Special Project 173 (RN400Q Residual)

Report No.
Special project 173

3130 FM 521 Fresno, Texas 77545, USA Phone: 281-431-2561 Fax: 281-431-1655 email: gmt.analytical.services@champ-tech.com
TO: Noel Brissard Date: August 6, 2008
FROM: Lijie Feng Cc: G. Cunningham

Nellie Chu W. Goss
Ming Xie L. Rodsjo
G. Cooper
J. Venter
A. Thompson
Residual Analysis of Cortron RN-400Q in Qatar Brine using HPLC/FLD

District: Corrosion and EHBS
EXECUTIVE SUMMARY
A LC/MS method was developed and qualified for determination of residual Cortron RN-400Q
in Qatar brine on December, 2007 (See Report AS20071926). An alternative method by
HPLC/FLD was requested by TS&D Corrosion and EHBS. The residual RN-400Q HPLC/FLD
method is successfully developed along with the use of a standard of RN-400Q, low TDS and
high TDS Qatar brines. A known concentration samples were prepared in the low and high TDS
brines respectively. The analysis results showed the samples in high TDS and low TDS brine
yielded 100±3 % recovery. The results are summarized in Table 1.
EXPERIMENTAL
The standards were prepared by dissolving RN-400Q standard in 5: 5 Acetonitrile:Water at 5.6,

11.2, 22.4 and 33.6 µg/mL, respectively. Both the standards and samples were analyzed using an
Agilent 1100 Series HPLC equipped with an Agilent 1200 Series FLD. Experimental
parameters and instrument conditions are summarized in Method 1 below.
Method 1. HPLC/FLD method for residual determination of Cortron RN-400Q in Qatar brine
Column: Zorbax Eclipse XDB C8, 5 µm, 4.6 x 150 mm
Mobile phase A: 0.1% Acetic acid in water
Mobile phase B: Acetonitrile
Gridient: T (min) %A %B
0.0 90 10
30.0 0 100
35.0 0 100
35.1 90 10
1
Report No. Special project 173
42.0 90 10
Flow rate: 1 ml/min
Column temperature: Ambient
Injection Volume: 50µL
FLD settings PMT 12, response time 4 sec, Excitation 248 nm, Emission 418 nm,
Emission after 14 minutes, 364 nm.
Diluent: 5:5 ACN: H2O
RESULTS AND DISCUSSION
The LC/FLD analysis results for RN400Q in Brine are summarized in table 1. The overlay
chromatogram of the standards and the corresponding calibration curves are shown in Figure 1
through Figure 4. The chromatograms of RN400Q in low TDS brine and high TDS brine are
shown in Figure 5 and Figure 6.
Table 1: LC/FLD Analysis Results

Peak Identification Experimental Recovery
in RN400Q Concentration (ppm)
222 ppm RN400Q in Peak 1 (RT = 11.5 min) 225 101.6%
low TDS Brine Peak 2 (RT = 13.0 min) 224 100.9%
Peak 3 (RT = 14.8 min) 223 100.5%
288 ppm RN400Q in Peak 1 (RT = 11.5 min) 281 97.6%
High TDS Brine Peak 2 (RT = 13.0 min) 282 97.9%
Peak 3 (RT = 14.8 min) 280 97.3%
2
Figure 1: Overlay Chromatogram of RN-400Q Calibration Standard

FLD1 A, Ex=248, Em=418, TT (RN400Q072908LJF CAL CURVE\RN400Q 2008-07-30 16-15-09\LJF3.D)
LU
Peak 1
80
Std1: 5.6 ug/ml
Std2: 11.2 ug/ml
70
Std3: 22.4 ug/ml
Peak 2
60 Std4: 33.6 ug/ml
50
40
30
20
Peak 3
10
0 5 10 15 20 25 30 min
Figure 2: Calibration Curve of Peak 1 (RT = 11.5 min)

P eak 1 , F L D 1 A
A rea = 2 3 .5 7 5 3 5 8 9 *A m t -4 .8 1 2 0 8 2 2
A re a R el. R es % (1 ): -2 .8 0 6 3 e-1
4
600
3
400
2
200 1
0 C orrelation : 0 .9 9 9 9 1
0 20 A m o u n t[n g /u l]
3

P eak 2 , F L D 1 A
A rea = 1 7 .1 6 5 6 7 5 8 *A m t -2 .5 4 9 5 6 5 3
A re a R el. R es % (1 ): 1 .2 8 0 7 e-1
500 4
400
3
300
2
200
1
100
0 C orrelation : 0 .9 9 9 9 5
0 20 A m o u n t[n g /u l]

P eak 3 , F L D 1 A
A rea = 3 .0 8 9 1 4 9 4 2 *A m t -0 .4 7 3 3 5 8 1
A re a R el. R es % (1 ): -1 .6 4 0
100
4
80
60 3
40 2
1
20
0 C orrelation : 0 .9 9 9 9 7
0 20 A m o u n t[n g /u l]
4
Figure 5: Chromatograms of the Prepared Samples in Low TDS Brine at 222 ppm (20
Times Dilution)
FLD1A,Ex=248,Em=418,TT(RN400Q072908LJFCALCURVE\RN400Q2008-07-3016-15-09\LJF7.D)
LU
25
Peak1
Peak2
20
15
10
Peak3
0
0 5 10 15 20 25 30 min
Figure 6: Chromatograms of the Prepared Samples in High TDS Brine at 288 ppm (20
Times Dilution)
FLD1A,Ex=248,Em=418,TT(RN400Q073108LJF\RN400Q2008-07-3117-15-30\LJF5.D)
LU
Peak1
30
Peak2
25
20
15
10
Peak3
0 5 10 15 20 25 30 min

Special Project 173 (RN400Q Residual)

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Special Project 173 (RN400Q Residual)

Uploaded by

Copyright:

Available Formats

Report No.

Special project 173

TO: Noel Brissard Date: August 6, 2008

FROM: Lijie Feng Cc: G. Cunningham

Residual Analysis of Cortron RN-400Q in Qatar Brine using HPLC/FLD

The standards were prepared by dissolving RN-400Q standard in 5: 5 Acetonitrile:Water at 5.6,

RESULTS AND DISCUSSION

Table 1: LC/FLD Analysis Results

Figure 1: Overlay Chromatogram of RN-400Q Calibration Standard

Figure 2: Calibration Curve of Peak 1 (RT = 11.5 min)

Figure 3: Calibration Curve of Peak 2 (RT = 13.0 min)

Figure 4: Calibration Curve of Peak 3 (RT = 14.8 min)

You might also like