?????????????????????? (qualitative analysis)

1
????????????????????
????????????????????

• ??????????????????????????????????????????????????
  ????????????????????????????????? ? ???????
• ?????????????????????????????????????? 2 ??????
• ?????????????????????? (qualitative analysis)
• ??????????????????????????????????????????????????
  ??????????????????????????????????????????????????
  ???????????????????????????
• ?????????????????????? (quantitative analysis)
• ??????????????????????????????????????????????????
  ??????? ? ??????????????

???? ????????????? ??????????????????????????????
???????????????????????? ?????????????????????????
?????????????? ????????
2
????????????????????

• ??????????????????????????????????????????????????
  ???????????????????????????????????
• ???????? 2 ?????? ??????????????????????
  (qualitative analysis) ??? ??????????????????????
  (quantitative analysis)
• ?????????????????????? ????????????????????????
  ??????????????????????????? ??????????????????????
  ????????????????????????????????????
• ?????????????????????? ?????????????????????????
  ???????????????

3
????????????????????(???)

• ?????????????????????? ??????????????????????????
  ????
• Gravimetric technique
• Volumetric or Titrimetric technique
• Spectrometic technique
• Mass spectrometric technique
• Electrochemical technique
• Chromatographic technique
• Nuclear or radiochemical technique
• Thermal technique

4
Gravimetric analysis

• ??????????????????????????????????????????????????
  ????????????????????????????????????????????????
• ??????? 1) ??????????????????????????????? 2)
  ??????????????????????????????? (analyte)
  ????????????????????????? (sample matrix)
  ???????????????????????????? ???
  3)?????????????????????????????????????
• ???????? physical separation ??? chemical
  alteration and separation

5
Gravimetric analysis (???)

• physical separation
• loss on drying ???? ?????????????? TSS
• ???????????????? (loss) ??????????????????????????
  ?? ???????? ???????????? (drying)
• loss on drying
• loss on ignition ???? ???????????????????????????
  ????????
• ????????????????? ?
• ????????????????????? ???? CaCO3 heat CO2
  CaO
• residue on ignition ???? ?????????????? volatile
  solid

6
Gravimetric analysis (???)

• ???????/??????????
• ?????????
• ????????
• Crucible
• Oven
• Muffle furnace
• Desiccator
• ????????????????????

7
Obtain the Samples
Prepare the Sample

• Carry Out the Gravimetric Analysis Method
• Obtain Weight or Volume Data on the Prepared
  Sample.
• . An initial sample weight or volume is always
  needed to the calculate results.
• Carry Out a Physical Operation on the Sample.
• Obtain the Required Data for the Sample
• .This is the final critical piece to most
  gravimetric analysis methods.

Work the Data This is requires weight data to be
used in percent (or similar) calculation can be
derived.
Calculate and Report the Results
8
Titration analysis

• ????????????????????????????????????????????????
  (standard solution) ????????????????????????
  ??????????????????????????????????? (end point)
  ??????????????????????????
• ??????? ??????????????????????? analyte ???
  reagent ??????????????????????????????????????????
  ?????????????????????????????????? visual
  indicator, ????????????????
• End-point detection change of color, change of
  electrical cell potential ???????

9
Titration analysis (???)

• ???????/??????????
• ????????
• ?????????????
• ????????????????????
• pH meter

10
Titration analysis (???)

• ???????????????????????????????
• Acid-Base Titrations ??????????????????????????
  ?????????????? TKN

???????????????????????????? indicator
???????????? Acid-Base Titrations
indicators Low pH color High pH colour Experimental colour change range/pH
Methyl orange red yellow 3.1-4.4
Methyl red red yellow 4.2-6.3
phenoplphthalein colourless red 8.3-10.0
11
Titration analysis (???)

• ??????????????????????????????? (???)
• Redox Titrations ???????????????????????????????
  ??, ?????????????????????????, ???????????????????
  ???????
• KI O (analyte) R (product) I2

12
Obtain the Samples
Prepare the Sample

• Carry Out the Titrimetric Analysis Method
• Obtain Volumetric Data on the Prepared Sample.
• Prepare a Solution of a Substantce With Which the
  Analyte Will React.
• Standize Solutions.
• .It is required to have known quantities to
  which to compare the sample. This is the
• Solution with which the analyte reactesthe
  titrant.
• 4. Obtain the Required Data for the Samples.
• This is the buret reading.

Work the Data This is requires stoichiometry
calculation from which the desired results can
be derived.
Calculate and Report the Results
13
Spectrometric analysis

• Colorimetric analysis
• ??????????????????????????????????????????????????
  ??????????????????????????????????????????????????
  ??????????????????????? ?????????????????????????
  ??????????????????????????????????????????????????
  ????????????????????????????????

14
Colorimetric Analysis

• ???????????????????
• ?????????????? (Lamberts law) ????????????
  ??????????????????????????????????????????????????
  ?

15
Colorimetric Analysis

• ???????????????????
• ??????????? (Beers law) ????????????????????????
  ??????????????????????????????????????
• Beer-Lamberts law
• Absorpbance (A) ?bc
• ????? c ???????????????????????????/????
• b ?????????????????????????????????
• ? molar absorptivity

16
??????????????????????????????????????????????????
???????????????
???????????????????? ???????????????????????????????????? ???????????????????????????????????? ????????
???????????????????? ?? ????? ????????
???????????????? DIN, PO43- ,Si ???????????????
?????????????????? DON, DOP NH3, PO43-
?????????? DON, NH3, PO43-
???????????? DON, DOP, (PO43-)
???????????? NH3 NO2- nitritation
???????????? NO2- NO3- nitratation
?????????????? NO3- (NH3, NO2-) ??????????????
17
???????????????????????????????????

• ??????????????????????????????
• ???????????????????????????????????? ???????
  ??????????
• ??????????????????????????????? ??????????
• ??????? (filtration)
• ????????

18
????????????????
??????
??????????????
????????
???????????????
????????????? 1-2 ????
??????????? 1-2 ????
???????????????????
19
??????????????????????????????????? (???)

• ???????? (matrix)
• Turbidity blank
• ????????????
• ????????????
• ??????????????????????? (low-nutrient seawater,
  LNSW)
• ????????????????????????????

20
??????????????????????????????????? (???)

• ??????????? (calibration curve)
• 1) ??????????????????????????? ????????
  ??????????????????????????????
  ??????????????????????????????????????????????
  0.8-1
• 2) ?????????????????? (???????????????
  ???????????????????????????????????????????????)
  ??????????????????????? ??????????????????????????
  ??????????????? 2 ???????????????????????????????
  ???????????????
• 3) ???????????????????????????????????????????????
  ? 5 ??????????? ?????????????) ???????????????????
  ??????????????????????????????????????????????????
  ??? ??????????????????? 3 ???
• ??????????????????? ?????????????????????????????
  ??????????????? reference cell
• 5) ????????????????????????????????????????????
  ???????????????????????????????????????? (linear
  regression)

21
??????????????????????????????????? (???)

• ???????????????
• Duplicate analysis
• Spiked sample
• CRM, SRM, LRM
• Control chart

22
??????????????????????????????????? (???)

• ?????????????? molar absorptivity
• A?bc
• ???????? molar absorptivity ???????????????????
  ??????????? diazotization 46000
• A (46000 x concentration)/(14 x10-6)