STANDARD OPERATING PROCEDURES
Contents
1. saa Soil Plant Spectral World Diagnostics Lab ii Centre Code METH09V01 Date July 30 2014 Author Dickens Ateku STANDARD OPERATING PROCEDURES NEAR INFRARED DIFFUSE REFLECTANCE SPECTROSCOPY METHOD FOR ANALYSING SOILS AND PLANTS USING BRUKER MULTI PURPOSE ANALYSER SPECTROMETER Contact Details Telephone 254 20 7224000 4235 4279 4163 Email icraf speclab cgiar org Laboratory Manager Soilspec_ Lab Manager cgiar org Website www http worldagroforestry org research land health Address Details World Agroforestry Centre Mailing P O Box 30677 00100 Nairobi Kenya Physical address United Nations Avenue Off Limuru Road Gigiri Nairobi Kenya aaa STANDARD OPERATING PROCEDURE Date July 31 2014 or Qoae Code METH 09V01 Agroforestry Title Method for analysing samples for spectral Author Dickens Ateku characteristics in Mid IR range using MPA METHOD DOCUMENT CONTROL LOG Name and position Signature Author s Dickens Ateku Alubaka Senior Laboratory signature for completeness and Technician correctness of document Verifiers Dickens Ateku Alubaka Senior Laboratory signature for completeness and Technician correctness of document Beatrice Mwangi Laboratory Technician signature for completeness and correctness of document Authorizer Elvis Weullow Deputy Laboratory signature for completeness and Manager correctness of d2. assistance from an authorized service representative or an individual with training in electronic repair The instruments require a third wire protective grounding conductor REQUIREMENTS Equipment a Rolling pin b PVC c 2mm sieve d Sample holders Small Petri dish 7cm diameter Duroplan gt Wide Petri dish 9 cm diameter Duroplan gt Vials gt Mug 9cm diameter Cuvette for liquids transmission e Spatula f Non fluffy cloth 4 IMPA SOP Agrotorest Centre Qoae Code METH 09V01 y Diagnostics Lab Title Method for analysing samples for spectral Author Dickens Ateku STANDARD OPERATING PROCEDURE Date July 31 2014 characteristics in Mid IR range using MPA NOTE No reagents or chemicals used PROCEDURE Sample Analysis a Power up the instrument and log into the OPUS software Technician must get himself herself familiarized with operating instructions of the instrument by going through the ICRAF soil and plant spectral diagnostic laboratory adopted version of user manual for MPA Module Select the advance data collection option in OPUS and load the ICRAF soil and plant diagnostics laboratory adopted method by selecting and opening ICRAF MPA_SPHEREMACROSAMPLEICRAF XPM for solid samples diffuse reflectance Refer page 23 of the MPA manual Or MPA_SAMPLECOMPARTMENTICRAF30 XPM for liquid samples transmission page 16 Create a folder that i
3. dentifies the batch of soils being analyzed on the computer connected to the instrument Sample scanning process in carried out in OPUS LAB software Refer page 33 of the MPA technical manual As a part of quality control the lab records spectra of selected standard soils Grey standard and Kaolinite every day These spectra are saved in a separate folder C ICRAF RAW DAILY STANDARDS All spectra recorded on test samples should be saved in a separate folder For example C ICRAF RAW SOTUBA SITE SOILS 0 for all Sotuba soils Refer page 33 of the MPA SOP manual Place the sample holder petri dish on the instrument against the Infra red light and start scanning Refer page 58 MPA manual 5 IMPA SOP QUALITY CONTROL Reference Material a Reference standards Infrared ICRAF laboratory uses Katumani High Black Cracking Clay Soil HBCCS and Mua soils Grey Standard and Kaolinite as reference standards Everyday new spectra are recorded on these samples before analyzing test samples and checked against the previous records Appropriate correction actions where necessary are implemented Normally no adjustments are required b Blanks A standard internal gold reference is used to correct the background c Calibration No calibration is required d Duplicates Not used e Quick Compare Perform opus quick compare of the standards to see how the instrument is performing refer to the MPA Technical manual 1 Data Validat
4. ion a Data Review gt Check the sample data and QC data to verify that the data to be reported is based on acceptable analyses and meet acceptable limits Verify that Mua standard spectra have been entered into the appropriate logs Verify that the results are saved in appropriate folder and format Place data in the laboratory database b Supervisor Review gt Check the sample data and QC data to verify that the data to be reported is based on acceptable analyses and meet acceptable limits gt lf any errors are found return data for repeat analysis REFERENCES 2 Multi Purpose Analyzer User Manual BRUKER OPTIC 2003 page1 page 48 eis roforest w Centre di Soil Plant Spectral Diagnostics Lab STANDARD OPERATING PROCEDURE Code METH 09V01 Date July 31 2014 Title Method for analysing samples for spectral characteristics in Mid IR range using MPA Author Dickens Ateku ANNEX 1 Work Flow Infra red Laboratory Workflow MPA amp ASD This laboratory uses infra red rays to analyze samples Objective To provide fast high through put cheap and accurate analysis optimization of analysis LEGEND Terminal point Action point Decision point Tape notes Stored data LOO Process route Operates in Near Infra Red Sample Compartment Transmission Mode This is used to analyze liquid samples Load the method
5. ion of diffuse reflected light is optimized and the detection of specular reflected light is minimized A DRIFT is an analyzing technique in FT IR spectroscopy that makes use of the phenomenon of diffuse reflection The key advantage of these techniques is that it enables analysis of strongly scattering and absorbing samples unlike transmission measurements and equally has high signal intensity ABBREVIATIONS AND DEFINITIONS DRIFT Diffuse Reflectance Fourier Transform spectroscopy OPUS Bruker s Optical User Software STD standard soil sample PVC Poly Vinyl Chloride SOP standard operating procedures NIR near infra red MPA Multi Purpose Analyze 3 MPA SOP Title Method for analysing samples for spectral Author Dickens Ateku pm Centre STANDARD OPERATING PROCEDURE Date July 31 2014 Soil Plant Spectral Code METH 09V01 Diagnostics Lab Title Method for analysing samples for spectral characteristics in Mid IR range using MPA Author Dickens Ateku RELATED DOCUMENT Multi Purpose Analyzer Technical Manual Sample Reception and Preparation SOP NIR Workflow nfrared Health and Safety RELATED FORMS Login form Recording sheet SAFETY AND ENVIRONMENT Electrical hazards Electrical systems must conform to the ICRAF standards No shock hazards exist inside the instruments Do not try to repair the faulty electrical system but call for
6. ocument Distribution of valid copies of this document G 149 Infrared Spectroscopy Laboratory Revise date before Historical dates of previous issues data Date to be filled in once the document has become obsolete and is archived retrieval Changes in this version compared to previous version Describe what has changed in the text of this version compared to the previous version 2 MPA SOP pia Agroforest Centre STANDARD OPERATING PROCEDURE Date July 31 2014 Qoae Code METH 09V01 y Diagnostics Lab characteristics in Mid IR range using MPA SCOPE AND APPLICATION This is a World Agroforestry Centre s Soil Plant Spectral Diagnostic Laboratory SOP for analysis of various chemical properties in both soils and plants using near IR spectra recorded with MPA module The technique involves shinning of near infrared light on the samples and capturing of the diffuse reflected light in to raw file known as the interferogram The spectrum thus recorded bears the qualitative and quantitative chemical aspect of the sample for further use with various data processing systems This SOP is applicable to those doing analysis on infrared laboratory using MPA spectrometer Module PRINCIPLE The MPA Module is designed for measurements in diffuse reflection and transmission The optics of a diffuse reflection accessory is designed in such a way that detect
7. then scan the sample Integrating Sphere Pa This method uses diffuse reflectance to analyze samples Direct Method Place petridish vials on integrating sphere window MPA Multi Purpose From Preparation Factory All the processes for sample preparation are outlined in the sample preparation workflow and SOP ASD ASD Analytical Device Operates in visible Near Infra Red UE e 4 19 Spectral Sample Scanning on lamp probe mug to Reflectance mode obtain spectra Put the sample petridish Rotating Arm Place a wide petridish or the sample cup on the rotating arm Samples Choose the method then scan the samples to obtain spectral signatures 7 IMPA SOP Scanning Data Processing All the data processes are illustrated in the SOP To Database Method not frequently used eis Agroforest Centre id STANDARD OPERATING PROCEDURE Date July 31 2014 Qoae Code METH 09V01 y Diagnostics Lab Title Method for analysing samples for spectral Author Dickens Ateku characteristics in Mid IR range using MPA 2 Infrared MPA spectrometer standards fact sheets MPA Instrument calibration standards These are standards used for all analysis in the ICRAF Soil Plant diagnostic laboratory gt Heavy black cracking clay soils HBCCS Katumani and MUA standards are r
8. un every day in the morning before you start any analysis and every time you start on a new site gt Grey card Kaolinite clay and White sand are commercial Standards which are run every day in the morning before you start any analysis and every time you start on a new site 3 Quality Control fact sheet PROCESS DESCRIPTION Background Measurement The instrument is set in a way that it forces the user to perform Background measurement after every 1 hour The measurement normally increases the signal to noise ratio of the spectrum produced improves the quality of the spectra Measurement of the selected soil standards The standards used in ICRAF infrared laboratory are HBCCS Katumani MUA Kaolinite Grey card and White Sand The measured spectra are used to monitor the performance of the instrument Check on the quality of the spectrum measured Always monitor the instrument moisture Ensure that the spectrum measured does not have any noise due to moisture and carbon dioxide The moisture noise peaks are expected at around 3600cm and 1600cm wave numbers while the carbon dioxide peak is expected at around 2400cm wave numbers 8IMPA SOP
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