ࡱ> #"$!&'mnopqrstuvwxyz{|}~QM 7bjbj== 0WWl    $ $ T L 4666666$ ~Zi Z     4 4 h 44 H " < ( 440 4 "4 May 31, 2002. Recalculation of alkalinity values for WOCE SR3/S4 cruise AA9404. Large changes in the lab temperature during titrations on this cruise were a problem in the early part of this cruise. The changing ambient lab temperature caused some variations in the titration temperatures for the early part of the cruise. Up to stations 22, the titration cell temperatures were up to about 24C. Normal conditions were 20C for a titration. The original alkalinity calculation did not correct for the expansion of the Plexiglas titration cell at the warmer temperatures, or for slight changes in the acid density with temperature and caused an overestimate of alkalinity in the early part of the cruise (see figure 1). The change in acid density was a small effect.  EMBED Excel.Chart.8 \s  Figure 1. Reduction in alkalinity due to correction of temperature induced changes in the titration cell volume and acid density. Corrections applied to alkalinity calculation. Acid density: The acid density at different temperatures was calculated based on measurements made with the Anton Parr density meter. The acid used for the density calibration was prepared in the same way as the one used on aa9404 and had a density of 1.021154 gm/cm3 (20C). The acid used on the aa9404 cruise had a density of 1.02136 gm/cm3 (20C), due to slight differences in the concentration. The equation for the change in density relative to 20C on the acid was: Density correction = 0.00000136*T3 - 0.00010924*T2 + 0.00257069*T - 0.01859167 where T is in centigrade, and the R2 value of the fit was 0.9998. The above correction was added to the acid density of 1.02136. Thermal expansion of Plexiglas cell: The thermal expansion of the plexiglas cell had to be corrected for. The coefficient of thermal expansion from the manufacturer (http://www.roehm.de/eng/plexiglas/) as 7 * 10-5 per K. To account for this change the equations in SOP12 of the DOE handbook were applied using the T of the cell during the titration (Tcell). The equation is: V(Tcell)=V20*(1+3*7*10-5*(Tcell-20.)). Where, V20 refers to the calibrated volume at 20C. Equilibrium constants: Equilibrium constants were calculated at the cell titration temperature and sample salinity. Addition of HgCL2 The calculated titration alkalinity values were multiplied by 1.0002 to correct for the addition of 100ml of saturated HgCl2 solution to each 500ml sample. Certified Reference Material analyses for alkalinity: The CRM values were used to calibrate the alkalinity cell volumes. Few CRM's were analysed at the start of the cruise when the cell temperatures were above 20C. This was also the first cruise that the alkalinity cell was subsequent cruises have less noisy data. In order to calculate the cell volume from the CRM analyses, an initial volume of 210.60ml (at 20C) was used and the alkalinity calculated with the above corrections applied (ie. cell volume corrected to titration T, acid density and equilibrium constants). The values for alkalinity were then averaged for all CRM's where the estimated cell volume was within 210.60 +/- 0.02ml, which corresponded to a titration temperature of 20 0.5C. The resultant average Talk was 2217.81 mmol/kg. The CRM value is designated as 2217.16 mmol/kg, which indicates the new cell volume should be 210.66ml (20C). The new cell volume was then used to recalculate the alkalinity values for all CRM's and samples. The results are: Alkalinity: 2217.10 2.77 mmol/kg (n=41) DIC from titration: 1996.31 1.77 mmol/kg (n=41) Batch 22 CRM: Bottled on April 1, 1994 Original certificate issued August 15, 1994 Total alkalinity not certified CERTIFIED VALUES Salinity 33.561 Total Dissolved Inorganic Carbon Mean: 1995.19 mol/kg Standard Deviation 0.71 mol/kg Number of Analyses 13 Total Alkalinity Mean: 2217.16 mol/kg Standard Deviation 1.51 mol/kg Number of Analyses 18 (on 8 bottles) Phosphate 0.27 mol/kg Silicate 1.99 mol/kg Nitrite 0.00 mol/kg Nitrate 0.20 mol/kg Note: Nutrient levels may have changed on storage; their stability has not been examined. The standard deviation of the titration alkalinity values is not particularly good. Likely reasons for that include errors in the corrections applied for temperature, and this was the first cruise that alkalinity was analysed using a closed cell. There were numerous problems with the original cell supplied from the USA and a new cell was made at CSIRO just before the cruise. The cell itself seemed to work well, but it did not leave any time for developing the method. CRM data from subsequent cruises shows less scatter. Duplicates: No alkalinity duplicates were analysed.  EMBED Excel.Chart.8 \s  TCO2 analyses with SOMMA system. An offset in TCO2 for CRM's was due to incorrectly calibrated gas loop volumes for the cruise. The offset of about 10.8 mmol/kg data was used to correct all samples. Hence, the average CRM value below shows good agreement with the assigned CRM value for TCO2. TCO2 data have been multiplied by 1.0004 to correct for dilution of 100ml saturated HgCl2 in 250ml sample.  EMBED Excel.Chart.8 \s   EMBED Excel.Chart.8 \s  S . / & ' [ ]       2 4 ` u .0v68V&7Bmn$ jR/Ujĩ@ UV CJOJQJ 5CJH*\CJH*CJH*jW@ UV jU 5CJ\CJNST!"   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