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ASTM D8469-22

(Test Method)

Standard Test Method for Analysis of Multiple Elements in Cannabis Matrices by Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

Standard Test Method for Analysis of Multiple Elements in Cannabis Matrices by Inductively Coupled Plasma Mass Spectrometry (ICP-MS)

SIGNIFICANCE AND USE
5.1 Medical and/or recreational marijuana (cannabis) has been legalized for adult use in many countries and states within the USA (5). Many jurisdictions that permit the use of medicinal and recreational marijuana require testing of cannabis and associated products to ensure safety from contaminants, especially the toxic “big four” elements such as As, Cd, Hg, and Pb (6), and other metals worthy of consideration (6). These heavy metals can accumulate in plants grown in polluted soils or contamination can occur during the manufacturing process (7). In addition to ensuring product safety, the analysis of mineral and other trace elements is required for labeling purposes when these products are sold as nutritional supplements. Trace element analysis of plant and nutritional supplement materials is a well-established application (8). Following acidic digestion to break down the plant-based samples' primary components, ICP-MS is often used for quantitative analysis because of its multi-element capability, high sensitivity, speed, robustness, and wide dynamic range.  
5.2 This test method covers the rapid determination of multiple elements in cannabis sample digests. The elements include the priority toxic elements (As, Cd, Hg, and Pb), as well as elements required by some states and elements of interest in the cannabis community (V, Cr, Cu, Zn, Sb, Ba, Se, Ag, Na, Al, K, Mn, Fe, Co, Ni, Mo, Tl, Th, and U). Irrespective of the number of elements being measured, test times are approximately a few minutes per test specimen, and detectability for most elements is in the low- to sub-ppb range.
SCOPE
1.1 This test method uses inductively coupled plasma mass spectrometry (ICP-MS) to determine multiple trace elements in cannabis and cannabis-related matrices following sample preparation using microwave-assisted acid digestion. This test method is applicable to the quantification of trace levels of elements in dried plant materials, concentrates, oils, extracts, tinctures of cannabis and cannabis-related products. Other matrices may be added provided that the lab validates the extra matrices using Practice D8282. Details are provided on the validation of both the sample preparation procedure and analytical method using certified reference materials (CRMs) and validation of the analytical method using spike recovery testing of several cannabis based samples.  
1.2 This test method should be used by analysts experienced in the use of microwave digestion and ICP-MS, matrix interferences, and procedures for their correction or reduction, and should only be used by personnel trained in the handling, preparation, and analysis of samples for the determination of trace elements in cannabis and cannabis products (1).2 This test method was developed using a single quadrupole ICP-MS equipped with a collision/reaction cell (CRC) that can be pressurized with helium (He) gas for the removal of polyatomic interferences using kinetic energy discrimination (KED). This test method can also be run using a triple quadrupole or “tandem” mass spectrometer (MS/MS) ICP-MS instrument, which is fitted with CRC technology. The ICP-MS method accounts for polyatomic interferences, which are the most common spectral overlaps in ICP-MS, isobaric interferences, and any potential doubly-charged ion interferences (M2+) that may arise from the presence of rare earth elements (REEs) in the samples, as the REE2+ ion interferences can affect the accuracy of the measurement of arsenic (As) and selenium (Se) in the samples. Table 1 lists elements for which the test method applies along with recommended analytical masses, and secondary masses for some elements. The priority toxic elements arsenic (As), cadmium (Cd), mercury (Hg), and lead (Pb), also sometimes referred to as the “big four” toxic trace elements are listed separately because of their toxicity, as discussed in 5.1.  
1.3 Certified reference materials (CRMs) should be matrix matc...

General Information

Status
Published
Publication Date
31-Jul-2022
ICS
11.120.99 - Other standards related to pharmaceutics
65.020.20 - Plant growing
Technical Committee
D37 - Cannabis
Drafting Committee
D37.03 - Laboratory
Current Stage
Ref Project

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ASTM D8469-22 - Standard Test Method for Analysis of Multiple Elements in Cannabis Matrices by Inductively Coupled Plasma Mass Spectrometry (ICP-MS)ASTM D8469-22 - Standard Test Method for Analysis of Multiple Elements in Cannabis Matrices by Inductively Coupled Plasma Mass Spectrometry (ICP-MS)
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ASTM D8469-22 - Standard Test Method for Analysis of Multiple Elements in Cannabis Matrices by Inductively Coupled Plasma Mass Spectrometry (ICP-MS)
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This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D8469 − 22
Standard Test Method for
Analysis of Multiple Elements in Cannabis Matrices by
1
Inductively Coupled Plasma Mass Spectrometry (ICP-MS)
This standard is issued under the fixed designation D8469; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope masses, and secondary masses for some elements.The priority
toxicelementsarsenic(As),cadmium(Cd),mercury(Hg),and
1.1 This test method uses inductively coupled plasma mass
lead (Pb), also sometimes referred to as the “big four” toxic
spectrometry(ICP-MS)todeterminemultipletraceelementsin
trace elements are listed separately because of their toxicity, as
cannabis and cannabis-related matrices following sample
discussed in 5.1.
preparation using microwave-assisted acid digestion. This test
method is applicable to the quantification of trace levels of
1.3 Certified reference materials (CRMs) should be matrix
elements in dried plant materials, concentrates, oils, extracts,
matched as closely as possible to the cannabis/plant matrix.
tinctures of cannabis and cannabis-related products. Other
In-house reference materials (RMs) are acceptable if no CRM
matricesmaybeaddedprovidedthatthelabvalidatestheextra
is available and/or the in-house RM is well characterized, but
matrices using Practice D8282. Details are provided on the
CRMs are preferred. NIST 1575a Pine Needles, NRC
validation of both the sample preparation procedure and
HEMP-1, and a NIST hemp sample (NIST number not
analytical method using certified reference materials (CRMs)
assigned yet) were analyzed to verify method bias. The
and validation of the analytical method using spike recovery
RM/CRMs should have a recovery between 80% to 120 %
testing of several cannabis based samples.
when concentrations are above the limit of quantification
(LOD) or within the concentration uncertainty (converted to
1.2 Thistestmethodshouldbeusedbyanalystsexperienced
in the use of microwave digestion and ICP-MS, matrix percent relative uncertainty) supplied on the certificate, which-
ever is greater. If acceptable values are not obtained, the
interferences, and procedures for their correction or reduction,
and should only be used by personnel trained in the handling, analytical solution may be reanalyzed once. If acceptability is
still not met, recalibrate and reanalyze the entire analytical
preparation, and analysis of samples for the determination of
2
traceelementsincannabisandcannabisproducts (1). Thistest sequence and/or prepare and digest new analytical portions.
method was developed using a single quadrupole ICP-MS
1.4 Multi-laboratory Validation (MLV)—This test method
equipped with a collision/reaction cell (CRC) that can be
was tested by analyzing an NRC hemp CRM, a NIST hemp
pressurized with helium (He) gas for the removal of poly-
SRM, and a NIST plant control sample (NIST 1575a Pine
atomic interferences using kinetic energy discrimination
Needles)byfourlaboratorieseachrunningasinglequadrupole
(KED). This test method can also be run using a triple
ICP-MS.
quadrupole or “tandem” mass spectrometer (MS/MS) ICP-MS
instrument, which is fitted with CRC technology.The ICP-MS
1.5 Gravimetric dilution (weight/weight), volumetric dilu-
method accounts for polyatomic interferences, which are the
tion (volume/volume), or a combination of the two techniques
most common spectral overlaps in ICP-MS, isobaric
(weight/volume) are acceptable methods for ICP-MS sample
interferences, and any potential doubly-charged ion interfer-
preparation.
2+
ences (M ) that may arise from the presence of rare earth
2+ 1.6 Units—The values stated in SI units are to be regarded
elements(REEs)inthesamples,astheREE ioninterferences
as the standard. No other units of measurement are included in
canaffecttheaccuracyofthemeasurementofarsenic(As)and
this standard.
selenium (Se) in the samples. Table 1 lists elements for which
the test method applies along with recommended analytical
1.7 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
1
This test method is under the jurisdiction of ASTM Committee D37 on
Cannabis and is the direct responsibility of Subcommittee D37.03 on Laboratory. mine the applicability of regulatory limitations prior to use.
Current edition approved Aug. 1, 2022. Published O
...

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1.1 This terminology is a compilation of definitions of technical terms used in the cannabis industry. Terms that are generally understood or adequately defined in other readily available sources are not included.  
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1.6 Abbreviated Terminology:  
1.6.1 Abbreviated terminology is intended to provide uniform contractions of terms relating to cannabis that have evolved through widespread common usage. The compilation in this standard has been prepared to avoid the occurrence of more than one abbreviated term for a given cannabis term and to avoid multiple meanings for abbreviated terms.  
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1.6.3 Acronyms and Initialisms—A word formed from the letters or parts of words of a longer word-phrase, usually from the initial letters or parts of the words. An acronym is pronounced as a word (for example, radar for radio detection and ranging). An initialism is pronounced as a series of letters (for example, DOT for Department of Transportation).  
1.6.4 The acronym or initialism description is the origin word-phrase for the acronym or initialism, not a definition.  
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Standard Guide for Sample Preparation of Cannabis and Hemp Inflorescence for Laboratory Analysis

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5.1 The sample preparation procedure for comminution impacts other downstream processes such as extraction and sonication, which ultimately affects the total analytical error (TAE) and measurement uncertainty.  
5.2 Factors that may influence the sample preparation process include the prevention of cross-contamination (carryover) from a prior sample and an inadequate cleaning procedure between preparation of samples, poor sample handling, storage (sample preservation), and moisture content (drying methods) of plant material being greater than 15 % (15). Samples with high moisture content are hard to process completely and may yield lower analyte (that is, cannabinoid) concentration during extraction and further processing. Lastly, water activity Specification D8197 is recommended, activity (aw) range (0.55 to 0.65) for dry cannabis or hemp flower or both.  
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5.4 In addition to sampling devices, this guide does not include the sample preparation of edibles, tinctures, oils/concentrates, beverages, and so forth in which the sample diversity poses significant sample preparation challenges to be put forward in additional work items.  
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1.1 In this guide, the basic steps in obtaining a test portion sample of either dried cannabis/hemp inflorescence are outlined.  
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ASTM D8452-22(Guide)
Standard Guide for Requirements for Medical-related Professionals within the Cannabis and Hemp Industries

SIGNIFICANCE AND USE
5.1 As patient use of cannabis and hemp for medical purposes increases and medical professionals are increasingly called upon to provide medical advice, the following requirements and expectations within the medical profession are increasingly significant, requiring:  
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1.4 This guide provides recommendations for articulating professional requirements for training and education or earning certificates. It is part of a series of guides denoting certification requirements for professions within the cannabis and hemp industries (Guides D8346, D8347, D8348), and supporting Practice D8403 for associated certificate programs.  
1.5 This guide's content does not supersede requirements for training or earning a certificate defined by jurisdictional entities such as government or other regional regulatory bodies.  
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5.1 Gas chromatography and flame ionization detection provides a rapid means to identify and quantify cannabinoids in a variety of samples of interest. This test method allows producers of cannabis products to improve and optimize the quality of their products. For example, hemp extractors can use it to determine the efficiency of extraction processes and to verify that products meet regulatory requirements, ensuring safety and quality of products.  
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Standard Guide for Assessing Spoilage of Hemp Seed Intended for Human Consumption

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3.1 This guide provides a method for rapid, visual, on-site assessment of spoilage of hemp seed that will assist in managing food quality and productivity while maintaining consumer safety. It can be augmented with a number of laboratory tests to determine spoilage.  
3.2 This guide provides a method to identify hemp seed samples that are likely to spoil by quantifying discolored (dark yellow or brown) dehulled seed. Samples from lots/batches that display more than 2 % discolored2 dehulled seed are generally considered to be compromised.  
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3.3.1 It is recommended that where possible, test results taken from samples are reported with a calculated margin of error to ensure statistical significance or relevant results.  
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1.1 This guide covers the recommended steps for a visual assessment of spoilage in hemp seed intended for human consumption. Additional recognized laboratory tests can be completed as necessary to augment this guide.  
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5.1 This standard will provide best practices for the sampling of harvested cannabis inflorescence with the intent to assure representative sampling.  
5.2 The laboratory results and their respective harvest batch associations have implications and significance to regulatory requirements, quality control considerations throughout the product’s life cycle, and the safety of the consumers who may be adversely affected by consumption of product that was not tested in a homogeneous manner (3).  
5.3 This standard does not address the appropriate sampling of processed cannabis materials such as such as extracts, seeds, edibles, topicals, etc.  
5.4 This standard addresses the sampling of cannabis inflorescence destined for human or animal consumption.  
5.5 This standard does not address pre-harvest field sampling or large untrimmed or unprocessed harvest batches.
SCOPE
1.1 Cannabis harvested materials require sampling strategies throughout their life cycle, from cultivation to the end consumer. For purposes of this standard, the term cannabis is inclusive of all cannabis inflorescence, including hemp varieties. The qualitative and quantitative characteristics of cannabis/hemp for human or animal consumption has safety implications throughout the life cycle from cultivation to end consumer. This standard provides best practice procedures and protocols for sampling batches of harvested cannabis inflorescence. Cannabis/hemp materials often exhibit variability across different parts within the same plant or across different plants within the same cultivar, or both, (1, 2).2 Thus, sampling strategies are required which yield a representative a sample across a harvest batch. Representative sampling is required to ensure that the qualitative and quantitative test results accurately reflect cannabinoid identification, potency, identification and concentration of terpenes, concentration of trace metals, microbiological activity, mycotoxins, and concentration of pesticides across the batch.  
1.2 Where procedural aspects of this practice differ from local regulatory or jurisdictional requirements, the local regulatory or jurisdictional authority’s directives shall take precedence.  
1.3 Units—The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system are not necessarily exact equivalents; therefore, to ensure conformance with the standard, each system shall be used independently of the other, and values from the two systems shall not be combined.  
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
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4.1 In this guide, steps are suggested for the effective development, control, and management of procedures and records required for an effective product recall/removal from the marketplace.  
4.2 This guide presents a systematic approach to procedures and documentation regarding the steps necessary to be taken in the event of a product recall or removal from the marketplace because of health, safety, or quality nonconformances.  
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Standard Guide for Intrusion Detection System (IDS)

SIGNIFICANCE AND USE
3.1 The intrusion detection system (IDS) safeguards various areas considered critical to operations. Intrusion detection devices include but are not limited to, door or window contact alarms that are activated when the device is separated, such as opening; and motion detection technology that uses a passive infrared to survey the area and sounds an audible notification alarm when a person or object moves into the protected space. Also included are glass-break detectors that use an audio sensor to pick up the actual frequency of broken glass. If the glass-break detector “hears” broken glass, an alarm is activated. If any of the devices are triggered when the system is armed, an alert is sent to a 24-h monitoring area for notification.
SCOPE
1.1 This guide covers the recommended intrusion detection system (IDS) for protecting resin cannabis, resin cannabis products, resin cannabis waste, currency, people, property, and assets.  
1.2 Units—The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered standard.  
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

  • Guide
    3 pages
    English language
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ASTM
ASTM D8205-20(Guide)
Standard Guide for Video Surveillance System

SIGNIFICANCE AND USE
3.1 The video surveillance system safeguards various areas considered critical to operations. The surveillance system uses cameras capable of capturing images and videos that can be compressed, stored, or sent over communication networks. The main difference between a digital video surveillance system and an analog video surveillance system is that a digital video surveillance system is capable of capturing and storing the video signal in a digital format. A digital video surveillance solution can be managed from anywhere and provide interoperability. The cameras can be networked and footage encrypted and digitally archived, which is considered crucial for most resin cannabis businesses because the video feed can be secured and shared with government authorities.
SCOPE
1.1 This guide covers the recommended video surveillance system for protecting resin cannabis, resin cannabis products, resin cannabis waste, currency, people, property, and assets.  
1.2 Units—The values stated in inch-pound units are to be regarded as the standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered standard.  
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations as defined by the Authority Having Jurisdiction (AHJ) prior to use.  
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

  • Guide
    3 pages
    English language
    sale 15% off