Mercury Determination in Fish by Cold Vapor Atomic Fluorescence Spectroscopy for 60 minutes. Samples were yellow in a color and clear solutions without any pre- Cipitate. Before analysis, each sample was , dliluted 1:10 with 2 percent (w/v) FIC and OimL of hydroxylamine hydrochloride was added to remove free bromine. For calibration standards, 4.0mLs of standard was added to polypropylene test tubes, All sample reagents were added to Often, warnings related to fish in specified bodies of water orto certain species each standard cup, except for the 4.0mLs ‘of fish limie recommended consumption for the entire population or those at high of deionized watee Table I summa risk such as women of child-bearing age. This technical note desribes the digestion procedure determination of mercury in fish issue using 2fally automated cold ‘vapor atomic fuorescence analyzer. esthe ——— Sample Preparation A variety ofcanned tuna samples were purchased along with a lyophilized doggish reference material (Dorm 2) provided by the National Research Council of Canada. The digestion procedure was molfied from Digestion I found inthe USEPA Method 1631 Appendix. Each of the tuna samples was opened and liquids drained. Samples were patted dry be tween paper towels. For each sample two separate aliquots of approximately 0.25 gram were tran ferred to S0mL. polypropylene test tubes, To each aliquot we added 5.0mL of 3: (wh) HySO4:HINO3, and let stand at oom temperature for 2 hours. Next the samples were heated to 80°C for 40 minutes. At this point all samples are liquefied, We added 15.0mLs of 6N FICL, 3.0mLs of 0.1N BrCl solution and 4.0mLs of de-ionized ‘water The BrClsolutionisthesamethatisidentified on USEPA Method 245.7. After mixing, the samples were heated to 60°C Lee ed Standard Volume (mL) Sample Volume(ml) After Addition Standard 40 “00 3:1 HS054N0, 50 50 then aOmin'@ BC 2 ee NHC z 15.0 15.0 ae GAIN BrCl 30a 3.0 i 5 Water soe (0.0 4.0 6Omin @ 60°C [tee 2% HCL 1:10 dilution T:10 dilution 7 30% Hydroxlamine hyérochloride On OLHAACP and QMI° Products: Your Best Defense Against CTC tL QMI° Aseptic Transfer System Controls contamination during sampling or inoculation of yogurt, cheese, culture, buttermilk and other fermented products. QMI° Aseptic Sampling System Identifies sources of contamination and/or documents process control. Validation studies have proven that OMI Products will control contamination during ‘sampling or inoculating. ‘Yor Test Rous On as scans Yow Sarple Don’t Take Chances. Take Action Against Contamination. | Quality Management, Inc. (QMI°) Phone # 651-501 2887 «Fax 681-501-5797 smal Ades: nf@gmisystemscom ‘Web Adres wregmisystems.com (QM products are manufactured under the following US, Patents: 4,941,517; 5,086,813; 5,199,473, “other patents pending Analysis Another analyzer that uses a dual detector approach for rou tine work in the sub-parts-perthousand (ppt) to high pacts perbillion (ppb) range wasalso employed. Ie has been designed for compliance with EPA methods 1631 and 245.7 and with European Standards EN-13506 and EN-12338. This analyzer provides a prescreen mode to protect the high sensitivity gold amalgamators from contamination. It was also employed in the di ditions were ct fluorescence mode forthe analysis, Instrument con Carrier gas: 0.3 LPM Argon Pump Speed: 5 mLmin Rinse time: 60 secs. Uprake time: Integration: 45 secs, Reductant: 10 percent Sil; in 10 percent HCI (ww) The original concentration ofthe calibration standards was entered into the calibration table. Original concentrations were (0.00, 1.00, 2.00, 6.00, 20.00, 50.00, and 100.0 ppb. The actual concentration of the standards was (standard volumeffinal volume}/{diution) or (4.0 mL/27mL}/10 of 0.0148 the original ‘concentration. The calibration fi is shown in Figure 1. The lin earty is excellent with a correlation coefficient of 0.9998, ELT cans Fie, I: Linear Caliration Fit This calibration curve was employed co determine the con- centration of mercury in digested sample solutions. ‘To calculate the concentration inthe original sample results were multiplied by 4.0 (the volume of standard added) and divided bythe sample ‘weight (approximately 0.254). The certified reference mate rial was further diluted (1:2) with 2 pereent HC to bring ie into calibration range. Results fra variety of tuna appear in Table 2. ‘Two replicates foreach aliquot were measured, Conclusions ‘The fist analyzer provides accurate and reproducible results for the determination of mercury in fish tissue, Its high sensitivitySCT etic) rtd Sample 4 test at rtech laboratories > From microbiology and chemistry a 10 sensory Processing, we've got everthing you need to make your produots and processes better, In one convenient location, fe ies 180 17026-accredited ‘Sample it in the NEW eo testing and pitt 5 arate A | oot | 0101 | 101 | poy Coast B | 0207 | 0302 | 0300 safer and smarter, Caratiomn, 2 | ozs | 02% | 022 | ar5 B | 0330 | o3 | 026 T Balam A | 0589 | oer | 0555 | yay B | 060s | 599 | asee essuaw, A | 0467 | 0456 | ase 8 | o6ss | asm | osse | O56 BPrime =A | 0317 | 0319 | 0318 B | 03 fos | oa | | sussoiam 4 | ane | 040s | 0406 | yyy 8 | oat | oma | oso fr amsoidwt A | 0398 | 0398 | age 8 | ova | omgs | osee | °MO smi | os | ooet | 0088 | 515 8 | 0258 | 0254 | o2ss Wroslowiny A | 0138 | 0139 | ore | B | ass | ors | 0136 sersoiaw, a | ase | osat | 0500 | 4, 8 | ast | cass | sss tom2 —-k | 42 | son | 4s | yy, | 93 B } a4 | ass | sas | MY | cet ‘will permit the determination of mercury even in fish where an ticipated mercury content is low. Sample preparation using the sulfuricinitric acid mixture followed by oxidation with bromine ‘monochloride results in complete dissolution without the need for microwave digestion, m References Appendix to Method 1631, Total Mercury in Tissue, Sale, Sediment ind Sol by Acid Digestion nd BrCl Onidation, EPA-821-R-O1-013, January 2001 Method 245.7, Mercury Water by Cold Vapor Atomic Fluorescence Spectrometry, EPAS21-R-01-008, January 2001 ‘ava ste eo pot maoge or Teepe lesan abe 9 baad dvelperf tome setiscapy that 00 a High Temp bog + Sterile, 18-07 '532-ml capacity VU estar tea a) SS oe eT