Doe ib - LQUIODRGOT LABORATORY MANAGEMENT SERVICES KUALITI ALAM SDN BHD [Page Toft WORK/QUALITY INSTRUCTIONS TsweNo. #1 [RevNo: 0) PRETREATMENT OF SOLID SAMPLES Tssue Dae 3007/2002 FOR METAL ANALYSIS USEPA SW 846 30508 Issued by : General Manager 2. SW846 Method 3050B Acid Digestion of Sediments, Siudges And Soils Purpose: To provide method for the acid digestion of sample prior to trace metals, analysis. Scope: ‘This method is applicable to acid digestion of sediments, sludges and soils for analysis by ICP-OES , FLA. Sample is refluxed with acid-peroxide digestate during which metals associated with particulates or solids are converted to a form (ree metals) Which can be determined by atomic absorption spectrometry or inductively coupled plasma spectroscopy. 4, Safety Precautions: 4.1.1 Hydrochloric acid and nitric acid are corrosive. Avoid contact with body. 4.1.2 Hydrogen peroxide is a strong oxidizing agent and corrosive. Handle it in fume hood and avoid contact with its vapours. Keep away flammable materials from it. 4,13 Follow the instructions in “Prosedur dan Peraturan Keselamatan Di Dalam Makmal”. 5. Equipment/Apparatus: 5.1.1 Block digester- able to maintain a temperature of 90- 95°C 5.1.2. Digestion vessel 250ml 5.13 Wateh glassDes ID = LQNTOODOOT LABORATORY MANAGEMENT SERVICES KUALITI ALAM SDNBED Page 2 of 2 WORK/QUALITY INSTRUCTIONS Tesue No. :1 [RevNo:0 PRETREATMENT OF SOLID SAMPLES Teoue Date: 300772002 FOR METAL ANALYSIS USEPA SW 846 30508, ‘Issued by + General Manager 5.1.4 Analytical balance- capable of accurate weighing to 0.01g, S.L5 Funnel 5.1.6 Graduated cylinder 5.1.7 Volumetric flasks 100m! 6. Materials/Reagents: (Reagent grade chemicals shall be used unless otherwise indicated) 6.1.1 Concentrated nitric acid 6.1.2 Nitric acid 1:1 6.1.3 Concentrated hydrochloric acid 6.1.4 Hydrogen peroxide 30% 6.1.5. Deionised water 6.1.6 Filter paper Whatman No.41 or equivalent 6.1.7 Stock standard solution: Silver (1000 mg/l), Arsenic(1000mgil), Barium(1000mg/), -Boron(1000mg/}, _Calefum(1000mg/!), Cadmium(1000mel), Cobalt(1000mg/l), _ Chromium(1000mg/1), Copper(1000mg/), _Iron(i000me/l), —_ Magnesium(1000mg/1), Nickel(1000me/l), _ Manganese(000mg/l), —-‘Lead(1000mg/1), ‘Zino(1000mg/l), Setenium(1000mg/1). Procedure: 7.1 Weigh 1 to 2 g (wet weight) sample to the nearest 0.01g, record weight and transfer sample to digestion vessel. 7.2 Ima hood, add 10ml of 1:1HNOs to the sample. Mix the slurry and cover with watch glass. Heat the sample to 95°C and reflux for 10 to 15 minutes without boiling.Doe ID = LQUI00200T LABORATORY MANAGEMENT SERVICES ‘KUALITL ALAM SDN BED [Page 3083 WORKIQUALITY INSTRUCTIONS, TsueNo, 71 [RevNo:0 PRETREATMENT OF SOLID SAMPLES Teave Date : 300072002 FOR METAL ANALYSIS. ‘USEPA SW 846 30508, Issued by + General Manager 73 14 18 16 16 1 18 Allow the sample to cool, add 5 ml of cone. HNOs and reflux for 30 minutes. Tf brown fume are generated repeat this step (add Sml of cone. HINO) until no brown fumes. Allow the solution to evaporate to approximately Sml without boiling for two hours. ‘Wait for the solution to cool. Add 2ml of deionised water and 3ml of 30% H202. Cover the vessel with a watch glass. Heat until effervescence subsides and cool the vessel. Continue to add 1 ml of 30% HO, with warming until the effervescence is minimal (Do not add more than 10ral of 30% HO2 in total), Heat until the volume has been reduced to approximately Smal or heat at 95°C without boiling for two hours. Continue fo add 1 ml of 30% 1,02 with warming until the ‘effervescence is minimal ( Do not add more than 10m! of 30% Ha in total), Heat until the volume has been reduced to approximately Sal or heat at 95°C without boiling for two hours. Add 10ml cone, HCE to the sample. Heat and reflux at 95°C for 15, minutes, Cool and filter the digestate through Whatman 41 and collect filtrate in a 100m! volumetric flask, Wash down vessel walls with two Sml portion of deionised water and add these rinsing to the flask. Make to volume and analyse by ICP-OES ot FLA. Quality control 7.8.1 Run a minimum of one method blank per sample batch. 7.8.2. To one sample out of every twenty (or one sample from each, group of sample if less than twenty are being anaylsed), add 5 ml of 16 clements (Ag, As, B, Ba, Ca, Cd, Co, Cr, Ca, Fe, Mg, Ni, Ma, Pb, Zn, Se) standard solution ( from step 7.9 Yinto 100ml of volumetric flask containing sample to be digested and mark up to 100ml using the same sample solution. This spiked sample is run in duplicate. The final concentration of each metals is 5 mg/l.LABORATORY MANAGEMENT SERVICES Doe ID = LQTOORROOT KKUALITI ALAM SDN BHD Page tor WORK/QUALITY INSTRUCTIONS TssueNo st JRevNo:0 ‘PRETREATMENT OF SOLID SAMPLES Tissue Dato 30/07/2002 FOR METAL ANALYSIS USEPA SW 846 30508 Tssved by : General Manager 19 Preparation of 16 elements standard solution 7.9.1 Transfer 50 ml of cach clement of the 1000 mg/l stock standard 79.2 793 194 195 196 19.1 solution into 1 litre volumetric flask, Mark up to 1 L using 2% HNO, Digestion procedure to improve solubility and recoveries of antimony, barium, lead and silver. ‘Add 2.5 ml cone. HNO3 and 10 ml cone, HCL to a 1 - 2g ‘sample (wet weight) and cover with a watchglass. Place the ‘sample in the vessel and reflux for 15 minutes. Filter the digestate through Whatman No. 41 filter paper and collect filtrate in a 100 ml volumetric flask. Wash the filter paper, while still in the funnel, with no more than 5 mi of hot ( ~95°C) HCI, then with 20 ml of hot (~95°C) reagent water. Collect washings in the same 100 ml volumetsic flask. Remove the filter and residue from the funnel, and place them back in the vessel. Add Sml of conc. HCI, place the vessel back on the heating source, and heat at 95°C 4 $°C until the filter paper dissolves. Remove the vessel from the heating source and wash the cover and sides with reagent water. Filter the residue and collect the filtrate in the same 100 ml volumetric flask. Allow filtrate to cool, then dilute to volume. If a precipitate forms on the bottom of a flask, add up to 10 ml of concentrated HCI to dissolve the precipitate. After precipitate is dissolved, dilute to volume with reagent water, ‘Analyse by ICP-OES ot FLAA.LABORATORY MANAGEMENT SERVICES KUALITI ALAM SDN BED WORKIQUALITY INSTRUCTIONS: Doe 1D : LQU1007227001 [Page 5005 Tssve No. #7 fRevNos0 PRETREATMENT OF SOLID SAMPLES FOR METAL ANALYSIS USERA SW 846 30508 Tesue Dale 30/07/2002, Tssued by : General Manager Caleulation: Concentration of the metals in the spiked sample, X + ¥ Where X= concentration of spiked sample Reference: original concentration of metal which is diluted by a factor of 0.95 Test Methods for Evaluating Solid Waste, United States Environmental Protection Agency November 1996 Third Edition ( SW 846 method 30508)Dos. No -LQIToORGoT LABORATORY MANAGEMENT SERVICES KUALITLALAM SDN BHD Page Tof 10 WORK / QUALITY INSTRUCTIONS Tssue No, +f] RevNo:6 Tesue Da 01/06/2005 DETERMINATION OF METALS BY ICP USEPA SW 846 Method 6010 B Issued by : General Manager 2 4. 5. Inductively Coupled Plasma- SW 846 Method 60108 Purpose : ‘To provide a method for the determination of metals in solution by inductively coupled plasma-atomic emission spectrometry (ICP-AES) where the results, are not meant for regulatory purposes under the Environmental Quality (Sewage and Industrial Effluent) Regulations 1979. Scope : This method is applicable for ground water, aqueous samples, TCLP and EP extracts, industrial and organic wastes, soils, sludges, sediments and other solid wastes that has been suitably extracted with acid, When analyzing groundwater for dissolved elements, semples that have been prefiltered and acidified will not need acid digestion Principle : Extract from the digested sample is nebulized and the resulting aerosol is transported to the plasma torch. Elemont-specific emission spectra are produced by a radio-frequency inductively coupled plasma. The spectra are dispersed by a grating spectrometer, and the intensities of the emission lines at specific wavelength are measured and used to determine the concentration of the elements of interest. Safety Precautions : 4.1 Pretreated samples contain strong acids. Avoid contact with the samples. 4.2 Follow the instructions in “Prosedur dan Peraturan Keselamatan Di Dalam Makmat”, ‘Equipment/Apparatus : 5.1 Inductively Coupled Plasma Emission SpectrometerDoe. No QU TOUGHT LABORATORY MANAGEMENT SERVICES KUALITL ALAM SDN BED Page 2 of 10 WORK./ QUALITY INSTRUCTIONS Issue No. #1] RevNor6 Trove Date: 01/06/2006 DETERMINATION OF METALS BY ICP USEPA SW 846 Method 6010 B Tssued by : General Manager 6 3.1.1 Emission spectrometer with inter-element correction software and/or background correction facility 5.1.2 Radio-frequeney generator compliant with FCC regulations 5.1.3 Mass flow controller for argon nebulizer gas supply. 5.14 Peristaltic pump 5.15 Autosampler 5.2. Volumetric flasks of suitable precision and accuracy 5.3. Volumetric pipettes of suitable precision and accuracy Reagents/materials : (Reagent or trace metals grade chemicals shall be used in all tests) 6.1 Nitric acid (cone), HNOs 6.2 Nitric acid (1:1), HNOs. Add 500ml concentrated HINOs to 400 ml ‘water and dilute to 1 liter in an appropriately sized beaker. 63 Hydrochloric acid (conc.), HCL 6.4 Hydrochloric acid (1:1), HCL. Add 500 ml concentrated HCI to 400 ml ‘water and diluted t0 I liter in an appropriately sized beaker. 6.5 Reagent Water. All references to water in the method refer to reagent water. Reagent water must be interference free. 6.6 Standard stock solutions may be purchased or prepared from ulira-high purity grade chemicals or metals (99.99% pure or greater), All salts must be dried for 1 hour at 105°C, unless otherwise specified. 6.7 Argon gas —high purity 68 Nitrogen gas 69 Compressed airLABORATORY MANAGEMENT SERVICES KUALITI ALAM SDN BED WORK / QUALITY INSTRUCTIONS Doe. No TL QI TOORONOT Page dof 10 Issue No. 21] Revo DETERMINATION OF METALS BY ICP Issue Date 01/06/2006 USEPA SW 846 Method 6010 B Issued by : General Manager 7 Preparation of Standard Solutions 7.1 Mixed calibration standard solutions Prepare mixed calibration standard solutions by combining appropriate ‘volumes of the stock solutions in volumetric flasks as listed below: ‘Table 1 : Low range calibration ‘neat Wardangh | — —Strdard onesies | Eguiant Vane (i) of 05" | “Qualiy Canto ™ gt Veomghicnatbal | Sunes eh SGT | SRT] Sead | Sa] Sandee) Sela [COV] TO 2 Hi 5 Ag [326068 | 1 | “s_ | 10 [or [03s [10 5 | 3 és__1193.96 | 1 |_5 { 1 | oi [os [10 | 5 [5 B [249677 | 1 | 5 | 1 | 01 [os [10 [5 | 5 Ba__|233527| 1 | 5 | 10 | 01 [os [| 10 [ 5 | 5 Ca__[317933 | 1 | 5 | 10 | o1 [os [to | 5 [5 Ca_|oesoz ti {5 [10 [or |os [10 [ 5s | 5 Co__[2286i6 | 1 | 5 | 10 [or fos | 10 [5 | 5 Cr__ (267.716 | 1 | 5 | 0 [or | os [io | 5s | 5 Cu__|324.752 | 1 | 8 [| 10 [or | os [10 [5 | 5 Fe [238204 | 1 | 5 | 10 | o1 | 05 [10 [5 | Mg_[285213.| 1 | 5 | 10 | or | os [10 [5 | 5 Ni [231.608 | 1 [5 [10 [01 [os | 10 [5 [5 Ma_|257.610, 1 | 5 | 10 | 01 [os | 10 | 5 | ~5 Pb [270353 | 1 | 5 | 10 | 01 [os | io [5 | 5 %__ 1213857 | 1 | 5 | 10 | 01 [05 | io [5 | 5 Se 1196026 [ 1 [5 | 10 | o1 [os [10 [5s [7s Table 2 : High range calibration emai] Wake | ——Sunaartomcetatin |” Bgnaie Valine (a) atv0ak | Qualiy Conor m eh ietea ten nz | Sandesh Sad] | Sa sist | Senet | ager [COV TOV aes 3 As__[is3.606 [1 | 35 [50 | 02 [30 25 | 35 Cd__[228.802 | 1 [25 | 50 | 02 | 5: 25_| 25 Gr __f267.716 | 2 | 50 | 100 | 94 | 30 | 25 Cu [324.752 [2 | 50_| 100 | 04 50 | 25 Ni_[231.604 [~4 [100 [200 | 0.4 50 | 25) Po [220.353 | 2 | 50 | 100 | 0.8 100_[ 25 Za [213.857 | 6 | 150 [300 | 1 150_|_25_]‘Dos, No 191 Toon aor LABORATORY MANAGEMENT SERVICES KUALITI ALAM SDN BED. Page For 10 WORK / QUALITY INSTRUCTIONS TsueNo. :1] RevNor 6 DETERMINATION OF METALS BY ICP Tssue Dato: 0106/2006 USEPA SW 846 Method 6010 B Tssved by + General Manager 72 73 14 18 16 Prepare the standard solutions as in Table 1 or 2, which ever is, applicable, For example, Standard 2 for low range calibration is 5 mg/l for all the elements. Prepare this concentration of working solution by transferring an amount equivalent to 0.5 ml of 1000 mg/l stock standard solution of each element into 100 ml of volumetric flask. ‘Mark up fo 100 ml using 2% HNOs ‘Altematively, for low range calibration prepare intermediate standard by transferring 10 ml of 1000ppm standard stock solution for each clement into 200ml volumetric flask. Mark up to 200ml using 2% HINO3 to give a SOmg/I solution. To prepare standard 3, pipette 20m! of intermediate siandard solution and transfer it to 100ml volumetric flask. Mark up to 100m! using 2% HNO3. To prepare standard 2, pipette 10mi of intermediate standard solution and transfer it to 100ml volumetric flask. Mark up to 100ml using HINO3. To prepare standard 1, pipette 2mI of intermediate standard solution and transfer it to 100ml volumetric flask. Mark up to 100ml using HNO3. For high range calibration, prepare standard 3 by transferring ‘appropriate volume of each stock 1000ppm solution, as stated in table 2 into 200ml volumetric flask. Mark up to 200ml using 2%4HNO3. For standard 2 and standard 1 prepare a serial dilution from standard 3. Use the three calibration standard solutions (Mixed Standard 1, 2, 3) to standardize the instrument. Preparation of the Quality Control solution, Prepare the Quality Control solution by mixing the appropriate amount of stock standard solution, as stated in Table 3, Mark up to 100 ml using 2% HNO,‘Bos. No LOI TOORDIOT LABORATORY MANAGEMENT SERVICES KVALITI ALAM SDN BED Page Sof 10 WORK / QUALITY INSTRUCTIONS TssueNo. iT] RevNo: 6 “Tssue Datos OV06R006 DETERMINATION OF METALS BY ICP USEPA SW 846 Method 6010B Issued by + Genecal Manager Table 3 : Preparation of Quality Control Solution QC Type [Elements | QC conc. Volume A Tow range] ICV) Each 3 i Dial intermediate siock of Soppm calibration element in 100m volumetric flask cov [ach 3 Toil intermediate soak of SOppm element in 100 volumetric flask High TeV| Each DS [BS ml stock soln oF 1000p range element 100m volumetric flask calibration [CCV] AS DB | Sil stock soln of 1000ppm in 100ml volumetric ask Ca DS [2S al stock soln of F000ppm in 100ml volumetric flask or 30 [SO stock soln of 1000ppm in 100ml volumetric flask a BO} S30 mt stock sin of 1000p Ie 1002 volumetric flask Pb 30) SmI sock soln of 1000ppar in 100m volumetric ask Ni TOO | 18m! stook soln of 1000ppi in 100ml vohuneirc ask Za TSO [Sia stock son of 1000ppm Ta a Torn volumes st Tow range [MS &) Each Z| Rie intermediate stock of ppm calibration | MSD | element jn 100ml volumetric ask High MS & AS 3 “0s intermediate stock spin oF range | MSD 100 pom in 100ml volumetric flask calibration Ca 2) Sosa inisomediete desk sola of 40 pom ia. 100m volumetric ask or 3 3.0 mi stock soln of 100 pom in “ral volumeti Magy Gr 3 Taal stock sol mi 100m volumes flask Pb 10 ‘nl tock so Fy Gal volumetric ask Ni 3 “Emi stock sla of 100ppm in 10Gel volumetie ask Za z im! sock soln of 10 pan 100ml volumetie askDoe. No: LOT TOOROIOOT LABORATORY MANAGEMENT SERVICES ‘KUALITI ALAM SDN BED Page 60f 10 WORK / QUALITY INSTRUCTIONS DETERMINATION OF METALS BY ICP USEPA SW 846 Method 6010 B Tsued by : General Manager Tisue Date 01/06/2006 TaueNe, #1] RevNo=6 8 Preparation of Blank ‘Two types of blanks are required for samples : 8.1.1 Calibration blank is used for all initial and continuing calibration blank determinations. HNO; 2 % is used as calibration blank. 8.1.1 Method blank is a solution contain all of the reagents in the same volumes as used in the processing of the sample and is, cartied through the complete sample preparation and analytical procedure. An acceptable method blank should not be higher ‘than the highest of, a) The method detection limit (MDL) ot b) 5% of the regulatory limit for that analyte or ©) 5%of the measured concentration in the sample 9. Procedure : ot 92 Set up instrument according to manufacturer's instructions with proper operating conditions. The instrument must be allowed to be thermally stable for 30 minutes of operation prior to calibration, ‘The plasma operating conditions must be optimized prior to use of the instrument. Follow the manufacturer's recommendation. 9.2.1 Intensity Check 9.2.1.1 Mn (257.610nm) 1ppm check Perform a calibration with calibration blank and Ippm Mn, Go to ‘Tools’, ‘Spectrometer Control’ and select ‘Plasma Axial’. Make sure the following setting is carried out. 1) Purge gas ~ normal 2) Sutter—auto 3) Hg lamp - off Go to ‘Align View", select ‘OK’, The instrument will perform the intensity check and provide the reading ofDos: No -EQi 1O0AO0OT LABORATORY MANAGEMENT SERVICES KUALITI ALAM SDN BED Page Tof 10 WORK / QUALITY INSTRUCTIONS TsweNo, #1] RevNo:6 ‘sue Date : 01/06/2006 DETERMINATION OF METALS BY ICP USEPA SW 846 Method 6010 B Issued by = General Manager peak intensity, The peak intensity should be more than 200,000.00 for axial viewing. 9.2.1.2 Cu 324.752nm) 1 ppm Perform a calibration with calibration blank and Ippm Cu, Go to “Align Value’, select ‘OK’. The instrument will perform the intensity check and provide the reading of peak intensity. 9.2.2. Background Equivalent Concentration (BEC) test 9.2.2.1 BEC axial test Go to ‘Method’ icon, select ‘BEC Radial’. Click on the ‘Manual’ icon, aspirate the blank and click on “Analyse Blank’. Aspirate the Mn Ippm solution and click on ‘Analyse Standard’. This completes the calibration. Aspirate the rinse solution. In the ‘Tools’ menu, click on “Spectrometer Control’. in the ‘Spectrometer Control” window, close the shutter by selecting the ‘Closed’ option. Click on the ‘Manual Analysis Control’ window to bring it to the front. For the ‘Read Delay’, select ‘Override Method’ and set the ‘Read Delay’ to 0. While continuing to aspirate the rinse solution, click on “Analyse Sample”. This will give you results in concentration units. Click on the ‘Spectrometer Control Window’ to bring it to the front. Change the shutter from ‘Closed? to the ‘Auto’ position which returns it to ‘Instrument Control’ Check the results. By taking the negative value and making it a positive value, this gives the BEC for Mn 257.610, It should be less than or equal to 0.04 mg/L. If it is not, refer to ‘Performance Problem’ in Chapter 5, ‘Troubleshooting in Hardware guide. 9.3 Calibrate the instrument according to the instrament manufacturer's recommendation, using mixed calibration standards solutions describedDoe. No TL QUTOOROOOT LABORATORY MANAGEMENT SERVICES KUALITI ALAM SDN BED Page 8 of 10 WORK / QUALITY INSTRUCTIONS TsueNo, RevNor6 DETERMINATION OF METALS BY ICP Tse Date : 01/06/2006 ‘USEPA SW 846 Method 6010 B Issued by : General Manager 10 94 95 in 7.1, Flush the system with calibration blank between each standard and each sample, If dilutions are performed, the appropriate factors must be applied to sample values, All results should be reported up to three significant figures. Inter-element spectral correction determination Inter-clement correction factors of each element are derived according to manufacturer’s instructions, ‘The factors are stored in the instrument and the results of each analyte are automatically corrected during each sample run, Quality Control 10.1 10.2 103 10.4 ‘A minimum of one method blank per sample batch is run to determine if there is any contamination resulting from the analytical process. To one sample out of every 20 (or one sample from each group of samples if less than 20 are being analysed), add identical known amounts of the metal of interest to 2 portions of the sample and analyse to confirm spike recovery. Recovery of added metal should be within 25% of the actual value and the relative difference between spiked duplicate should be within + 20% Instrument standardization must be checked using the following QC samples: 10.3.1 Check calibration with an Initial Calibration Verification (ICV) following intial calibration 10.3.2 Verify calibration with the Continuing Calibration Verification (CCV) Standard immediately following daily calibration, after every 10 samples and atthe end of an analytical run. 10.3.3 Analyse a calibration blank immediately following daily calibration, after every 10 samples and, at the end of the analytical ran, ‘The results of the ICV and CCV should agree within 10% of the expected value and RSD < 5% from replicate (minimum of two)Doe. No sLQUTDOROOOT LABORATORY MANAGEMENT SERVICES KUALITI ALAM SDN BID Page Sof 10 WORK / QUALITY INSTRUCTIONS TsueNo, 11] RevNo:6 Tse Date : 0170672005 DETERMINATION OF METALS BY ICP USEPA SW 846 Method 6010 B Issued by + General Manages Tnlegrations. If not, terminate the analysis, correct problem and re- calibrate the instrument, Note: The ICV is in the correct concentration range that will provide an adequate test of the inter-clement correction factors. Hence it also serves as the Interference Check Solution. 10.5 The results of the calibration blank should be less than three times the IDL or less than 1/10 the concentration of the action limit of interest. If not, repeat the analysis two more times and average the results, If the average is not within the above stated limits, terminate the analysis, correct the problem, recalibrate and reanalyze the previous 10 samples. Ji. Calculations: Concentration of metal, mg/l = instrument read out, mg/l x dilution factor Total metal (mg/kg) = Concentration of metal (mg/l) Weight of sample used for digestion (g) x 100 12. References: States Environmental jon (SW 846 method 12.1 Test Methods for Evaluating Solid Waste, Unit Protection Agency, November 1996, Third E 12.2 601OB: standard method for Inductively Coupled Plasma-Atomic Emission Spectrometry). 12.3 Test Methods for Evaluating Solid Waste, United States Environmental Protection Agency, November 1996, Third Edition ( SW 846 method 30508) 124 Concepts, Instrumentation, and Techniques in Inductively Coupled Plasma Optical Emission Spectrometry, Perkin Elmer 1997LABORATORY MANAGEMENT SERVICES KUALI] ALAM SDN BED WORK / QUALITY INSTRUCTIONS Bos No sLQIToORO0OT Page 10of 10 TemuoNo, 71 | RevNo:6 DETERMINATION OF METALS BY ICP USEPA SW 846 Method 6010 B Tiave Date : 01/06/2006, Issued by + General Manager EXPLANATORY NOTES: Equivalence of QC scheme: SW846 Method 6010 B and APHA 3120B SW846 Method 6010 B Equivalent APHA 3120B requirement Calibration Blank — after daily calibration, every 10 samples and at end of run, Should be within 3 times IDL or less than 1/10 of action level. Calibration Blank — beginning each nm and altemating with each sample, Examine data for carry-over. ‘Method Blank- each batch. Examine for contamination and carry-over. ‘Method Blank- each batch, Examine for contamination and carry-over. TCV ~ after initial calibration. Should be within + 10% Instrument Quality Control Sample — within each run. Should be within + 5% CCV- after daily calibration, every 10 samples, and at the end of run, Should be within + 109% Instrument Check Standard — beginning of each run and every 10 samples. Should be within + 5% Thteference Check Sample ~ beginning of cach run, Should be within + 20% of true value. Can be substituted by ICV Test for matrix interference — serial dilution with calibration blank to 1 mg/l Results of diluted sample to be + 5% of original result. Matrix Spiked Duplicate — one per matrix batch. Must be within + 25% of actual value and + 20% RPD Re-analysis of any sample — just before end of run. Should be within 5%, Method Quality Control — every rin. Within + 5% of certified valuc.