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Standard Operating Procedure Issue

for the Collection of Lot Samples of Date: Rev.: 3


Agricultural Food Products for Physical, 06/24/13
Chemical and Microbiological Analyses PROPRIETARY
Foreign Trade Service Corporation
Page #:
Procedure 4300-P, SOP for Sample Collection
1 of 36

1 Purpose

1.1 These Standard Operating Procedures will serve as a guide for training in sampling technique,
both as a written instruction and for on the job instruction by supervisors or certified master samplers. In
general, these procedures for sampling agricultural products from a Lot are based on USDA and FDA
procedures, as well as ISO standards.1 Samplers will refer to 4300-P SOP while completing their formal training
and will have access to a copy will conducting field sampling. Competence in sampling, collecting exhibits,
photography, observation, report preparation, sample identification, handling, packaging, transport and shipping
is demonstrated by satisfactorily completing written or practical examination.

1.2 Further, in accordance with the Food Safety Modernization Act (FSMA), training in these
procedures and their practical application will ensure that FTS samplers meet the FSMA requirement that,
“individuals who conduct sampling of foods (for laboratory analysis) are qualified by training and experience to
do so.”2 Using these SOPs, samplers will be trained to collect samples of foods, from all types of packaging and
bulk-storage, for physical, chemical and microbiological analyses.

1.3 The scope3 of operations includes the sampling of all foods for commercial and technical
purposes:

a) to serve as a representative sample of product offered for sale


b) for examination to verify that the product meets a commercial, official or contractual
specification or standard
c) for laboratory tests to determine the characteristics, stability or safety of a food
d) for process quality control
e) for end product quality control
f) to identify known or unknown material or the source of a given material
g) to determine the composition or flavor profile of a material
h) to monitor changes in properties over time, as in shelf life studies
i) for tests in support of a government regulatory action
j) as arbitration samples; preshipment or retention samples
k) as forensic evidence

1.4 This procedure will guide samplers in the collection of samples representative of the Lot;
maintaining the integrity of the sample and documenting a clear chain of custody,4 so that the samples will

1
ISO 7002, Agricultural food products – Layout for a standard method of sampling from a lot
2
FDA Food Safety Modernization Act, Title II, Sec. 202
3
ISO 7002, 4.3-4.4
4
FDA Investigations Operations Manual (FDA IOM), Chapter 4, 4.1.4.1 (4)
Copyright 2013 Foreign Trade Service Corp.
Standard Operating Procedure Issue
for the Collection of Lot Samples of Date: Rev.: 3
Agricultural Food Products for Physical, 06/24/13
Chemical and Microbiological Analyses PROPRIETARY
Foreign Trade Service Corporation
Page #:
Procedure 4300-P, SOP for Sample Collection
2 of 36

serve as forensic evidence for laboratory analysis in support of an FDA enforcement action or other legal
activity.5

1.5 Samplers will be certified in writing as Master Samplers by an officer of the Foreign Trade
Service Corp., upon satisfactory completion of training to the SOP, by written and practical tests, and with the
written recommendation of the Laboratory Manager or Sampling Operations Manager.

2 Scope / Field of Application

2.1 This Standard Operating Procedure applies to samplers and the sampling of foods and medical
devices for commercial purposes; physical, chemical and microbiological analyses food safety or general
quality and condition or in support of an FDA enforcement action.

3 Definitions and Acronyms


3.1 Composite sample: A bulk sample comprised of approximately equal portions collected from
the units sampled from a Lot.
3.2 Consignment: A quantity of some commodity delivered at one time and covered by one set of
documents. The consignment may consist of one or more Lots or parts of Lots (ISO 7002, A.9).
3.3 Continuous or in-line sampling: Samples collected directly at specific intervals and locations
on a production line of a manufacturing process.
3.4 Counter samples: One or more substantially equivalent representative samples taken from the
same package for use as commercial samples, control or preshipment samples, arbitration samples, joint
examinations, referee samples or as retention samples for laboratory analysis.
3.5 Entry: A lot or consignment arriving at a US Customs port of entry for import into the United
States.
3.6 Entry documents: Commercial Invoice, Packing List, Bill of Lading and other documents
submitted to U.S. Customs for the purpose of paying duty and clearing goods for import into the United States.
3.7 FDA Notice of Action: An official document stating FDA’s intention to release, sample, detain
or refuse entry of foods, drugs or medical devices, intended for import into the United States.
3.8 Inspection: The process of examining, measuring, testing, gauging or otherwise comparing the
unit (sample) with applicable requirements (ISO 7002, A.15).
3.9 Laboratory sample: A sample as prepared for sending to the laboratory for inspection or testing
(ISO 7002 A.19).

5
FDA Investigations Operations Manual (FDA IOM), Chapter 4, 4.1.4.1 (4)
Copyright 2013 Foreign Trade Service Corp.
Standard Operating Procedure Issue
for the Collection of Lot Samples of Date: Rev.: 3
Agricultural Food Products for Physical, 06/24/13
Chemical and Microbiological Analyses PROPRIETARY
Foreign Trade Service Corporation
Page #:
Procedure 4300-P, SOP for Sample Collection
3 of 36

3.10 Line Item: Each unique Lot of product listed in an Entry document submitted to U.S. Customs.
3.11 Lot: For the purpose sampling and testing, a “Lot” is defined as that quantity of product
representing one run, batch or chop of product, produced by one manufacturer, of the same origin, type and
grade, identically labeled or coded and presumed to be uniform.
3.12 Lot sample: The collection of subsamples or portions collected from a Lot or a composite
sample representing those individual portions.
3.13 Lot size: The number of items (packages) or quantity of material constituting the Lot (ISO 7002,
A.22). Lot size may be indicated by an upper case letter “N” followed by the quantity, as N = 700.
3.14 Master Sampler: A sampler-inspector certified as being qualified by training and experience to
inspect and collect samples of food, commodities and medical devices.
3.15 Portion: The number of items or quantity of material constituting each subsample.
3.16 Random sampling: The taking of n items from a Lot of N items in such a way that all possible
combinations of n items have the same probability of being chosen (ISO 7002, A.34).
3.17 Representative sample: A sample drawn so as to reflect as accurately as possible the properties
of interest of the lot from which it is taken (ISO 7002, A.38).
3.18 Sampler-inspector: Field technician responsible for inspection and collecting samples from
Lots held in public or private storage.
3.19 Sampling plan: The predetermined procedure for the sample selection, withdrawal and
preparation of samples from a Lot to yield the required information so that a decision can be made regarding the
acceptance of the Lot (ISO 7002, A.43).
3.20 Sample size: The number of items (packages) or quantity of material constituting the sample.
The number of subsamples or sampled units may be designated by a lower case “n,” as in n = 20.
3.21 SCR: Acronym for “Sample Collection Report,” a written report describing the lot and product
that was sampled, owner and manufacturer, method of sampling, quantity sampled, sample identification, chain
of custody and signed and dated by the sampler.
3.22 Subsample: Individual portions collected from a Lot. Each subsample is individually packaged,
numbered and labeled.
3.23 Stratified sampling; zone sampling: The sampling of a lot that can be differentiated into sub-
lots (called strata or zones), in such a way that specified portions of the sample are drawn at random from
different strata (ISO 7002, A.46)

Copyright 2013 Foreign Trade Service Corp.


Standard Operating Procedure Issue
for the Collection of Lot Samples of Date: Rev.: 3
Agricultural Food Products for Physical, 06/24/13
Chemical and Microbiological Analyses PROPRIETARY
Foreign Trade Service Corporation
Page #:
Procedure 4300-P, SOP for Sample Collection
4 of 36

4 Responsibilities

4.1 The Laboratory Manager ensures that this procedure is established, implemented and maintained.

4.2 The Quality Manager oversees the day-to-day operations of document control.

4.3 The Sampling Operations Manager ensures that samplers are instructed, trained and qualified to
execute the procedure.

4.4 Samplers are responsible for following this procedure in its entirety. Samplers must be
physically strong and able to lift and carry heavy objects.

5 Required

5.1 General Requirement for Samplers

Samplers must be able to


a) read and write English6
b) observe and report conditions and exceptions of packaging and storage that
might affect the quality and safety of the Lot as well as the integrity of the sample.
c) complete a sample collection report
d) use entry documents and warehouse receiving and inventory records to
identify lots
e) take documentary digital photos, collect exhibits and collect valid samples, without bias and
with the care and knowledge that (s)he might be required to testify with respect to the sample,
recorded observations and sample chain of custody.7

5.2 Individuals collecting samples from Lots in warehouses located on waterfront facilities must be
citizens of the United States or legal aliens, must not have a felony conviction, and must apply for and be
issued a Transportation Worker Identification Credential.8

5.3 Samplers are responsible for obeying a facility’s rules for safety and personal conduct when on
the property of a public or private warehouse, terminal, processing plant or any other location where
sampling is conducted.

5.4 Training for samplers will include written or on-the-job instruction in the following:

6
FDA-IOM, Ch. 1, 1.1, Ch. 4, 4.4.10
7
FDA IOM, Ch. 4, 4.1.2, 4.1.3; ISO 7002, 8.1
8
Maritime Transportation Security Act of 2002
Copyright 2013 Foreign Trade Service Corp.
Standard Operating Procedure Issue
for the Collection of Lot Samples of Date: Rev.: 3
Agricultural Food Products for Physical, 06/24/13
Chemical and Microbiological Analyses PROPRIETARY
Foreign Trade Service Corporation
Page #:
Procedure 4300-P, SOP for Sample Collection
5 of 36

a) collection of samples, photos and exhibits as forensic evidence for use alone or for tests that
might be used as evidence in court
b) packing, labeling, sealing, transporting and shipping samples, especially those samples that must
remain chilled or frozen.
c) aseptic sampling
d) basic level training in warehouse sanitation, storage pests and microbiological food safety
e) use of sampling tools such as triers, grain probes, drills, drum thiefs, sterile pipettes, sterile bags
and scoops
f) sampling of foods that are fresh, processed, solid, free flowing particles, powders, liquid and
viscous fluids; in frozen, chilled and ambient storage
g) sampling portions from whole fish and meat
h) sampling from cartons, cases, pails, drums, tanks, bulk boxes, super sacks, bladders, rail cars and
barges

5.5 Most sampling assignments can be accomplished by one sampler working alone and
unsupervised; however, some procedures involve repetitive heavy lifting, such as meat drilling and wharf
examinations, and might require two samplers.

6 Procedure

6.1 GENERAL SAMPLING AND INSPECTION PROCEDURES

6.1.1 These sampling procedures are to ensure the collection of unbiased representative lot samples for
inspection and testing and maintain the condition, integrity and chain of custody of those samples delivered to
the client or the laboratory9. The field application of these methods is identified, where applicable, in the
procedures10. Before collecting samples, the sampler must

a) identify and inspect the Lot and storage area to ensure that the correct Lot is sampled
b) inspect the Lot to verify the packaging is intact and free from damage that would affect the
safety or quality of the product
c) inspect the area where the Lot is stored to ensure that it is held under sanitary conditions; i.e.,
no evidence of exposure to water, debris, insects, rodents, birds or other animals.
d) verify the quantity by a physical count or when not practicable, examining the current
public warehouse inventory record for the lot
e) identify* the Lot by marks, Lot number, product codes and Lot location and cross-referencing

9
ISO 7002, 4.3
10
ISO 7002, 4.4
Copyright 2013 Foreign Trade Service Corp.
Standard Operating Procedure Issue
for the Collection of Lot Samples of Date: Rev.: 3
Agricultural Food Products for Physical, 06/24/13
Chemical and Microbiological Analyses PROPRIETARY
Foreign Trade Service Corporation
Page #:
Procedure 4300-P, SOP for Sample Collection
6 of 36

the same, when applicable, using FDA Notice of Action, U.S. Customs Entry or shipping
records, packing lists, bills of lading, and commercial invoices referenced with the ocean
container, truck, warehouse receipts, warehouse inventory and warehouse Lot locations; shipping
marks, package labels and brand; product type, style, grade, packaging and declared net
weights11,12.

*Do not sample a Lot that does not match the Lot identified in the Entry and other supporting
documentation.

6.1.2 SAMPLE COLLECTION REPORTS

6.1.2.1 Complete a Sample Collection Report (SCR). Record relevant observations and exceptions, Lot
and sample identification, shipping or transport method and chain of custody in FTS Form 4310-SCR for FDA
detentions. Use FTS Form 4319-MEAT for meat drilling and FTS Form 4300-WS for all other sampling reports
and wharf examinations. Include documentary photos when applicable. Only the sampler who prepared and
signed the SCR may edit the SCR13.

6.1.2.2 The SCR form is a template that serves as an instruction for the completion of the report. The
forms ask for certain information, such as the name of the warehouse, Lot number, marks etc., and a space is
provided for the sampler to enter the information requested. The sampler should enter all pertinent and available
information in the space provided or enter “NA” when not applicable or unavailable. If an error is made, strike
through the mistake with a single line, make the necessary correction, and initial next to the correction. Never
obliterate or erase a mistake with a pen, pencil, tape or correction fluid.

6.1.2.3 Sampling reports must be signed and dated by the sampler-inspector. Representation by
concerned third parties, as witnesses to sampling or for joint collection of arbitration samples or claims, shall be
clearly stated in the SCR14. When sampling is witnessed or samples collected jointly with another party, the
SCR must be signed by both samplers15.

6.1.2.4 Use New York Board of Trade (NYBOT) sampling orders for reporting sampling of Exchange
coffee and cocoa.

6.1.2.5 Sampling reports are hand-written, but occasionally a more formal Certificate of Sampling might
be required. Certificates of Sampling are usually typed and might include documentary photos and other
relevant attachments.

11
FDA IOM, Ch. 4: 4.2.6, 4.2.6.1
12
ISO 7002, 4.9
13
FDA IOM, Ch. 4:4.10; Attachment A
14
ISO 7002, 4.8.2
15
ISO 7002, 4.8.4
Copyright 2013 Foreign Trade Service Corp.
Standard Operating Procedure Issue
for the Collection of Lot Samples of Date: Rev.: 3
Agricultural Food Products for Physical, 06/24/13
Chemical and Microbiological Analyses PROPRIETARY
Foreign Trade Service Corporation
Page #:
Procedure 4300-P, SOP for Sample Collection
7 of 36

6.1.3 SAMPLE IDENTIFICATION

6.1.3.1 Label all subsamples and exhibits with the FTS Sample/Job Number. Counter label packaging
units from which subsamples were collected. For samples that will be forwarded or delivered to a client or
laboratory, sample labels may include the date of sampling, sampler’s initials, corresponding subsample number
and a Lot reference; i.e., U.S. Customs Entry Number and Line Item number.16

6.1.3.2 Counter or Control samples are duplicate samples collected at the same time from the same
package usually for use as commercial control samples, preshipment samples or laboratory retention samples.
Counter samples must be identically labeled, but may be differentiated by a letter code, such as samples “A”
and “B”. In some cases, multiple counter samples could be required and should be labeled accordingly. Place
the subsamples into a master packaged for transport or shipping. Counter label the master package as above and
place a tamper evident seal on the master package. Enclose the original SCR with the sealed sample and retain a
file with seal numbers, copies of photos, records and documents used to identify the Lot.17

6.1.4 SAFETY

6.1.4.1 In case of a fire or other emergency, be aware of the nearest exit from the facility where you are
working. Make sure to check in and out with warehouse personnel and that they are aware of your location in
the warehouse. Watch out for forklifts and conveyors and keep your eye on the load when cargo is being
handled or lifted near you. Watch out for load shifts, particularly with stacked bags, such as cocoa beans. When
opening an intermodal container, open one door only at first and stand clear in case there is pressure on the door
causing it to spring open. Sampling is destructive by nature and some damage and spillage is unavoidable.
Whenever possible, take care to avoid unnecessary contamination or exposure of the food. To avoid slipping
hazards and debris that might attract pests, clean up your area when sampling is completed. Where and when
appropriate, to ensure personal health and safety, wear a dust mask, steel toed shoes, protective clothing and
gloves, hard hat, safety glasses, ear protection, safety vest, safety harness18.

6.1.5 EQUIPMENT

6.1.5.1 In general, equipment used for sampling various food groups and sample types are specified in
the procedures. Sampling equipment and supplies are stored in Newark, NJ, Humble, TX and Suffolk, VA and
will be shipped to samplers at other locations when needed. Contact the Sampling Operations Manager for
supplies.

6.15.2 Lighting is often poor in warehouses so a flashlight is an important piece of equipment that a
sampler should never be without. When selecting a container for the sample and method of transporting the
sample, consider that ambient conditions might affect or alter the condition of the sample. Most fresh or
16
FDA IOM, Ch. 4: 4.3.2.2
17
ISO 7002, 4.13
18
ISO 7002, 4.8.3
Copyright 2013 Foreign Trade Service Corp.
Standard Operating Procedure Issue
for the Collection of Lot Samples of Date: Rev.: 3
Agricultural Food Products for Physical, 06/24/13
Chemical and Microbiological Analyses PROPRIETARY
Foreign Trade Service Corporation
Page #:
Procedure 4300-P, SOP for Sample Collection
8 of 36

perishable agricultural food products are sampled in cold storage. Meat, poultry, fish and seafood, frozen
vegetables and fruit concentrates are held in freezer storage. Many low moisture foods, snack foods, many
processed and canned foods are stored without temperature or humidity control. Where applicable, the
procedures will specify container types and transport or shipping conditions that should maintain the samples in
a state similar to that under which they were stored19.

6.2 RESEALING AND REPAIR OF SAMPLED PACKAGES

6.2.1 Sampling is destructive by nature. Restore sampled Lots as circumstances allow by reclosing and
resealing inner and outer packaging. Re-close barrels, drums and cases; sew tape or otherwise secure bags or
cartons.20 Notify the owner and warehouse, if conditions exist after sampling that expose the contents. Wipe
packaging surfaces clean and remove spilled contents.

6.2.2 There are instances when you will backfill sampled packages with product from another master
package. If the product is on FDA detention, notify the party in possession of the goods that there is an empty
master package. The empty package must be retained pending release of the product for entry into the United
States. Make a note in the SCR that product was back filled. If the empty package is used to transport or ship
the samples to the laboratory, it should be noted on the SCR and the package should be retained by the
laboratory as an exhibit. Every package in a Lot that is refused entry by FDA must be accounted for at the time
a Lot is re-exported or destroyed.

6.2.3 When required, place tamper evident seals on packages, drums or similar containers opened for
sampling.

6.3 DELIVERY OF SAMPLES

6.3.1 In general, transport frozen or chilled samples in coolers with ice, dry ice or chill packs.
However, certain frozen products, such as frozen blocks of shrimp, are sufficiently chilled to be transported or
shipped in coolers or insulated cartons without additional ice, dry ice or chill packs. If chilled or frozen samples
are shipped to a laboratory, use an overnight delivery service. When dry ice is required in a package, use only
FedEx. Obey regulations for HAZMAT labeling and weight of dry ice not to exceed 2.3Kg (5 Lbs.).21

6.3.2 Maintain a clear chain of custody until the samples are delivered to the laboratory or a courier
service or picked up by laboratory personnel. A copy of an airway bill or receipt for the samples will serve as
evidence that custody of the samples has been transferred to the courier or laboratory.

19
ISO 7002, 4.10 & 4.11
20
FDA IOM, Ch. 4: 4.3.2.1
21
U.S. Code of Federal Regulations, Title 49, Ch. 1: Sec. 173.217
Copyright 2013 Foreign Trade Service Corp.
Standard Operating Procedure Issue
for the Collection of Lot Samples of Date: Rev.: 3
Agricultural Food Products for Physical, 06/24/13
Chemical and Microbiological Analyses PROPRIETARY
Foreign Trade Service Corporation
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Procedure 4300-P, SOP for Sample Collection
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6.4 SAMPLING PLANS

6.4.1 Sample size, sample type, portions and the number of units sampled is determined by the food,
lot size, sampling plan and type of tests. A sampling plan for each job will be provided by the Sampling
Operations Manager or Laboratory Manager.

6.4.2 For all other samples collected for chemical and microbiological analysis, we refer to FDA
sampling plans. The exceptions are sampling plans established by food industry and trade associations; i.e.,
ASTA, MICA, AFI, NYBOT etc. When sampling for grading, sensory and other physical tests, FTS often
follows USDA-AMS sampling plans22. In any case, sampling plans and methods will be assigned by the
Sampling Operations Manager or Laboratory Manager.

6.4.3 Sequential sampling is a method by which the samples are taken in increments depending on the
absence or presence of critical defects or attributes in a given number of sampled units. Sequential sampling
plans have and rejection numbers “c” for “n” samples. In the case where there is a zero tolerance for live
insects, the sampler might be directed to stop sampling, if live insects are observed in the product.

6.4.4 The sampling plan might direct that the individual subsamples are combined into one or more
composite samples. Sometimes, in order to achieve sufficient weight for each laboratory sample, multiple units
of prepackaged products are needed for each subsample; such as, combining several small retail-packaged units
of a spice to meet the 100g subsample requirement for microbiological tests. When such units are combined to
make a subsample, label each accordingly and place them in a larger master package.

6.5 SAMPLING AND INSPECTION METHODS (PRINCIPAL)

6.5.1 Whenever samples are collected for microbiological tests or tests for filth, samplers will wear lab
coats or clothing free from loose dirt and animal hairs; hair nets or ball caps or other appropriate head covering
and examination gloves. When sampling in a food manufacturing facility, remove any jewelry, wrist watches,
cell phones, keys, pens etc. and place them where they could not accidently fall into processing equipment,
samples, open packages or bulk storage unit.

6.5.2 For the sampling and inspection of foods for foreign material, follow the general procedure for
Wharf Examination (6.20). Note any necessary modification in the method in the SCR or Sampling and
Inspection report.

22
ISO 7002, 8.1 Note: The usual default-sampling plan is ISO 2859-1. In general, when samples are collected from Lots that are
detained by FDA, sample size is determined according to the Sample Schedule Charts in the FDA IOM, FDA Compliance Policy
Guides; FDA Bacteriological Analytical Manual (FDA BAM); FDA Import Seafood Compliance Program CPG 7303.844
Attachments A-6 and D. When sampling detained products for conditions or tests not covered in existing guidelines, the Sampling
Operations Manager will contact the Compliance Officer or FDA Office of Field Science.

Copyright 2013 Foreign Trade Service Corp.


Standard Operating Procedure Issue
for the Collection of Lot Samples of Date: Rev.: 3
Agricultural Food Products for Physical, 06/24/13
Chemical and Microbiological Analyses PROPRIETARY
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Procedure 4300-P, SOP for Sample Collection
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6.5.3 Take precautions to ensure the safety of the food product that is to be sampled. Never place
packages or samples directly on the floor when sampling. If it is necessary to remove a package from a pallet to
facilitate sampling, use a small stack of pallets covered by a clean corrugated slip-sheet as a workbench. Make
sure that there are no conditions in the surrounding area to that might affect the integrity of the product.
Samplers must wash their hands before and after sample collection. It is always a safe practice to wear
examination gloves when collecting the sample. Change into a clean pair of gloves, if the gloves were worn
while handling or opening packages and after handling objects such as cell phones. As a rule, change gloves as
frequently as necessary.

6.5.4 Select random packages for sampling so that there is no bias in the sample.23 Do not accept
packages presented by the client for sampling. Always collect samples from packages that are chosen by you,
the sampler. In some cases, by prior arrangement or rule, the warehouse will prepare a random package sample
pallet at the time of unloading and samples will be collected from the sample pallet.

6.5.5 When inserting a trier into a package, keep the open side face down until the trier is fully
inserted. Then twist the trier so that the opening is face up. Collect the sample through the open end by moving
the trier in a short back a forth motion.

6.5.6 Grain probes are either partitioned or non-partitioned. Use a partitioned grain probe to collect
subsamples from multiple sites in a bulk storage system. Insert the probe with the opening closed. Open the
probe to collect subsample portions. Reclose and remove the probe. Empty the contents onto a canvas sheet,
stainless steel table or if possible, empty the portions directly into individual sample containers. Use a non-
partitioned grain probe for composite samples.

6.5.7 Samples should always be collected into appropriate unused clean containers strong enough to
protect the product from damage and cross-contamination. When filling the container, ensure that headspace is
reduced to limit to the degree possible any change of state of the product. Collect pesticide test samples,
samples for melamine analysis and all other residue test samples into metal bags or glass containers, such as
mason jars. Never collect residue samples into paper or plastic bags. Collect aseptic samples into sterile bags or
sterile containers. Collect samples for sensory examination into clean jars or metal bags. Samples of dried fruit
should be collected into moisture-barrier plastic bags. Produce, tree nuts, beans, grain, pulses, spices, herbs and
spice seeds may be collected into heavy weight or multi-ply cloth or paper bags, sterile twirl bags or plastic
bags. Processed foods, Individually Quick Frozen (IQF) products and other packaged frozen foods should be
collected as packaged whenever possible. Perishable and frozen foods should be held and transported as near as
possible to the temperature at which they were stored24.

23
FDA IOM Ch. 4: 4.3.7.2
24
ISO 7002, 4.11
Copyright 2013 Foreign Trade Service Corp.
Standard Operating Procedure Issue
for the Collection of Lot Samples of Date: Rev.: 3
Agricultural Food Products for Physical, 06/24/13
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6.6 ASEPTIC SAMPLING

6.6.1 Equipment List:

a) flashlight
b) digital camera, min 5 megapixel
c) sampling report worksheet, notepad or notebook
d) hair net
e) examination gloves
f) lab coat
g) sterile sample bags (twirl bags) or another type of sterile container
h) sterile scoop, sterile pipette, sterile drum thief or other sterilized tool
i) ethanol or isopropyl alcohol
j) torch or lighter
k) tape
l) knife or box cutter
m) sampling report worksheet, notepad or notebook

6.6.2 Samplers will wear lab coats or clothing free from loose dirt and animal hairs; hair nets or ball
caps or other appropriate head covering and examination gloves. Aseptic sampling is a method of collecting a
sample from pre-packaged or bulk packaging into sterile sample containers using sterile or aseptic gloves,
scoops, triers, pipettes and other devices. If a tool such as a probe, knife, drill bit or saw is required to collect
the sample, the tool or portion of the tool that is in contact with the food must be sterilized prior to its use. This
can be achieved by applying autoclaving. Alternatively, apply alcohol to the tool area that will be in contact
with the food product and flame it off or use a sanitizer spray. Prior to collecting a sample from a bulk bag by
using a probe, first sanitize the area where the probe is to enter the bag.

6.6.3 Take care when opening the package to avoid introducing dust or other debris from the package
or your clothing. Sterile scoops should not be removed from its packaging until immediately before use. Keep
the package in a clean place. Do not rest the scoop on a non-sterile surface between samples. If the scoop must
be set down, place back in the package from which it was removed. Do not allow the scoop to contact any other
surface other than the food that is being sampled.

6.6.4 With a clean gloved hand, remove the sterile scoop or sterile tool from its package and insert it
into the exposed food material. Open the sterile twirl bag or container. Collect the required portion into the
sterile twirl bag or other sterile container. Replace the sampling scoop or tool in the food material or back into
its original package.

6.6.5 Sterile bags such as Whirl Pack™ bags should remain closed until immediately prior to receiving
the sample. To open, remove the perforated strip at the top of the bag and use the two plastic tabs to spread
Copyright 2013 Foreign Trade Service Corp.
Standard Operating Procedure Issue
for the Collection of Lot Samples of Date: Rev.: 3
Agricultural Food Products for Physical, 06/24/13
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sides of the bag apart. After filing the bag with the sample, fold the excess bag material over the front of the bag
expelling the air. Hold each end of the wire closure and twirl the bag. Twist or fold the ends so that the closures
secure the bag without the possibility of the wires puncturing the bag.

6.6.6 If the scoop or tool comes in contact with a non-sterile surface other than the food you are
sampling, sterilize the tool or use a new one. Change gloves as frequently as necessary. When collecting
subsamples for microbiological tests where there is a zero (negative) tolerance or the subsamples are to be
composited for analysis you may use the same tool for the same lot. Otherwise, use different sterile tools each
subsample and always for each lot.

6.6.7 Make sure that the samples are temperature controlled when held and transported.

Supplemental to this procedure and as a general guideline, refer to the FDA procedures for collecting aseptic
samples25.

6.7 DRILLING MEAT (FROZEN BEEF TRIMMINGS)

6.7.1 Equipment List:

a) Hand-held drill ½ inch drive and power corded


b) 1 inch diameter auger bit, 6 inch length
c) Template, 12 hole, (2x3x2x3x2)
d) extension cord
e) hair nets
f) lab coat
g) examination gloves
h) sanitizer
i) bucket
j) bulk sample bags, plastic
k) cooler with ice or freezer packs
h) flashlight
i) digital camera, min 5 megapixel
j) sampling report worksheet, notepad or notebook
k) tape

6.7.2 When sampling frozen beef trimmings for fat claim analysis, collect 1 lbs. samples by drilling
holes with a minimum 3/4 inch auger bit through a 12 hole-template placed on top of the block of frozen beef.
Use aseptic procedure. When available, collect samples from cartons that have been collected at random by the

25
FDA IOM Ch. 4: 4.3.6 through 4.3.6.1.4
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receiving warehouse and placed on a designated and labeled sample pallet. Sample that number of cartons that
represent 6% of the lot. Record the bar code from each box sampled and include the bar codes in the sample
collection report, FTS Form 4319. Composite the sample and place it in a package that will limit loss of
moisture. Label the sample with the FTS Job Number, PO Number or Lot Number. Hold and transport meat
sample to the laboratory at refrigerated temperature. This procedure is based on the North American Guidelines
for the Settlement of Fat Claims, March 15, 2012, of the Meat Importing Council of America, Inc. (MICA)26.

6.7.4 Whenever sampling meat, use aseptic technique. Samplers will wear lab coats or clothing free
from loose dirt and animal hairs; hair nets or ball caps or other appropriate head covering and examination
gloves. Collect samples in a clean environment. Sanitize the drill bit and work area as frequently as necessary.
After handling and opening boxes or after handling other non-sterile items, such as cell phones, change gloves!
It is critical that before contacting meat, examination tables or food handling equipment that you make sure that
a new pair of sterile gloves are worn.27 When finished sampling, clean and sanitize all sampling equipment and
the work area. Remove meat shavings, blood and other debris. Reseal cartons.

6.8 COCOA, COFFEE, SUGAR

6.8.1 Equipment List:

a) flashlight
b) coffee trier or cocoa trier
c) dust mask
d) sample seals
e) twine
f) sugar-sample jars and lids
g) black electrical tape for sealing jar
h) large plastic bag for compositing A& B sugar samples
i) razor knife for cutting sugar bags
j) 8.5 x 11 inch label-seal for sampled sugar bags
k) Styrofoam peanuts or bubble-wrap for packing and shipping sugar samples
l) preprinted sample labels, usually 10 per page format such as Avery 5963
m) digital camera, minimum 5 megapixels
n) sampling report worksheet, notepad or notebook
o) Sugar Sample Check List
p) Storage Labels for sugar samples “B” shipping carton
q) US Customs Form 6479, Laboratory Sample Label

26
MICA North American Guidelines for the Settlement of Fat Claims, Rev. March 15, 2012.
27
Title 9 CFR 416.4 - Sanitary operations. (a) All food-contact surfaces, including food-contact surfaces of utensils and equipment,
must be cleaned and sanitized as frequently as necessary to prevent the creation of insanitary conditions and the adulteration of
product.
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6.8.1 Collect cocoa and coffee NYBOT Exchange samples using a trier. Collect composite samples
from 20% of the bags in the chop when sampling lots for the first time and 25% when resampling.28 Label the
samples with the Chop Number, Exchange ID Number and when necessary, the Cargo Number. Coffee appeal
samples must have the word “APPEAL” written in read on the sample bag. Identify Exchange lots in the
warehouse by the chop number on the pallet tags attached to bags at the corners of the Chop. Use cargo
numbers and bag marks as a cross reference. Samples must be sealed and delivered to the Exchange. Collect
bulk samples of coffee or cocoa using a grain probe or vacuum sampler. Scrape weave of sacks with tip of trier
to close trier holes. Collect a counter-sample when collecting commercial non-Exchange samples. All cocoa and
coffee samples are composite samples. A representative of the warehouse and the sampler must sign 2 copies of
the sampling order. The sampler takes one copy. For coffee samples, place the signed order in the sample bag
before sealing the sample. Do not do this with cocoa samples. Deliver the signed cocoa orders separate from but
together with the samples.

6.8.2 Inspect cocoa and coffee bags for slack weight, wet stains, clumping, mold and webbing,
cocoons and live insects. When applicable, record and report exceptions and damage in the chop on the
sampling corresponding sampling order.

6.8.3 For sugar sampling, use a razor knife to cut an “X” into the flat area at the center of ten bags.
Each cross-cut should be about 4 inches in length, sufficient for collecting a sample but small enough that the
opening can be sealed with an 8.5 x 11” pressure sensitive label. There will be five sample sets as follows: For
each sample set, use a scoop to collect a one pound portion of sugar from each of two bags. Mix the portions
together in a large plastic bag. Transfer one pound of the blended portion into each of two sample jars. Label
one jar “A” and the other jar “B.” Repeat this process with the remaining eight opened bags so that there will be
five sets of samples collected from the ten bags. In addition to labeling the jars as A and B, also number the five
sets 1A through 5A and 1B through 5B. Wrap electrical tape around the base of the lid and jar, to attach the lid
to the jar. The tape will keep the lid from coming off and will act as a moisture barrier. Use bubble wrap or
Styrofoam peanuts when packing the jars for shipment, to prevent breakage spillage. The “A” set of samples is
sent to the U.S. Customs lab for testing. Be sure to include US Customs Form 6479 “Laboratory Sample Label”
with the samples sent to US Customs. Sample set B1 thru B5 is shipped to a storage warehouse, as directed, to
be held in reserve. There are four “Storage Labels” that will be placed on each side of the cartons used for the
“B” set of sugar samples, that includes the Entry Number, Job Number, Customer Name and Discard Date.
Complete the “Sugar Sample Check List” form and send it with copies of shipping Air Bill to the Houston
Office, preferably scanned and sent by email.

28
NYBOT Cocoa and Coffee Rules
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6.9 SPICES

6.9.1 Equipment:

a) flashlight
b) digital camera, minimum 5 megapixels
c) examination gloves
c) sampling report worksheet, notepad, notebook
d) trier
e) scoop
e) No. 4 paper bags
e) tape
f) Sharpie marking pen
g) brush to clean powdery spices from bags
h) dust mask

6.9.2 Collect samples of spices for ASTA cleanliness analysis (American Spice Trade Association,
Inc..29 In general, collect subsamples based on the square root of the Lot but not more than 10 subsamples.
Examine the outer packaging of edible seed and pulses for signs of rodent droppings, gnawing and insect
infestation. Sample sizes are as follows:

a) Collect ¾ to 1 Lb subsamples of high-density items using a trier: Black and White Pepper,
Cassia, Cinnamon, Nutmeg (whole or broken), Ginger, Cloves, Allspice/Pimento, Tumeric, CelerySeed, Poppy
Seed, Sesame Seed, Caraway Seed, Cardamom Seed, Anise Seed, Coriander Seed, Cumin Seed, Dill Seed and
Fennel Seed.
b) Collect ½ to ¾ Lb subsamples of low-density items using a gloved hand or scoop. Avoid causing
damage that could be mistaken for insect damage. Low-density items are Chillies, capsicums, Mace, Sage,
Oregano Leaves, Basil Leaves, Laurel Leaves, Thyme Leaves, Rosemary Leaves, Tarragon Leaves, Marjoram
Leaves and Savory Leaves.

6.9.3 When ground bulk-packed spices are packed in multiwall paper bags, cut a three-sided opening
in the top portion of the bag and fold it back. Frame the opening with plastic tape. Remove leafy samples
carefully by hand or with a scoop. Sample ground spices with a scoop. Avoid spilling the powdery ground spice
on the outer surface of the bag. Close the flap and brush off any powder that is on the outside of the taped frame
around the cut area. Tape the flap securely by placing plastic tape crosswise over the cut area and tape frame. If
a trier is used, seal the trier hole with tape or FTS trier-hole seals.

29
ASTA Cleanliness Specifications for Unprocessed Spices, Seeds and Herbs 2007
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6.10 FLOUR AND OTHER POWDERS

6.10.1 Equipment:

a) flashlight
b) digital camera, min 5 megapixel
c) sampling report worksheet, notepad, notebook
d) examination gloves
e) dust mask
f) trier
g) scoop
h) No. 2, 3 or 4 paper bags or twirl bags (Whirl-pack type)
i) tape
j) Sharpie marking pen
k) brush to clean powder from bags
l) knife or box cutter

6.10.2 Collect bulk-packaged samples using a scoop. When powders are packed in multiwall paper bags
cut a three-sided opening in the top portion of the bag and fold it back. Frame the opening with plastic tape.
Remove the sample carefully with a scoop. Avoid spilling powder on the outer surface of the bag. Close the flap
and brush off any powder that is on the outside of the taped frame around the cut area. Tape the flap securely by
placing plastic tape crosswise over the cut area and tape frame.

6.11 TREE NUTS AND DRIED FRUITS

6.11.1 Equipment:

a) flashlight
b) digital camera, minimum 5 megapixel
c) examination gloves
d) sampling report worksheet, notepad, notebook
e) cocoa trier
f) knife or box cutter
g) scoop
h) No. 2, 3, 4 paper bags; 5 or 10 lbs. lined paper bags; large 4 mil plastic bags
i) tape
j) Sharpie marking pen
k) stainless 12 inch No. 4 or No. 8 wire mesh sieve and pan
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l) plastic tote for sieve test (cashews)

6.11.1 Collect three portions for each subsample. Follow AFI or USDA-AMS sampling plans for grade
samples. Collect subsamples of approximately 500g each of tree nuts, but in the case of samples collected into
jars, the minimum portion should be approximately 250g. Collect composite samples of approximately 5.5 Kg
from each Lot or chop for dried fruits, except dates and figs. For dates and figs, collect approximately 2.5 lb
subsamples as specified by Lot size in the USDA-AMS sampling plan.

6.11.2 Collect core samples of dried fruits: Do not sample the top layer. Place dried fruit into moisture
barrier bags to retain properties for moisture and water activity tests.

6.11.3 Examine tree nut and dried fruit packaging for signs of insect infestation and report taints or
odors of fermenting fruit or rancid nuts.

6.12 GENERAL GUIDELINES FOR SAMPLING CASHEWS

6.12.1 Equipment List:

See 6.11.1

6.12.1 When applicable, record the packaging dates and codes that appear on the carton, tin, bulk-box
or package corresponding to each subsample. Examine the master cartons for evidence of infestation, rodent,
bird filth and other damage. Record the warehouse Lot number, container number, warehouse, Lot location,
quantity and grade, number of subsamples, number of pallets sampled, producer and shipping marks. Be sure to
sign and date the sampling report.

6.12.2 Occasionally, some packages are damaged in-transit. If not representative of the general
condition of the Lot, do not sample damaged cartons, but take photos. Do not sample previously opened
cartons.

6.12.3 Care must be taken to prevent damaging kernels when collecting, handling samples. Breakage
can occur to cashew splits, 450 count wholes and low moisture kernels from rough handling. Do not drop,
throw, or otherwise mishandle the samples.

6.12.4 Use a scoop to collect samples or draw by gloved-hand and collect three equal random portions
totaling approximately 500g for each subsample. Wear clean examination gloves when sampling by hand and
change gloves as frequently as necessary. Hold the fingers tightly closed in the form of a scoop. This will

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prevent pieces and other debris from falling back into the package. Do not squeeze the hand sample or collect
pieces resulting from the insertion of the hand.

6.12.5 When the quality appears to be uniform from package to package, a composite sample may be
collected. If a composite sample is collected, note that fact on the SCR.

6.12.6 Label each subsample or composite sample and corresponding sampled packaging unit with the
corresponding sample reference number, date, subsample number and sampler’s initials.

6.12.7 Collect samples for sensory analysis into clean glass jars.

6.12.8 Collect all other subsamples into No. 2 heavy weight paper bags or plastic jars. Collect
composite samples into double-wall paper bags or large 6mil plastic bags.

6.12.9 Seal samples and when necessary refrigerate until examined to avoid cross contamination by
insects.

6.12.10 Freeze all retention samples of cashews.

6.12.11 Determine the level of sampling intensity by the quality history of the producer or the Lot, the
origin, trends, market influences, complaints and current inspection data. Collect samples in accordance with
the AFI Sampling Plan (Figure 1.)

Lot Size – N AFI Sample Plan


(cartons) Normal (n) Intensive (2n)
≤ 50 3 6
51-350 6 12
351-1050 13 26
Bulk Boxes 6 12
Figure 1. Sampling Plan for Cashew Kernels

6.12.12 Cashew shipments often arrive as two more lots as determined by grade, loaded in the same
ocean container. If the Lot is from a single producer, treat the cartons in a mixed container as one Lot when
conducting the wharf examination. Follow the modified sampling plan (Figure 2.). The modified plan assumes
that,

a) The producer is packing kernels under insanitary conditions and the probability that any random
carton of cashews contains insect infestation is the same, regardless of grade.

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b) Cashew quality is less variable than infestation in the Lot, so a smaller sample size is sufficient
for determining grade.

MODIFIED AFI SAMPLING PLAN


LOT SIZE SAMPLE SAMPLE SAMPLE SAMPLE SAMPLE
by grade & SIZE (AFI) SIZE SIZE SIZE SIZE
packer 1 lot 2 lots 3 lots 4 lots ≥ 5 lots
Full Container 13
601 – 700 10 7
501 – 600 10 7 5
401 – 500 7 7 5 5
351 – 400 7 7 5 5
201 – 350 7 5 5 3
101 – 200 7 3 3 3
51 – 100 3 3 3 3
≤ 50 3 3 3 3
total sample 13 13-14 13-15 13 –14 ≥ 15
Figure 2. Modified AFI Sampling Plan for split-lot container loads.

Note: The default plan for all claims is the AFI intensive (2n) sample plan (Figure 1.).

6.12.13 Ship cashew samples to the grading lab in approved sample jars packed into specially designed
Foreign Trade Service™ shipping boxes consisting of Styrofoam molds inserted into 275 Lb. Test double wall
cartons. Label cartons “Fragile.”

6.12.14 Unless otherwise directed, ship samples by FedEx 2nd Day AM service. Send a copy of the
FedEx Airbill or pick-up record and tracking information to orders@ftslabs.com.

6.12.15 Send the original sampling report with the samples and send digital documentary photos to
orders@ftslabs.com.

6.12.16 When sampling locally in Newark, deliver the samples to the Newark office. Place the samples
on the receiving bench in the grading lab and present the sample-inspection reports to the Operations Manager
or person entering the data into the electronic Sample Log file.

6.13 EDIBLE SEED AND PULSES

6.13.1 Equipment List:

a) flashlight
b) digital camera, minimum 5 megapixels
c) examination gloves
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c) sampling report worksheet, notepad, notebook


d) trier
e) scoop
e) No. 2, 3 or 4 paper bags
e) tape
f) Sharpie marking pen

6.13.2 Collect 10 x 1 lb subsamples of edible seed and a 2.5 kg composite sample of pulses. Sample
from bags using a trier and from cartons using a gloved hand or scoop.

6.13.3 Examine the outer packaging of edible seed and pulses for signs of rodent droppings, gnawing
and insect infestation; report taints or odors of rancidity.

6.14 FRESH AND FROZEN PRODUCE

6.14.1 Equipment List

a) flashlight
b) digital camera, minimum 5 megapixels
c) examination gloves
d) sampling report worksheet, notepad, notebook
e) case hammer or carpenter hatchet
f) 1 inch box nails
g) scoop
h) No. 4 paper bags; No. 5 or 10 lbs lined paper bags; large 4 mil plastic bags
i) tape
j) Sharpie marking pen

6.14.2 Vegetables and Fruits may be fresh or frozen. Because fresh fruits and vegetables are perishable,
the sampler must expedite the sample collection and forwarding of samples to the laboratory. The sampler
should take special care to protect the integrity of the product when collecting the sample and when packing the
samples for shipment to the testing lab. Even if the samples do not require temperature control, the sampler
should pack the fresh produce samples in an insulated shipping carton. The insulated carton can add protection
during shipment to the testing lab. Make sure that there is no headspace between the samples and the top of the
shipping carton. Fill this headspace in with layers of bubble wrap to prevent the samples from moving around
during shipment and causing damage to the produce. If the produce is frozen, the sampler will pack the samples
in coolers or insulated cartons with frozen gel pack to maintain the temperature.

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6.15 PROCESSED PRODUCTS: CANNED, BOTTLED OR OTHERWISE PACKAGED FOR RETAIL

6.15.1 Equipment List

a) flashlight
b) digital camera, minimum 5 megapixels
c) examination gloves
d) sampling report worksheet, notepad, notebook
e) case hammer or carpenter hatchet
f) 1 inch box nails
g) tape
h) Sharpie marking pen
i) carton or tote for transporting samples

6.15.2 Sample one or more packages to represent each subsample so that there is sufficient weight of
product or ingredient to satisfy the amount of sample required for testing. Because dented cans are reported by
laboratories as a defect, avoid causing dents in canned products when sampling and shipping canned samples.
Restore the lot by backfilling from another master carton and use the empty master carton to transport the
samples. Make sure to note on the collection report that the empty master carton was used for that purpose.

6.16 FROZEN FISH, SEAFOOD AND OTHER FROZEN FOODS

6.16.1 Equipment List

a) flashlight
b) digital camera, minimum 5 megapixels
c) examination gloves
d) sampling report worksheet, notepad, notebook
e) large Coleman/Igloo-type coolers or Styrofoam insulated shipping cartons
f) coat for wearing in freezer/cold storage, hat and gloves
g) large serrated knife or saw
h) hammer, ice pick, chisel
i) large 3 or 4 mil plastic bags
j) chill packs or dry ice
k) strapping tape
l) tape
m) Sharpie marking pen

6.16.2 Pre-chill coolers used to transport samples. Whenever possible, collect intact packages or
packaged Individually Quick Frozen (IQF) portions as subsamples. When required, remove portions of bulk
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seafood or aseptically cut/saw and remove sections of whole fish. Keep samples in a frozen state and deliver or
ship the samples to the laboratory so that they arrive in a frozen state.

6.17 FRUIT CONCENTRATES AND OTHER LIQUIDS

6.17.1 Equipment List

a) flashlight
b) digital camera, minimum 5 megapixels
c) examination gloves
d) sampling report worksheet, notepad, notebook
e) large Coleman/Igloo-type coolers or Styrofoam insulated shipping cartons
f) drum thief, aseptic thief or sterile pipette
g) ladel
h) bung wrench
i) 2 pair of pliers, wrench, socket tool, flathead screwdriver
j) 500 or 1000ml leak-proof wide mouth bottles; twirl bags
k) lock ties/zip-ties
l) FTS drum seals for open head drums
m)chill packs or dry ice
n) strapping tape
o) tape
p) Sharpie marking pen
q) paper towels

6.17.2 Liquids cover a wide range of food products. Liquid products are shipped in retail and bulk
packaging and in ambient, refrigerated, and frozen temperature. Retail packaged product may be in plastic or
glass bottles or aseptic packages. When sampling retail packaged liquid products, first consider the product
temperature and packaging type. If the product is at ambient temperature and packaged in plastic bottles or an
aseptic pouch, no special steps need to be taken when packing the samples for shipment to laboratory. If the
product is in glass bottles, the sampler must individually wrap each sample bottle in bubble wrap to insure that
the bottle does not break during shipment to the testing lab. Whether you are dealing with ambient,
refrigerated, or frozen product and regardless of the packaging type, the sampler must always place the bottled
product into a leak-proof bag before packing for shipment to the testing lab. In the event of leakage during
shipment the liquid sample will be captured in the leak-proof bag. If the product is refrigerated or frozen, the
sampler must take steps to insure that the product retains its temperature until it reaches the testing lab.

6.17.3 There are various types of Bulk containers in which liquids are packed or contained; including,
drums, tanks, bladders, barrels and pails. Collection of samples from bulk containers presents many challenges.
Opening and resealing of the bulk container is the first thing the sampler must consider. Can the bulk container
be opened and be securely resealed after sampling? Some bulk containers are not designed to be re-sealable.
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This is because most bulk liquids are used to produce other products and bulk packages are designed for single
use and direct flow into processing systems from openings located underneath the bulk-package. Examples are
product packaged in bladders with in drums or in crates. There are some bladders are fitted with a bunghole or
cap that can be opened and re-sealed. However, when there is no bung or cap the only way to sample the
product is to cut the bladder open. DO NOT cut open a bladder unless there is written approval from the owner
of the product. A record of the written approval must be retained in the job file.

6.17.4 In order to cut open a bladder, the sampler must find a corner at the top of the bladder where
there is some free space and the bladder is easily separated from the liquid. The sampler should make a small
cut into the bladder at the designated corner. The size of the cut should only be large enough for the sterile
drum thief to enter and exit the bladder without touching the sides of the hole. After the sample has been
collected, the sampler must seal the bladder by using a plastic zip-tie to cinch the bladder together below the cut
at the top corner. The sampler will then place a sterile bag over the cut in the top corner and use a second
plastic zip-tie to cinch the bag closed around the cut.

6.17.5 When collecting samples of liquids from bulk containers, the sampler will use leak proof sample
bottles or Whirl-Pack bags for each sample. When collecting the sample, always leave some head space in the
top of the sample bottle or bag to allow the product to expand. If using a bottle or jar to contain the sample,
always place the sample bottle into a Whirl Pack bag to protect against leakage. Remove the head-space in the
bag by twirling or rolling and twist-tie the closure. Label the outer sample bag as well as the sample bottle.

6.17.6 The preferred tool for sampling liquids from a bulk container is an aseptic drum thief. Sampling
thiefs come in many different lengths and diameters. The sampler should always use a thief that is long enough
to reach the bottom of the bulk container. This allows a representative sample to be collected from the top,
middle, and bottom of the bulk container. When sampling a free flowing liquid the thief should be inserted into
the bulk container and the sampler should swirl the thief around in an effort to mix the product together, in the
event that there is separation in the product. After performing the mixing then the sample can be collected by
pulling the thief out and allowing the product to flow into the sample container. If the product is not free
flowing, it will not be possible to swirl to thief in order to mix the product. When product is not free flowing,
(such as thick honey or juice concentrate) it may be necessary to use an aseptic scoop or spoon to scrape the
product off the thief into the sample bottle. In cases where the liquid product is in a frozen state the sampler
will have to use a different sampling tool to collect the sample; i.e., an aseptic scoop or spoon and on occasion a
sterile knife may be used.

6.17.7 Fruit concentrates might be packed in open-head or tight-head drums with bungs; pails and bulk
aseptic packages or bladders. The product is usually held in freezer storage. The product should be thawed,
partially or completely prior to sampling.

6.17.8 Before opening the package for sampling, check the packaging for swelling indicative of gas
produced by fermentation. Drums under pressure from fermenting juice can explode when opened projecting
the bung cap or lid upward causing serious injury to the sampler.
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6.17.9 Separation of water and solids occurs when the product is frozen. Before drawing the sample,
use the thief as a stir rod and mix the product. Collect the sample into a leak-proof wide-mouth bottle using a
sterile drum thief. Allow headspace for gas expansion. Place the bottle in a Whirl-Pack™ type bag, twirl and
secure the wire closure. Keep the sample cool and re-freeze prior to transporting to the laboratory.

6.18 OILS AND LIQUID FATS AND SOLID FATS

6.18.1 Equipment List

a) flashlight
b) digital camera, minimum 5 megapixels
c) examination gloves
d) sampling report worksheet, notepad, notebook
e) electronic top-to-bottom tube mixer
f) drum thief, aseptic thief or sterile pipette
g) bailer or zone sampler
h) ladle
i) bung wrench
j) 2 pair of pliers, wrench, socket tool, flathead screwdriver
k) 500 or 1000ml leak-proof wide mouth bottles; twirl bags
l) lock ties/zip-ties
m)FTS drum seals for open head drums
n) chill packs and coolers when applicable
o) strapping tape
p) tape
q) Sharpie marking pen
r) paper towels
s) extension cord

6.18.2 Collect samples of oil and liquid fats from drums and tank cars using a core sampler that is long
enough to take a cross section of the entire depth. When sampling from deep storage tanks, use a bailer or zone
sampler with sufficient chain length.

6.18.3 Liquefy milk fat by heating with SpaceKraft Bins using the SpaceKraft heating element. Heat
bin for approximately 50 hours.

6.18.4 Homogenize the heated liquid milk fat by inserting a pre-cleaned and sanitized electronic Top-
to-Bottom Tube Mixer through a standard 2” bung and mix for 1 hour.

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6.18.5 Remove the mixer and immediately insert a pre-cleaned and sanitized Coliwasa-Composite
Liquid Sampler through the bung hole and collect an aseptic 250 – 300 ml core sample. Collect sample into
Whirl-Pack® bag.

6.18.6 Replace bung plug and affix tamper evident seal indicating product was sampled.

6.18.7 Prepare sample collection field report and note any off-odors coming from the product or other
observations that might affect the integrity of the sample.

6.18.8 Place samples in Styrofoam insulated shipping cartons with chill packs or dry ice as directed.

6.18.9 Seal cartons with tape and place tamper evident seals across tape on top and bottom of shipping
cartons.

6.18.10 Maintain custody of samples and hand-deliver to courier service for overnight shipment. If dry
ice is used, samples must be shipped via FedEx.

6.19 MEALS AND GRAINS

6.19.1 Equipment List

a) flashlight
b) digital camera, minimum 5 megapixels
c) examination gloves
d) sampling report worksheet, notepad, notebook
e) scoop
f) tape
g) Sharpie marking pen
h) safety vest
i) trier
j) partitioned or open handle grain probe, 3.5, 4, 8, 10 or 12 foot length
k) canvas sampling cloth at least as long as the partitioned probe probe
l) cotton draw string or paper sample bags or other suitable containers for collecting the sample into
m) FTS seals for resealing of hatches on rail cars and other bulk containers
n) ladder
o) bucket
p) bolt Cutters
q) safety Harness
r) safety Glasses
s) hard Hat
t) safety Lanyard
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u) steel-toed shoes

6.19.2 Meals and grain products can be found in many types of packaging and storage systems; such as,
retail packages, corrugated bulk boxes, poly woven super sacks, jute bags, multi-wall paper bags, bulk trailer,
hopper bottom trailer, inter-modal bulk shipping containers, silos, bins, barges and railroad cars. Special
techniques and tools will be required to collect samples from these various bulk storage and packaging systems.

6.19.3 Retail Packaging: When collecting samples of meal or grain product in retail packages the entire
retail package will usually be collected. Exception: when sampling basmati rice you should follow the FDA
Guideline for Sampling Basmati Rice.

6.19.4 Bulk Packaging: When sampling from rail cars and trucks there should be another sampler or
warehouse person present as a safety precaution. When sampling from bulk packages the sampler will need to
use the appropriate sampling tool and safety equipment for the specific package type. The sampler must also
collect stratified samples from various zones within the bulk package; for example, sampling from top, middle,
and bottom of the storage unit using a partitioned grain probe or an open handle grain probe. A partitioned grain
probe is used when collecting subsamples from the various zones. Standard procedures also require that the
sampler collect probes from a least five different sites in large bulk bins or hoppers, hopper trucks, barges or rail
cars. The sampler must include in the Sample Collection Report a sketch of the position of the sites probed and
sampled in the bulk container.

6.20 (Reserved)

6.21 SAMPLING FOR TAINTS, HEAVY METALS, PESTICIDES AND OTHER RESIDUE TESTS

6.21.1 Equipment List

a) flashlight
b) digital camera, minimum 5 megapixel
c) examination gloves
d) sampling report worksheet, notepad, notebook
e) knife or box cutter
f) Mason jars
g) metalized sample bags
h) plastic bags, 3-4 mil

6.21.2 Because compounds present in plastic jars, plastic and paper bags, might be the same or mimic
the residue responsible for a taint or for which the sample will be tested, special sample containers will be used.
For taints, collect samples into Mason or Ball jars. For pesticides, economic adulterants, and other residues,
collect samples into metalized bags. For heavy metals analysis, use plastic bags.

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6.21.3 Use preprinted adhesive labels to identify samples collected for taints, heavy metals, pesticide
residues and other residues.

6.22 SAMPLING FOODS AND MEDICAL DEVICES DETAINED BY FDA

6.22.1 Basic Equipment List:

a) flashlight
b) digital camera, minimum 5 megapixel
c) examination gloves
d) lab coat
e) hair net
d) sampling report worksheet, notepad, notebook
e) knife or box cutter
f) tape
g) tamper evident seals
h) sterile sample bags, jars, metalized bags, paper bags
i) sterile scoops, sterile drum thief
j) trier or probe
k) 12 inch diameter No. 4 or No. 8 wire mesh sieve and pan
l) sanitizer spray or alcohol
m) coolers

For additional equipment, refer to the specific equipment lists for the various sampling protocols and food types
listed in this SOP.

6.22.2 The sampler is responsible for collecting samples according to the assigned sampling plan and
will follow one or more of the procedures and techniques contained in this SOP, relevant ISO Procedures or
other official procedures (FDA, USDA). The FDA Investigations Operations Manual advises that

“Your training and experience will enable you to become proficient in most sampling operations.
However, in new or unusual situations it is your responsibility to use imagination and ingenuity in getting the
job done and, if necessary, to consult with your supervisor.”30

30
FDA-IOM Ch. 4, 4.3.1 - Responsibility
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6.22.3 The sampler will complete the Sample Collection Report (SCR) worksheet at the time that
samples are collected and will enter information for every item in the report.

6.22.4 Label the subsamples or sample with the Entry Number, Line Item Number, date of the
sampling, the sub-sample number and the hand written initials of the person performing the sampling31.
Counter-label the package from which the sample is collected with the same information that appears on the
corresponding sample label.

6.22.5 Take documentary digital photos of a pallet-load of product from the sampled Lot. Photograph
each side of one package and of one or more of the subsamples. When practical, take photos that document any
relevant exceptions or conditions of package integrity or storage conditions. Record such exceptions in the
Notes and Observations pages of the SCR.

6.22.6 When making a correction to the SCR, draw a single line through that information which is
incorrect, enter the correction above or near the error, date and initial the correction. Only the sampler may
correct the SCR.

6.22.7 Samples are to be packaged and sealed. Hand-deliver or ship the samples to the private
laboratory that will be testing the samples. Maintain a clear chain of custody and obtain proof of delivery if
hand-delivered or retain a copy of the Airbill with tracking information. In some cases, the laboratory may send
a representative to take custody of the samples directly from the sampler or sampling office.

6.22.8 Prepare a shipping Airbill when forwarding samples by FedEx or another courier service. The
Airbill must include a sample reference number and billing reference.

6.22.9 Copies of the completed SCR, digital photos, and shipping Airbills are sent as soon as possible to
Sampling Operations Manager by email. The original SCR and exhibits are sent directly to the laboratory with
the samples.

6.22.10 Some of the information contained in the SCR worksheet may be entered in advance; such as,
Lot identification information taken from the U.S. Customs Entry documents and the FDA Notice of Action.
The sampler will use the pre-entered Lot identification information in the SCR worksheet, warehouse records
and other available documents to identify that the Lot presented for sampling is the correct Lot. At the same
time, the Lot identification information is used to verify that the Lot being sampled is the Lot described in the
US Customs Entry, Commercial Invoice, Packing List and FDA Notice of Detention.

6.22.11 Even though there may be some pre-entered Lot identification information in the SCR, there
will be additional information that must be entered by the sampler at the time of sampling and inspection:

31
FDA- IOM Ch. 4: 4.5.2.1
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a) brand name of the product as it appears on the package label


b) labeled size or the net weight as it appears on the package label
c) product codes, carton numbers, date codes, production and expiration dates, batch or lot codes

Note: If there is no product code, the sampler must write NONE in the space for product code.

d) actual quantity present at the time of sampling verified by count or warehouse inventory report.
e) warehouse or freezer lot number as it appears on the Lot

Note: If there is no warehouse lot number, write NONE in the space for warehouse/freezer lot number.

f) Notes and Observations of exceptions, insanitation, storage, damaged packaging, shortages and other
conditions that might affect the integrity and safety of the food and Lot samples.
g) Date of sampling
h) Name and signature of the sampler must appear on all pages completed by the sampler.

6.22.12 Make copies of the SCR. Send the original SCR with the samples and send the copy to the
Sampling Operations Manager for retention in the job file.

6.22.13 Sampler will label the samples and sampled packages by hand or by use of printed labels. There
are certain types of packages and conditions, such as a frozen product, where it is difficult to place an adhesive
label on the samples or packages. In that case, label a tag and tie it on the package or otherwise affix the label
tag to the package or bulk container. The subsample number on the label must link the subsample to the
package from which the subsample is collected32.

6.22.14 Precautions:
a) DO NOT USE magic markers, etc. to identify subsample bags, because compounds in the ink may
affect the test results. Use stick on labels to identify subsample bags and similar sample containers. Collect
samples in the container in which the dealer is packaging the product. If the dealer is packaging the product in
plastic bags, collect sample in these bags. If the firm is not packing the product, collect the samples in paper
bags, cardboard cartons, etc. Do not use plastic bags as this may interfere with the analysis, unless the bags are
certified as contaminant free.
b) Detention samples must be delivered as promptly as possible to the laboratory if regulatory action is
to be taken against actionable lots.
c) Hold samples in cold storage until ready to be shipped or delivered to the laboratory. If the sample is
of semi-perishable fruit or vegetable (such as apples, pears, butternut squash), and is shipped for overnight
delivery, it can be shipped to the laboratory unrefrigerated; provided that, the receiving laboratory is advised to
refrigerate the samples on receipt.

32
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d) Use aseptic technique, where applicable, when collecting samples of finished products from bulk
containers.

6.23 DIGITAL DOCUMENTARY PHOTOS

6.23.1 Equipment List:

a) Digital camera, minimum 5 megapixels


b) sampling report worksheet, notebook or notepad
c) Sharpie marker and pen

6.23.2 Photos are documentary samples (DOC) or exhibits33. Photos are an important part of the
sampling and inspection procedure. There must be a set of photos for each Line Item and each size or lot code
of product sampled for analysis. There are often different sizes of packaged shrimp that will be sampled and
recorded in the SCR, and there must be a set of photos for each size. Typically, there are four to five different
photos in a documentary photo set for a product on detention. Examples of these photos are as follows:

a) a full pallet of product (Figure 1. Photo 1)


b) one side of a master carton (Figure 1. Photo 2)
c) end of the master carton (Figure 1. Photo 3)
d) a sample collected from the Lot (Figure 1. Photo 4)

Note: When photographing an example of the sample, it is best to photograph the sample together with the open
package from which the sample was collected.

6.23.3 Use a digital camera that has a minimum capability of five megapixels. Take photos of each
subject in triplicate to ensure that at least one shot will be clear and useable. Although convenient, do not use a
cell phone camera, as they do not always produce acceptable photos when enlarged for reports. Review the
photos in your digital camera’s photo viewer to ensure they are sharp, not blurry. You must stand close enough
to what you are photographing so that the subject nearly fills the frame. You must remove all plastic shrink-
wrap or stretch-wrap from the pallet you are photographing to prevent glare and whiteout caused by the
warehouse lights or camera flash.

33
FDA-IOM Ch. 4: 4.5.2.4
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Photo # 1 Photo # 2

Photo # 3 Photo # 4

Figure 1. Example of documentary photos to be included in a SCR.

Note: In this example, there is only one side-view photo. The second side identically marked and not needed. Notice also,
that these pictures are of large size examination gloves. If there were other size gloves, there would be a set of similar
photos for each size.

6.23.4 Photograph insects, rodent droppings, gnawed packaging, and wet stains, visible mold, bird
droppings and feathers, dead animals, holes in the warehouse roof above the Lot, and any other damage,
exceptions or evidence of insanitation. When possible, draw circles or arrows to indicate the location of the
subject of the photograph, on or in the packaging and collect specimens as exhibits. Number the exhibits in the
same manner as subsamples so that the exhibits correspond to the photo documenting the condition reported in
the SCR Notes and Observations.

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6.24 WHARF EXAMINATION OF PACKAGE CONTENTS FOR FOREIGN MATTER

6.24.1 Equipment List:

a) flashlight
b) digital camera, minimum 5 megapixel
c) examination gloves
d) sampling report worksheet, notepad, notebook
e) knife or box cutter
f) scoop
g) No. 2, 3, 4 paper bags; 5 or 10 lbs. lined paper bags; large 4 mil plastic bags
h) jars, vials or similar containers for collecting insects, rodent dropping and other foreign matter
i) tape
j) twine and bag needle
k) Sharpie marking pen
l) stainless 12 inch No. 4 or No. 8 wire mesh sieve and pan
m) large plastic tote for whole bag-whole package screening (sieve test).
n) partitioned or open handle grain probe or trier

6.24.2 The “Wharf Exam” is a screening or sieve exam of nuts, beans, large seeds and similar free
flowing low-moisture foods. Select cartons, bags or other packaging units for sampling as randomly as possible.
A Sample Pallet with randomly selected cartons prepared at the time of unloading by the warehouse serves as a
random sample. Otherwise, and when the entire lot is not available, request that the warehouse position a
representative set of 3-6 pallets for sampling. For safety purposes, the sample pallets should be away from
forklift operations. Collect live insects and other foreign matter found in the sampling. Place the specimens in
sealed containers when required or destroy and discard them to prevent contamination of warehouse spaces.

6.24.3 When screening cashews, open one tin or flexible package from each sample carton.

6.24.4 Storage pest insects exhibit geotaxis, in that they occupy different strata in a bulk container
depending on the species. Most pests can be found in the first few inches of the top layer, but some seek the
moist warmer core of the load. Use an open handle or partitioned grain probe when examining Gaylord-type
bulk boxes, super sacks or other bulk containers. Probe five times, once in the center and one foot from each
corner. Otherwise, collect the sample by gloved-hand or scoop directly from five sites below and within the top
layer.

6.24.5 Empty the entire contents of 25 Lbs. Net Wt. tins or flexible cashew package into a large
sanitized plastic or stainless steel tote. When conducting a non-FDA related wharf exam and packages are 50-
100 Lbs. Net Wt., screen at least half, but not necessarily the entire contents of the package. For bulk product in

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large jute or woven plastic bags, probe the bag in 5 locations with a trier and screen the combined sample
portions. Do not screen powders or similar fine material.

6.24.6 Thoroughly mix samples in a tote that have been emptied from packages into the tote. Debris and
insects will gravitate to the bottom of the tote during mixing. If the entire contents of the tote are not to be
screened, return the top portion from the tub to the original package. Pass the debris-containing bottom layer of
the tote (about 1 or 2 kilos) over a mechanical rocker-type or hand-held, 12in diameter, U.S. Number 4 or
Number 8 sieve and pan.

6.24.7 When working in a processing facility, wear clean powder-free examination gloves, lab coat and
hairnet or hat. Depending on the sample type, subsamples are collected from the tote using a sterile or sanitized
scoop or gloved hand. Each subsample should consist of three random portions and weigh a total of between
250g and 500g.

6.24.8 Examine the debris retained in the pan for insects, insect filth and other foreign matter. Collect
specimens into the appropriate container when required.

6.24.9 Record observations in the sample collection report. Findings must correspond with the
subsample numbers on the sample and sampled package. Itemize the number and type of insect (beetles,
caterpillars/larvae or moths) and note the presence of webbing, frass, and tunneling. Describe insects as live or
dead and by species, if known; quantify rodent droppings and bird feathers; describe by type and dimension any
other foreign matter especially hard or sharp objects. Record all findings on the report as specifically as
possible. Number the sample containers of specimens to correspond with the subsample number and job
number.

6.24.10 Describe the contents of a package unit as "critically infested,” when the degree of insects and
insect damage is so great that it is too numerous to quantify and the product appears to be unsalvageable.

Note: The Wharf Examination procedure is a modification of USDA-AMS 172-A and FDA Wharf
Examination.34

6.25 EXHIBITS

6.25.1 Collect package labels as exhibits when appropriate. Always collect 3 labels as exhibits. Do not
remove labels from bulk containers35.

34
FDA IOM Ch. 4: Sampling Schedule 8
35
FDA IOM Ch 4: 4.4.9.2
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6.25.2 Collect specimens of insects, rodent dropping and other filth into vials and label as exhibits.
When it is necessary to identify unknown insects or material removed in wharf examinations, collect the
material into sealed containers and label as exhibits.

6.26 PACKAGING, TRANSPORT, SHIPMENT AND DELIVERY OF SAMPLES

6.26.1 A sample must be in a controlled environment. If the sample was collected in ambient storage
and it is not for microbiological tests, it can be held and transported at ambient temperature. If the sample was
collected from a product that was chilled or frozen, it must be packaged so that it will remain in a chilled or
frozen state during transport and shipping. Pre-chill coolers used to contain samples36. Pack frozen samples
according to FDA guidelines and ship frozen samples by overnight courier37. If frozen samples cannot be
shipped the same day, store the samples in a freezer until such time as they can be shipped. Samples from
products held in ambient storage that are collected for microbiological tests should be chilled. Samples that will
be tested for moisture or water activity should be collected in Whirl-Pack™ type bags or jars with a minimum
of headspace. When sampling certain foods from bulk packaging for organoleptic examination, place samples in
glass jars to prevent taints from other sources38.

6.26.2 Use bubble wrap or packing peanuts to protect all fragile samples and to minimize free space and
movement during shipment. For liquid samples collected in glass or plastic leak-proof bottles, place each bottle
or jar into a Whirl-Pack™ bag and twirl closed so that any liquid that might leak will be contained. For fruit
concentrates and other sugary foods that ferment, allow headspace for gas expansion.

6.26.3 After securing the shipping carton with tape, place tamper-evident seals across the top and
bottom flaps of the shipping carton. Record the seal numbers.

6.26.4 All packages of samples will be shipped by FedEx Priority Overnight or UPS Next Day Air.
Frozen products require special handling and labeling. All frozen products are shipped in insulated shipping
cartons. When samples are shipped with dry ice, a Hazardous Material (HAZMAT) Label for Dry Ice must be
placed on the outside of the shipping cartons on two sides. This label will list the shipper and the receiver and
the amount of dry ice in the carton. The HAZMAT label is an FAA regulation and must be on the carton.
Samples shipped with dry ice will be shipped via FedEx Priority Overnight.

6.26.5 When filling out the Airbill some items are very important. On each air bill a box or line offers a
space to enter a billing reference number. This number is important for it helps to establish the continuing chain
of custody by identifying the sample that was shipped. It also aids in tracking the shipment and accounting for
the shipping charges for a specific job. The sampler must not forget to write this number in. The second item
identifies whether or not the package contains DRY-ICE. If the package contains dry ice, this must be indicated
on the Airbill and the package MUST be labeled with the HAZMAT label. The third important item is the
36
FDA IOM Ch.4: 4.5.3.5
37
FDA IOM Ch 4: 4.5.3.5.1
38
FDA IOM Ch. 4: 4.3.9
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“Account billed to” information. Unless instructed otherwise, ship all samples using the third-party shipping
account number of the lab or client.

Figure 2. An example of a FedEx Airbill.

6.26.6 The customer or shipper’s copy of an Airbill and the tracking history of Airbill number and
receipt of the package by the laboratory, document a clear chain of custody of the samples from the sampler to
the laboratory. It is essential that a copy of the receipt is kept on file.

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Revision History

Date Revision Number Revised By Reason for Revision


08/01/12 0
Original

Jeffrey Abels
11/27/12 1 Internal audit 11/15/12-change to 6.5.1 to
add “clothing free from loose dirt and
animal hairs” and “ball caps.” Correction
Jeffrey Abels to reference for Wharf Exam from section
6.24 to 6.20. Change to 6.3.1 to allow for
certain frozen products to be transported or
shipped without additional ice, dry ice or
chill packs.
12/14/12 2 Added collection of samples with a trier or
scoop, ground spices, exam for infestation,
to Section 6.9.3; 6.15.2 revision to dented
can and backfill procedure; 6.23.2
Jeffrey Abels clarification to photos of sizes and lot
codes products such as shrimp
6/24/13 3 Revision to Sec. 1.1 to include requirement
to have access to SPO in field. Change in
order and numbering of Sections 6.20,
Jeffrey Abels 6.24-6.26. Revision to Sec. 6.22.2
“Responsibility” clause.

Copyright 2013 Foreign Trade Service Corp.

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