This method is for determining the hydrogen content of light and middle distillates boiling in the range of approximately 15°C to 350°C on an as received basis, and hydrocarbons boiling above 350°C by dilution, using low resolution pulsed nuclear magnetic resonance (NMR). The range of quantitation is from 9.5 to 15.4 mass-% hydrogen. The concentration limits of the method may be extended if appropriate pure compounds are obtained as reference standards.

This method is for developing precision statements as reported in UOP methods and relative bias of the same method between different laboratories. The calculation of precision, in terms of repeatability and intermediate precision (within a laboratory), reproducibility (between laboratories) and relative bias (between laboratories) is described. Precision statements in methods having a 98 or later suffix were developed by the procedure described; methods having an 88 through 97 suffix used UOP 888-88, while methods with suffixes earlier than 88 used UOP 666-82.

The features of UOP 999 are as follows:

Minimum of 16 analyses required with emphasis on multiple concentration levels
Better identification of the components of variation and repeatability estimates
Alignment with ASTM repeatability, intermediate precision, and reproducibility definitions
Relative bias between laboratories with 95% confidence interval

UOP 999 is the minimum guideline for estimating the initial precision for new or revised methods. Once a new or revised method is in use, a reference sample, if available, should be run on a regular basis. When 16 analyses have been completed, individual and range control charts are to be used to estimate the long-term UOP repeatability and are to be maintained on an ongoing basis. The example calculations in UOP 999 are made using Minitabâ, a statistical software package. The details of the calculations are in UOP 999-97 Supplement.

This method is for determining total trace arsenic in liquid organics and heavy petroleum fractions by microwave digestion and Inductively Coupled Plasma – Mass Spectrometry (ICP-MS). The lower limit of quantitation for arsenic is 5 ng/g (mass-ppb).

Sample preparation by conventional extraction and digestion, such as that used in UOP Method 946, Arsenic in Petroleum Naphthas by HG-AAS, is time consuming and is problematic for high-boiling samples as it is possible for arsenic to be volatilized at the extreme sample preparation conditions required. UOP Method 986, Arsenic in Heavy Petroleum Fractions using Microwave Digestion and Graphite Furnace-AAS, uses microwave digestion, however due to sensitivity limitations of the GF-AAS, multiple digestions must be combined for analysis. A comparison of the methods is shown in Table 1

This method is for determining the total water in solid materials such as catalysts and zeolites (molecular sieves). Other materials may be applicable. This test is quantitative over a range of 0.2 to approximately 30 mass-% water. Common interferences are discussed in Notes.

This method is for organic analysis of distillate or petroleum fractions boiling in the range of 36 – 435°C using comprehensive two-dimensional gas chromatography (GCxGC) coupled with a flame ionization detector (FID). Results, expressed in mass-% can be reported in three different formats: 1) molecular types indexed to n-alkanes; 2) molecular type homologous series by carbon number and 3) user specified resolved compounds or molecular type groups. Individual compounds and molecular type groups are identified by their location, as plotted on a chromatographic two-dimensional image. Olefins, unless specifically identified, are lumped with other molecular types, typically cycloparaffins. Heteroatomic species, when resolved, can be determined; otherwise they are lumped with other aromatic hydrocarbons. The lower limit of detection for a single molecular component is typically below 0.004 mass-% with the specified equipment. .

This method is for determining trace concentrations of chloride, fluoride, and bromide in liquid organics by Combustion Ion Chromatography (CIC). This method has a lower limit of quantitation of 0.1 mg/kg (mass-ppm) for fluoride and chloride, and 0.2 mg/kg for bromide.

This method is for determining sulfur in liquid hydrocarbons at concentrations ranging from 10 to 1500 ng/g (mass-ppb). A direct measurement procedure (Part A) is used for samples above 100 ng/g. A trap & release procedure (Part B) is used for samples between 10 and 200 ng/g where high precision is required. This method is also applicable to highly volatile samples, such as pentane, through the use of a cooled sampling system.

Higher concentrations can be determined by ASTM Method D5453, "Standard Test Method for Determination of Total Sulfur in Light Hydrocarbons, Spark Ignition Engine Fuel, Diesel Engine Fuel, and Engine Oil by Ultraviolet Fluorescence" and D7183, "Standard Test Method for Determination of Total Sulfur in Aromatic Hydrocarbons and Related Chemicals by Ultraviolet Fluorescence" using the cooled sampling system described herein for highly volatile matrices.

Halogens interfere at concentrations greather than approximately 0.3%. The method has reduced sensitivity to sulfur present as a sulfate. For Part A, nitrogen content must not exceed sulfur by more than 100-fold to prevent a positive bias to the results.

This method is for determining sulfur in liquefied petroleum gas (LPG) and gaseous hydrocarbons at concentrations ranging from 0.2 to 100 mg/kg (mass-ppm).

LPG samples are expanded into the gas phase before analysis. If any heavy sulfur compounds are present in the LPG that do not volatilize quantitatively with the LPG, they may be under-reported. The method can also be applied to the analysis of hydrogen and other gas samples. Halogens interfere at concentrations greater than approximately 0.3%.

This method is similar to ASTM Method D6667, “Total Volatile Sulfur in Gaseous Hydrocarbons and Liquefied Petroleum Gases by Ultraviolet Fluorescence,” and ASTM Method D7551, “Total Volatile Sulfur in Gaseous Hydrocarbons and Liquefied Petroleum Gases and Natural Gas by Ultraviolet Fluorescence,” but uses a different sample introduction system which may improve precision and accuracy.

This method is for determining sulfur in liquefied petroleum gas (LPG) and gaseous hydrocarbons at concentrations ranging from 10 to 1400 ng/g (0.01 to 1.40 mass-ppm). A trap & release procedure is used to increase the sensitivity of the analysis.

Higher concentrations can be determined by ASTM Method D6667, "Standard Test Method for Determination of Total Volatile Sulfur in Gaseous Hydrocarbons and Liquefied Petroleum Gases by Ultraviolet Fluorescence," or ASTM Method D7551, "Total Volatile Sulfur in Gaseous Hydrocarbons and Liquefied Petroleum Gases and Natural Gas by Ultraviolet Fluorescence," by using the instrument without the trap & release module.

LPG samples are expanded into the gas phase before analysis. If any heavy sulfur compounds are present in the LPG that do not volatilize quantitatively with the LPG, they may be underreported.

Halogens interfere at concentrations greater than approximately 0.3%. The method can also be applied to the analysis of hydrogen and other gas samples.

This method is for the determination of pentane-insolubles in petroleum oils and is applicable to samples that are fluid at about 37 degrees C or lower temperatures. This method covers the range of 0.01 to about 20 mass-% pentane-insolubles. Solid particulate materials interfere. The data provided by this method may be used as an index to coking tendency of petroleum oils when considering their suitability as charge stocks to cracking or other processes.

More viscous or solid materials such as asphalts may be handled by using the modification described in the Appendix.

A similar test method for heptane-insolubles, for samples that are fluid at 80 degrees C, is UOP Method 614, Heptane-Insoluble Matter in Petroleum Oils by Membrane Filtration, which also mentions toluene-insolubles in a Note. ASTM Method D 4055, Pentane Insolubles by Membrane Filtration, is also similar in technique, but is written for particulates in lubricating oils rather than asphaltenes.