2 API STANDARD 19C

ASTM American Society for Testing and Materials

FTU Formazin turbidity unit

LOI loss on ignition

NTU nephelometric turbidity unit

4 Standard Proppant Sampling Procedure

4.1 General

Before any sample is taken, consider what tests will be performed; each test will require different
volumes. It is important that both the supplier and customer obtain the best representative sample
possible. Unless the sample is truly representative of a total shipment or container, testing and correlation
with specifications/standards is difficult. It is unlikely that sampling/testing methods in the field duplicate
the producer’s system. The standard procedures included within this document assist in obtaining
representative samples; however, there are inherent variations associated with sampling, testing
equipment, and procedures that can lead to inconsistent results. A sample that is representative of a
truckload, 23,000 kg (50,700 lb), or a railcar load, 90,000 kg (198,000 lb), can be the initial source of wide
variation when making comparisons. All parties shall ensure uniform samples. The customer and supplier
shall agree on sampling and testing methods/techniques.

For the best representation, continuous sampling is ideal. Although many proppant suppliers utilize
automatic sampling, it is usually impractical at the job site. If sampling is conducted while unloading a
container or at the well site, consideration should be given to the number and frequency of samples.

If bulk containers are filled from a flowing stream of proppant material, sampling procedures in
accordance with 4.5 shall be applied. If bulk containers are filled using sacked proppant material,
sampling procedures in accordance with 4.6 shall be applied.

4.2 Particle Segregation

It is important to have a basic understanding of segregation when sampling proppant. Depending on the
size, shape, distribution, and mechanisms involved, there is usually a certain amount of error or variability
involved in sampling due to segregation. The sampling procedures described here are the result of much
experience and are designed to minimize the effects of segregation of particles by size.

Particles, such as proppants, will naturally find the path of least resistance when moved or when force is
applied. During transfer or movement, particles of differing size and mass naturally separate or
segregate. The degree of segregation depends on the mechanisms involved in the transfer or movement.

There are several forces, such as gravity, acting on a stream of particles as it flows. Within a moving
stream, fine particles drop through the voids or gaps and coarser particles move to the outside. The fine
particles migrate and usually rest close to the area where they land. The heavier, coarser particles
bounce or roll much further, stratifying the material by particle size.

4.3 Equipment

The following equipment shall be used to compile representative proppant material samples.

4.3.1 Sampling Device

With a minimum slot opening six times the largest particle diameter sampled.

For example, a 12/20 fracturing proppant may contain particles as large as 2.36 mm, the size of the
opening in a U.S. alternative No. 8 (ASTM 2.36 mm) test sieve.
 MEASUREMENT OF AND SPECIFICATIONS FOR PROPPANTS USED IN HYDRAULIC FRACTURING AND GRAVEL-PACKING OPERATIONS 3

The minimum slot opening is defined as:

6 x 2.36 mm = 14.2 mm or 0.557 in.

The length of the slot shall be longer than the thickness of the stream being sampled. The volume of the
sampler shall be large enough so as to not overflow while cutting through the entire stream. An example
of a sampling device is shown in Figure 1.

Key
1 Sampler body: aluminum; 160 mm x 210 mm x 65 mm (6.25 in. x 8.25 in. x 2.5 in.)
2 Handle: common round pipe of sufficient strength to support the sampler plus about 1.6 kg (3.5 lb) proppant;
length as needed
3 Pipe coupling to accept handle (two locations)
4 Sample opening: 15 mm (0.6 in.)

Figure 1—Typical Box Sampling Device

4 API STANDARD 19C

4.3.2 Sample Reducer (16:1)

Of appropriate size for handling sack-size samples and reducing the material to 1/16 of the original mass.
See Figure 2.

Key
1 Main body: 370 mm x 480 mm x 110 mm (14.5 in. x 19 in. x 4.5 in.)
2 Splitter plate: eight locations, 51 mm x 51 mm x 51 mm (2 in. x 2 in. x 2 in.)
3 Discharge plate: 370 mm x 300 mm x 3.2 mm (14.5 in. x 12 in. x 0.125 in.)
4 Discharge chute: 57 mm x 57 mm x 76 mm (2.25 in. x 2.25 in. x 3 in.)
5 Hopper: 370 mm x 240 mm x 150 mm (14.5 in. x 9.5 in. x 6 in.)
6 Gate: 370 mm x 190 mm x 3.5 mm (14.5 in. x 7.5 in. x 0.125 in.)
7 Hand knob: diameter 38 mm (1.5 in.)
8 Support stand assembly: 710 mm x 380 mm x 690 mm (28 in. x 15 in. x 27 in.)

Figure 2— Typical 16:1 Sample Reducer

 MEASUREMENT OF AND SPECIFICATIONS FOR PROPPANTS USED IN HYDRAULIC FRACTURING AND GRAVEL-PACKING OPERATIONS 5

4.3.3 Sample Splitter

Of appropriate size.

Key
1 Main body: 290 mm x 280 mm x 165 mm (11.5 in. x 11 in. x 6.5 in.)
2 Handle
3 Gate plate
4 Hopper
5 Pan
6 Splitter vanes: 16 locations, 15 mm (0.6 in.)

Figure 3—Typical Sample Splitter

6 API STANDARD 19C

4.4 Number of Required Samples—Bulk

4.4.1 Proppants for Hydraulic Fracturing

A minimum of one sample per 9000 kg (20,000 lb), or fraction thereof, shall be obtained. All samples per
bulk container shall be combined and tested.

4.4.2 Gravel-packing Proppant

A minimum of one sample per 4500 kg (10,000 lb), but no fewer than two samples per job, shall be
obtained, combined, and tested.

4.5 Sampling—Bulk Material

All samples shall be obtained from a flowing stream of proppant by a manual or automatic sampler.
Samples shall not be taken from a static pile. The sampling device shall be used with its length
perpendicular to the flowing proppant stream. The sampler shall be passed at a uniform rate from side to
side through the full stream width of moving proppant. This shall be done as the material is moving to or
from a conveyor belt into a blender, truck, railcar, or bulk container. Approximately 2000 kg (4400 lb) of
proppant material shall be allowed to flow prior to taking the first sample. The number of samples taken
shall comply with 4.4. During sampling, the sampling receptacle shall be passed completely across the
moving proppant stream in a brief interval of time so as to sample the entire stream with each pass.
Under no circumstances shall the sampling receptacle be allowed to overflow.

4.6 Sampling—Sacked and Bagged Material

4.6.1 Sacks Up to 50 kg (110 lb)

Only whole sacks are to be used for sampling proppant materials.

4.6.2 Totes/Bulk Bags/Super Sacks: Weighting up to 2000 kg (4400 lb)

Unless the product can be sampled in a free-flowing state, the sample of large bags presents the same
problems as a static pile. Follow the same sample frequency as described in 4.4, using the sampling
method described in 4.5, but allow approximately 50 kg (110 lb) to be discharged from the bulk bag
before sampling.

5 Sample Handling and Storage

5.1 Sample Reduction

Place the contents of the combined bulk sample of proppant, or an entire sack up to 50 kg (110 lb), in the
16:1 sample reducer (see Figure 2) or equivalent. Obtain a reduced sample of approximately 1/16 of the
original mass of the total sack’s contents, typically 3 kg (6.6 lb).

5.2 Sample Splitting

An appropriately sized sample reducer and sample splitter shall be used to prepare representative
samples for testing. Place the reduced sample, obtained according to 5.1, or the sample obtained during
bulk material loading operations (refer to 4.5) in the sample splitter (see Figure 3) or equivalent. Split the
sample to the desired quantity to permit performance tests as specified in this document.

5.3 Sample, Record Retention, and Storage

The proppant supplier shall maintain records of all tests conducted on each shipment for a minimum of
one year. Physical samples of an amount sufficient to conduct all tests recommended herein, but in no
 MEASUREMENT OF AND SPECIFICATIONS FOR PROPPANTS USED IN HYDRAULIC FRACTURING AND GRAVEL-PACKING OPERATIONS 7

cases less than 0.25 kg (0.5 lb), shall be retained in storage for a minimum of six months. Any material
subsequently taken for testing shall be split from the retained sample. Samples shall be sealed in a type
of container that is sufficient to protect the sample from contamination and moisture. Samples shall be
stored in a cool, dry place.

6 Sieve Analysis

6.1 Purpose

The purpose of this section is to provide specifications for recognized proppant sizes and a standard
procedure to ensure a consistent methodology for sieve analysis.

6.2 Description

The procedure and equipment described in 6.3 through 6.6 are the most widely utilized in the hydraulic
fracturing and gravel-packing industry. Alternate methods may be used, but shall be correlated with these
standard methods.

6.3 Apparatus and Materials

6.3.1 Sieve Sets (Two)

Complying with the requirement of ASTM Sieve Series, 200 mm (8 in.) diameter or equivalent.

One set is a working or compliance set, and the other a master or calibration set to be used for calibration
or standardization only. Compliance and calibration sieves are defined in ASTM E11.

NOTE For informational purposes, an excerpt from E11 is included in this document as Annex A.

Table 1—ASTM Test Sieve Sizes

Sieve-opening Sizes
µm
3350/ 2360/ 1700/ 1700/ 1180/ 1180/ 850/ 600/ 425/ 425/ 212/
1700 1180 1000 850 850 600 425 300 250 212 106
Typical Proppant/Gravel-pack Size Designations

6/12 8/16 12/18 12/20 16/20 16/30 20/40 30/50 40/60 40/70 70/140

Stack of ASTM Sieves a,b

4 6 8 8 12 12 16 20 30 30 50
Upper designating
6 8 12 12 16 16 20 30 40 40 70
sieve in bold type
8 10 14 14 18 18 25 35 45 45 80
10 12 16 16 20 20 30 40 50 50 100
12 14 18 18 25 25 35 45 60 60 120
Lower designating
14 16 20 20 30 30 40 50 70 70 140
sieve in bold type
16 20 30 30 40 40 50 70 100 100 200
pan pan pan pan pan pan pan pan pan pan pan

a Sieve series as defined in ASTM E11 (U.S. Alternative designation); refer to Annex A for opening size in µm.

b Test sieve stacked in order from top to bottom, largest opening on top.