UOP 826-2010 Carbon Dioxide in Amine Solution.pdf

1、 IT IS THE USERS RESPONSIBILITY TO ESTABLISH APPROPRIATE PRECAUTIONARY PRACTICES AND TO DETERMINE THE APPLICABILITY OF REGULATORY LIMITATIONS PRIOR TO USE. EFFECTIVE HEALTH AND SAFETY PRACTICES ARE TO BE FOLLOWED WHEN UTILIZING THIS PROCEDURE. FAILURE TO UTILIZE THIS PROCEDURE IN THE MANNER PRESCRIB

2、ED HEREIN CAN BE HAZARDOUS. MATERIAL SAFETY DATA SHEETS (MSDS) OR EXPERIMENTAL MATERIAL SAFETY DATA SHEETS (EMSDS) FOR ALL OF THE MATERIALS USED IN THIS PROCEDURE SHOULD BE REVIEWED FOR SELECTION OF THE APPROPRIATE PERSONAL PROTECTION EQUIPMENT (PPE). COPYRIGHT 1981, 2010 UOP LLC. All rights reserve

3、d. Nonconfidential UOP Methods are available from ASTM International, 100 Barr Harbor Drive, P.O. Box C700, West Conshohocken, PA 19428-2959, USA. The UOP Methods may be obtained through the ASTM website, www.astm.org, or by contacting Customer Service at serviceastm.org, 610.832.9555 FAX, or 610.83

4、2.9585 PHONE. Carbon Dioxide in Amine Solution UOP Method 826-10 Scope This method is for determining carbon dioxide in amine solution using a commercially available total inorganic carbon analyzer. The lower limit of quantitation is 20 mg/L. References ASTM Method D513, “Total and Dissolved Carbon

5、Dioxide in Water,” www.astm.org ASTM Method D1293, “pH of Water,” www.astm.org UIC Application Note 9, “Determination of Carbon Dioxide in Amine Gas Scrubbing Solutions,” UIC Total Inorganic Carbon Analyzer Instrument Manual, Outline of Method The analyzer is purged of atmospheric CO2 and an aliqu

6、ot of the sample is injected. Acid is added to evolve the CO2 and the evolved gas is scrubbed to remove potentially interfering gases. The CO2 is then measured using coulometric titration. Apparatus References to catalog numbers and suppliers are included as a convenience to the method user. Other s

7、uppliers may be used. However, at this writing, UIC is the only known manufacturer of the apparatus required for this analysis. Balance, analytical, readable to 0.0001 g Balance, laboratory, readability 0.01-g Bottle, 500-mL, clear glass, with poly-lined cap, VWR, Cat. No. 89043-070, if needed, see

8、Procedure pH meter, conforming to the requirements given in ASTM Method D1293, “pH of Water” Scrubber, 500-mL, Ace Glass, Cat. No. 4055-06, if needed, see Procedure Syringe, 250-L, glass, cemented needle, VWR, Cat. No. 60373-061 or 60375-263 2 of 3 826-10 Total inorganic carbon analyzer, UIC, Model

9、CM140, with CM5015 coulometer; includes CM5014 analyzer and CM5130 acidification module. Contact the manufacturer for options, accessories, spare parts, and supplies necessary for the specific installation. The following options and supplies are listed in Application Note 9: Auxiliary scrubber assem

10、bly, with 100-mL flask, threaded, Cat. No. CM210-017 Ring stand, with clamp, for holding glassware Reagents and Materials References to catalog numbers and suppliers are included as a convenience to the method user. Other suppliers may be used. References to water mean deionized or distilled. Refer

11、to UIC Application Note 9 and the total inorganic carbon analyzer instrument manual for reagents and materials needed for this analysis. The following reagents and materials are listed in Application Note 9: Carbon anode solution, Cat. No. CM300-002 Carbon cathode solution, Cat. No. CM300-001 Extern

12、al carrier gas (optional, see Application Note 9) Post scrubbing solution, 20% silver nitrate; prepared from reagent water containing 3% hydrogen peroxide and acidified with nitric acid to a pH of 2. Potassium iodide, Cat. No. 300-003 Pre scrubbing solution, 40 to 45% potassium hydroxide solution (o

13、ptional, see Application Note 9) Procedure The analyst is expected to be familiar with general laboratory practices and the equipment being used. Assemble the instrument and analyze samples as described in UIC Application Note 9, “Determination of Carbon Dioxide in Amine Gas Scrubbing Solutions,” an

14、d the instrument manual. ASTM Method D513, “Total and Dissolved Carbon Dioxide in Water,” may also be used for reference. SO2 and H2S will interfere with the analysis of CO2. If these compounds are present in the samples to be analyzed, insert an additional scrubber filled with a silver nitrate solu

15、tion as described in Application Note 9. Calibration is not required, but check the instruments performance by analyzing a small amount of calcium carbonate or sodium bi carbonate and sodium carbonate as described in Application Note 9. Calculations All calculations are performed by the instrument.

16、For additional information, refer to the total inorganic carbon analyzer instrument manual. Precision Repeatability Based on 8 tests performed on each of three samples by one analyst, the within day estimated standard deviations (esd) were calculated at the concentrations listed in the Table. Two an

17、alyses 3 of 3 826-10 performed in one laboratory by the same analyst on the same day should not differ by more than the repeatability allowable difference shown in the Table with 95% confidence. The data in the Table represent short-term estimates of the repeatability of the method. When the test is

18、 run routinely, use of a control standard and a control chart is recommended to generate an estimate of long-term repeatability. Table Repeatability, mg/L Concentration Within- Day esd Allowable Difference 40 2.2 5 3693 29.1 69 30669 774.4 1831 Reproducibility There is insufficient data to calculate

19、 the reproducibility of the test at this time. Time for Analysis The elapsed time and labor requirement for one analysis is less than 0.5 hour. Suggested Suppliers Ace Glass, Inc., 1430 North West Blvd., Vineland, NJ 08362-0688 USA (856-691-3333) UIC, Inc., Joliet, IL 60434-0863 USA (815-744-4477) VWR International, 1310 Goshen Pkwy., West Chester, PA 19380 USA (610-431-1700)