[Header] Format=SMU ver=3 appl=GUMWB32 MR=0 SUR=0 SUP=0 UIP=1 UCR=0 status=2 FUEB=0 [Title] Title='Standardising a sodium hydroxide solution' Ref='' Date='08/29/2007' Version='' Author='' Description=11 Description[0]='This is the example A2 of the EURACHEM /' Description[1]='CITAC Guide "Quantifying Uncertainty in Analytical Measurement", Second' Description[2]='Edition.' Description[3]='' Description[4]='A' Description[5]='solution of sodium hydroxide (NaOH) is standardised against the titrimetric' Description[6]='standard potassium hydrogen phtalate (KHP).' Description[7]='' Description[8]='The titrimetric standard KHP is dried and weighed. After the preparation of the' Description[9]='NaOH solution a' Description[10]='sample of the KHP is dissolved and then titrated using the NaOH solution.' PictureCount=1 DCount=1 [Model] Model=15 Model[0]='{Molar mass of KHP}' Model[1]='' Model[2]='M_KHP = 8 * M_C + 5 * M_H + 4 * M_O + M_K;' Model[3]='' Model[4]='{Volume delivered by the piston burette, excluding repeatability}' Model[5]='' Model[6]='V_T = V_nominal * f_V\minus\calibration * f_V\minus\temperature;' Model[7]='' Model[8]='{mass of KHP weighed, excluding repeatability}' Model[9]='' Model[10]='m_KHP = m_container\sp\and\sp\KHP - m_container\sp\less\sp\KHP;' Model[11]='' Model[12]='{calculation of the concentration of the NaOH solution}' Model[13]='' Model[14]='c_NaOH = (k_mL * m_KHP * P_KHP) / (M_KHP * V_T) * f_repeatability;' CE=1 CTC=1 [Components] CompOrder=3 Comp=16 Comp[0]=M_KHP_ Comp[1]=M_C_ Comp[2]=M_H_ Comp[3]=M_O_ Comp[4]=M_K_ Comp[5]=V_T_ Comp[6]=V_nominal_ Comp[7]=f_V\minus\calibration_ Comp[8]=f_V\minus\temperature_ Comp[9]=m_KHP_ Comp[10]=m_container\sp\and\sp\KHP_ Comp[11]=m_container\sp\less\sp\KHP_ Comp[12]=c_NaOH_ Comp[13]=k_mL_ Comp[14]=P_KHP_ Comp[15]=f_repeatability_ [COMP 0] Type=Temp Definition='Molar mass of KHP' Unit='g/mol' Description=0 Fcov=2 NomUnit= UncUnit= CovID=1 UncID=0 Vnom=204.2212 Ustd=0.00376530211271287 Neff=10000 HB=0 HC=0 HR=0 IO=0 PictureCount=1 DCount=1 [COMP 1] Type=TypBRectang Definition='Atomic weight of carbon' Unit='g/mol' Description=3 Description[0]='The atomic weight of carbon and its uncertainty are taken from data listed in' Description[1]='the latest IUPAC table of atomic weights. The IUPAC quoted data is considered' Description[2]='to be of rectangular distribution.' Vnom=12,0107 Hlim=0,0008 PictureCount=1 DCount=1 [COMP 2] Type=TypBRectang Definition='Atomic weight of hydrogen' Unit='g/mol' Description=3 Description[0]='The atomic weight of hydrogen and its uncertainty are taken from data listed in' Description[1]='the latest IUPAC table of atomic weights. The IUPAC quoted data is considered' Description[2]='to be of rectangular distribution.' Vnom=1,00794 Hlim=0,00007 PictureCount=1 DCount=1 [COMP 3] Type=TypBRectang Definition='Atomic weight of oxygen' Unit='g/mol' Description=3 Description[0]='The atomic weight of oxigen and its uncertainty are taken from data listed in' Description[1]='the latest IUPAC table of atomic weights. The IUPAC quoted data is considered' Description[2]='to be of rectangular distribution.' Vnom=15,9994 Hlim=0,0003 PictureCount=1 DCount=1 [COMP 4] Type=TypBRectang Definition='Atomic weight of potassium' Unit='g/mol' Description=3 Description[0]='The atomic weight of potassium and its uncertainty are taken from data listed' Description[1]='in the latest IUPAC table of atomic weights. The IUPAC quoted data is' Description[2]='considered to be of rectangular distribution.' Vnom=39,0983 Hlim=0,0001 PictureCount=1 DCount=1 [COMP 5] Type=Temp Definition='Volume delivered by piston burette' Unit='mL' Description=0 Fcov=2 NomUnit= UncUnit= CovID=1 UncID=0 Vnom=18.64 Ustd=0.0127107853415908 Neff=1334 HB=0 HC=0 HR=0 IO=0 PictureCount=1 DCount=1 [COMP 6] Type=Const Definition='Volume indicated by burette' Unit='mL' Description=14 Description[0]='The nominal volume is not associated with any uncertainties. The uncertainty of' Description[1]='the real volume of the burette has three components, repeatability, calibration' Description[2]='and temperature. The latter two are included in the uncertainty budget as' Description[3]='separate factors. Repeatability of the volume delivery is taken into account' Description[4]='via the combined repeatability term for the experiment, f_repeatability_.' Description[5]='Another factor influencing the result of the titration, which can also be' Description[6]='attributed to the automatic titration system, of which the burette is one part,' Description[7]='is the bias of the end-point detection. The titration is performed under a' Description[8]='protective atmosphere (Ar) to prevent absorption of CO_2_, which would bias the' Description[9]='titration. There are no indications that the end-point determined from the' Description[10]='shape of the pH-curve does not correspond to the equivalence-point, because a' Description[11]='strong acid is titrated with a' Description[12]='strong base. No further uncertainty contributions are introduced to cover the' Description[13]='bias of the end-point detection.' Vnom=18,64 PictureCount=1 DCount=1 [COMP 7] Type=TypBTriangl Definition='Uncertainty contribution to the volume due to uncertainty in calibration of the burette' Unit='' Description=11 Description[0]='The limits of accuracy for a' Description[1]='20 mL piston burette are indicated by the manufacturer as typically ±0.03 ml.' Description[2]='No further statement is made about the level of confidence or the underlying' Description[3]='distribution. An assumption is necessary to work with this uncertainty' Description[4]='statement. In this case a' Description[5]='triangular distribution is assumed. Since f_V\minus\calibration is a' Description[6]='multiplicative factor to the nominal volume, which is only used to introduce' Description[7]='the calibration uncertainty, it has the value 1. The halfwidth of limits' Description[8]='corresponds to the relative uncertainty as stated by the manufacturer (i.e.' Description[9]='0.03 mL /' Description[10]='20 mL).' Vnom=1 Hlim=0,0015 PictureCount=1 DCount=1 [COMP 8] Type=TypBNormal Definition='Uncertainty contribution to the volume due to temperature variation' Unit='' Description=15 Description[0]='The laboratory temperature can vary by ±3°C. The uncertainty of the volume due' Description[1]='to temperature variations can be calculated from the estimate of the possible' Description[2]='temperature range and the coefficient of the volume expansion. The volume' Description[3]='expansion of the liquid is considerably larger than that of the burette, so' Description[4]='only the volume expansion of the liquid is considered. The coefficient of' Description[5]='volume expansion for water is 2.1\cdot\10^-4^°C^-1^, which is used here also' Description[6]='for the NaOH solution. This leads to a' Description[7]='possible volume variation of ±(19 \cdot\ 3 \cdot\ 2.1\cdot\10^-4^/1.96) mL =' Description[8]='±0.006 mL. A' Description[9]='rectangular distribution is assumed for the temperature variation Since' Description[10]='f_V\minus\temperature is a' Description[11]='multiplicative factor to the nominal volume, which is only used to introduce' Description[12]='the temperature uncertainty, it has the value 1. Its uncertainty is calculated' Description[13]='as 0.006 mL /' Description[14]='19 mL.' Vnom=1 Uexp=0,0003 Fcov=1 PictureCount=1 DCount=1 [COMP 9] Type=Temp Definition='Mass of KHP weighed' Unit='g' Description=0 Fcov=2 NomUnit= UncUnit= CovID=1 UncID=0 Vnom=0.3888 Ustd=0.00012247448713916 Neff=10000 HB=0 HC=0 HR=0 IO=0 PictureCount=1 DCount=1 [COMP 10] Type=TypBRectang Definition='Mass of container and KHP' Unit='g' Description=10 Description[0]='Repeatability of the wheighing is taken into account via the combined' Description[1]='repeatability term, f_repeatability_. Any systematic offset across the scale' Description[2]='will also cancel due to the wheighing by difference. The only contributing' Description[3]='source of uncertainty is the linearity of the balance. The calibration' Description[4]='certficate of the balance quotes ±0.15 mg for the linearity. The manufacturer' Description[5]='recommends using a' Description[6]='rectangular distribution to convert this linearity contribution into a' Description[7]='standard uncertatiny. This uncertainty is not correlated with the uncertainty' Description[8]='of m_container\sp\less\sp\KHP, since they are independent observations and the' Description[9]='linearity effects are not correlated.' Vnom=60,5450 Hlim=0,00015 PictureCount=1 DCount=1 [COMP 11] Type=TypBRectang Definition='Mass of container less KHP' Unit='g' Description=10 Description[0]='Repeatability of the wheighing is taken into account via the combined' Description[1]='repeatability term, f_repeatability_. Any systematic offset across the scale' Description[2]='will also cancel due to the wheighing by difference. The only contributing' Description[3]='source of uncertainty is the linearity of the balance. The calibration' Description[4]='certficate of the balance quotes ±0.15 mg for the linearity. The manufacturer' Description[5]='recommends using a' Description[6]='rectangular distribution to convert this linearity contribution into a' Description[7]='standard uncertatiny. This uncertainty is not correlated with the uncertainty' Description[8]='of m_container\sp\and\sp\KHP, since they are independent observations and the' Description[9]='linearity effects are not correlated.' Vnom=60,1562 Hlim=0,00015 PictureCount=1 DCount=1 [COMP 12] Type=Result Definition='Concentration of the sodium hydroxide solution' Unit='mol/L' Description=0 Fcov=2 NomUnit= UncUnit= CovID=1 UncID=0 Vnom=0.102136159706791 Ustd=9.67818987998781E-5 Neff=570 HB=1 HC=0 HR=1 IO=0 PictureCount=1 DCount=1 [COMP 13] Type=Const Definition='Conversion factor 1000 ml = 1L' Unit='mL/L' Description=0 Vnom=1000 PictureCount=0 DCount=0 [COMP 14] Type=TypBRectang Definition='Purity of the KHP' Unit='' Description=3 Description[0]='In the supplier''s catalogue, the purity of the KHP is given as 1.0000±0.0005.' Description[1]='No further information concerning the uncertainty is given. Therefore this' Description[2]='value is assumed to be of rectangular distribution.' Vnom=1 Hlim=0,0005 PictureCount=1 DCount=1 [COMP 15] Type=TypBNormal Definition='Repeatability of the titration' Unit='' Description=9 Description[0]='All uncertainty contributions due to repeatability of one of the operations are' Description[1]='combined in this factor. It includes at least the repeatability of the' Description[2]='wheighings and of the volume delivered by the burette. The magnitude of this' Description[3]='uncertainty contribution is assessed during the method validation stage. The' Description[4]='data shows that the overall repeatability of the titration experiment is 0.05%.' Description[5]='Since f_repeatability is a' Description[6]='multiplicative factor to the result, which is only used to introduce the' Description[7]='repeatability uncertainty, it has the value 1' Description[8]='with an uncertainty of 0.0005.' Vnom=1 Uexp=0,0005 Fcov=1 PictureCount=1 DCount=1 [Correlations] Description=0 [CalCorr] CNT=20 R[0,12]=-0.0194574 R[5,12]=-0.7196345 R[9,12]=0.3324335 R[0,1]=0.98134 R[0,3]=0.1840013 R[0,2]=0.053667 R[0,4]=0.0153334 R[5,7]=0.8980265 R[5,8]=0.4399413 R[9,10]=0.7071068 R[9,11]=-0.7071068 R[12,7]=-0.6462509 R[12,15]=0.5276615 R[12,8]=-0.3165969 R[12,14]=0.3046455 R[12,10]=0.235066 R[12,11]=-0.235066 R[12,1]=-0.0190943 R[12,3]=-0.0035802 R[12,2]=-0.0010442