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 2008 UOP LLC. All rights reserved. Non
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4、 PHONE. Chloride in Liquid Hydrocarbons by Dry Colorimetry UOP Method 799-08 Scope This method is for determining the sum of organic chloride and hydrogen chloride (HCl) in liquid hydrocarbons at concentrations ranging from approximately 0.5 to 500 mass/volume-ppm (mg/L). Other halogens, if present,
5、 are determined as chloride. References ASTM Method D 4052, “Density and Relative Density of Liquids by Digital Density Meter,” www.astm.org ASTM Method D 4307, “Preparation of Liquid Blends for Use as Analytical Standards,” www.astm.org Instrument instruction manual, C.I.Analytics PN 2010-Cl-man UO
6、P Method 999, “Precision Statements in UOP Methods,” www.astm.org Outline of Method A commercial chloride analyzer utilizing dry colorimetric detection is set up according to the manufacturers specifications. The sample is subjected to pyrolysis which converts the organic chlorides to HCl. The pyrol
7、ysis product is then passed to a detector where the HCl causes a color change on sensitized paper. The measured color change is proportional to the quantity of chloride in the sample. Calibration is performed using blends of known concentrations of chloride in a liquid hydrocarbon. Apparatus Referen
8、ces to catalog numbers and suppliers are included as a convenience to the method user. Other suppliers may be used. Chloride analyzer, with Dry Colorimetric Detector (DCD), C.I.Analytics, 2010L. Stock replacement parts as recommended by the manufacturer. Regulator, air, two-stage, high purity, with
9、stainless steel diaphragm, delivery pressure range 30-700 kPa (4-100 psi), Matheson Tri-Gas, Cat. No. 3122-590 2 of 4 799-08 Regulator, nitrogen, two-stage, high purity, with stainless steel diaphragm, delivery pressure range 30-700 kPa (4-100 psi), Matheson Tri-Gas, Cat. No. 3122-580 Regulator, oxy
10、gen, two-stage, high purity, with stainless steel diaphragm, delivery pressure range 30-700 kPa (4-100 psi), Matheson Tri-Gas, Cat. No. 3122-540 Reagents and Materials References to catalog numbers and suppliers are included as a convenience to the method user. Other suppliers may be used. Air, comp
11、ressed gas, 99.99% minimum purity Chlorobenzene, 99.9% minimum purity, Burdick if the isooctane is not halogen-free, find another source for the isooctane. Calculate the chloride concentration to three significant figures in each of the Calibration Blends using Equation 1. 3 of 4 799-08 6.112A5.35C
12、= (1) where: A = concentration of chlorobenzene in Calibration Blend, mg/kg C = concentration of chlorine in blend, mg/kg 35.5 = atomic weight of chlorine 112.6 = molecular weight of chlorobenzene Determine the density of the calibration blend, either by using ASTM Method D 4052, “Density and Relati
13、ve Density of Liquids by Digital Density Meter,” or by using a literature value for the density of isooctane. Calibration Calibrate the instrument as described in the instrument manual. After all required parameters are entered into the instrument, the calibration factors are calculated by the instr
14、ument software. Sample Analysis Analyze the samples according to the instrument manufacturers instructions. Calculations All calculations are performed by the instrument software and printed out automatically. Results will be shown in mass/volume-ppm (mg/L). If results in mass-ppm (mg/kg) are desire
15、d, determine the density of the sample using ASTM Method D 4052. Convert mg/L to mg/kg using Equation 2. SBD = (2) where: B = chloride, mg/L D = chloride, mg/kg S = density of the sample, g/mL Report the results to one significant figure below one mg/L (or mg/kg), and to two significant figures at o
16、r above one mg/L (or mg/kg). Note In refinery applications, it may be advantageous to analyze for chloride using an online analyzer. Similar online analyzers using dry colorimetric detection are available from the suggested supplier and may be substituted. Precision Analyses of the samples used for
17、the precision statement were performed by the suggested vendor. Repeatability and Site Precision A nested design was carried out by two analysts, with each analyst performing analyses on two separate days, performing two analyses each day for a total of eight analyses. Using a stepwise 4 of 4 799-08
18、 analysis of variance procedure, the within-day estimated standard deviations (esd) were calculated at the concentration means listed in the Table. Two analyses performed in one laboratory by the same analyst on the same day should not differ by more than the repeatability allowable differences show
19、n in the Table with 95% confidence. Two analyses performed in one laboratory by different analysts on different days should not differ by more than the site precision allowable differences shown in the Table with 95% confidence. Table Repeatability and Site Precision, Chloride, mg/kg Repeatability S
20、ite Precision Mean Concentration Within- Day esd Allowable DifferenceWithin- Lab esd Allowable Difference 0.5 0.004 0.01 0.049 0.30 50 0.28 1.1 1.25 7.6 The data in the Table represent short-term estimates of the repeatability of the method. When the test is run routinely, use of a control standard
21、and a control chart is recommended to generate an estimate of long-term repeatability. Reproducibility There is insufficient data to calculate the reproducibility of the test at this time. Time for Analysis The elapsed time and labor requirement for one analysis is one hour, including calibration. E
22、ach succeeding analysis requires 0.3 hour. Suggested Suppliers C.I.Analytics, 2085 Industrial Blvd., Chambly, Quebec, Canada J3L 4C5 (450-658-4965) Grace, 2051 Waukegan Rd., Deerfield, IL 60015 (847-948-8600) Matheson Tri-Gas, 166 Keystone Drive, Montgomeryville, PA 18936 (215-648-4000) VWR International, 1310 Goshen Parkway, West Chester, PA 19380 (610-431-1700)
