Advanced technics in the. (TIC/TOC/TNb)

Transcription

1 Advanced technics in the determination of sum parameters (TI/T/Tb) Andreas Martens, Elementar Analysensysteme Gmb, anau, Germany БЕОГРАД,

2 What is a sum parameter?

3 Definition: sum parameter A composite parameter achieved by the determination of a general characteristic (x) of various chemical compounds (x i ) as sum without specification of a single compound. i i =1 x i = x 1 + x x i

4 sum parameters...are commonly used in water and waste water analyses for the determination of its contamination with organic compounds. Typical sum parameters are: BD x - biological oxygen demand D - chemical oxygen demand T - total organic carbon

5 sum parameters BD x and B are indirect methods to determine the amount of organic carbon by the determination of the biological and chemical oxygen demand during the decomposition of its compounds. Disadvantage: slow insufficient or wrong oxidation depending from biological activity heavy metal containing reagents no automation

6 sum parameters BD 5 - biological oxygen demand after 5 days DI DI Disadvantage: particulates are not sufficiently oxidized Reference: Fonds der chemischen Industrie - Umweltbereich Wasser

7 sum parameters D - chemical oxygen demand DI Disadvantage: higher or fluctuating results, if dichromate is consumed due to the oxidation of sulfur containing compounds Reference: Fonds der chemischen Industrie - Umweltbereich Wasser

8 sum parameters E European tandard Water analysis - Guidlines for the determination of the total organic carbon (T) and dissolved organic carbon (D) The E 1484 approves the determination of T and D as appropriate method to determine the contamination of water with organic compounds.

9 sum parameters E European tandard Determination ti of T and D by: Wet chemical - UV-persulfat method ombustion method

10 Determination of T and D Wet chemical - UV-persulfat method Advantage: large sample volume (up to 20mL) high sensitivity Disadvantage: insufficient oxidation of particulates not applicable for electrolytes not for highly contaminated samples not for solid samples

11 Determination of T and D ombustion method Advantage: quantitative oxidation of all carbon containing compounds low matrix influence applicable for waste water and solids Disadvantage: lower injection volume (up to 3mL) problematically with salts lower sensitivity

12 onclusion The combustion method has the largest potential to be state of the art, when the disadvantages can be minimized.

13 T E European tandard - total carbon TI - total inorganic carbon ( 2 3 ) T - total organic carbon (+ -, -, - ) TI + T = T (additive determination) T = T - TI (difference method) Direct method: T = (T - TI) after external acidification

14 E European tandard T - total organic carbon P - non-purgable organic carbon P (V) - purgable organic carbon T = P + P or TI + P + P = T P = T -TI -P P = 0 P = T

15 Additive determination TI + T = T or TI + P + P = T liqui T II liqui i T trace

16 P direct (after external acidification) o P 850 o salts & ashes arrier Gas

17 TI/P - determination 2 TI >800 o P P >800 o salts & ashes arrier Gas

18 TI/P/ P - determination o P RT o or higher salts & ashes arrier Gas

19 Dynamic 2-zone-furnace Determination ee of TI and T in solids without acidification by the temperature ramp method.

20 Difference method T = T - TI or P = T - TI - P vario T cube

21 vario T cube arrier Gas Flow TI/T analysis

22 vario T cube Acid Dosing TI/T analysis

23 Flushing with sample vario T cube TI/T analysis

24 Dosing (TI-Measurement) vario T cube TI/T analysis

25 TI-Measurement vario T cube TI/T analysis

26 vario T cube T-Measurement TI/T analysis

27 vario T cube TI/T-Waste TI/T analysis

28 Flushing with sample vario T cube P analysis

29 vario T cube combines for the very first time 110 years of experience in elemental analysis and more than 30 years of experience in T analysis

30 vario T cube TE PWER F EXPERIEE ets new standards in T analysis measuring range for T from 2 ppb to ppm optional up to 50mg abs. in solids Makes auto-dilution unnessesary.

31 vario T cube TE PWER F EXPERIEE ets new standards in T analysis with new detectors free of spectral peak area (arbit tr. units) R 2 = 0, ,05 0,1 0,15 0,2 0,25 0,3 0,35 0,4 0,45 T [mg/l] interferences, e.g. of 2 and with extraordinary linearity over the entire detection range.

32 vario T cube TE PWER F EXPERIEE ets new standards in T analysis Also available for T b determination: LD 0.2ppm 200ppm ED 0.2ppm 500ppm ew DIR detectors with outstanding performance in T b determination. Working range: 0.05ppm 50,000ppm

33 vario T cube TE PWER F EXPERIEE ets new standards in T analysis with its integrated automatic sample feeder for liquids

34 vario T cube TE PWER F EXPERIEE ets new standards in T analysis available with 120 positions for up to 300 mg 80 positions for up to 1 g also applicable for liquids and suspensions by capsule sealing technique with its revolutionary automated analysis of solids

35 vario T cube TE PWER F EXPERIEE ets new standards in T analysis with its unique reusable ash/salt crucible for complete matrix separation, e.g. no restrictions on salt content in liquids and solids

36 vario T cube liquid id solid samples samples ombustion tubes

37 vario T cube ombustion tube for solids ombustion tube for liquids ombustion tubes

38 vario T cube TE PWER F EXPERIEE ets new standards in T analysis with no restrictions on the particle size in liquids o need any more for inaccurate suspension method

39 vario T cube TE PWER F EXPERIEE Applications from liquids to... reagent water drinking water waste water... sea water saline solutions electrolytes...

40 vario T cube TE PWER F EXPERIEE... to solids particles suspensions slurries... soils residues solids...

41 vario T cube TE PWER F EXPERIEE Approved methods, once again improved with ID-3 * counter gas membrane drying chemical drying condensation * 3-step intensive drying system

42 vario T cube TE PWER F EXPERIEE omprehensive math data processing tatistics Manual and automatic peak integration Base line correction Peak substraction

43 vario T cube TE PWER F EXPERIEE Automatic ti alibration by fixed volume and different conc. Dilution series Automatic outlier elimination

44 vario T cube TE PWER F EXPERIEE Automatic alibration by fixed concentration and different volumes auto-dilution-effect without dilution errors Multi-point-calibration from a single standard solution

45 vario T cube TE PWER F EXPERIEE Analysis of well water for animals (liquid samples, particles) Method ample T [mg/l] mean [%] well water 76,520 RD (absolute) 0,271 RD (relative) % 0,354

46 vario T cube TE PWER F EXPERIEE Analysis of hard digestible silicon carbid compounds (ib) Method ample T [mg/l] mean [%] ib 30,82 RD (absolute) 0,0683 RD (relative) % 0,0261 vario T cube shows excellent oxidation behaviour even in case of hard digestable compounds like ib ceramics with decomposition temperaturesres of approx o.

47 vario T cube TE PWER F EXPERIEE Analysis of sea water (liquid samples, salt) Method ample T [mg/l] T measurement of n = 50 sea water samples Method ample T [mg/l] T measurement of n = 50 sea water samples. External sample acidification was performed under stirring in the vials of the automatic sample feeder, followed by automatic stripping of 2 with synthetic air. mean [%] orth ea 24,282 mean [%] orth ea 12,209 RD (absolute) 0,160 RD (absolute) 0,074 Excellent for the analysis of brine solutions

48 vario T cube TE PWER F EXPERIEE Analysis of river sediments (solid sample) Method Analysis of 25 dried river sediments (Elbe/Germany) measured in solid mode Method Analysis of 25 dried river sediments (unte/germany) measured in solid mode n T [%] n T [%] mean [%] 25 5,396 mean [%] 25 4,202 RD (absolute) 0,088 RD (absolute) 0,070 Reference value (variomax) 5,35 % Reference value (variomax) 4,22 %

49 vario T cube TE PWER F EXPERIEE TE FAT I Analytical method: atalytic high temperature digestion tandards: I 8245, EPA 415.1, European standard acc. to E 1484, EV 12260, European Pharmacopoeia 6.0, vol.1 (20244) 2008, U..Pharmacopoeia-F, UP ; DI Measured parameters: T; T, TI/P; D; P optional T b Digestion temperature: free selectable up to 1200 o, standard operating temperature in dependency on the chosen catalyst between o

50 vario T cube TE PWER F EXPERIEE TE FAT II Measuring range (ppm): : 0 60,000 ppm (cube) alternatively high% : % (up to 50mg abs. ) Detection limit: : 0 25,000 ppm (trace) : ppm(ld); 500 ppm(e) : 0 50,000 ppm (DIR) : ± 6 µg/l D (cube) : ± 3 µg/l D (trace) : ± 0.02 mg/l D (DIR) Precision: i <1% at > 5 mg/l /L

51 vario T cube TE PWER F EXPERIEE TE FAT III Injection volume (liquid-mode): ample weight (solid-mode): ml (cube) ml (trace) organic substance mg or up to 1 g soil (depends on the sample matrix) Particel size: Duration of analysis: liquid mode: inner tube diameter 0.8 mm solid mode: free selectable in dependency on the chosen capsule size 2-3 min. for T (solids) 3-4 min. per parameter (liquids)

52 vario T cube TE PWER F EXPERIEE TE FAT IV Gas: synthetic air (hydrocarbon 0.1 mg L -1 and 2 1 mg L -1 ) or oxygen (grade 4.5) Gas flow: 200 ml min min -1 at 1 bar pre-pressure pressure Dimensions: Weight: 55 x 42 x 55 cm (L x W x ) basic unit 55 x 42 x 72 cm (L x W x ) basic unit with autosampler for liquids approx. 60 kg Power supply: 100/110/200/230 V, 50/60 z, 1.6 kw

53 vario T cube TE PWER F EXPERIEE Instrument control and data processing peration and control under Windows XP or Windows Vista. All instrument functions are digitally controllable, the comprehensive operation software includes e.g. automatic leak test, extensive fault diagnostics, monitoring of maintenance cycles, sleep- / awake function, statistical evaluation and almost unlimited memory capacity for storage of analytical data and graphics. Integration to data network and LIM. The possibility of remote control and diagnosis via the internet. In full compliance with 21 FR Part 11 (option).

54 ELEMETAR Analysensysteme Gmb Thank you for your attention. ХВАЛА!

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