SLA SOP-00077/13

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ACT1 BY GC FID

1.0 INTRODUCTION

1.1 This method is used for determining ACT-1 Activator in the Benfield solution at its working concentration,
and in water samples such as stripper condensate in concentrations of 50 – 1,000 ppm.

2.0 SCOPE

2.1 Samples are collected using special procedures that include the addition of Triethylenetetramine (Trien).
Trien prevents adsorption of the ACT-1 activator on the surfaces of the containers and syringes. The
treated samples are analyzed for ACT-1 via GC with an FID detector. Peak areas are measured with an
electronic integrator, and external standards (also treated with Trien) are used to quantify the results.

3.0 DEFINITIONS

3.1 SAP – Systems Application Program

3.2 FID – Flame Ionization Detector

4.0 REFERENCE METHOD

4.1 Test Codes

4.1.1 LC-OPL

4.2 Primary Reference

4.2.1 UOP 177073 rev 1 – “Analysis of UOP Benfield Activator ACT-1 by Gas Chromatography”.

4.3 Deviations
Table #1: Deviations from primary reference method (UOP 177073 rev1).
Reference Deviation
The reference method stated specific instrumentation and Bureau Veritas Laboratories is using a newer model Varian
operational settings for the GC 6890 split/splitless instrument. Through assistance of PCLI
R&D method development was done to have the system
work on the new instrument. Some setting may vary
slightly from the reference method. Validation of the
system was done to ensure proper operation.
The reference method states calculate a K factor after The system is calibrated with 3 standards, the equation of
calibration and to use the average “K” value for calculation the line is used for calculation of result in electronic form to
of results. make calculations easier. The line equation method is also
a more accurate way of achieving the final result.

5.0 REGULATORY CRITERIA

5.1 None.

6.0 SAFETY

6.1 General Safety requirements for this SOP are provided in a critical task analysis (CTA). In addition to the
CTA, additional guidance on Bureau Veritas Laboratories Environment, Health and Safety (EHS) program
are found in various Safe Work Procedures, Safety Policies, and the Safety Guide (See MEHS WI-00013).
Chemical wastes and sample disposal protocols are outlined in the Corporate Environmental Waste
Management Policy (MEHS WI-00069).
6.2 The use of personal protective equipment (PPE), including safety glasses and lab coats are mandatory in all
Bureau Veritas Laboratories. It is the responsibility of the analyst to read and understand the CTA attached
to this SOP and ensure that any additional identified hazard controls are used (e.g. nitrile gloves, splash
goggles, fume hoods, respirators, etc).
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6.3 Material safety data sheets for all chemical reagents are available to personnel using this method. Training
on the interpretation of MSDS sheets is provided during WHMIS training upon hire. Staff performing this
method shall review the associated MSDS sheets for chemicals used in this procedure and ensure they
understand the associated hazards and safety controls required to work safely with each chemical.
6.4 General information for chemical waste and sample disposal is described in the Health and Safety work
instructions. Disposal of all samples, extracts and reagents must be done in accordance with local,
provincial and federal laws and regulations. Chemical wastes and sample disposal protocols are described
in SLA WI-00007.

7.0 SAMPLE HANDLING, PRESERVATION, HOLDING TIME

7.1 Containers Used

7.1.1 Various size glass bottles

7.2 Sample Size

7.2.1 20g

7.3 Sample Preservation

7.3.1 Samples are transported from the client to the lab at the ambient temperature.
7.3.2 In the lab, samples are kept at room temperature.

7.4 Analytical Holding Time

7.4.1 Samples are analyzed the day that they are received. Samples are then kept on the warehouse
shelf for 3 months then disposed of.

8.0 INTERFERENCES

8.1 None

9.0 DETECTION LIMITS

9.1 Reporting Detection Limit

9.1.1 The lowest reportable value is 0.1%.

9.2 Measurement of Uncertainty

9.2.1 Trial processes will determine site precision. Site Precision is defined as: The value below which
the absolute difference between two individual test results obtained under site precision conditions
may be expected to occur with a probability of approximately 95%. It is defined as 2.77 times the
standard deviation of the results obtained under site precision conditions.

9.2.2 Site Precision Conditions are defined as: Conditions under which test results are obtained by one
or more operators in a single site location practicing the same test method on a single
measurement system which may be comprised of multiple instruments, using test specimens taken
at random from the same sample material, over an extended period of time, spanning at least a 15
day interval.

9.2.3 (NOTE: Referenced from SLA WI-00038 “Measurement Uncertainty Policy for Industrial.”)

9.3 Precision and Bias

9.3.1 Repeatability
9.3.1.1 The repeatability for this method has been set at 10%.

9.3.2 Reproducibility
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9.3.2.1 The reproducibility for this method has been set at 20%.

10.0 GLASSWARE CLEANING

10.1 The syringe is flushed thoroughly with Type 1 water to prevent blockage.
10.2 Volumetric Flasks are cleaned with soap and water and then air dried.
11.0 APPARATUS AND MATERIALS
11.1 5 µL syringe with Handle, Fisher Cat. # 14815202 or equivalent
11.2 Various size volumetric flasks
11.3 Disposable pipette
11.4 Agilent 6890N GC/FID; split splitless
11.5 Spatula
11.6 Analytical Balance
11.7 Various Class A volumetric pipettes

12.0 REAGENTS AND STANDARD PREPARATION

12.1 Trien solution
12.1.1 Dissolve exactly 16.67grams Trien Solution into a 1L “Class A” volumetric flask and dilute to the
mark with Type 1water.
12.2 1% ACT-1
12.2.1 Dissolve exactly 1.538g of Benfield Activator Solution into a 100ml “Class A” volumetric flask
and dilute to the mark with the solution in 12.1.1.
12.3 0.05%, 0.1%, 0.25% ACT-1 & 0.15% QC.
12.3.1 Using a “Class A” volumetric pipette add 5ml of solution 12.2 to 100ml “Class A” volumetric
flask, dilute to the mark with the solution in 12.1.1. Label as 0.05% ACT-1.
12.3.2 Using a “Class A” volumetric pipette add 10ml of solution 12.2 to 100ml “Class A” volumetric
flask, dilute to the mark with the solution in 12.1.1. Label as 0.1% ACT-1.
12.3.3 Using a “Class A” volumetric pipette add 25ml of solution 12.2 to 100ml “Class A” volumetric
flask, dilute to the mark with the solution in 12.1.1. Label as 0.25% ACT-1.
12.3.4 Using a “Class A” volumetric pipette add 15ml of solution 12.2 to 100ml “Class A” volumetric
flask, dilute to the mark with the solution in 12.1.1. Label as 0.15% ACT-1 QC.
12.3.5 Invert ALL solutions at least ten times to ensure proper mixing.
12.3.6 Store all standards in the fridge in a glass bottle.

12.4 Expiry Date and Storage Conditions

12.4.1 The default expiry date is as specified on the manufacturer’s label.
(NOTE: If the label lists, i.e. March 2006, as an expiry date, the product is valid until the last day
of March 2006.)
12.4.2 If no expiry date is specified, refer to CAM WI-00010 Preparation and Labeling of Reagents and
Standards.
12.4.3 All prepared reagents are stored at room temperature.

13.0 SAMPLE PREPARATION

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13.1 Sample Preparation

13.1.1 Weigh 5g +/- 0.001 of Lean Carbonate, Benfield Solution or Water Sample into a 50ml volumetric
flask. Dilute to the mark with the solution in 12.1.1
13.1.2 Invert at least 10 times to ensure proper mixing.

14.0 ANALYTICAL DETERMINATION

NOTE: A flush is to be run after each sample.

14.1 Preparation of Apparatus

14.1.1 Load Method ACT-1.M
14.1.2 Allow 15 minutes to warm up.

14.2 Instrument Method Settings

14.2.1 Refer to Attachment 1.

14.3 Procedure Sample Analysis

14.3.1 Open Chemstation software.

14.3.2 Ensure the detector is lit before injecting any samples or standards. This is done by clicking on the
FID icon and ensuring beside “flame” it says “on”.
14.3.3 If the flame is “off” then click on the re-ignite button, if this does not work then shut down the
software and re-start (if there are still continuing problems contact the shift lead).
14.3.4 Load the ACT-1.M method by:
14.3.4.1 Clicking on Method, then load method and select ACT-1.M.
14.3.5 Click on “Sample Info”.
14.3.6 Create a new sub-directory at the beginning of each month using the following format
(SEPT2017) this would represent September 2017.
14.3.7 For the QC, beside “Sample Name” enter the QC information in the following format (QC0927-1)
this would represent the QC 0.15% injection 1 for run day September 27th.
14.3.8 For the QC, beside “Signal 2” enter the QC information in the following format (QC0927-1.D)
this would represent the QC 0.15% injection 1 for run day September 27th. The “D” represents the
file type which is Data. “Signal 2” can only accept a total of 10 characters including the “.D”.
14.3.9 For the Lean Carbonate sample, beside “Sample Name” enter the information in the following
format (LC0927-1). This would represent the Lean Carbonate sample, injection 1 for run day
September 27th.
14.3.10 For the sample Lean Carbonate, beside “Signal 2” enter the sample information in the following
format (LC0927-1.D) this would represent the Lean Carbonate sample for September 27 th the first
injection.
14.3.11 Modify 14.3.8 and 14.3.10 for each injection by changing the injection number for whatever
injection you are running.
14.3.12 Click
14.3.13 Run 1 injection for the QC.
14.3.14 Run 2 injections for the sample.
14.3.15 Rinse syringe several times with 1% Trien and discard waste
14.3.16 Fill the 5 µl syringe as follows.
14.3.16.1.1 2.0 µl 1% Trien solution.
14.3.16.1.2 1.0 µl air.
14.3.16.1.3 1.0 µl sample.
14.3.16.1.4 1.0 µl air.
14.3.16.1.5 Wipe off needle.
14.3.17 Inject sample
14.3.18 As soon as the injection is complete press the “start” button on the instrument.
14.3.19 Once the injection is completed print out the chromatogram and calculate as per SLA FCD-00207
(the one saved in the current calibration month).
14.3.20 Save the file in that months calibration folder in the following format
14.3.20.1 LC-“current analysis date” (LC-2015-04-13).
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14.3.20.2 Print out a copy of the final calculation and attach to the chromatograms and the
Lean Carbonate worksheet.
14.3.21 Do 1 injection of water at the end of the analysis as per 14.3.16.1 to 14.3.16.5 but substituting
“water” for the “sample”.
14.3.22 Rinse the syringe several times with 1% Trien solution and place back in the box for
storage.

14.4 Calibration

14.4.1 Click on “Sample Info”.

14.4.2 Create a new sub-directory for that day using the following format (APRCAL) this would
represent April’s calibration (location is P:\ACT-1\Calibrations\.
14.4.3 For the STD, beside “Signal 2” enter the STD information in the following format (CAL-05-1.D)
this would represent the calibration STD 0.05% injection 1 data file.
14.4.4 Modify 14.4.3 for each injection by changing the injection number for whatever injection you are
running.
14.4.5 Inject each standard 3 times.
14.4.6 Repeat 14.4.3 and 14.4.4 in the Sample name section.
14.4.7 Repeat 14.4.3 for the other 2 calibrations STDs.
14.4.8 Instrument is calibrated with 0.05%, 0.10% and 0.25% ACT-1 standards.
14.4.9 Instrument will be calibrated when one or more of the following criteria applies.
14.4.9.1 Column has been replaced.
14.4.9.2 New standards have been prepared.
14.4.9.3 QC is trending outside of 3 Sigma.
14.4.10 Fill the 5 µl syringe as follows with the first standard
14.4.10.1 2.0 µl 1% Trien solution.
14.4.10.2 1.0 µl air.
14.4.10.3 1.0 µl standard.
14.4.10.4 1.0 µl air.
14.4.10.5 Wipe off needle.
14.4.11 Inject the standard.
14.4.12 As soon as the injection is complete press the “start” button on the instrument.
14.4.13 Once the injection run is complete repeat 14.4.10 two more times for the same standard.
14.4.14 Once the 3 injections of the first standard are complete repeat 14.4.10 for the other 2 calibration
standards.
14.4.15 Once all injections are complete, calculate and ensure all criteria have been met as per SLA
FCD-00207.
14.4.16 The correlation must be at minimum 0.995 to proceed with analysis.

14.5 Integration

14.5.1 For efficiency purposes this should be done after each injection is complete
14.5.2 Open up the “offline” copy of Chemstation.
14.5.3 Go to “File”.
14.5.4 Then “Load Signal”.
14.5.5 Load the chromatogram of interest.
14.5.6 Integrate the peak using the integration tool.
14.5.7 Peaks are integrated as per COR WI-00044 “Manual Integration of Chromatographic Peaks”.
14.5.8 The peak of interest will be at approximately 15min +/- 0.5min.
14.5.9 Once the peak has been integrated print the chromatogram, review and initial all raw data.

15.0 QUALITY CONTROL REQUIREMENTS

15.1 Quality Control (QC Sample)

15.1.1 A 0.15% QC is run each running day.

15.1.2 Calculate the result using SLA FCD-00207.
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15.1.3 If the QC result is outside 3 Sigma range repeat analysis once.

15.1.4 If it is still outside the 3 Sigma control limit suspend analysis and notify Management.
15.1.5 If the recheck is within the 3 Sigma control limits proceed with analysis.

15.2 Control Charting

15.2.1 All QC results must be documented on the ACT-1 QC control chart

15.2.2 Corrective action is required when errors, deficiencies or out of control situations exist. If a
corrective action is called for, the action must be carried out as per COR WI-00055
“Environmental Procedure for Control Charting.”

16.0 DATA INTERPRETATION AND CALCULATION

16.1 Calculations

16.1.1 Calibration value

16.1.1.1 Calculate the calibration curve y-intercept, slope, and correlation as per SLA FCD-00207,
with a minimum correlation of 0.995.
16.1.1.2 Save the file on the P:\ACT-1\Calibrations\
16.1.1.3 This file will be used for calculations for that month.

16.1.2 Sample value

16.1.2.1 Calculate the sample value using SLA FCD-00207
16.1.2.2 Print a copy of the calculation and attach to the chromatograms and the Lean
Carbonate worksheet.
16.2 Reporting

16.2.1 Report the result on the Lean Carbonate worksheet SLA FCD-00038.
16.2.2 Include all chromatogram printouts and calculation printouts.

17.0 MAINTENANCE REQUIREMENTS

17.1 Annual PM is performed by an outside provider.
17.2 Daily PM is done using the “ACT-1 GC PM Form” SLA FCD-00208.
17.3 Non-Routine Maintenance such as flow checks, column replacement or troubleshooting is recorded in the
PLEQ15 GC Non-Routine Maintenance Logbook stored at the Instrument.
18.0 ATTACHMENTS
18.1 Instrument Method Settings.