Inorganic Chloride By iC

Question 1

Preparation of Samples

Answer 1

• begin heating DI water, when boiling reduce heat
• sample should be shaken for 2 minutes vigorously and intermittently vented
• required 200mL if sample should be immediately poured in graduate and placed in separatory funnel
• for crude oils, pour up 200mL of toluene into separatory funnel (do not use toluene for anything but crude oils)
• for crude oils pour up 200mL of heated DI water (do not use heated DI water for hydrocarbons other than crude oils)
• place stopper in separatory funnel, cover stopper with rag and invert separatory funnel and vent
• mix sample for 2 minutes being careful to vent frequently at start of mixing (failure to vent can risky in the separatory funnel exploding)
• mixing sample for 2 minutes, return funnel to ring stand and remove stopper
• allow sample mixture to settle and separate. FOR CRUDE OILS ONLY use the electrostatic separator to aid separation
• allow 5 minutes for sample to settle after mixing and shocking
• filter crude oils through fluted filter paper into 25mL graduate. For other hydrocarbons DO NOT use filter paper (can add chlorides to sample)
• after filtering, fill vials and dilute sample if necessary (check with chloride strip to determine if dilution necessary)
• refer to fluoride example to run chromeleon samples

Question 2

Results

Answer 2

• graphs should be examined for correct integration
• if no peak, and dilution was done, you can run sample straight
• never report an area smaller or larger than smallest and largest area of calibration

Question 3

Troubleshoot

Answer 3

• never allow instrument to run out of eluent. Do not add eluent during run
• when refilling eluent bottle try not to let air into line
• from Robinson panel, if pressure seems abnormally high, could indicate plug in a line, if abnormally low, could indicate leak
• if you fee sample did not run well, rerun to verify
• if standard hits and it still runs weird, call for resample and notify chemist over area
• if area count of sample outside range of calibration, you will need to either dilute sample or dilute more if it was diluted

Question 4

Purpose

Answer 4

Determine the amount of salt in crude oils and hydrocarbons which are not vapor at room temperature and pressure. Ion chromatography used to determine amount of salt present as sodium chloride by measuring chloride content. Value is used to calculate amount of salt present in units of pounds per thousand barrels (PTB-lb/1000bbl). Knowing amount of salt in crude oil is important in evaluating effectiveness of desalters. Chloride in crude oil can have corrosive effects as well as negatively impact catalysts on refining units.