700 CMR 19.05
Sampling, Testing, and Examination for Total Sulfur, Pyrrhotite, and Framboidal Pyrite
All applicants and licenses shall conduct sampling, testing, and examination for total sulfur,
pyrrhotite, and framboidal pyrite in accordance with the requirements and standards identified
in this 700 CMR 19.05. Sampling, testing, and examination results and analysis shall be
reported in the GSR report in accordance with 700 CMR 19.06.
(1) Sampling, testing, and examination shall be conducted by a certified professional geologist,
licensed professional geologist or an equivalent acceptable to the State Geologist.
(2) Sampling, testing, and examination results provided in GSR report under 700 CMR 19.06
shall be from samples obtained by the lead geologist or designated party assigned by the lead
geologist. Testing and examination shall be conducted on representative samples from the
Aggregate Manufacturer’s active mining location(s).
(a) Sampling. Aggregate shall be sampled from the stockpile(s), in accordance with ASTM
D75 Standard Practice for Sampling Aggregates or AASHTO R 90 Standard Practice for
Sampling Aggregate Products. Sampling shall be conducted by certified technicians that are
independent from and not affiliated with Aggregate Manufacturers. Technicians shall be
certified with the American Concrete Institute (ACI) Aggregate Testing Technician – Level 1
certification, Northeast Transportation Training and Certification Program (NETTCP)
Soils & Aggregate Inspector certification, or an equal certification approved by MassDOT.
Aggregate samples shall be a composite of all onsite aggregate stockpiles of the same source,
recombined, and sampled randomly from the combined sample. Aggregate stockpile samples
shall be protected from the environment and sealed. The geology of the aggregate stockpile
samples shall be analyzed and be of the same geology of previously examined cores
identified in 700 CMR 19.06(2)(b). If the geology differs, samples from the previously
sampled and stored cores shall be obtained for the testing and examination identified in
700 CMR 19.05(2)(b).
(b) Testing and Examination. Testing and examination shall be conducted by laboratories
that are independent from and not affiliated with Aggregate Manufacturers. Independent
laboratories utilized for testing shall be recognized by the National Cooperation for
Laboratory Accreditation (NACLA) in Construction Materials Engineering and Testing
(CMET), AASHTO Resource, or an equal program approved by MassDOT and the State
Geologist. Independent laboratory results shall be determined by the preparer and
documented on a report form meeting the standard methods identified in 700 CMR
19.05(2)(b): Table 1. The GSR shall include a description of each test performed and a
summary of the results.
Level 1 total sulfur content testing and Level 2 petrographic examination (when required)
shall be conducted on a composite sample of all onsite aggregate stockpiles of the same
source (and previously sampled and stored cores when requested by the State Geologist) and
reported annually, per the requirements identified in 700 CMR 19.00. Level 2 petrographic
examination shall be conducted when the Level 1 total sulfur content test result is greater
than or equal to 0.1% and less than 1.0%, as identified in 700 CMR 19.05(2)(b): Table 1.
If the manufacturer blends aggregate from multiple sources or areas with geological
differences, then each source or area blended into the aggregate shall be tested and examined
separately.
Testing requirements are determined from current research and available information.
As research evolves, testing requirements will be adjusted to reflect the most recent and
proven research at any given time. MassDOT, in consultation with the State Geologist,
reserves the right to request further information when deemed necessary. If a concrete
structure exhibits distress or deterioration due to iron sulfide reaction, the aggregate source
shall be subjected to further sampling, testing, and examination through the aggregate source
licensing program, as specified in 700 CMR 19.05.
Table 1: Total Sulfur Content, Pyrrhotite, and Framboidal Pyrite Testing Requirements
Method
Quality Characteristic
Limits
Level 1 Total Sulfur Content Testing
ASTM D4239[1]
Total Sulfur
Content(%)
Acceptable: Permitted for use in Concrete
< 0.1
Additional:
Level 2 Petrographic
Examination for Pyrrhotite and Framboidal
Pyrite Content Required
0.1 to < 1.0
Rejectable: Prohibited from use in
Concrete
> 1.0
Level 2 Petrographic Examination (if required)
ASTM C295[2]
Pyrrhotite
and/or
Framboidal
Pyrite
Acceptable: Permitted for use in Concrete
No Presence
Rejectable: Prohibited from use in
Concrete
Presence
[1]
ASTM D4239 Standard Test Method for Sulfur in the Analysis Sample of Coal and Coke Using
High-Temperature Tube Furnace Combustion shall be modified for the testing of aggregate
accordingly.
[2]
Scanning electron microscope (SEM) / energy-dispersive x-ray spectroscopy (EDS) can be
conducted to confirm the presence of pyrrhotite and framboidal pyrite. Pyrrhotite (Fe1-xS; where
x = 0 to 0.17) shall be considered present when observing iron to sulfur ratios in the range of 0.8
to 1.0 detect 4C (Fe7S8), 5C (Fe9S10), 6C (Fe11S12) and 11C (Fe10S11), respectively. Framboidal
pyrite shall be considered present when observing clustered microcrystals in a framboidal shaped
structure, with an iron to sulfur ratio of 0.5 to detect FeS2.
(3) Testing Exceptions.
(a) Statistically Insignificant Risk Exception. Subject to the regional and site geology
analysis reported in the GSR, as required in 700 CMR 19.06(2)(a) and (2)(b), an applicant
or licensee may, in lieu of the testing requirements provided in 700 CMR 19.05(2), obtain
an opinion signed by a certified professional geologist, licensed professional geologist or an
equivalent acceptable to the State Geologist, that there is a statistically insignificant risk that
the area of operation for a given year contains iron sulfide deposits (pyrrhotite and
framboidal pyrite). This testing exception shall be contingent on completion of the regional
and site geology analysis as described in 700 CMR 19.06(2)(a) and (b). The regional and site
geology analysis shall be included in the Geological Source Report (GSR) submitted with
the license application.
(b) Continuous Extraction Site Operations Exception. Subject to the regional and site
geology analysis reported in the GSR, as required in 700 CMR 19.06(2)(a) and (2)(b), an
applicant or licensee may, in lieu of the testing requirements provided in 700 CMR 19.05(2),
may certify that they will continue to source aggregate from the same extraction site for
which a previous year’s GSR was submitted and will not expand operations beyond the
maximum radius of 250 feet beyond the farthest drill hole or exposed quarry faces used for
identifying geology, as provided in 700 CMR 19.06(2)(b)20. This exception of testing shall
be contingent on completion of the regional and site geology analysis as described in
700 CMR 19.06(2)(a) and (b). The regional and site geology analysis shall be included in
the Geological Source Report (GSR) submitted with the license application. If, during the
relevant license year, an aggregate manufacturer operates a new or expanded extraction site,
this exception shall no longer apply and a new GSR must be submitted in accordance with
700 CMR 19.06.
(c) Natural Sand Exception. Subject to the regional and site geology analysis reported in
the GSR, as required in 700 CMR 19.06(2)(a) and (2)(b), an applicant or licensee may, in
lieu of the testing requirements provided in 700 CMR 19.05(2), obtain confirmation signed
by a certified professional geologist, licensed professional geologist or an equivalent
acceptable to the State Geologist, that the aggregate source is a natural sand deposit. This
testing exception shall be contingent on completion of the regional and site geology analysis
as described in 700 CMR 19.06(2)(a) and (b). The regional and site geology analysis shall
be included in the Geological Source Report (GSR) submitted with the license application.
(d) Manufactured Sand Exception. Testing exception for manufactured sand shall be
subject to the regional and site geology analysis reported in the GSR, as required in
700 CMR 19.06(2)(a) and (2)(b), and the test results of the quarried rock used in the
manufactured sand, as required in 700 CMR 19.05(2).