аЯрЁБс>ўџ œžўџџџ–џџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџџьЅС!` №П†”bjbj\­\­ .ž>Ч>Чz;џџџџџџЄ```````tќ6ќ6ќ6ќ6D@7ьtЋIђ88ˆР8Р8Р8Р8Р8.ю89 ŽHHHHHHH$JhMPДHБ`о;Р8Р8о;о;ДH``Р8Р8eIЊCЊCЊCо;`Р8`Р8ŽHЊCо;ŽHЊCЊC``ЊCР8,8 vmХЬАЦќ6ј@fЊCвCМ{I0ЋIЊCUM^BBUMЊCUM`ЊC(О9h&:JЊCp:<Ќ:29x†9$Њ9ДHДH C О9О9О9ЋIо;о;о;о;tttdи$tttиttt``````џџџџ Methods Spectrophotometric pH Measurements The pH measurements of seawater were made using the spectrophotometric techniques of Clayton and Byrne (1993). The pH of the samples using the m-cresol purple (mCP) is determined from pH = pKind + log [(R - 0.0069)/(2.222 - 0.133 R)] (1) where Kind is the dissociation constant for the indicator and R (A578/A434) is the ratio of the absorbance of the acidic and basic forms of the indicator corrected for baseline absorbance at 730 nm. The pH of the samples is perturbed by the addition of the indicator. The magnitude of this perturbation is a function of the difference between the seawater acidity and indicator acidity; therefore this correction was quantified for each batch of dye solution. To a sample of seawater ((5ml), a volume of 2 milli-molar mCP (0.008 ml) was added and the absorbance ratio was measured. From a second addition of mCP and absorbance ratio measurement, the change in pH per ml of added indicator ((pH) was calculated. From a series of such measurements over a range of seawater pH, the first addition of indicator used to calculate pH was described as a linear function of the pH measured with the subsequent addition of indicator (i.e. standard addition correction due to the indicator as a function of pH). In the course of routine seawater pH analyses, this correction was applied to every measured pH; i.e. the corrected pH is calculated as pH = 1.0013(pHi) – 0.0083 (2) This equation was applied twice for double addition indicator runs, and once for single addition indicator runs to yield pseudo replicate runs for every pH sample when a second addition of indicator was added. Clayton and Byrne (1993) calibrated the m-cresol purple indicator using TRIS buffers (Ramette et al., 1977) and the pH equations of Dickson (1993). They found that pKind = 1245.69/T + 3.8275 + (2.11 x 10-3) (35 - S) (3) where T is temperature in degrees Kelvin and is valid from 293.15 to 303.15 K (20 to 30oC) and S = 30 to 37. The values of pH calculated from equations (1) and (3) are on the total scale in units of mol (kg-soln)-1. The total proton scale (Hansson, 1973) defines pH in terms of the sum of the concentrations of free hydrogen ion, [H+], and bisulfate, [HSO4-] pHT = -log[H+]T = -log{[H+] + [HSO4-] }= -log{[H+](1 + [SO42-]/KHSO4)} (4) where the concentration of total sulfate, [SO42-] = 0.0282 ( S/35 and KHSO4 is the dissociation constant for the bisulfate in seawater (Dickson, 1990a). Lee et al. (1996) have redetermined the value of pKind from 273.15 to 313.15 K (0 to 40oC) using a 0.04 m TRIS buffer (Ramette et al., 1977). The pH of the TRIS buffer was determined from the emf measurements made with the H2,Pt| AgCl,Ag electode system (Millero et al., 1993a). At 273.15 K (25oC) the buffer had a pH of 8.076 and yielded spectrophotometric values of pH that were in excellent agreement (( 0.0001) with those found using equations (1) and (3). These results from 273.15 to 313.15 K (0 to 40oC) were fitted to the equation (S = 35) pKind = 35.913 - 216.404/T - 10.9913 log (T) (5) with the standard error of 0.001 in pKind where the constant is on the total scale in {mol (kg-H2O) -1}. The values of pH calculated from equations (1) and (5) are on the total scale in units of {mol (kg-H2O)-1}. The conversion from the total scale (pHT) {mol (kg-H2O)-1} to the seawater scale (pHSWS) in {mol (kg-soln)-1} can be made using (Dickson and Riley, 1979; Dickson and Millero, 1987): pHSWS = pHT - log{(1 + [SO42- ]/KHSO4 + [F-]/KHF )/(1 + [SO4-2]/KHSO4])} - log (1 - 1.005x10-3 S) (6) where the total concentration of fluoride, [F-] = 0.000067 ( 35/S, and KHF is the dissociation constant for hydrogen fluoride (Dickson and Riley, 1979). The seawater pH scale (pHSWS) was used in further calculations of the internal consistency (Millero et al., 1993b) of the four parameters since the carbonate constants used are on this scale (Dickson and Millero, 1987). The pH system is automated and makes measurements of discrete pH approximately every twelve minutes on a sample volume of 25 cm3. A microprocessor controlled syringe pump (Kloehn 50300) and sampling valve aspirates and injects the seawater sample into the 10 cm optical cell at a precisely controlled rate. The syringe rinses and primes the optical cell with 20 cm3 of sample and the software permits five minutes for temperature stabilization. A refrigerated circulating temperature bath (Neslab RTE-17) regulates the temperature of the sample at 25 ( 0.01 КC. An Agilent 8453 UV/VIS spectrophotometer measures the background absorbance of the sample. The automated syringe and sampling valves aspirates 4.90 cm3 seawater and 0.008 cm3 of indicator and injects the mixture into the cell. After the software permits five minute for temperature stabilization, a Guildline 9540 digital platinum resistance thermometer measures the temperature and the spectrophotometer acquires the absorbance at 434, 578 and 730 nm. During the Hawaii to Alaska portion of the cruise, the pH system was converted to an underway mode, in which a Seabird thermosalinograph was inserted on a flowing line from which the syringe pump could draw a sample every ten minutes. The measurement process was the same as the procedure above, with the exception of the input salinity coming from the Seabird. The water jacket enclosing the 10 cm optical cell was thermostated with the same underway seawater to yield true in situ measurements totaling 1250 runs. Eight stations of discrete measurements were made at the temperature of the surface waters relative to when the measurement was made and were later normalized to 25oC. Potentiometric Measurements TA Titration system The titration systems used to determined TA consisted of a Metrohm 665 Dosimat titrator and an Orion 720A pH meter that is controlled by a personal computer (Millero, et al., 1993c). Both the acid titrant in a water jacketed burette and the seawater sample in a water jacketed cell were controlled to a constant temperature of 25 SYMBOL 177 \f "Symbol" 0.1SYMBOL 176 \f "Symbol"C with a Neslab (RTE-17) constant temperature bath. The plexiglass water jacketed cell used is shown in Figure 4. The cells had fill and drain valves which increased the reproducibility of the cell volume. Our TA system consists of a manifold which allows the automated measurement of six samples in sequence. A set of pumps, valves and relays are used to rinse, fill and drain the TA cell. The titration is controlled programmatically using National Instrument’s Labwindows/CVI environment. The titration is made by adding HCl to seawater past the carbonic acid end point. A typical titration records the emf reading after the readings become stable (SYMBOL 177 \f "Symbol" 0.05 mV) and adds enough acid to change the voltage to a pre-assigned increment (13 mV). A full titration (25 points) takes about 15 minutes. Using two automated systems a 36-bottle station cast can be completed in six hours. Electrodes The electrodes used to measure the emf of the sample during a titration consisted of a ROSS 8101 glass pH electrode and an Orion 90-02 double junction Ag/AgCl reference electrode. The filling solution used in the reference electrode was a 0.7 M NaCl solution to maintain a consistent junction potential between the solution and electrode. Standard acids The HCl used throughout the cruise was made, standardized, and stored in 500 mL glass bottles in the laboratory for use at sea. The 0.243402 Б 0.000022 M HCl solutions were made from 1 M Mallinckrodt standard solutions in 0.45 M NaCl to yield an ionic strength equivalent to that of average seawater (( 0.7 M). The acid was originally tested on seawater of a known TA to determine the reliability of the acid and later sent for final standardization using a coulometric technique (Taylor and Smith, 1959; Marinenko and Taylor, 1968) by Dickson’s group. Volume of the cells The volumes of the cells used at sea were determined in the laboratory by making numerous measurements of seawater with a known total alkalinity. Once the TA values agree to Б 1.0 m№mol kg-1, the volume of the cell is determined to Б 0.01 mL from the value required to reproduce the TA. Measurements on Certified Reference Material samples were made to confirm the volume and reproduce the known TA to Б 0.5 m№mol kg-1. Volume of Titrant The volume of HCl delivered to the cell is traditionally assumed to have small uncertainties (Dickson, 1981) and equated to the digital output of the titrator. Calibration of the burette of the Dosimat with Milli-Q water at 25SYMBOL 176 \f "Symbol"C indicate that the system delivers 3.000 mL (the value for a titration of seawater) to a precision of SYMBOL 177 \f "Symbol" 0.0004 mL. This uncertainty results in an error of SYMBOL 177 \f "Symbol" 0.4 SYMBOL 109 \f "Symbol"mol kg-1 in TA and TCO2. Since the titration systems are calibrated using standard solutions, the error in the accuracy of volume delivery will be partially canceled and included in the value of cell volumes assigned. The laboratory precision of the system is Б 1.0 m№mol kg-1. Evaluation of the Carbonate Parameters The total alkalinity of seawater was evaluated from the proton balance at the alkalinity equivalence point, pHequiv = 4.5, according to the exact definition of total alkalinity (Dickson, 1981) TA = [HCO3-] + 2[CO32-] + [B(OH)4-] + [OH-] + [HPO42-] + 2[PO43-] + [SiO(OH)3-] - [H+] - [HSO4-] - [HF] - [H3PO4] (7) At any point of the titration, the total alkalinity of seawater can be calculated from the equation (V0 TA - VM)/(V0 + V) = [HCO3-] + 2[CO32-] + [B(OH)4-] + [OH-] + [HPO42-] + 2[PO43-] + [SiO(OH)3-] - [H+] - [HSO4-] - [HF] - [H3PO4] (8) where V0 is the volume of the cell, M is the molarity of the acid titrant, and V is the volume of acid added. In the calculation all the volumes are converted to mass using the known densities of the solutions (Millero et al., 1993c). A computer program has been developed in Labwindows/CVI to calculate the carbonate parameters (pHsw, E*, TA, TCO2, and pK1) in seawater solutions. The program is patterned after those developed by Dickson (1981), Johansson and Wedborg (1982) and Dickson (DOE, 1994). The fitting is performed using the STEPIT routine (J.P. Chandler, Oklahoma State University, Stillwater, OK 74074). The STEPIT software package minimizes the sum of squares of residuals by adjusting the parameters E*, TA, TCO2 and pK1. The computer program is based on equation (8) and assumes that nutrients such as phosphate, silicate and ammonia are negligible. This assumption is valid only for surface waters. Neglecting the concentration of nutrients in the seawater sample does not affect the accuracy of TA, but does affect the carbonate alkalinity. The pH and pK of the acids used in the program are on the seawater scale, [H+]sw = [H+] + [HSO4-] + [HF] (Dickson, 1984). The Mehrbach et al (1973) dissociation constants were used in the program as fit by Dickson and Millero (1987) for carbonic acid, from Dickson (1990a) for boric acid, from Dickson and Riley (1979) for HF, from Dickson (1990b) for HSO4- and from Millero (1995) for water. The program requires as input: the concentration of acid, volume of the cell, salinity, temperature, measured emf (E) and volume of HCl (VHCl). To obtain a reliable TA value from a full titration at least 25 data points should be collected (9 data points between pH 3.0 to 4.5). The precision of the fit is better than 0.4 SYMBOL 109 \f "Symbol"mol kg-1 when pK1 is allowed to vary and 1.5 SYMBOL 109 \f "Symbol"mol kg-1 when pK1 is fixed. Our titration program has been compared to the titration programs used by others (Johansson and Wedborg, 1982; Bradshaw et al.,1981; Bradshaw and Brewer, 1988) and the values of TA agree to within SYMBOL 177 \f "Symbol" 1 SYMBOL 109 \f "Symbol"mol kg-1. Accuracy of Measurements The spectrophotometric pH and potentiometric TA of CRM used during the cruise have been measured in the laboratory before the cruise to characterize the pH of the standard and make sure our titration systems were performing to the desired precision. During the cruise, titrations on CRM were made to insure that the two titration systems were giving consistent values. The values of pH and TA for CRM #73 are summarized in Table 2. The precision of the potentiometric measurements of batch #73 were Б 3.0 Еmol kg-1 for TA and Б 0.006 for pH. For spectrophotometric measurements the average values agreed to Б 0.002 for CRM batch #73 and Б 0.003 for TRIS buffer solution. The deviations are within 2У for most of the measurements. Small correction factors were made to the TA to account for the offset with the CRM. To correct the TA values, a ratio of the CRM value to the measured value, for each system, was taken and multiplied to each of the sample measurements. For pH, the average value was subtracted from the CRM value for each system, and this value was added to each of the sample measurements. These correction factors were made at the end of each station. The TA values for System A appeared to drift over the course of the cruise, however, the correction factors made accounted for this drift as is evident in the duplicate results. Table 2: Summary of Certified Reference Material Measurements TA m№mol kg-1pH @ 25oCTotal RunsSystem A2253.6 Б 4.17.826 Б 0.00653System B2257.2 Б 2.07.826 Б 0.00560Combined2255.5 Б 3.07.826 Б 0.006113        Spectrophotometer   CRM Batch 73 7.8417Б 0.00209TRIS 8.0525 Б 0.,яђ% ( a d f i   е ж В Г ‰ŒАВ !ž ./067ABCDNOWXYefopruyЎЏБМНШЬORst§ўDEГДFIЁјѓящятяняняжяЯяЧящяТяКяТяТянТяняТяняТянТяТянТянянТяГяняняКяняТяжяТянян jД№h%0dhСsIh%0dH* h%0dH*hА h%0dH* jD№h%0d jЛ№h%0d h%0dH* h%0dCJH* h%0dCJh%0d h%0d5h%0dCJ$aJ$F+,ц — н†Щ2Cwэ‰єяяргФИФФгФг­рг­ргр $dрa$gd%0d Цdрgd%0d$ Цdрa$gd%0d Ца№dрgd%0d$ Цhdрa$gd%0dgd%0d $dрa$gd%0d†”§ЁзикнRSUW‚ƒ’”ЏВХЧ-.048=>ACNOQTXЖЗФХбг23<?IJgop†‡ˆ‹ŒІ &z{67jkЌШбвйклуфш№ќїќђќїќђќїќїќђќїќђќїќїќїђќїќђќїќїђќїќђќђќыќїќїќуќмќмќмќмќђќмќмќмќђќеќЮќмќмќђќмќмќ h–wh%0d jБ№h%0d hwnh%0dhnTXh%0dH* jД№h%0d h%0dH* h%0dH*h%0dQ№ёѕїБВЖжзщ5 6 L M Q R h i ####§#$\%l%Л%М%š&›&™'Ў'Ц(Ш(д(и(Œ*Ž*š*ž* *Ђ*Ш*H,I,_,`,Ч,Ш,о,п,--,---2-3-I-J-P-S-`-a-Њ.Ќ.њіяічітініеіеіеіеіеіеінініЭіЦініЛіГіЛіГіЌніеіеіеіеіеіеіеіеіЭіЄіЛh%0dCJEHњџ hгVh%0dhќ9dh%0dH*hЛCГh%0dOJQJ jЛ№h%0dh%0dCJEHjh%0dU h%0d6 h%0d5hѓF=h%0dH* hwnh%0dh%0d h%0dH*@ЖЗзш!?!§#$\%k%™'Ў'Ђ*Ш*Р./J0Ž0њюовУУУУУЛУЛУАУЛУЛУЛ $dрa$gd%0ddрgd%0d$ Цhdрa$gd%0d Цhdрgd%0d$ ЦhЦdрa$gd%0d $ Цha$gd%0dgd%0dЌ.И.М.О.Р./ь/ј/K0T0U0V0^0_0a0k0l0m0t0u0}0~0€0ˆ0‰0‹0Ё0Ђ0Ѓ0Љ0Њ0В0Г0Д0С0Т0Ф0Х0э0R1T1U1a1b1n1o1p1x1y1{1…1†1‡1Ž11™1š1œ1Є1Ѕ1Ї1Г1Д1Е1Л1М1Ф1Х1ќєќьчќпќдХЖдХЖдХЖдЖдХЖдХЖдХЖдЖдХЖдХдХдќдЊдЊдХЖдХЖдХЖдЖдХЖдХЖдХЖдЖдХhMSЃh%0dH*mHsHhMSЃh%0dCJEHmHsHhMSЃh%0dCJEHњџmHsHhMSЃh%0dmHsHh%0dCJEHњџ h%0d6h UЏh%0d6hќ9dh%0dH*h%0dCŽ0э0Q1‘1о1Щ2 6V6Z:s:ЄAЅAІAхAїїїїьнннвУУУЗ $$Ifa$gd%0d$„аdр`„аa$gd%0d $dрa$gd%0d$ Цhdрa$gd%0d $dрa$gd%0ddрgd%0d Х1Ц1г1д1ж1з1о1х1ц1,3.3;3<3D3E3К4М4Т4У4X6Y6Z6\6]6b6c6k6l6m6q7r7s7"8%8н8о8є8ѕ8ћ8§899"9#999:9@9B9C9J9K9Я9ж9::4:5:ёцзцШцФМФДФЏФДФДФДФЇФДЁФЇФДЇФД›ФДФ“Ф“ФЇФДФ“Ф“ФЇ›ФДФŽФ“Ф“ h%0d6jh%0dU h%0dEH h%0dCJh%0dCJEH h%0dH*h%0dCJEHњџhќ9dh%0dH*h%0dhMSЃh%0dCJEHњџmHsHhMSЃh%0dCJEHњџmHsHhMSЃh%0dmHsHhMSЃh%0dCJEHmHsH85:8:9:O:P:V:X:Z:s:v: :Ё:v<x<ІAхAцAыAьAюABBBB$B&B@BBB’BќєќєќьќфнќнќеќПЎ—Ў—}c}H}H}Ў—5h  h%0d5CJH*OJPJQJ\^JaJnH tH 2h  h%0d5CJOJPJQJ\^JaJnH tH 2h  h%0d5CJOJPJQJ\^JaJnH tH ,h  h%0dCJOJPJQJ^JaJnH tH  h  h%0dCJPJaJnH tH *h  h%0d5OJPJQJ\^JnH tH h\}$h%0dH* h\}$h%0dh%0dCJ$aJ$h%0dCJEHjh%0dUh%0dхAцAчAшAщAъAыAЖЊЊЊЊЊ $$Ifa$gd%0dIkd$$If–l”;жћџ8'=і=6ііжџжџжџжџ4ж4ж laіgpж џџyt%0dыAьAюABB*B@BVJJJJJ $$Ifa$gd%0dЉkdy$$If–l”џжrћџdl8' џџџџџџџџџџџџџџџџ'џџџџџџџџџџџџџџџџ'Tџџџџџџџџџџџџџџџџ'џџџџџџџџџџџџџџџџ'Ьџџџџџџџџџџџџџџџџі=6ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџџџџ4ж4ж laіgpж2џџџџџџџџџџyt%0d@BBBTBnBpBŒB’BVJJJJJ $$Ifa$gd%0dЉkdr$$If–l”,жrћџdl8' 'џџџџ'Tџџџџ'џџџџ'Ьџџџџі=6ііжџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laіgpж2џџџџџџџџџџyt%0d’B”BІBРBТBоBфBVJJJJJ $$Ifa$gd%0dЉkd‡$$If–l”џжrћџdl8' џџџџ'џџџџџџџџ'Tџџџџџџџџ'џџџџџџџџ'Ьџџџџџџџџі=6ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laіgpж2џџџџџџџџџџyt%0d’B”BфBцB8C:CLCNC`CbC†C”C–CиCкCDpp ppp$p+p,pJpKpUpVprrrrЊsЌsИsМsfuhutuzuЊuЌuИuОuv€>€B€H€В€яияияияияОияияиМияияОияияияИ­ИЅИ­И И­ИЅИ­ИЅИМИ›И…*hM1h%0d5OJPJQJ\^JnH tH  h%0do( h%0dH*h4Uh%0dH*h7`’h%0dOJQJh%0dU2h  h%0d5CJOJPJQJ\^JaJnH tH ,h  h%0dCJOJPJQJ^JaJnH tH  h  h%0dCJPJaJnH tH 1фBцBјBCC0C8CVJJJJJ $$Ifa$gd%0dЉkdЊ$$If–l”џжrћџdl8' џџџџ'џџџџџџџџ'Tџџџџџџџџ'џџџџџџџџ'Ьџџџџџџџџі=6ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laіgpж2џџџџџџџџџџyt%0d8C:C>CBCDCHCLCVJJJJJ $$Ifa$gd%0dЉkdЭ$$If–l”џжrћџdl8' џџџџ'џџџџџџџџ'Tџџџџџџџџ'џџџџџџџџ'Ьџџџџџџџџі=6ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laіgpж2џџџџџџџџџџyt%0dLCNCRCVCXC\C`CVJJJJJ $$Ifa$gd%0dЉkd№$$If–l”џжrћџdl8' џџџџ'џџџџџџџџ'Tџџџџџџџџ'џџџџџџџџ'Ьџџџџџџџџі=6ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laіgpж2џџџџџџџџџџyt%0d`CbC†CŠCŒCC”CVJJJJJ $$Ifa$gd%0dЉkd$$If–l”џжrћџdl8' џџџџ'џџџџџџџџ'Tџџџџџџџџ'џџџџџџџџ'Ьџџџџџџџџі=6ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laіgpж2џџџџџџџџџџyt%0d”C–CАCДCЖCдCиCVJJJJJ $$Ifa$gd%0dЉkd6$$If–l”џжrћџdl8' џџџџ'џџџџџџџџ'Tџџџџџџџџ'џџџџџџџџ'Ьџџџџџџџџі=6ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laіgpж2џџџџџџџџџџyt%0dиCкCфCшCъCppVJJJJJ $$Ifa$gd%0dЉkdY $$If–l”џжrћџdl8' џџџџ'џџџџџџџџ'Tџџџџџџџџ'џџџџџџџџ'Ьџџџџџџџџі=6ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laіgpж2џџџџџџџџџџyt%0d003332    Certified Values   CRM Batch 732253.57.8417       The precision of the instruments was tested by making duplicate or replicate measurements of samples throughout the cruise. These samples were taken from the same Niskin bottle, equilibrated for an equal amount of time, and then measured on each system for duplicates and the same system for replicates. A total of 62 duplicate samples were made on the titration systems yielding a precision of 0.3 Б 2.3 m№mol kg-1 for TA and -0.001 Б 0.008 for pH. These results validate the correction factors applied to each system as the deviations between the two systems are within the experimental error of the titrators (Б 3.0 m№mol kg-1). A total of 59 and 74 replicate samples run on Systems A and B, respectively, and 1051 replicate samples were made on the spectrometer. Results showed that the average replicate difference for TA were 0.1 Б 1.2 m№mol kg-1 for System A, 0.1 Б 1.0 m№mol kg-1 for System B. Finally, 0.0004 Б 0p p p ppppVJJJJJ $$Ifa$gd%0dЉkd| $$If–l”џжrћџdl8' џџџџ'џџџџџџџџ'Tџџџџџџџџ'џџџџџџџџ'Ьџџџџџџџџі=6ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laіgpж2џџџџџџџџџџyt%0dpp$p&p'p)p+pVJJJJJ $$Ifa$gd%0dЉkdŸ $$If–l”џжrћџdl8' џџџџ'џџџџџџџџ'Tџџџџџџџџ'џџџџџџџџ'Ьџџџџџџџџі=6ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laіgpж2џџџџџџџџџџyt%0d+p,p9p@pApHpJpVJJJJJ $$Ifa$gd%0dЉkdТ $$If–l”џжrћџdl8' џџџџ'џџџџџџџџ'Tџџџџџџџџ'џџџџџџџџ'Ьџџџџџџџџі=6ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laіgpж2џџџџџџџџџџyt%0dJpKpMpOpQpSpUpVJJJJJ $$Ifa$gd%0dЉkdх $$If–l”џжrћџdl8' џџџџ'џџџџџџџџ'Tџџџџџџџџ'џџџџџџџџ'Ьџџџџџџџџі=6ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laіgpж2џџџџџџџџџџyt%0dUpVpWpF€H€В€VKKK? $$Ifa$gd%0d $dрa$gd%0dЉkd$$If–l”џжrћџdl8' џџџџ'џџџџџџџџ'Tџџџџџџџџ'џџџџџџџџ'Ьџџџџџџџџі=6ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laіgpж2џџџџџџџџџџyt%0d.0025 for spectrophotometric pH. Table 3: Summary of Duplicate/Replicate Measurements      TA m№mol kg-1pHTotal RunsDuplicates0.3 Б 2.3-0.001 Б 0.00862    Replicates   System A0.1 Б 1.2-0.001 Б 0.00459System B0.1 Б В€Д€И€М€Р€Ф€Ш€ЖЊЊЊЊЊ $$Ifa$gd%0dIkd+$$If–l”Jжёџ)'8і86ііжџжџжџж4ж4ж laі]pж џџyt%0dВ€Д€Ш€Ъ€Ю€д€ж€т€ц€XZln„’”рт‚”””4”5”]”^”n”„”…”†”яияиОЄО‰ОяОияияОияияи‡ияияияОияƒhsAGU5hM1h%0d5CJH*OJPJQJ\^JaJnH tH 2hM1h%0d5CJOJPJQJ\^JaJnH tH 2hM1h%0d5CJOJPJQJ\^JaJnH tH ,hM1h%0dCJOJPJQJ^JaJnH tH  hM1h%0dCJPJaJnH tH  Ш€Ъ€Ю€ш€ъ€№€VJJJJJ $$Ifa$gd%0dЉkdВ$$If–l”жrёџНЩ С4)'Ьџџџџ' џџџџџџџџ'јџџџџџџџџ'sџџџџџџџџ'ѕџџџџџџџџі86ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laі]pж2џџџџџџџџџџyt%0d24RXVJJJJJ $$Ifa$gd%0dЉkdе$$If–l”;жrёџНЩ С4)'Ьџџџџ' џџџџџџџџ'јџџџџџџџџ'sџџџџџџџџ'ѕџџџџџџџџі86ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laі]pж2џџџџџџџџџџyt%0dXZ^bdhlVJJJJJ $$Ifa$gd%0dЉkdј$$If–l”жrёџНЩ С4)'Ьџџџџ' џџџџџџџџ'јџџџџџџџџ'sџџџџџџџџ'ѕџџџџџџџџі86ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laі]pж2џџџџџџџџџџyt%0dln„ˆŠŽ’VJJJJJ $$Ifa$gd%0dЉkd$$If–l”жrёџНЩ С4)'Ьџџџџ' џџџџџџџџ'јџџџџџџџџ'sџџџџџџџџ'ѕџџџџџџџџі86ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laі]pж2џџџџџџџџџџyt%0d’”ІКМкрVJJJJJ $$Ifa$gd%0dЉkd>$$If–l”жrёџНЩ С4)'Ьџџџџ' џџџџџџџџ'јџџџџџџџџ'sџџџџџџџџ'ѕџџџџџџџџі86ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laі]pж2џџџџџџџџџџyt%0dртє””””VJJJJJ $$Ifa$gd%0dЉkda$$If–l”жrёџНЩ С4)'Ьџџџџ' џџџџџџџџ'јџџџџџџџџ'sџџџџџџџџ'ѕџџџџџџџџі86ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laі]pж2џџџџџџџџџџyt%0d1.00.000 Б 0.00374Spec 0.0004 Б 0.00251051Combined-0.1 Б 1.1-0.001 Б 0.003133Spec - Titrator 0.015 Б 0.0131414 ”””””/”4”VJJJJJ $$Ifa$gd%0dЉkd„$$If–l”жrёџНЩ С4)'Ьџџџџ' џџџџџџџџ'јџџџџџџџџ'sџџџџџџџџ'ѕџџџџџџџџі86ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laі]pж2џџџџџџџџџџyt%0d4”5”>”I”J”Y”]”VJJJJJ $$Ifa$gd%0dЉkdЇ$$If–l”жrёџНЩ С4)'Ьџџџџ' џџџџџџџџ'јџџџџџџџџ'sџџџџџџџџ'ѕџџџџџџџџі86ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laі]pж2џџџџџџџџџџyt%0d]”^”n”p”q””„”VJAAJJ $Ifgd%0d $$Ifa$gd%0dЉkdЪ$$If–l”џжrёџНЩ С4)'Ьџџџџ' џџџџџџџџ'јџџџџџџџџ'sџџџџџџџџ'ѕџџџџџџџџі86ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laі]pж2џџџџџџџџџџyt%0d„”…”†”VTЉkdћ$$If–l”ўжrёџНЩ С4)Ьџџџџ' џџџџџџџџ'јџџџџџџџџ'sџџџџџџџџ'ѕџџџџџџџџі86ііжџџџџџџџџџџџџџџџџџџџџжџџџџџџџџџџџџџџџџџжџџџџџжџџџџџ4ж4ж laі]pж2џџџџџџџџџџyt%0d,1hАа/ Ар=!А"А# $ %ААаАа аw$$If–g!vh5ж=#v=:V –l”;і=6і,ж5ж=9ж/ж џaіgpж џџyt%0dї$$If–g!vh5ж 5ж5жT5ж5жЬ#v #v#vT#v#vЬ:V –l”џі=6і,ж5ж 5ж5жT5ж5жЬ9ж/ж џџџџџџрџaіgpж2џџџџџџџџџџyt%0d$$If–g!vh5ж 5ж5жT5ж5жЬ#v #v#vT#v#vЬ:V –l”,і=6і,ж5ж 5ж5жT5ж5жЬ9ж/ж џ/ж  џ/ж џџџџџџрџaіgpж2џџџџџџџџџџyt%0d!$$If–g!vh5ж 5ж5жT5ж5жЬ#v #v#vT#v#vЬ:V –l”џі=6і,ж5ж 5ж5жT5ж5жЬ9ж/ж џ/ж џџџџџџрџ/ж џџџџџџрџ/ж  џaіgpж2џџџџџџџџџџyt%0d!$$If–g!vh5ж 5ж5жT5ж5жЬ#v #v#vT#v#vЬ:V –l”џі=6і,ж5ж 5ж5жT5ж5жЬ9ж/ж џ/ж џџџџџџрџ/ж џџџџџџрџ/ж  џaіgpж2џџџџџџџџџџyt%0d!$$If–g!vh5ж 5ж5жT5ж5жЬ#v #v#vT#v#vЬ:V –l”џі=6і,ж5ж 5ж5жT5ж5жЬ9ж/ж џ/ж џџџџџџрџ/ж џџџџџџрџ/ж  џaіgpж2џџџџџџџџџџyt%0d!$$If–g!vh5ж 5ж5жT5ж5жЬ#v #v#vT#v#vЬ:V –l”џі=6і,ж5ж 5ж5жT5ж5жЬ9ж/ж џ/ж џџџџџџрџ/ж џџџџџџрџ/ж  џaіgpж2џџџџџџџџџџyt%0d!$$If–g!vh5ж 5ж5жT5ж5жЬ#v #v#vT#v#vЬ:V –l”џі=6і,ж5ж 5ж5жT5ж5жЬ9ж/ж џ/ж џџџџџџрџ/ж џџџџџџрџ/ж  џaіgpж2џџџџџџџџџџyt%0d!$$If–g!vh5ж 5ж5жT5ж5жЬ#v #v#vT#v#vЬ:V –l”џі=6і,ж5ж 5ж5жT5ж5жЬ9ж/ж џ/ж џџџџџџрџ/ж џџџџџџрџ/ж  џaіgpж2џџџџџџџџџџyt%0d!$$If–g!vh5ж 5ж5жT5ж5жЬ#v #v#vT#v#vЬ:V –l”џі=6і,ж5ж 5ж5жT5ж5жЬ9ж/ж џ/ж џџџџџџрџ/ж џџџџџџрџ/ж  џaіgpж2џџџџџџџџџџyt%0d!$$If–g!vh5ж 5ж5жT5ж5жЬ#v #v#vT#v#vЬ:V –l”џі=6і,ж5ж 5ж5жT5ж5жЬ9ж/ж џ/ж џџџџџџрџ/ж џџџџџџрџ/ж  џaіgpж2џџџџџџџџџџyt%0d!$$If–g!vh5ж 5ж5жT5ж5жЬ#v #v#vT#v#vЬ:V –l”џі=6і,ж5ж 5ж5жT5ж5жЬ9ж/ж џ/ж џџџџџџрџ/ж џџџџџџрџ/ж  џaіgpж2џџџџџџџџџџyt%0d!$$If–g!vh5ж 5ж5жT5ж5жЬ#v #v#vT#v#vЬ:V –l”џі=6і,ж5ж 5ж5жT5ж5жЬ9ж/ж џ/ж џџџџџџрџ/ж џџџџџџрџ/ж  џaіgpж2џџџџџџџџџџyt%0d!$$If–g!vh5ж 5ж5жT5ж5жЬ#v #v#vT#v#vЬ:V –l”џі=6і,ж5ж 5ж5жT5ж5жЬ9ж/ж џ/ж џџџџџџрџ/ж џџџџџџрџ/ж  џaіgpж2џџџџџџџџџџyt%0d!$$If–g!vh5ж 5ж5жT5ж5жЬ#v #v#vT#v#vЬ:V –l”џі=6і,ж5ж 5ж5жT5ж5жЬ9ж/ж џ/ж џџџџџџрџ/ж џџџџџџрџ/ж  џaіgpж2џџџџџџџџџџyt%0d…$$If–]!vh5ж8#v8:V –l”Jі86і,ж5ж89ж/ж џ/ж aі]pж џџyt%0d!$$If–]!vh5жЬ5ж 5жј5жs5жѕ#vЬ#v #vј#vs#vѕ:V –l”і86і,ж5жЬ5ж 5жј5жs5жѕ9ж/ж џ/ж џџџџџџрџ/ж џџџџџџрџ/ж  џaі]pж2џџџџџџџџџџyt%0d!$$If–]!vh5жЬ5ж 5жј5жs5жѕ#vЬ#v #vј#vs#vѕ:V –l”;і86і,ж5жЬ5ж 5жј5жs5жѕ9ж/ж џ/ж џџџџџџрџ/ж џџџџџџрџ/ж  џaі]pж2џџџџџџџџџџyt%0d!$$If–]!vh5жЬ5ж 5жј5жs5жѕ#vЬ#v #vј#vs#vѕ:V –l”і86і,ж5жЬ5ж 5жј5жs5жѕ9ж/ж џ/ж џџџџџџрџ/ж џџџџџџрџ/ж  џaі]pж2џџџџџџџџџџyt%0d!$$If–]!vh5жЬ5ж 5жј5жs5жѕ#vЬ#v #vј#vs#vѕ:V –l”і86і,ж5жЬ5ж 5жј5жs5жѕ9ж/ж џ/ж џџџџџџрџ/ж џџџџџџрџ/ж  џaі]pж2џџџџџџџџџџyt%0d!$$If–]!vh5жЬ5ж 5жј5жs5жѕ#vЬ#v #vј#vs#vѕ:V –l”і86і,ж5жЬ5ж 5жј5жs5жѕ9ж/ж џ/ж џџџџџџрџ/ж џџџџџџрџ/ж  џaі]pж2џџџџџџџџџџyt%0d!$$If–]!vh5жЬ5ж 5жј5жs5жѕ#vЬ#v #vј#vs#vѕ:V –l”і86і,ж5жЬ5ж 5жј5жs5жѕ9ж/ж џ/ж џџџџџџрџ/ж џџџџџџрџ/ж  џaі]pж2џџџџџџџџџџyt%0d!$$If–]!vh5жЬ5ж 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