SENSORS FOR LPG CONTAMINANTS PHASE I: GAS DETECTION … · sensors for lpg contaminants phase i:...

SENSORS FOR LPG CONTAMINANTS PHASE I: GAS DETECTION TUBE

PROOF OF CONCEPT

FINAL REPORT

SwRI Project No. 08-12889 PERC Docket No. 12117

Prepared for:

Propane Education and Research Council (PERC) 1140 Connecticut Ave., NW, Suite 1075

Washington DC 20036

April 2007

This report must be reproduced in full,

unless SwRI approves a summary or

abridgement

SENSORS FOR LPG CONTAMINANTS

PHASE I: GAS DETECTION TUBE PROOF OF CONCEPT

FINAL REPORT

SwRI Project No. 08-12889 PERC Docket No. 12117

Prepared for:

Propane Education and Research Council (PERC) 1140 Connecticut Ave., NW, Suite 1075

Washington DC 20036

Prepared by:

Scott A. Hutzler, Research Scientist James E. Johnson, Principal Engineer

Southwest Research Institute 6220 Culebra Road

San Antonio, TX 78238

April 2007

Approved: Edwin C. Owens, Director Fuels and Lubricants Technology Department Fuels and Lubricants Research Division

SwRI Project No. 08-12889 April 2007

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Table of Contents Section Page Number

EXECUTIVE SUMMARY............................................................................................................. 1

1.0 BACKGROUND................................................................................................................ 1 2.0 OBJECTIVES .................................................................................................................... 1 3.0 TASK 1. SAMPLING METHODS................................................................................... 2

3.1 Summary of Findings ............................................................................................... 2 4.0 TASK 2 - GAS DETECTION TUBES - SELECTION AND PROCEDURE ................... 3

4.1 Summary of Findings ............................................................................................... 3 5.0 TASK 3 - GAS DETECTION TUBES - LABORATORY EVALUATION..................... 6

5.1 Technical Approach.................................................................................................. 6 5.2 Summary of Findings ............................................................................................... 7

6.0 TASK 4 - IN-LINE FILTRATION - LABORATORY EVALUATION........................... 8 6.1 Technical Approach.................................................................................................. 8 6.2 Summary of Findings ............................................................................................... 9

7.0 CONCLUDING REMARKS ........................................................................................... 10 APPENDIX ................................................................................................................................... 11

8.0 LPG SAMPLING............................................................................................................. 12 9.0 GAS DETECTOR TUBE BASICS.................................................................................. 14

9.1 Principle of Operation ............................................................................................ 14 9.1.1 Gas Sampling Methods ............................................................................... 15 9.1.2 Reaction Principles...................................................................................... 15 9.1.3 Temperature Effects .................................................................................... 16 9.1.4 Correcting Tube Results.............................................................................. 17 9.1.5 Storage of Gas Detector Tubes.................................................................... 18 9.1.6 Summary ..................................................................................................... 18

10.0 SENSIDYNE PRODUCT SPECIFICATION SHEETS .................................................. 19 10.1 Ammonia (Tube No. 105SC).................................................................................. 19 10.2 Ammonia (Tube No. 105SD) ................................................................................. 20 10.3 Carbon Disulfide (Tube No. 141SA)...................................................................... 21 10.4 Carbon Disulphide (Tube No. 141SB) ................................................................... 22 10.5 Carbonyl Sulphide (Tube No. 239S) ...................................................................... 23 10.6 Chlorine (Tube No. 109SA) ................................................................................... 24 10.7 Ethyl Mercaptan (Tube No. 165SA)....................................................................... 25 10.8 Hydrogen Fluoride (Tube No. 156S)...................................................................... 26 10.9 Hydrogen Sulfide (Tube No. 120SB) ..................................................................... 27 10.10 Hydrogen Sulfide (Tube No. 120SD)..................................................................... 28 10.11 Methyl Alcohol (Tube No. 119SA) ........................................................................ 29 10.12 Methyl Alcohol (Tube No. 119U) .......................................................................... 30


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Table of Contents Section Page Number

10.13 Methyl Mercaptan (Tube No. 164SA).................................................................... 31 10.14 Methyl Mercaptan (Tube No. 164SH).................................................................... 32 10.15 Nitrogen Dioxide (Tube No. 117SA) ..................................................................... 33 10.16 Sulfur Dioxide (Tube No. 103SC).......................................................................... 34 10.17 Sulfur Dioxide (Tube No. 103SD).......................................................................... 35 10.18 Sulfur Dioxide (Tube No. 103SE) .......................................................................... 36 10.19 Water Vapor (Tube No. 177SA)............................................................................. 37

11.0 GAS DETECTOR TUBE DETAILS ............................................................................... 38 12.0 GAS DETECTOR TUBE TEST DATA .......................................................................... 44 13.0 GAS DETECTOR TUBE PLOTS.................................................................................... 48 14.0 GAS DETECTOR TUBE PHOTOS ................................................................................ 70 15.0 FILTRATION TEST DATA............................................................................................ 89 16.0 FILTRATION PHOTOS.................................................................................................. 93 17.0 REFERENCES................................................................................................................. 95

List of Tables Table Page Number 1. Contaminant Matrix .................................................................................................................. 4 2. Gas Detector Tube Operating Characteristics......................................................................... 38 3. Gas Detector Tube Interferences ............................................................................................ 39 4. Gas Detector Tube Results...................................................................................................... 44 5. Glass Fiber Filter (GFF) Results............................................................................................. 89 6. Millipore Filter Results ........................................................................................................... 91

List of Figures Figure Page Number 1. Permeation Tube Apparatus...................................................................................................... 6 2. Millipore High Pressure Filter Holder, 25 mm ......................................................................... 8 3. In-line Filtration Apparatus....................................................................................................... 9 4. Configuration for a Manual Sampling via ASTM D1265 ...................................................... 12 5. Typical Visual Indicator Sampling System (from GPA Standard 2174-93)........................... 13 6. Example Detector Tube Specification for Ammonia from Sensidyne.................................... 14 7. Example of a Manual Detector Tube Pump............................................................................ 15 8. Sulfur Dioxide (103SC), Tube #3 (left) and #5 (right), 25 ppm............................................. 48 9. Sulfur Dioxide (103SD), Tube #2 (left) and #4 (right), 25 ppm............................................. 48


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List of Figures (continued) Figure Page Number 10. Sulfur Dioxide (103SD), Tube #6 (left) and #7 (right), 49 ppm............................................. 49 11. Sulfur Dioxide (103SC), Tube #8 (left) and #9 (right), 49 ppm............................................. 49 12. Sulfur Dioxide (103SC), Tube #10 (left) and #11 (right), 99 ppm......................................... 50 13. Sulfur Dioxide (103SC), Tube #12 (left) and #13 (right), ~200 ppm..................................... 50 14. Sulfur Dioxide (103SD), Tube #14 (left) and #15 (right), 49 ppm......................................... 51 15. Hydrogen Sulfide (120SD), Tube #16 (left), #18 (middle), #20 (right), 15 ppm .................. 51 16. Hydrogen Sulfide (120SD), Tube #17 (left), #28 (right), 49 ppm......................................... 52 17. Hydrogen Sulfide (120SD), Tube #19 (left), #30 (middle), #25 (right), 29 ppm .................. 52 18. Hydrogen Sulfide (120SB), Tube #21 (left), #22 (left-center), #23 (right-center),

#24 (right), 15 ppm ................................................................................................................. 53 19. Hydrogen Sulfide (120SB), Tube #26 (left), #27 (middle), #29 (right), 29 ppm .................. 53 20. Hydrogen Sulfide (120SB), Tube #31 (left), #32 (middle), #33 (right), 49 ppm .................. 54 21. Hydrogen Sulfide (120SB), Tube #34 (left), #35 (right), 111 ppm ....................................... 54 22. Hydrogen Sulfide (120SB), Tube #36 (left), #37 (right), 111 ppm ....................................... 55 23. Hydrogen Sulfide (120SB), Tube #40 (left), #41 (right), 169 ppm ....................................... 55 24. Carbonyl Sulfide (239S), Tube #43 (left), #44 (right), 7 ppm............................................... 56 25. Carbonyl Sulfide (239S), Tube #45 (left), #46 (right), 10 ppm............................................. 56 26. Carbonyl Sulfide (239S), Tube #47 (left, 22 ppm), #48 (right, 20 ppm)............................... 57 27. Methyl Mercaptan (164SA), Tube #49 (left), #50 (middle), #51 (right), 20 ppm ................. 57 28. Methyl Mercaptan (164SA), Tube #52 (left), #53 (middle), #54 (right), 50 ppm ................. 58 29. Methyl Mercaptan (164SA), Tube #55 (left), #56 (middle), #57 (right), 84 ppm ................. 58 30. Methyl Mercaptan (164SH), Tube #58 (left, 175 ppm), #59 (middle, 171 ppm), #60

(right, 175 ppm) ...................................................................................................................... 59 31. Methyl Mercaptan (164SH), Tube #61 (left), #62 (right), 347 ppm....................................... 59 32. Carbon Disulfide (141SB), Tube #63 (left), #64 (middle), #65 (right), 10 ppm ................... 60 33. Carbon Disulfide (141SB), Tube #66 (left,), #67 (right), 24 ppm......................................... 60 34. Carbon Disulfide (141SB), Tube #68 (left), #69 (right), 42 ppm.......................................... 61 35. Carbon Disulfide (141SA), Tube #70 (left), #71 (right), 42 ppm.......................................... 61 36. Carbon Disulfide (141SA), Tube #72 (left), #72A (right), 86 ppm....................................... 62 37. Carbon Disulfide (141SA), Tube #73 (left), #74 (right), 198 ppm........................................ 62 38. Carbon Disulfide (141SA), Tube #75 (left), #76 (right), 339 ppm........................................ 63 39. Ethyl Mercaptan (165SA), Tube #77 (left), #78 (center), #79 (right), 8 ppm ........................ 63 40. Ethyl Mercaptan (165SA), Tube #80 (left), #81 (left-center), #82 (right-center,),

#83 (right), 19 ppm ................................................................................................................. 64 41. Ethyl Mercaptan (165SA), Tube #84 (left), #85 (right), 41 ppm............................................ 64 42. Ethyl Mercaptan (165SA), Tube #86, 126 ppm...................................................................... 65 43. Methyl Alcohol (119U), Tube #88 (left), #89 (center), #90 (right), 50 ppm.......................... 65


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List of Figures (continued) Figure Page Number 44. Methyl Alcohol (119SA), Tube #93 (left), #94 (right), 0.06%............................................... 66 45. Methyl Alcohol (119SA), Tube #95, 0.11%........................................................................... 66 46. Ammonia (105SD), Tube #100, 3 ppm................................................................................... 67 47. Ammonia (105SD), Tube #101, 10 ppm................................................................................. 67 48. Ammonia (105SC), Tube #102 (left), #103 (right), 20 ppm................................................... 68 49. Ammonia (105SD), Tube #104 (left), #105 (right), 20 ppm .................................................. 68 50. Ammonia (105SD), Tube #106 (left), #106 (right), 44 ppm .................................................. 69 51. Sulfur Dioxide (103SC), Tube #3 (left) and #5 (right), bag sampling, 25 ppm...................... 70 52. Sulfur Dioxide (103SD), Tube #2 (left) and #4 (right), bag sampling, 25 ppm ..................... 70 53.Sulfur Dioxide (103SD), Tube #7 (left) and #6 (right), bag sampling, 49 ppm....................... 71 54. Sulfur Dioxide (103SC), Tube #8 (left) and #9 (right), bag sampling, 49 ppm...................... 71 55. Sulfur Dioxide (103SC), Tube #11 (left) and #10 (right), bag sampling, 99 ppm.................. 72 56. Sulfur Dioxide (103SC), Tube #13 (left) and #12 (right), bag sampling, ~200 ppm ............. 72 57. Sulfur Dioxide (103SD), Tube #15 (left) and #14 (right), bottle sampling, 49 ppm .............. 73 58. Hydrogen Sulfide (120SD), Tube #16 (left, 100 mL bag sample), #18 (middle,

50 mL bag sample), #20 (right, 100 mL bottle sample), 15 ppm ........................................... 73 59. Hydrogen Sulfide (120SD), Tube #17 (left, 50 mL bag sample), #28 (right,

50 mL bottle sample), 49 ppm ................................................................................................ 74 60. Hydrogen Sulfide (120SD), Tube #19 (left, 50 mL bag sample), #30 (middle,

50 mL bottle sample), #25 (right, 50 mL bottle sample), 29 ppm .......................................... 74 61. Hydrogen Sulfide (120SB), Tube #21 (left, 100 mL bottle sample), #22

(left-center, 300 mL bag sample), #23 (right-center, 100 mL bag sample), #24 (right, 50 mL bag sample), 15 ppm.................................................................................. 75

62. Hydrogen Sulfide (120SB), Tube #26 (left, 300 mL bag sample), #27 (middle, 100 mL bag sample), #29 (right, 100 mL bottle sample), 29 ppm ......................................... 75

63. Hydrogen Sulfide (120SB), Tube #31 (left, 100 mL bag sample), #32 (middle, 50 mL bag sample), #33 (right, 100 mL bottle sample), 49 ppm ........................................... 76

64. Hydrogen Sulfide (120SB), Tube #34 (left, 100 mL bottle sample), #35 (right, 100 mL bag sample), 111 ppm ............................................................................................... 76

65. Hydrogen Sulfide (120SB), Tube #36 (left, 50 mL bottle sample), #37 (right, 50 mL bag sample), 111 ppm ................................................................................................. 77

66. Hydrogen Sulfide (120SB), Tube #40 (left, 50 mL bottle sample), #41 (right, 50 mL bag sample), 169 ppm ................................................................................................. 77

67. Carbonyl Sulfide (239S), (left to right) Tube #43 (100 mL bottle sample, 7 ppm), #44 (100 mL bag sample, 7 ppm), #45 (100 mL bottle sample, 10 ppm), #46 (100 mL bag sample, 10 ppm), #47 (100 mL bottle sample, 22 ppm), #48 (100 mL bottle sample, 20 ppm).......... 78


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List of Figures (continued) Figure Page Number 68. Methyl Mercaptan (164SA), Tube #49 (left, 100 mL bottle sample), #50 (middle,

100 mL bag sample), #51 (right, 100 mL bag sample), 20 ppm............................................. 78 69. Methyl Mercaptan (164SA), Tube #52 (left, 100 mL bottle sample), #53 (middle,

100 mL bag sample), #54 (right, 100 mL bag sample), 50 ppm............................................. 79 70. Methyl Mercaptan (164SA), Tube #55 (left, 100 mL bottle sample), #56 (middle,

100 mL bag sample), #57 (right, 100 mL bag sample), 84 ppm............................................. 79 71. Methyl Mercaptan (164SH), Tube #58 (left, 100 mL bottle sample, 175 ppm), #59

(middle, 100 mL bottle sample, 171 ppm), #60 (right, 100 mL bag sample, 175 ppm) ......... 80 72. Methyl Mercaptan (164SH), Tube #61 (left, 100 mL bottle sample), #62 (right, 100 mL

bottle sample), 347 ppm.......................................................................................................... 80 73. Carbon Disulfide (141SB), Tube #63 (left, 200 mL bottle sample), #64 (middle, 200 mL

bag sample), #65 (right, 400 mL bag sample), 10 ppm .......................................................... 81 74. Carbon Disulfide (141SB), Tube #66 (left, 200 mL bottle sample), #67 (right, 200 mL

bag sample), 24 ppm............................................................................................................... 81 75. Carbon Disulfide (141SB), Tube #68 (left, 200 mL bottle sample), #69 (right, 200 mL

bag sample), 42 ppm............................................................................................................... 82 76. Carbon Disulfide (141SA), Tube #70 (left, 100 mL bottle sample), #71 (right, 100 mL

bag sample), 42 ppm............................................................................................................... 82 77. Ethyl Mercaptan (165SA), Tube #77 (left, 400 mL bottle sample), #78 (center, 200 mL

bottle sample), #79 (right, 100 mL bottle sample), 8 ppm...................................................... 83 78. Ethyl Mercaptan (165SA), Tube #80 (left, 400 mL bottle sample), #81 (left-center,

200 mL bottle sample), #82 (right-center, 100 mL bottle sample), #83 (right, 200 mL bag sample), 19 ppm............................................................................................................... 83

79. Ethyl Mercaptan (165SA), Tube #84 (left, 200 mL bottle sample), #85 (right, 200 mL bag sample), 41 ppm............................................................................................................... 84

80. Ethyl Mercaptan (165SA), Tube #86 100 mL bottle sample, 126 ppm.................................. 84 81. Methyl Alcohol (119U), Tube #88 (left, 100 mL bottle sample), #89 (center, 100 mL

bottle sample), #90 (right, 100 mL bag sample), 50 ppm....................................................... 85 82. Methyl Alcohol (119SA), Tube #93 (left, 100 mL bottle sample), #94 (right, 100 mL

bottle sample), 0.06% ............................................................................................................. 85 83. Methyl Alcohol (119SA), Tube #95 (left, 100 mL bottle sample), new tube (right), 0.11% . 86 84. Ammonia (105SD), Tube #100, 100 mL bottle sample, 3 ppm.............................................. 86 85. Ammonia (105SD), Tube #101, 100 mL bottle sample, 10 ppm............................................ 87 86. Ammonia (105SC), Tube #102 (left, 100 mL bottle sample), #103 (right, 100 mL bottle

sample), 20 ppm...................................................................................................................... 87 87. Ammonia (105SD), Tube #104 (left, 100 mL bottle sample), #105 (right, 100 mL bottle

sample), 20 ppm...................................................................................................................... 88


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List of Figures (continued) Figure Page Number 88. Ammonia (105SD), Tube #106 (left, 100 mL bottle sample), #106 (right, 100 mL bottle

sample), 44 ppm...................................................................................................................... 88 89. Glass Fiber Filter Recovered Weights, Run A........................................................................ 90 90. Glass Fiber Filter Recovered Weights, Run B........................................................................ 90 91. Millipore Filter Recovered Weights, Run A........................................................................... 92 92. Millipore Filter Recovered Weights, Run B ........................................................................... 92 93. Millipore Filters, Run A.......................................................................................................... 93 94. Millipore Filters, Run B.......................................................................................................... 93 95. GFF Filters, Run A ................................................................................................................. 94 96. GFF Filters, Run B.................................................................................................................. 94

Abbreviations ASTM American Society for Testing and Materials GC Gas Chromatography GDT Gas Detection Tubes GFF Glass Fiber Filter GPA Gas Processors Association HC Hydrocarbon LP Liquefied Petroleum LPG Liquefied Petroleum Gas PPM Parts Per Million SwRI Southwest Research Institute


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Naming Conventions Throughout this document the term LPG (Liquefied Petroleum Gas) will be used repeatedly. In order to eliminate confusion, the term LPG will refer to those product grades composed primarily of propane (e.g., HD-5). Where necessary, the actual state of the sample (i.e., gas or liquid) will be clarified. Specific compounds, such as propane or methane and other hydrocarbons will be referred to by name. Although butane is considered one of the four major LP-gases, its use is primarily industrial. Our primary concern in this document is with LPG for domestic and commercial use and those that are suitable for internal combustion engines (i.e., LPG-based).

Organization of the Report The report is organized into the following subject areas: Executive Summary

• Background (Section 1.0)

• Objectives (Section 2.0)

• Task 1 - Sampling Methods (Section 3.0)

• Task 2 - Gas Detection Tubes - Selection and Procedure (Section 4.0)

• Task 3 - Gas Detection Tubes - Laboratory Evaluation (Section 5.0)

• Task 4 - In-line Filtration - Laboratory Evaluation (Section 6.0)

• Concluding Remarks (Section 7.0) Appendix

• LPG Sampling (Section 8.0)

• Gas Detector Tube Basics (Section 9.0)

• Sensidyne Product Specification Sheets (Section 10.0)

• Gas Detector Tube Details (Section 11.0)

• Gas Detector Tube Test Data (Section 12.0)

• Gas Detector Tube Plots (Section 13.0)

• Gas Detector Tube Photos (Section 14.0)

• Filtration Test Data (Section 15.0)

• Filtration Photos (Section 16.0) Miscellaneous

• References (Section 17.0)


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EXECUTIVE SUMMARY 1.0 BACKGROUND

There is currently a need for a means to detect contaminants in LPG. Although there are

instruments available to meet this need, their cost and complexity is beyond the reach of local

retailers and distributors. As such, a simple-to-use device is needed to detect common

contaminants in LPG. In previous work [1] we investigated a large number of candidate

sensors/devices and performed a trade-off study based on a set of criteria that we defined (e.g.,

complexity, cost, detection limits, etc.). Based on that study, gas detection tubes (GDT) were

ranked the highest in part due to their low investment cost, sensitivity to a wide range of low level

contaminants, and ease of use.

Contamination of LPG during transport continues to be a significant problem for some industries.

Field methods for the early and cost-effective detection of contaminants will lead to longer life of

LPG-fueled systems. The end result will be greater consumer confidence in the quality of their

fuel and fewer fuel-related problems in the field.

2.0 OBJECTIVES

The global objective of this effort was to perform a proof-of-concept evaluation of gas detection

tubes with respect to gas-phase LPG contaminants. At the same time, we investigated the use of

an in-line filtration system to show that liquid-phase insolubles could also be captured. Our

expectation was that the gas detection tubes would work sufficiently well to be used as an

inexpensive screening tool for batch samples at the retail or distributor level. Any indication of

contamination would prompt further testing for verification. The in-line filter pads would

concentrate any liquid-phase, insoluble contaminants allowing visual detection.

Specifically, this effort addressed the following:

1) Sampling methods for capturing a representative sample of LPG (Task 1)

2) Selection of gas detection tubes relevant to LPG (Task 2)

3) Laboratory evaluation of selected gas detection tubes (Task 3)

4) Laboratory evaluation of an in-line filter for detecting liquid-phase contaminants (Task 4)


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3.0 TASK 1. SAMPLING METHODS

Procedurally, the most difficult task will be collecting a representative sample. Since both gas

and liquid-phase contaminants exist we must consider each separately. Furthermore, the

analytical techniques proposed herein require different testing conditions. Filtration requires a

liquid sample while the gas detector tubes require a gas sample at or near atmospheric pressure.

We expect that batch sampling will be the preferred method, so we have tried to incorporate our

procedures into common sampling practices.

3.1 Summary of Findings

We began by analyzing the relevant sampling techniques described in the following documents:

• ASTM D1265 (Standard Practice for Sampling Liquefied Petroleum (LP) Gases (Manual

Method)

• ASTM D3700 (Standard Practice for Obtaining LPG Samples Using a Floating Piston

Cylinder)

• GPA Standard 2174 (Obtaining Liquid Hydrocarbon Samples for Analysis by Gas

Chromatography)

These methods describe two primary methods of sampling: a manual method and a method that

utilizes a floating piston cylinder. When collecting samples for compositional analysis, floating

piston cylinders are used to minimize vaporization and loss of light components (see Appendix

Section 8.0 for typical sampling configurations). For most of the tests specified in ASTM D1835

(Standard Specification for Liquefied Petroleum (LP) Gases), this sampling technique is not

necessary. The contaminant matrix under consideration consists primarily of various forms of

sulfides and mercaptans, water, methanol, and ammonia. These contaminants range from semi-

volatile to volatile. Regardless of the contaminant volatility, the optimal solution would be to use

a floating piston cylinder. This would prevent loss of volatile compounds and limit the

compositional change in the overall sample. This would be the best practice if the end user could

bear the burden of obtaining the appropriate hardware. However, given that the gas detector

tubes are intended to serve as a pre-screening tool, we feel that a liquid sample drawn directly

from the source (according to ASTM D1265) should suffice in most cases. In the worst-case

scenario, it might make volatile, low concentration contaminants difficult to detect.


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Cylinders that are stainless steel, or better yet, Teflon-lined would help to prevent loss of sulfur

compounds and other surface-active agents to the cylinder walls. Evidence in the literature

suggests that even in unlined steel cylinders, this loss would be minimal provided the analysis

was carried out within a few days. Nevertheless, this would be a preferred option for the end user

to consider.

In summary, the accuracy of the sampling technique is a factor in the accuracy of the analysis.

The end user should acquire the best equipment within their means to acquire a representative

sample. To a large extent, the relative accuracy of the gas detection tubes (10-25%) may mask

large changes due to sampling effects. In subsequent sections we will discuss the sampling

requirements specific to the particular analysis. For the most part, users should expect very little

change in their sampling procedures. The primary task will be interfacing the apparatus to the

LPG source whether it's bulk storage or a sample container.

4.0 TASK 2 - GAS DETECTION TUBES - SELECTION AND PROCEDURE


The objective of this task was to select the gas detector tubes to test, locate a supplier, and

develop a test plan. In order to accomplish this, we needed to generate a contaminant matrix with

approximate concentration levels. This information is not readily available for a large number of

compounds. GPA Standard 2140 provides some insight into a few basic classes of compounds.

Upon request, some very useful information was provided by PERC regarding LPG contaminants

and their typical concentration range.

A search for companies that provide gas detection tubes and related hardware resulted in a wide

selection of potential suppliers including:

• Sensidyne, Inc.

• Draeger Safety, Inc.

• Gastec Corporation

• RAE Systems

• Mine Safety Appliances (MSA)

Each of these companies provides a wide array of detector tubes and each carries its own form of

hand-held detector tube pump. Because of the specific tube requirements, mixing tubes and


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devices from different companies is not usually recommended. Factors to be considered when

selecting a source for gas detection tubes include concentration range, cross interferences, and, of

course, availability. For a brief review of gas detector tube characteristics, please see Section 9.0

in the Appendix.

Cross-referencing our contaminant list with available detector tubes resulted in the contaminant

matrix shown in Table 1. The broadest assortment of tubes appeared to be from Sensidyne, Inc.,

so we selected them as our supplier. They also provide a substantial amount of readily available

technical information on their tubes and sampling techniques. Undoubtedly, some of the other

suppliers could meet future needs in this area. The product specification sheets for the Sensidyne

detector tubes can be found in Section 10.0 in the Appendix. A compilation of tube operating

characteristics and tube interferents can be found in Table 2 and Table 3, respectively, of

Section 11.0 in the Appendix. Studying the list of tubes and their interferents, it appears that in

cases where a particular interferent may coexist with the analyte of interest, the concentration

needs to be excessively high to create a problem. Some tubes use pre-treat tubes to remove the

offending interferent and, in some cases, the effect of the interferent causes an identifiable color

change.

Table 1. Contaminant Matrix

Compound Sensidyne Part Number

Concentration Range (Sample Volume)

Ammonia 105SC 10 - 260 ppm (100mL) 5 - 130 ppm (200 mL)

Ammonia 105SD 1 - 20 ppm (100mL) 0.2 - 1 ppm (200 mL)

Carbon Disulfide 141SA 30 - 500 ppm (100 mL)

Carbon Disulfide 141SB 2 - 50 ppm (200 mL) 0.2 - 20 ppm (400 mL)

Carbonyl Sulfide 239S 5 - 60 ppm (100 mL) Chlorine 109SA 1 - 40 ppm (100 mL)

Ethyl Mercaptan 165SA 4 - 160 ppm (100 mL) 2 - 80 ppm (200 mL) 1 - 40 ppm (400 mL)

Hydrogen Fluoride 156S 0.5 - 30 ppm (300 mL) 0.25 - 15 ppm (600 mL)

Hydrogen Sulfide 120SB

6 - 300 ppm (50 mL) 3 - 150 ppm (100 mL) 1 - 50 ppm (300 mL)

0.75 - 37.5 ppm (400 mL)

Hydrogen Sulfide 120SD 2 - 60 ppm (50 mL) 1 - 30 ppm (100 mL)


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Methanol 119SA 500 - 60,000 ppm (100 mL) Methanol 119U 20 - 1,000 ppm (100 mL) Methyl Mercaptan 164SA 5 - 140 ppm (100 mL) Methyl Mercaptan 164SH 50 - 1,000 ppm (100 mL) Nitrogen Dioxide 117SA 20 - 1000 ppm (100 mL) Sulfur Dioxide 103SC 30-300 ppm (100 mL) Sulfur Dioxide 103SD 1 - 60 (100 mL)

Sulfur Dioxide 103SE 0.5 - 10 ppm (100 mL) 0.25 - 5 ppm (200 mL)

Water 177SA 1.7 - 33.8 mg/L (100 mL)

As mentioned earlier, gas detector tubes are designed to operate at or near atmospheric pressure.

For this application, there are two primary options for obtaining low-pressure samples: sampling

bags or flow-through samplers. These techniques are relatively common, so we chose to

experiment with both, as either could be readily applied in the field. Sampling bags, such as

Tedlar bags, are made of an inert material with low gas permeability. These can be filled quickly

and removed to a convenient location for testing. We chose Tedlar sample bags with an on/off

sampling valve. With a small piece of tubing, the detector tube can be quickly interfaced to the

valve and a test performed. Flow-through samplers are equally convenient and became our

preferred method of sampling. A flow-through sampler is simply a small container made of an

inert material, such as Teflon or polyethylene, with three small holes drilled in the lid of the

container. A low-pressure (near atmospheric), low-flow (0.1-2 L/min) gas-phase sample enters

through one hole via Teflon tubing connected to the primary sample container. The second hole

serves as a purge port. The gas detector tube is inserted in the third hole for testing. As we will

show later, both techniques are effective at capturing a representative sample.

On a side note, Draeger Safety recently introduced an electronic tube detector to the market that

uses an optical system to detect the colorimetric changes in the detector tubes and report the

results digitally. This device is handheld, incorporates a mass flow controller for precision gas

metering, and uses chips that contain ten embedded capillary detector tubes. Although it appears

to be a very nice device, at approximately $2,000/unit we felt the hand-operated pumps were

more cost efficient. Nevertheless, this may be an improvement over the traditional tubes and

hand-operated pumps.


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5.0 TASK 3 - GAS DETECTION TUBES - LABORATORY EVALUATION

5.1 Technical Approach

To accomplish the testing, we needed to generate a series of test gases containing pure propane

and a selected contaminant at a known concentration level. The most cost-effective way to

achieve this is with the use of permeation tubes in conjunction with a u-tube submerged in a

constant temperature bath (Figure 1). At a given temperature, a permeation tube will emit a

known concentration of its compound. For testing, propane "standards" were prepared by

regulating the flow of chemically pure propane over a permeation tube held at a fixed

temperature. The flow of modified propane was then collected in a sampling bag (e.g., Tedlar

bag) or directed into a flow-through sampler.

VICI (Valco Instruments Co., Inc.) was chosen as a supplier for gas permeation tubes and related

equipment. They can provide permeation tubes with essentially any chemical compound. We

needed a relatively high output from the permeation tubes in order to span a wide range of

concentrations. As a result, VICI could not certify the tube's permeation rate. Therefore, most of

the tubes are rated at ±15% of the stated output. We took this uncertainty into account when

calculating the range of possible values at a given flow and temperature.

Drying and Filter Column

Settling Chamber

Manometer (one side

vented to atm.)

Permeation Tube

Constant Temp. Oil Bath

U-Tube with Stoppers

Gas Sample Collection Bag

Low and High Range Flow Meters

Propane Tank (2 stg. Regulator)

Nitrogen Tank (2 stg. Regulator)

60 psi Pressure Gage

Needle Valve

By-pass Line

Ventilated Hood

Flow Temp. Sensor

Figure 1. Permeation Tube Apparatus


Page 7


With the exception of chlorine, nitrogen dioxide, and hydrogen fluoride, test gases in a range of concentrations were prepared for each of the contaminants listed in Table 1. Those test gases were then tested with their respective detector tubes using the bag sampling and/or bottle sampling (flow-through) technique. The results of those tests are tabulated in Table 4 of Section 12.0 in the Appendix. The results are also illustrated graphically in Figure 8 to Figure 50 of Section 13.0 of the Appendix. The vertical bars in each plot represent the range of possible concentrations for that test gas based on the uncertainties in the system (i.e., permeation tube, flow meter, etc). Photographs of many of the used detector tubes have been included in Figure 51 to Figure 88 of Section 14.0 of the Appendix. Generally, the results from the detector tube tests were good and, in some cases, excellent. For a given test case, we found the detector tubes to be repeatable even between the two sampling techniques. We had the most difficulty in maintaining low flow rates to achieve high concentrations. Flow rates above 200 mL/min of propane typically generated the best results. Notable exceptions are as follows:

• While very repeatable, the hydrogen sulfide data appeared to have a large positive bias in almost all cases. This may be a function of the permeation tube having an output different than specified.

• The carbon disulfide data showed a strong negative bias. Upon investigation, we discovered that this particular tube requires the pump to be modified by removing an internal flow control orifice. Since we hadn't done this, we may have been restricting the flow resulting in the lower than expected results.

• The methyl alcohol detector tubes are the only ones that appear to be affected by the propane itself. The propane causes tube #119U to fade making it difficult to detect the pale blue color change. Tube #119SA turns completely brown, although the green color change is still visible. Unfortunately, this is the high concentration (i.e., low-resolution) tube so accuracy is reduced. Nevertheless, it should be able to detect gross quantities of methanol.

• We were never able to generate a water/propane test gas that gave satisfactory results. Even at what should have been a high water concentration, the tube gave a weak response. We used the water detector tubes to test the humidity in the room and they seemed to respond fine. Thus the problem was obviously with our test gas.

Lastly, all of the detector tubes were tested against the chemically pure propane. As before, the methanol tubes were the only ones found to respond to the propane itself.


Page 8

6.0 TASK 4 - IN-LINE FILTRATION - LABORATORY EVALUATION

An obvious shortcoming of the gas detection tubes is that they only work for gas-phase samples.

Some of the more problematic contaminants are heavy oils or insolubles that remain primarily in

the liquid-phase. We proposed to use an in-line filter to capture these insolubles. This approach

is taken from ASTM D2276 (Standard Test Method for Particulate Contaminant in Aviation Fuel

by Line Sampling), which is used to measure particulate contamination in jet fuels. In this

method, a fixed volume of the fuel is passed through a filter and the resulting filter is analyzed

gravimetrically or given a visual rating. The gravimetric method is not really applicable to a field

application. However, the visual rating system may be applicable and would complement the gas

detection tubes without adding additional complexity or significant cost to the system.

6.1 Technical Approach

For testing, we selected an in-line, high-pressure, stainless steel filter holder (Figure 2) distributed

by Millipore (~$350). This holder accepts a standard 25mm filter and can handle differential

pressures of 1,000 psi (large safety margin). We opted for the smaller diameter filter to help

concentrate the contaminants and aid in visualization. In actual practice, a larger filter may be

desirable depending on the level of contamination, line sizes, or flowrates.

Figure 2. Millipore High Pressure Filter Holder, 25 mm

ASTM D2276 appeared to be a good starting point for visually rating membrane filters containing

insoluble debris. The visual rating system consists of two parts: color and particle density. Since

it is designed for fuel, the color rating varies from white, to yellow, to brown, and finally to black.

Our planned approach was to inject known quantities of test dust into a liquid propane sample to

document the capture of debris on the in-line filter. Several variations of test dust exist: Al

Ultrafine, A2 Fine, A3 Medium, and A4 Coarse. For these tests we chose the A2 test dust. This

dust contains a good distribution of particles ranging in size from 1 to 120 µm.


Page 9

For aviation fuel, we typically use 0.8µm cellulose-based membrane filters. This filter should

work reasonably well for this application too. For comparison, we also ran tests using a glass-

fiber filter (0.7µm). We expected that either filter type would be sufficient to generate a visual

rating for our propane application.

The test apparatus is illustrated in Figure 3. Various portions of test dust were weighed out in

duplicate and made into slurries with heptane. These slurries were then added into the loop

followed by purging of the loop with liquid propane. We performed a gravimetric analysis on all

of the test filters to determine the percent recovery (although we know from experience that the

results can be poor when trying to recover all of the test dust). The data for the filtration runs are

tabulated in Table 5 and Table 6 of Section 15.0 in the Appendix for the glass fiber and Millipore

filters, respectively. Graphical depictions of the data are also available in Section 15.0 in the

Appendix. Photographs of the filter pads are available in Section 16.0 in the Appendix.

Propane Tank with Dip Tube

Ball Valve

Funnel for Introducing Particulate Matter

Vent

Multiple Out of Plane Elbows to Promote Mixing

Mixing Pot

Liquid Flow

Flow to Atmosphere

Filter Housing

Figure 3. In-line Filtration Apparatus


Despite what some of the gravimetric analyses indicate, the filters generally appear to increase in

dirt content from low to high concentration. However, the uniform color and small particle sizes

of the test dust precluded any possibility of applying the color rating or the particle density chart.

That is not to say that the test was a complete failure. We have demonstrated that standard

membrane or glass fiber filters can be used to capture insoluble materials in a stream of liquid


Page 10

propane. Real-world dirt or bottom sludge will be far from uniform. In fact, although it's not

apparent in the photographs, some of the blank runs were actually capturing metal particles and

an oily black residue.

Implementing this capability in the field could be as simple as inserting an in-line filter holder in

the sampling line upstream of a sample cylinder. For the sampling apparatus shown in Figure 4

of Section 8.0 in the Appendix, this would be just to the right of Control Valve A. So

conceivably, in the process of collecting a small cylinder of LPG for testing gas-phase analytes

with the gas detector tubes, the in-line filter holder could be collecting the insoluble residues for

visual analysis. To gauge the amount of LPG that has passed through the filter, one could simply

use the size of the portable cylinder that is being filled (or multiples thereof if the cylinder is

filled/purged prior to filling). The result is a single process that creates a pre-screening tool for

both gas-phase and liquid-phase contaminants.

7.0 CONCLUDING REMARKS

Overall, we felt that the gas detector tubes passed the proof of concept test. The tubes appeared

to perform as stated and in a very repeatable manner. The extensive network of suppliers makes

this pre-screening tool accessible to the general public. Furthermore, the cost is not prohibitive;

the detector tube pumps range in cost from $150 to $350 and the tubes are normally $50/10 tubes

(a few tubes are $50/5 tubes). The addition of an in-line filter holder creates a powerful

combination of tests that provide access to certain liquid and gas-phase contaminants. These tests

are simple to carry out and require minimal training. Future testing on this capability should be

expanded to include real-world samples.


Page 11

APPENDIX


Page 12

8.0 LPG SAMPLING

The issue of sampling LPG in containers other than laboratory testing apparatus is addressed in

ASTM D1265 entitled ”Standard Practice for Sampling Liquefied Petroleum (LP) Gases (Manual

Method).” For custody transfer operations, the samples must be in the liquid phase only.

Furthermore, if corrosive compounds or sulfur compounds are to be analyzed, the sample

containers and valves should be made of stainless steel. A typical sampling container is shown in

Figure 4. The sample bottle contains an outage tube (ullage) at the top. Ullage volume is needed

for allowance of thermal expansion. By following the procedures outlined in D1265, this

particular sample bottle will always provide 20% outage (ullage) and 80% liquid. The D1265

sampling method is manual and requires some minor training of personnel that acquire LPG

samples.

Figure 4. Configuration for a Manual Sampling via ASTM D1265

For compositional analysis by gas chromatography, a more precise sampling technique is

necessary. GPA Standard 2174-93 entitled “Obtaining Liquid Hydrocarbon Samples for Analysis

by Gas Chromatography” incorporates a floating piston cylinder arrangement with one typical

configuration shown in Figure 5 (other arrangements are discussed in the standard). Unlike the

manual method, which is vented to atmosphere, the floating piston cylinder regulates the flow

into the cylinder without loss of product.


Page 13

Figure 5. Typical Visual Indicator Sampling System (from GPA Standard 2174-93)


Page 14

9.0 GAS DETECTOR TUBE BASICS

This section was excerpted from Reference [1].

9.1 Principle of Operation

Gas detector tubes are thin glass tubes that contain detection reagent(s) that are sensitive to

specific target compounds. The reagent(s) produce a distinct layer of color change when exposed

to the target compound. Calibration scales are printed on the tubes, which indicate the

concentration of the substance being measured. To provide long-term stability (shelf life up to 3

years), the tubes are hermetically sealed to protect the reagents. Hundreds of variations of

detector tubes currently exist to measure a wide variety of chemical compounds. An example of

a detector tube specification sheet (sold by Sensidyne) for ammonia is shown in Figure 6. There

are actually several tubes for ammonia depending on the concentration range. Some measure as

low as 1 ppm while others measure as high as 30%.

Figure 6. Example Detector Tube Specification for Ammonia from Sensidyne


Page 15

9.1.1 Gas Sampling Methods

Gas sensors and detection systems may utilize several different methods to draw gas through the

detector tubes. The most common are described below.

Vacuum method

The sample is drawn into the detector tube by manually operating a vacuum pump. This

is probably the most widely used technique (Figure 7).

Injection method

The sample is first drawn into a syringe before being injected into the detector tube.

Motor-driven pump method

The sample is drawn through the detector tubes by a motor-driven pump at a prescribed

rate for a prescribed time.

Diffusion method

The sample is not drawn but is allowed to diffuse slowly into the detector tubes.

Figure 7. Example of a Manual Detector Tube Pump

9.1.2 Reaction Principles

Detector tubes generally react to chemical compounds in one of the following ways:

1. The sample reacts directly with a detecting reagent.

2. The sample reacts directly with several detecting reagents.

3. The sample reacts in a two-step reaction. The sample is first oxidized in a pretreatment

layer before reacting with the detecting reagent.


Page 16

Substances that are chemically similar to the target compound may also react in the tube affecting

the results. These substances are called interferents and their effects may vary on the detector

tube type.

Interferences in direct reaction type detector tubes

1. The detector tube reagent(s) will also react with the interferents, giving a higher

indication. An example of such an interferent is hydrogen sulfide in an ethyl mercaptan

detector tube. Common interferences and their effects are normally documented on the

specification sheet for the detector tube and are usually concentration dependent.

2. If the detector tube contains a pH indicator then acids and bases will react as interferents

giving a higher indication.

Interferences in compound reaction type detector tubes

If a substance generated by the primary reaction(s) is the same as the target compound

then a higher indication will be given.

Interference in two-step reaction type detector tubes

If interferents consume the pretreatment oxidizer then its ability to oxidize the target

compound will be inhibited resulting in a lower indication.

9.1.3 Temperature Effects

Most detector tubes are either based on chemical reactions or physical adsorption, both of which

can be greatly affected by tube temperature. These effects are described below.

Influences on reaction rate

Chemical reaction rates are generally proportional to temperature. Below 20°C (68°F),

reactions will slow down and the sample will not completely react in the manner desired.

Some of the sample will diffuse further into the tube and react there creating a long pale

color change giving a higher indication. Above 20°C (68°F), reactions will accelerate

causing the sample to completely react in a shorter distance than normal. This gives a

shorter layer of color change resulting in a lower indication.


Page 17

Influences on physical adsorption

Chemical adsorption is inversely proportional to temperature. Below the prescribed

temperature, some of the sample will physically adsorb onto the detector tube reagent that

has already reacted with previous sample. Thus the subsequent sample will never reach

fresh reagent and react in the normal manner giving a lower than expected indication. At

higher temperature, adsorption/desorption will cause the sample to diffuse further into the

tube giving a higher than expected indication.

9.1.4 Correcting Tube Results

Detector tubes are generally resistant to minor fluctuations in temperature, pressure, and

humidity. When conditions are outside of predetermined limits the detector tube specification

sheet will normally provide instructions for correcting the results. Cases that may involve the

need to correct the indicated measurement are as follows.

Correction for temperature

Detector tubes are generally designed to be used at ambient temperatures 20-40°C (32-

104°F) and are calibrated based on a tube temperature (not sample temperature) of 20°C

(68°F). However, some tubes are more sensitive to temperature than others and may give

erroneous results at temperatures other than 20°C. For these tubes, a chart is generally

provided to correct the readings.

Correction for humidity

Most detector tubes are calibrated based on a specific relative humidity (e.g., 50%) but

their indications are not affected when the humidity is in the range of 0 to 99%.

Correction for atmospheric pressure

Since gas concentration is proportional to pressure, gas detector tubes are calibrated at

normal atmospheric pressure (760 mmHg). Their indications are not usually affected

within ±10% of this pressure. At pressures outside of this range, mathematical

corrections are applied to negate the effect.


Page 18

9.1.5 Storage of Gas Detector Tubes

Detector tubes contain sensitive reagents and storage in a dark, cool (0-10°C (32-50°F)) place is

recommended. Some detector tubes require refrigeration.

9.1.6 Summary

Summary of gas detector tube attributes:

• Very simple to operate - uses a manual or automatic pump to draw air through tube,

therefore technology should be dependable

• Tube selection process may require some standardization - a series of tubes in a particular

order to specifically identify a contaminant

• Good for bulk contamination or analyte specific detection

• Detection limits are tube dependent and there are a variety of tubes from which to choose

• Tube concentrations vary from ppm to % level

• Minor temperature and pressure effects

• Tube selection is critical because some tubes respond to multiple analytes; however, the

interferents usually respond with a different color so the interference is known


Page 19

10.0 SENSIDYNE PRODUCT SPECIFICATION SHEETS

10.1 Ammonia (Tube No. 105SC)


Page 20

10.2 Ammonia (Tube No. 105SD)


Page 21

10.3 Carbon Disulfide (Tube No. 141SA)


Page 22

10.4 Carbon Disulphide (Tube No. 141SB)


Page 23

10.5 Carbonyl Sulphide (Tube No. 239S)


Page 24

10.6 Chlorine (Tube No. 109SA)


Page 25

10.7 Ethyl Mercaptan (Tube No. 165SA)


Page 26

10.8 Hydrogen Fluoride (Tube No. 156S)


Page 27

10.9 Hydrogen Sulfide (Tube No. 120SB)


Page 28

10.10 Hydrogen Sulfide (Tube No. 120SD)


Page 29

10.11 Methyl Alcohol (Tube No. 119SA)


Page 30

10.12 Methyl Alcohol (Tube No. 119U)


Page 31

10.13 Methyl Mercaptan (Tube No. 164SA)


Page 32

10.14 Methyl Mercaptan (Tube No. 164SH)


Page 33

10.15 Nitrogen Dioxide (Tube No. 117SA)


Page 34

10.16 Sulfur Dioxide (Tube No. 103SC)


Page 35

10.17 Sulfur Dioxide (Tube No. 103SD)


Page 36

10.18 Sulfur Dioxide (Tube No. 103SE)


Page 37

10.19 Water Vapor (Tube No. 177SA)


Page 38

11.0 GAS DETECTOR TUBE DETAILS

Table 2. Gas Detector Tube Operating Characteristics



Temp. Range

Temp. Correction

Pressure Correction

Humidity Correction Color Change

Ammonia 105SC 10 - 260 ppm (100mL)** 5 - 130 ppm (200 mL) 0-40°C N Y N pale purple → pale yellow

Ammonia 105SD 1 - 20 ppm (100mL)** 0.5-10 ppm (200mL) 0.2-4 ppm (500mL)

0-40°C N Y N pale purple → pale yellow

Carbon Disulfide 141SA 30 - 500 ppm (100 mL)** 20°C Y N N pink → yellow

Carbon Disulfide 141SB 2 - 50 ppm (200 mL)** 0.8 - 20 ppm (400 mL) 0-40°C Y Y N pink → yellow

Carbonyl Sulfide 239S 5 - 60 ppm (100 mL)** 0-40°C Y Y N pink → yellow Chlorine 109SA 1 - 40 ppm (100 mL) 0-40°C N Y N white → yellowish-orange

Ethyl Mercaptan 165SA 4 - 160 ppm (100 mL) 2 - 80 ppm (200 mL)** 1 - 40 ppm (400 mL)

0-40°C Y Y N white → yellow

Hydrogen Fluoride 156S 0.5 - 30 ppm (300 mL)** 0.25 - 15 ppm (600 mL) 0-40°C Y Y Y yellowish-green → pink


6 - 300 ppm (50 mL) 3 - 150 ppm (100 mL)**

1 - 50 ppm (300 mL) 0.75 - 37.5 ppm (400 mL)

0-40°C N Y N white → dark brown

Hydrogen Sulfide 120SD 2 - 60 ppm (50 mL) 1 - 30 ppm (100 mL)** 0-40°C N Y N white → pale brown

Methanol 119SA 500 - 60,000 ppm (100 mL)** 20°C Y Y N yellowish-orange → light green Methanol 119U 20 - 1,000 ppm (100 mL)** 0-40°C Y Y N yellow → pale blue Methyl Mercaptan 164SA 5 - 140 ppm (100 mL)** 0-40°C Y Y N white → reddish-yellow Methyl Mercaptan 164SH 50 - 1,000 ppm (100 mL)** 0-40°C N Y N pale-yellow → orange Nitrogen Dioxide 117SA 20 - 1000 ppm (100 mL) 0-40°C Y Y N white → yellowish-orange Sulfur Dioxide 103SC 20-300 ppm (100 mL)** 0-40°C N Y N purple → yellow Sulfur Dioxide 103SD 1 - 60 ppm (100 mL)** 0-40°C N Y N pink → yellow Sulfur Dioxide 103SE 0.5 - 10 ppm (100 mL)** 0-40°C N Y N pink → yellow


Page 39



Temp. Range

Temp. Correction

Pressure Correction

Humidity Correction Color Change

0.25 - 5 ppm (200 mL) Water 177SA 1.7 - 33.8 mg/L (100 mL)** 0-40°C Y Y N greenish-yellow → purple

**This is the standard sampling volume for which the graduations on the tube are designed

Table 3. Gas Detector Tube Interferences

Compound Sensidyne Part Number Interference and Cross-Sensitivity

Ammonia 105SC

Coexistence: >2 ppm chlorine → lower readings sulfur dioxide at >1/5 ammonia concentration → lower readings amines → higher readings Interference: amines → similar stain and higher readings

Ammonia 105SD

Coexistence: amines → higher readings Interference: amines → similar stain

Carbon Disulfide 141SA

Coexistence: sulfur dioxide → higher readings >400 ppm hydrogen sulfide → higher readings chlorine → higher readings Interference: >50 ppm sulfur dioxide → similar stain >400 ppm hydrogen sulfide → similar stain chlorine → white stain


Page 40


Carbon Disulfide 141SB

Coexistence: sulfur dioxide → higher readings >120 ppm hydrogen sulfide → higher readings chlorine → higher readings Interference: >15 ppm sulfur dioxide → similar stain >100 ppm hydrogen sulfide → similar stain chlorine → pale pink stain

Carbonyl Sulfide 239S

Coexistence: sulfur dioxide at 1/5 carbonyl sulfide concentration → higher readings carbon disulfide at 1/10 carbonyl sulfide concentration → higher readings hydrogen sulfide at 1/2 carbonyl sulfide concentration → higher readings > 0.1% n-butane → lower readings

Chlorine 109SA

Coexistence: >1 ppm chlorine dioxide, bromine → higher readings nitrogen dioxide at 1/2 chlorine concentration → higher readings Interference: >0.1 ppm bromine → similar stain >0.3 ppm chlorine dioxide → similar stain nitrogen dioxide → pale yellow stain

Ethyl Mercaptan 165SA

Coexistence: >1 ppm methyl sulfide → lower readings >1 ppm nitrogen dioxide →lower readings >0.2 ppm chlorine → lower readings Interference: >150 ppm carbon monoxide → dark grey stain >200 ppm ethylene → dark grey stain >40 ppm hydrogen sulfide → dark brown stain acetylene → pale brown stain >1 ppm methyl mercaptan → reddish-yellow stain


Page 41


Hydrogen Fluoride 156S

Coexistence: chlorine → higher readings hydrogen chloride → higher readings Interference: chlorine → similar stain hydrogen chloride → similar stain


Coexistence: >12 ppm sulfur dioxide → higher readings >550 ppm mercaptans → higher readings >2 ppm nitrogen dioxide → lower readings

Hydrogen Sulfide 120SD

Coexistence: >10 ppm sulfur dioxide → higher readings >300 ppm mercaptans → higher readings >2 ppm nitrogen dioxide → lower readings

Methanol 119SA

Coexistence: C4+ paraffins, alcohols, ketones, aromatic hydrocarbons → higher readings >50 ppm esters → higher readings Halocarbons → overall brown stain. (Light green stain indicates methanol content.) Interference: C4+ paraffins, alcohols, esters, ketones, aromatic hydrocarbons → similar stain

Methanol 119U

Coexistence: C4+ paraffins, alcohols, esters, ketones, aromatic hydrocarbons, halocarbons → higher readings Interference: C4+ paraffins, ketones, aromatic hydrocarbons, halocarbons → overall brown stain


Page 42


Methyl Mercaptan 164SA

Coexistence: >1 ppm methyl sulfide → lower readings >0.2 ppm chlorine → lower readings Interference: >150 ppm carbon monoxide → dark grey stain >200 ppm ethylene → dark grey stain >40 ppm hydrogen sulfide → dark brown stain >20 ppm acetylene → dark brown stain >1 ppm ethyl mercaptan → yellow stain

Methyl Mercaptan 164SH

Coexistence: >650 ppm hydrogen sulfide → higher readings >1,000 ppm nitrogen dioxide → higher readings chlorine at 1/3 mercaptan concentration → lower readings Interference: >5,000 ppm nitrogen dioxide → yellow stain carbon monoxide → grey stain ethylene → grey stain

Nitrogen Dioxide 117SA

Coexistence: >5 ppm chlorine, bromine, iodine, ozone → higher readings Interference: chlorine, bromine, iodine, ozone → similar stain

Sulfur Dioxide 103SC

Coexistence: chlorine at 1/5 sulfur dioxide concentration → higher readings nitrogen dioxide at 1/5 sulfur dioxide concentration → higher readings hydrogen sulfide at 100x sulfur dioxide concentration → lower readings Interference: chlorine → similar stain >100 ppm nitrogen dioxide → pink stain


Page 43


Sulfur Dioxide 103SD

Coexistence: nitrogen dioxide at same sulfur dioxide concentration → higher readings chlorine at 2x sulfur dioxide concentration → higher readings Interference: >20 ppm nitrogen dioxide → pale pink stain chlorine →pale pink stain

Sulfur Dioxide 103SE

Coexistence: > 3 ppm nitrogen dioxide → unclear stain and higher readings hydrogen chloride → higher readings Interference: nitrogen dioxide → pale pink stain hydrogen chloride →pale pink stain

Water 177SA

Coexistence: >0.02% ammonia → purple or reddish-purple stain + higher readings >0.2% nitrogen dioxide → unclear stain >0.3% methanol, ethanol, ethyl acetate → unclear stain >0.5% acetone → unclear stain


Page 44

12.0 GAS DETECTOR TUBE TEST DATA

Table 4. Gas Detector Tube Results

SampleVolume

Target Concentration


(Low)


(High) Measured

Concentration Corrected

ConcentrationTube ID

Tube Type Contaminant Sample

TechniquemL ppm ppm ppm ppm ppm

2 103SD Sulfur Dioxide Bag 100 25 21 29 30 31 3 103SC Sulfur Dioxide Bag 100 25 21 29 26 27 4 103SD Sulfur Dioxide Bag 100 25 21 29 30 31 5 103SC Sulfur Dioxide Bag 100 25 21 29 26 27 6 103SD Sulfur Dioxide Bag 100 49 41 58 55 57 7 103SD Sulfur Dioxide Bag 100 49 41 58 55 57 8 103SC Sulfur Dioxide Bag 100 49 41 58 55 57 9 103SC Sulfur Dioxide Bag 100 49 41 58 55 57

10 103SC Sulfur Dioxide Bag 100 99 82 117 105 108 11 103SC Sulfur Dioxide Bag 100 99 82 117 105 108 12 103SC Sulfur Dioxide Bag 100 198 167 227 225 232 13 103SC Sulfur Dioxide Bag 100 200 169 228 210 217 14 103SD Sulfur Dioxide Bottle 100 49 41 58 55 57 15 103SD Sulfur Dioxide Bottle 100 49 41 58 58 60

16 120SD Hydrogen Sulfide Bag 100 15 13 17 22 22 18 120SD Hydrogen Sulfide Bag 50 15 13 17 11 22 20 120SD Hydrogen Sulfide Bottle 100 15 13 17 22.5 23 17 120SD Hydrogen Sulfide Bag 50 49 41 58 37 76 28 120SD Hydrogen Sulfide Bottle 50 49 41 58 35 72 19 120SD Hydrogen Sulfide Bag 50 29 25 34 19 39 30 120SD Hydrogen Sulfide Bottle 50 29 25 34 20 41 25 120SD Hydrogen Sulfide Bottle 50 29 25 34 22 45 21 120SB Hydrogen Sulfide Bottle 100 15 13 17 23 23 22 120SB Hydrogen Sulfide Bag 300 15 13 17 61 21


Page 45

SampleVolume



(Low)


(High) Measured





23 120SB Hydrogen Sulfide Bag 100 15 13 17 21 21 24 120SB Hydrogen Sulfide Bag 50 15 13 17 12 25 26 120SB Hydrogen Sulfide Bag 300 29 25 34 115 39 27 120SB Hydrogen Sulfide Bag 100 29 25 34 41 42 29 120SB Hydrogen Sulfide Bottle 100 29 25 34 42 43 31 120SB Hydrogen Sulfide Bag 100 49 42 58 64 65 32 120SB Hydrogen Sulfide Bag 50 49 42 58 32 65 33 120SB Hydrogen Sulfide Bottle 100 49 42 58 64 65 34 120SB Hydrogen Sulfide Bottle 100 111 94 126 150 154 35 120SB Hydrogen Sulfide Bag 100 111 94 126 132 135 36 120SB Hydrogen Sulfide Bottle 50 111 94 126 74 152 37 120SB Hydrogen Sulfide Bag 50 111 94 126 69 141 38 120SB Hydrogen Sulfide Bag 100 111 94 126 141 144 39 120SB Hydrogen Sulfide Bag 50 111 94 126 72 147 40 120SB Hydrogen Sulfide Bottle 50 169 143 194 74 152 41 120SB Hydrogen Sulfide Bag 50 169 143 194 65 133

43 239S Carbonyl Sulfide Bottle 100 7 5 9 5 5 44 239S Carbonyl Sulfide Bag 100 7 5 9 5 5 45 239S Carbonyl Sulfide Bottle 100 10 8 12 7 7 46 239S Carbonyl Sulfide Bag 100 10 8 12 6 6 47 239S Carbonyl Sulfide Bottle 100 22 17 27 10 10 48 239S Carbonyl Sulfide Bottle 100 20 15 25 8 8

49 164SA Methyl Mercaptan Bottle 100 20 17 23 24 25 50 164SA Methyl Mercaptan Bag 100 20 17 23 21 22 51 164SA Methyl Mercaptan Bag 100 20 17 23 21 22 52 164SA Methyl Mercaptan Bottle 100 50 41 58 50 51


Page 46

SampleVolume



(Low)


(High) Measured





53 164SA Methyl Mercaptan Bag 100 50 41 58 50 51 54 164SA Methyl Mercaptan Bag 100 50 41 58 50 51 55 164SA Methyl Mercaptan Bottle 100 84 71 95 95 98 56 164SA Methyl Mercaptan Bag 100 84 71 95 95 98 57 164SA Methyl Mercaptan Bag 100 84 71 95 95 98 58 164SH Methyl Mercaptan Bottle 100 175 147 200 250 257 59 164SH Methyl Mercaptan Bottle 100 171 144 196 225 231 60 164SH Methyl Mercaptan Bag 100 175 147 200 250 257 61 164SH Methyl Mercaptan Bottle 100 347 294 397 380 391 62 164SH Methyl Mercaptan Bottle 100 347 294 397 360 370

63 141SB Carbon Disulfide Bottle 200 10 8 11 4 4 64 141SB Carbon Disulfide Bag 200 10 8 11 4 4 65 141SB Carbon Disulfide Bag 400 10 8 11 6 2 66 141SB Carbon Disulfide Bottle 200 24 20 27 7 7 67 141SB Carbon Disulfide Bag 200 24 20 27 7 7 68 141SB Carbon Disulfide Bottle 200 42 35 49 10 9 69 141SB Carbon Disulfide Bag 200 42 35 49 9 9 70 141SA Carbon Disulfide Bottle 100 42 35 49 10 20 71 141SA Carbon Disulfide Bag 100 42 35 49 7 14 72 141SA Carbon Disulfide Bottle 100 86 71 100 25 50

72A 141SA Carbon Disulfide Bag 100 86 71 100 23 46 73 141SA Carbon Disulfide Bottle 100 198 168 226 80 158 74 141SA Carbon Disulfide Bag 100 198 168 226 80 158 75 141SA Carbon Disulfide Bag 100 339 287 388 145 284 76 141SA Carbon Disulfide Bag 100 339 287 388 150 294

77 165SA Ethyl Mercaptan Bottle 400 8 7 9 18 9


Page 47

SampleVolume



(Low)


(High) Measured





78 165SA Ethyl Mercaptan Bottle 200 8 7 9 10 10 79 165SA Ethyl Mercaptan Bottle 100 8 7 10 4 8 80 165SA Ethyl Mercaptan Bottle 400 19 16 22 35 18 81 165SA Ethyl Mercaptan Bottle 200 19 16 22 18 19 82 165SA Ethyl Mercaptan Bottle 100 19 16 22 11 23 83 165SA Ethyl Mercaptan Bag 200 19 16 22 21 22 84 165SA Ethyl Mercaptan Bottle 200 41 35 49 35 36 85 165SA Ethyl Mercaptan Bag 200 41 35 49 35 36 86 165SA Ethyl Mercaptan Bottle 100 126 104 149 75 155 87 165SA Ethyl Mercaptan Bag 100 126 107 144 saturated, >80 indeterminate

0 0 0 88 119U Methyl Alcohol Bottle 100 50 41 58 60 62 89 119U Methyl Alcohol Bottle 100 50 41 58 60 62 90 119U Methyl Alcohol Bag 100 50 41 58 60 62 91 119U Methyl Alcohol Bottle 100 96 80 114 unreadable unreadable 92 119U Methyl Alcohol Bag 100 96 80 114 unreadable unreadable 93 119SA Methyl Alcohol Bottle 100 598 506 685 0.075 773 94 119SA Methyl Alcohol Bottle 100 598 506 685 0.075 773 95 119SA Methyl Alcohol Bottle 100 1148 972 1314 0.15 1546

100 105SD Ammonia Bottle 100 3 2 3 2 2 101 105SD Ammonia Bottle 100 10 8 11 10 10 102 105SC Ammonia Bottle 100 20 17 24 18 19 103 105SC Ammonia Bottle 100 20 17 24 19 20 104 105SD Ammonia Bottle 100 20 17 24 22 23 105 105SD Ammonia Bottle 100 20 17 24 20 21 106 105SD Ammonia Bottle 100 44 37 49 40 41 107 105SD Ammonia Bottle 100 44 37 49 40 41


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13.0 GAS DETECTOR TUBE PLOTS

27 27

20

21

22

23

24

25

26

27

28

29

30

100 mL Bag 100 mL Bag

ppm

Figure 8. Sulfur Dioxide (103SC), Tube #3 (left) and #5 (right), 25 ppm

31 31

20

21

22

23

24

25

26

27

28

29

30

31

32


ppm

Figure 9. Sulfur Dioxide (103SD), Tube #2 (left) and #4 (right), 25 ppm


Page 49

57 57

40

42

44

46

48

50

52

54

56

58

60


ppm


57 57

40

42

44

46

48

50

52

54

56

58

60


ppm



Page 50

108 108

80

85

90

95

100

105

110

115

120


ppm


232

217

150

160

170

180

190

200

210

220

230

240


ppm

Figure 13. Sulfur Dioxide (103SC), Tube #12 (left) and #13 (right), ~200 ppm


Page 51

57

60

30

35

40

45

50

55

60

65

100 mL Bottle 100 mL Bottle

ppm


22 2223

10

12

14

16

18

20

22

24

100 mL Bag 50 mL Bag 100 mL Bottle

ppm

Figure 15. Hydrogen Sulfide (120SD), Tube #16 (left), #18 (middle), #20 (right), 15 ppm


Page 52

76

72

30

35

40

45

50

55

60

65

70

75

80

50 mL Bag 50 mL Bottle

ppm

Figure 16. Hydrogen Sulfide (120SD), Tube #17 (left), #28 (right), 49 ppm

39

41

45

20

25

30

35

40

45

50

50 mL Bag 50 mL Bottle 50 mL Bottle

ppm

Figure 17. Hydrogen Sulfide (120SD), Tube #19 (left), #30 (middle), #25 (right), 29 ppm


Page 53

23

2121

25

10

12

14

16

18

20

22

24

26

100 mL Bottle 300 mL Bag 100 mL Bag 50 mL Bag

ppm

Figure 18. Hydrogen Sulfide (120SB), Tube #21 (left), #22 (left-center), #23 (right-center), #24 (right), 15 ppm

39

4243

20

25

30

35

40

45


ppm

Figure 19. Hydrogen Sulfide (120SB), Tube #26 (left), #27 (middle), #29 (right), 29 ppm


Page 54

65 65 65

40

45

50

55

60

65

70


ppm

Figure 20. Hydrogen Sulfide (120SB), Tube #31 (left), #32 (middle), #33 (right), 49 ppm

154

135

80

90

100

110

120

130

140

150

160

100 mL Bottle 100 mL Bag

ppm

Figure 21. Hydrogen Sulfide (120SB), Tube #34 (left), #35 (right), 111 ppm


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152

141

90

100

110

120

130

140

150

160


ppm


152

133130

140

150

160

170

180

190

200


ppm



Page 56

5 5

4

5

6

7

8

9

10


ppm

Figure 24. Carbonyl Sulfide (239S), Tube #43 (left), #44 (right), 7 ppm

7

6

5

6

7

8

9

10

11

12

13


ppm

Figure 25. Carbonyl Sulfide (239S), Tube #45 (left), #46 (right), 10 ppm


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10

8

0

5

10

15

20

25

30


ppm

Figure 26. Carbonyl Sulfide (239S), Tube #47 (left, 22 ppm), #48 (right, 20 ppm)

25

22 22

15

17

19

21

23

25

27

100 mL Bottle 100 mL Bag 100 mL Bag

ppm

Figure 27. Methyl Mercaptan (164SA), Tube #49 (left), #50 (middle), #51 (right), 20 ppm


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51 51 51

40

42

44

46

48

50

52

54

56

58

60


ppm


98 98 98

70

75

80

85

90

95

100


ppm



Page 59

257

231

257

140

160

180

200

220

240

260

280

100 mL Bottle 100 mL Bottle 100 mL Bag

ppm

Figure 30. Methyl Mercaptan (164SH), Tube #58 (left, 175 ppm), #59 (middle, 171 ppm), #60 (right, 175 ppm)

391

370

290

310

330

350

370

390

410


ppm

Figure 31. Methyl Mercaptan (164SH), Tube #61 (left), #62 (right), 347 ppm


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4 4

2

0

2

4

6

8

10

12


ppm

Figure 32. Carbon Disulfide (141SB), Tube #63 (left), #64 (middle), #65 (right), 10 ppm

7 7

5

10

15

20

25

30


ppm

Figure 33. Carbon Disulfide (141SB), Tube #66 (left,), #67 (right), 24 ppm


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9 9

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35

40

45

50

55


ppm

Figure 34. Carbon Disulfide (141SB), Tube #68 (left), #69 (right), 42 ppm

20

14

10

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30

35

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45

50

55


ppm

Figure 35. Carbon Disulfide (141SA), Tube #70 (left), #71 (right), 42 ppm


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50

46

40

50

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70

80

90

100

110


ppm

Figure 36. Carbon Disulfide (141SA), Tube #72 (left), #72A (right), 86 ppm

158 158

110

130

150

170

190

210

230

250


ppm



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284

294

260

280

300

320

340

360

380

400


ppm


9

10

8

0

2

4

6

8

10

12

400 mL Bottle 200 mL Bottle 100 mL Bottle

ppm

Figure 39. Ethyl Mercaptan (165SA), Tube #77 (left), #78 (center), #79 (right), 8 ppm


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18

19

23

22

15

16

17

18

19

20

21

22

23

24

400 mL Bottle 200 mL Bottle 100 mL Bottle 200 mL Bag

ppm

Figure 40. Ethyl Mercaptan (165SA), Tube #80 (left), #81 (left-center), #82 (right-center,), #83 (right), 19 ppm

36 36

30

32

34

36

38

40

42

44

46

48

50


ppm

Figure 41. Ethyl Mercaptan (165SA), Tube #84 (left), #85 (right), 41 ppm


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155

90

100

110

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130

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150

160

100 mL Bottle

ppm

Figure 42. Ethyl Mercaptan (165SA), Tube #86, 126 ppm

62 62 62

40

45

50

55

60

65

100 mL Bottle 100 mL Bottle 100 mL Bag

ppm

Figure 43. Methyl Alcohol (119U), Tube #88 (left), #89 (center), #90 (right), 50 ppm


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773 773

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550

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650

700

750

800


ppm

Figure 44. Methyl Alcohol (119SA), Tube #93 (left), #94 (right), 0.06%

1546

900

1000

1100

1200

1300

1400

1500

1600

100 mL Bottle

ppm

Figure 45. Methyl Alcohol (119SA), Tube #95, 0.11%


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2

1

1.5

2

2.5

3

3.5

4

100 mL Bottle

ppm

Figure 46. Ammonia (105SD), Tube #100, 3 ppm

10

6

7

8

9

10

11

12

100 mL Bottle

ppm

Figure 47. Ammonia (105SD), Tube #101, 10 ppm


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19

20

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25


ppm

Figure 48. Ammonia (105SC), Tube #102 (left), #103 (right), 20 ppm

23

21

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25


ppm

Figure 49. Ammonia (105SD), Tube #104 (left), #105 (right), 20 ppm


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41 41

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38

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46

48

50

52


ppm

Figure 50. Ammonia (105SD), Tube #106 (left), #106 (right), 44 ppm


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14.0 GAS DETECTOR TUBE PHOTOS

Figure 51. Sulfur Dioxide (103SC), Tube #3 (left) and #5 (right), bag sampling, 25 ppm

Figure 52. Sulfur Dioxide (103SD), Tube #2 (left) and #4 (right), bag sampling, 25 ppm


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Figure 53. Sulfur Dioxide (103SD), Tube #7 (left) and #6 (right), bag sampling, 49 ppm



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Figure 56. Sulfur Dioxide (103SC), Tube #13 (left) and #12 (right), bag sampling, ~200 ppm


Page 73

Figure 57. Sulfur Dioxide (103SD), Tube #15 (left) and #14 (right), bottle sampling, 49 ppm

Figure 58. Hydrogen Sulfide (120SD), Tube #16 (left, 100 mL bag sample), #18 (middle, 50 mL bag sample), #20 (right, 100 mL bottle sample), 15 ppm


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Figure 59. Hydrogen Sulfide (120SD), Tube #17 (left, 50 mL bag sample), #28 (right, 50 mL bottle sample), 49 ppm

Figure 60. Hydrogen Sulfide (120SD), Tube #19 (left, 50 mL bag sample), #30 (middle, 50 mL bottle sample), #25 (right, 50 mL bottle sample), 29 ppm


Page 75

Figure 61. Hydrogen Sulfide (120SB), Tube #21 (left, 100 mL bottle sample), #22 (left-center, 300 mL bag sample), #23 (right-center, 100 mL bag sample), #24

(right, 50 mL bag sample), 15 ppm

Figure 62. Hydrogen Sulfide (120SB), Tube #26 (left, 300 mL bag sample), #27 (middle, 100 mL bag sample), #29 (right, 100 mL bottle sample), 29 ppm


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Figure 63. Hydrogen Sulfide (120SB), Tube #31 (left, 100 mL bag sample), #32 (middle, 50 mL bag sample), #33 (right, 100 mL bottle sample), 49 ppm

Figure 64. Hydrogen Sulfide (120SB), Tube #34 (left, 100 mL bottle sample), #35 (right, 100 mL bag sample), 111 ppm


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Figure 67. Carbonyl Sulfide (239S), (left to right) Tube #43 (100 mL bottle sample, 7 ppm), #44 (100 mL bag sample, 7 ppm), #45 (100 mL bottle sample, 10 ppm), #46 (100 mL bag

sample, 10 ppm), #47 (100 mL bottle sample, 22 ppm), #48 (100 mL bottle sample, 20 ppm)

Figure 68. Methyl Mercaptan (164SA), Tube #49 (left, 100 mL bottle sample), #50 (middle, 100 mL bag sample), #51 (right, 100 mL bag sample), 20 ppm


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Page 80

Figure 71. Methyl Mercaptan (164SH), Tube #58 (left, 100 mL bottle sample, 175 ppm), #59 (middle, 100 mL bottle sample, 171 ppm), #60 (right, 100 mL bag sample, 175 ppm)

Figure 72. Methyl Mercaptan (164SH), Tube #61 (left, 100 mL bottle sample), #62 (right, 100 mL bottle sample), 347 ppm


Page 81

Figure 73. Carbon Disulfide (141SB), Tube #63 (left, 200 mL bottle sample), #64 (middle, 200 mL bag sample), #65 (right, 400 mL bag sample), 10 ppm

Figure 74. Carbon Disulfide (141SB), Tube #66 (left, 200 mL bottle sample), #67 (right, 200 mL bag sample), 24 ppm


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Figure 75. Carbon Disulfide (141SB), Tube #68 (left, 200 mL bottle sample), #69 (right, 200 mL bag sample), 42 ppm

Figure 76. Carbon Disulfide (141SA), Tube #70 (left, 100 mL bottle sample), #71 (right, 100 mL bag sample), 42 ppm


Page 83

Figure 77. Ethyl Mercaptan (165SA), Tube #77 (left, 400 mL bottle sample), #78 (center, 200 mL bottle sample), #79 (right, 100 mL bottle sample), 8 ppm

Figure 78. Ethyl Mercaptan (165SA), Tube #80 (left, 400 mL bottle sample), #81 (left-center, 200 mL bottle sample), #82 (right-center, 100 mL bottle sample), #83

(right, 200 mL bag sample), 19 ppm


Page 84

Figure 79. Ethyl Mercaptan (165SA), Tube #84 (left, 200 mL bottle sample), #85 (right, 200 mL bag sample), 41 ppm

Figure 80. Ethyl Mercaptan (165SA), Tube #86 100 mL bottle sample, 126 ppm


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Figure 81. Methyl Alcohol (119U), Tube #88 (left, 100 mL bottle sample), #89 (center, 100 mL bottle sample), #90 (right, 100 mL bag sample), 50 ppm

Figure 82. Methyl Alcohol (119SA), Tube #93 (left, 100 mL bottle sample), #94 (right, 100 mL bottle sample), 0.06%


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Figure 83. Methyl Alcohol (119SA), Tube #95 (left, 100 mL bottle sample), new tube (right), 0.11%

Figure 84. Ammonia (105SD), Tube #100, 100 mL bottle sample, 3 ppm


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Figure 85. Ammonia (105SD), Tube #101, 100 mL bottle sample, 10 ppm

Figure 86. Ammonia (105SC), Tube #102 (left, 100 mL bottle sample), #103 (right, 100 mL bottle sample), 20 ppm


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Figure 87. Ammonia (105SD), Tube #104 (left, 100 mL bottle sample), #105 (right, 100 mL bottle sample), 20 ppm

Figure 88. Ammonia (105SD), Tube #106 (left, 100 mL bottle sample), #106 (right, 100 mL bottle sample), 44 ppm


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15.0 FILTRATION TEST DATA

Table 5. Glass Fiber Filter (GFF) Results

Run Sample Added Test Dust (mg)

Filter Pre-Weight(mg)

Filter Post-Weight(mg)

Recovered Test Dust (mg) % Recovery

A Heptane Blank 0.0 36.6 36.3 -0.3 N/A A Propane Blank 0.0 36.6 36.0 -0.6 N/A A A2 0.5 36.2 37.0 0.8 148% A A2 1.2 36.2 37.2 1.0 85% A A2 2.3 36.7 39.7 3.0 130% A A2 4.5 36.0 38.7 2.7 60% A A2 6.5 36.9 41.0 4.1 63% A A2 8.4 36.5 42.3 5.8 69% A A2 10.0 36.3 43.7 7.4 74% A A2 20.4 36.4 49.0 12.6 62% A A2 30.3 37.2 54.0 16.8 55% A A2 40.2 36.8 71.6 34.8 87% B A2 0.6 36.0 37.1 1.1 193% B A2 1.0 36.3 36.4 0.1 10% B A2 2.0 36.0 37.5 1.5 75% B A2 4.0 35.9 37.4 1.5 37% B A2 6.1 36.7 42.1 5.4 89% B A2 8.1 36.0 41.2 5.2 64% B A2 10.5 36.4 45.1 8.7 83% B A2 20.3 35.9 53.7 17.8 88% B A2 30.5 36.2 58.9 22.7 74% B A2 40.5 36.8 58.7 21.9 54%


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-5.0

0.0

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20.0

25.0

30.0

35.0

40.0

45.0

0.0 0.0 0.5 1.2 2.3 4.5 6.5 8.4 10.0 20.4 30.3 40.2

Test Dust Samples (mg)

A2 T

est D

ust (

mg)

Added Test Dust (mg) Recovered Test Dust (mg)

Figure 89. Glass Fiber Filter Recovered Weights, Run A

0.0

5.0

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35.0

40.0

45.0

0.6 1.0 2.0 4.0 6.1 8.1 10.5 20.3 30.5 40.5


A2 T

est D

ust (

mg)


Figure 90. Glass Fiber Filter Recovered Weights, Run B


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Table 6. Millipore Filter Results

Run Sample Added Test Dust (mg)

Filter Pre-Weight(mg)

Filter Post-Weight (mg)

Recovered Test Dust(mg) % Recovery

A Heptane Blank 0.0 22.8 22.9 0.1 N/A A A2 0.5 19.9 20.5 0.6 111% A A2 1.1 23.0 23.9 0.9 80% A A2 2.2 23.2 24.0 0.8 37% A A2 4.2 23.1 26.7 3.6 86% A A2 6.0 23.1 26.6 3.5 58% A A2 8.1 23.0 26.8 3.8 47% A A2 10.4 22.8 29.8 7.0 67% A A2 20.3 22.7 35.4 12.7 63% A A2 30.5 22.7 40.2 17.5 57% A A2 40.1 23.0 60.6 37.6 94% B Propane Blank 0.0 20.1 20.2 0.1 N/A B Heptane Blank 0.0 20.4 20.4 0.0 N/A B A2 0.6 20.3 20.5 0.2 36% B A2 1.1 20.6 21.4 0.8 74% B A2 2.5 23.0 24.7 1.7 68% B A2 4.6 19.9 22.0 2.1 46% B A2 6.2 20.2 24.8 4.6 74% B A2 8.2 20.2 26.7 6.5 79% B A2 10.6 23.1 30.9 7.8 73% B A2 20.6 23.1 35.5 12.4 60% B A2 40.5 23.0 62.4 39.4 97%


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0.0

5.0

10.0

15.0

20.0

25.0

30.0

35.0

40.0

45.0

0.0 0.5 1.1 2.2 4.2 6.0 8.1 10.4 20.3 30.5 40.1


A2 T

est D

ust (

mg)


Figure 91. Millipore Filter Recovered Weights, Run A

0.0

5.0

10.0

15.0

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30.0

35.0

40.0

45.0

0.0 0.0 0.6 1.1 2.5 4.6 6.2 8.2 10.6 20.6


A2 T

est D

ust (

mg)


Figure 92. Millipore Filter Recovered Weights, Run B


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16.0 FILTRATION PHOTOS

Propane

Blank Heptane

Blank 0.5 mg 1.1 mg 2.2 mg 4.2 mg 6.0 mg 8.1 mg 10.4 mg 20.3 mg

A2 Test Dust Added

Figure 93. Millipore Filters, Run A

Propane

Blank Heptane


A2 Test Dust Added

Figure 94. Millipore Filters, Run B


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Heptane

Blank Propane


A2 Test Dust Added

Figure 95. GFF Filters, Run A

0.6 mg 1.0 mg 2.0 mg 4.0 mg 6.1 mg 8.1 mg 10.5 mg 20.3 mg 30.5 mg 40.5 mg

A2 Test Dust Added

Figure 96. GFF Filters, Run B


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17.0 REFERENCES

Cited

1. "Investigation of Portable or Handheld Devices For Detecting Contaminants in LPG,"

PERC Docket No. 11296, March 2005.

Sampling

• ASTM D1265-05, Standard Practice for Sampling Liquefied Petroleum (LP) Gases

(Manual Method).

• ASTM D3700-07, Standard Practice for Obtaining LPG Samples Using a Floating Piston

Cylinder.

• GPA 2140-97, Liquefied Petroleum Gas Specifications and Test Methods.

LPG Contaminants

• GPA 2140-97, Liquefied Petroleum Gas Specifications and Test Methods

• ASTM D1835, Standard Specification for Liquefied Petroleum Gases

• Propane Education and Research Council (PERC) (www.propanecouncil.org)

Gas Detection Tubes

• Sensidyne, Inc., www.sensidyne.com

• GASTEC Corporation. www.gastec.co.jp

• Draeger Safety. http://www.draeger.com/index.html

• RAE Systems. http://www.raesystems.com

• Mine Safety Appliances (MSA), Co. www.msanet.com

Manuals

• "Sensidyne Gas Detector Tube Handbook." Sensidyne, Inc. www.sensidyne.com

• "Model AP-20S Gas Detection Pump Instruction Manual." Sensidyne, Inc.

www.sensidyne.com


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Filtration

• ASTM D2276-06 Standard Test Method for Particulate Contaminant in Aviation Fuel by

Line Sampling

• www.millipore.com

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