U5</scope><scope>8BQ</scope><scope>8FD</scope><scope>JG9</scope><scope>L7M</scope><orcidid>https://orcid.org/0000-0003-2517-6347</orcidid><orcidid>https://orcid.org/0000-0003-1504-0323</orcidid></search><sort><creationdate>20230104</creationdate><title>Evaluation of calibration approaches for quantitative analysis of sludge by laser induced breakdown spectrometry</title><author>Thiengo, Fernanda Ferreira ; de Carvalho Elias, Aline ; Luz, Maciel Santos ; Intima, Danielle Polidrio ; Gaubeur, Ivanise ; Naozuka, Juliana ; Piovezani Rocha, Fbio Rodrigo ; Nomura, Cassiana Seimi</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c211t-9e8380dff218a1c717ee91fdb4b5724a0578033ca15327588fa4d2bff2ac14123</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2023</creationdate><topic>Ablation</topic><topic>Calcium</topic><topic>Calibration</topic><topic>Chemical analysis</topic><topic>Confidence intervals</topic><topic>Copper</topic><topic>Emission</topic><topic>Errors</topic><topic>Laser induced breakdown</topic><topic>Organic matter</topic><topic>Pollution monitoring</topic><topic>Quantitative analysis</topic><topic>Scientific imaging</topic><topic>Semisolids</topic><topic>Sludge</topic><topic>Spectrometry</topic><topic>Spectroscopy</topic><topic>Zinc</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Thiengo, Fernanda Ferreira</creatorcontrib><creatorcontrib>de Carvalho Elias, Aline</creatorcontrib><creatorcontrib>Luz, Maciel Santos</creatorcontrib><creatorcontrib>Intima, Danielle Polidrio</creatorcontrib><creatorcontrib>Gaubeur, Ivanise</creatorcontrib><creatorcontrib>Naozuka, Juliana</creatorcontrib><creatorcontrib>Piovezani Rocha, Fbio Rodrigo</creatorcontrib><creatorcontrib>Nomura, Cassiana Seimi</creatorcontrib><collection>CrossRef</collection><collection>Engineered Materials Abstracts</collection><collection>Solid State and Superconductivity Abstracts</collection><collection>METADEX</collection><collection>Technology Research Database</collection><collection>Materials Research Database</collection><collection>Advanced Technologies Database with Aerospace</collection><jtitle>Journal of analytical atomic spectrometry</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Thiengo, Fernanda Ferreira</au><au>de Carvalho Elias, Aline</au><au>Luz, Maciel Santos</au><au>Intima, Danielle Polidrio</au><au>Gaubeur, Ivanise</au><au>Naozuka, Juliana</au><au>Piovezani Rocha, Fbio Rodrigo</au><au>Nomura, Cassiana Seimi</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Evaluation of calibration approaches for quantitative analysis of sludge by laser induced breakdown spectrometry</atitle><jtitle>Journal of analytical atomic spectrometry</jtitle><date>2023-01-04</date><risdate>2023</risdate><volume>38</volume><issue>1</issue><spage>131</spage><epage>141</epage><pages>131-141</pages><issn>0267-9477</issn><eissn>1364-5544</eissn><abstract>Sludge is a semi-solid organic waste from sewage treatment stations, whose disposal is a serious environmental issue. Application as a soil fertilizer is feasible due to its high organic matter and nutrient (
e.g.
Ca, Fe, Zn, and Cu) contents, but it critically depends on a previous chemical analysis. In this sense, laser-induced breakdown spectrometry (LIBS) deserves attention for skipping sample decomposition and due to the multi-elementary capacity. LIBS quantitative analysis requires proper calibration approaches to overcome matrix effects, mainly for complex samples as sludge. This work aims to propose an analytical method to directly determine Ca, Fe, Zn, and Cu in sludge by LIBS, after the evaluation of different calibration approaches: external calibration (EC), internal standard calibration (ISC), multi-energy calibration (MEC) and slope ratio calibration (SRC). EC, carried out using four certified reference materials (CRMs) with a similar composition to sludge samples, did not yield accurate analytical results. The differences between sample and standard ablated masses were successfully compensated for using carbon as the internal standard, except for Cu. MEC yielded accurate results for all analytes (relative errors <5%), requiring only a single standard for calibration. Its main drawback is the need for at least 3 interference-free emission lines. The simplest and more practical calibration approach, also applicable with a single standard, but requiring only the response monitored at a single emission wavelength, was SRC, which yielded accurate results, as demonstrated by agreement with certified values at the 95% confidence level and relative errors <21%.
Sludge disposal is a serious environmental issue and its use in agriculture depends on chemical analysis.</abstract><cop>London</cop><pub>Royal Society of Chemistry</pub><doi>10.1039/d2ja00292b</doi><tpages>11</tpages><orcidid>https://orcid.org/0000-0003-2517-6347</orcidid><orcidid>https://orcid.org/0000-0003-1504-0323</orcidid></addata></record> |
| fulltext | fulltext |
| identifier | ISSN: 0267-9477 |
| ispartof | Journal of analytical atomic spectrometry, 2023-01, Vol.38 (1), p.131-141 |
| issn | 0267-9477 1364-5544 |
| language | eng |
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| source | Royal Society Of Chemistry Journals 2008-; Alma/SFX Local Collection |
| subjects | Ablation Calcium Calibration Chemical analysis Confidence intervals Copper Emission Errors Laser induced breakdown Organic matter Pollution monitoring Quantitative analysis Scientific imaging Semisolids Sludge Spectrometry Spectroscopy Zinc |
| title | Evaluation of calibration approaches for quantitative analysis of sludge by laser induced breakdown spectrometry |
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