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PETRON INDUSTRIES INC.

CALCIMETER

5921 THOMAS FOAD . PO. BOX 41166 . HOUSTON, TX 772411166

[713] 937-7982 FAX [713] 937-884s
-Fd' '*r'
 Petron Automatic Calcimeter
Operation Work Instruction .

.
1.0 Scope
This work üNtruction defines the steps to operating the caicimeter to detérmine the
pe¡centage of caicium carbonate (CaCO3) and dolomite ifl the formation sample.

2,0 Parts and Tools Checklist

2 .1 Calcimeter:

. Peton automatic calcimeter with plexiglass reaction cell

. Sample delivery spoon
. Magnetic spinbar

2.2 Accessories:

. A¡alytical balance
. Morta¡ and pestle
'. Spatula
Vacuum grcase
. Weigh paper
. Hydrochloric acid, (.I0%\, reagent grade, labo¡atory staüdard
. Calcium Carbona¡e, reagent grade, labor¿tory standard
. Graduated cylinder (10 ml), or other liquid measuring device

3.0 Description
The pa¡ts listed above a¡e used as foilows:

Plexiglass rcaction cell with top O-dng Vessel that holds the HCL and sample
du ng the reaction; ¡etai¡s intemal
prcssu¡e.

A¡alytical electronic baiance Accu¡ately weighs the requircd amount

of sample.

Sample spoon Hoids the 0.5 g¡am CaCO3 sample.

Magnetic spinbar Agitates the HCL and sample to ensure

sample reaction.

Pd.on l¡dnfria I¡.. I Hoút n,'faa I l7l3) 971-1942

Calcimclcr Opentions !Vo.k lr$ruction
 Mortar and pestle Used to g¡ind the fo¡mation sample
into a powder.

Spatula Used to t¡ar(fer po\rdered sample to

the sample delivery spoon on the
electronic balance for weighing.

Vacuum grcase Lubricates the O rings and screw

threads on the rcaction cell and the
plexiglass fixturc maintai¡ed on the
front of the calcimeter.

Weigh paper Keeps the sample powder off the

electronic balanae.

Hydroclioric acid Acid ¡eagent that reacts with calcium

ca¡bo0ate (CaCOr) and dolomite
(CaMg(CO3)t.

Gmduated cylinder Used to measurc the amount of HCL.

(or other Liquid measuring device)

Petbn ¡ndüírié lft. / Húürlor, Tds / (?ll) 93?-7942

c¡lciñétd opéúlioft work lrul¡tction
4_0 Operating Work Instructions
Arrange a work area so that the elecfonic balance, autornatic aalcirnete¡, and
measümg rools and devices are comfonably .¡rua¡ed ¡D close pro\imiry.

Note: Peíorm at q stable and constanf room temperoture; ensure that fhis
is the calíbration femperature thaf will be maíntained d.urtng the
oPeratíon.

1.1 Sample Preparution

4.1.1 Use only thoroughly washed and dried cuttings samples. Turn the
switch on the back of the calcimete¡ to the ON position. Ensule that
the 3-way switch on the front palel is in the STOP position. Warm
up fo¡ approximately one hour and verify the caiibration (see the
Calibration P¡ocedure).

4.1.2 G¡iDd the cuttings sample to a fine powde¡ ar leasr 100 mesh with
the morta¡ and pestle.

Note: me r)olume in fhe sample deliyery spoon ís detemin¿d lry

fhe densíty of the sample. A lower density lrould J)íeld
morc volune than a higher densiry.

1.2 Equipment and Process Preparation

4.2.r Lubdcate üe O-rings atrd sc¡ew th¡eads on the reaction cell and
fixture with a light coating of vacuum g¡ease pe¡iodically. Veriry
that the O-¡ing seals and prcssu¡e connections are in good
condition. Check fo¡ dirt or debris on the threads and O-rings
which might prevent a good seal.

Place a weigh pape¡ on the electronic baiance to keep any sample

powder off the balance.

Place the sample delivery spool in the center of the weighing

paper. Close the lid to the elect¡onic balalce, Tare o¡ set the scale
to ze¡o to accuÉtely measu¡e only the weighi of the sample.

4.2.4 With the spatula transfe¡ exactly 0.5 g¡ams of sampie into the
sample delivery spoon on the electronic balance.

Pcton Indnr¡i6 rbc, / Housbn, fexa I Ql]) 937-1942

Cálcincl¿. Op€rálións Wo.k Iútnction
800002 Reeüion 0
 4.2.5 Place the loaded sample delivery spoon itr position in the
calcimeter. Keep the spoon in a horizontal position.

A. Hook the sample delivery spoon with the ú,eighed sample to

the hanger on the plexiglass reaction cell fixture that is
attached to the calcimeter, holding the spoon in place against
the electromagnet.

Note: To prevent losíng patl of the sample, hold the sample

delívery spoon snugry agaínst the electromagnet
\)híle settíng the three wqy sa¡tch on the front of the
calcimeter to the LOAD posíÍion.

B. Put the 3-way switch into LOAD positiol to activare rhe

elecÍomagnet to hold the sample delivery spoon in place.

4.2.6 Prepa¡e the reaction cell.

A. First, place the magnetic spinbar into the plexiglass reactio¡r

cel¡.

B. Then measure 10 rnl of HCL (10%) into a graduated cylinder.

Tra¡sfer the HCL to the reaction cell.

Zero the calcimete¡'s digital display usi¡g the SIGNAI ZERO

potentiometer on the front of the calcimete¡.

Note: This is scaled lfom zero to 100% and is wry sensitiye and
somewhat dílrtcuh fo set directb) on zero (0.0%).
Consíder the calc¡meter zeroed íf the display ís 0.0%,
+ /- 0.1%. If the dígita.l displÍy shows .¿ seies oÍ asterisks
(+**) the pressure values are out oÍ range for the sÍ p
chart to record

P.Lon Indürn6Inc. / Hoüsbn,lda I Q13) 1-19&2

Calcimcl¿rOpc.atio rvo.k¡rutnction
8000072 Resion 0 4
 4.2.8 Ensure that the pressurc ¡elief valve on top of the ¡eaction cell
fixture is i[ the closed position (turn clockwise, fj¡ge¡ tight)

4.2 9 Sc¡ew the plexiglass ¡eaction cell to the fixtu¡e,bn the calcimete¡.
Tighren (nugly.

A. Ihe pressure i¡ lhe reacrion cell \ ill rise immediarely as úe

reaction cell is tighteried. This is ¡eflected on the digital
display. If this does not occur the¡e is a pressure leak.

B. Bleed the pressu¡e off by opening the p¡essure ¡elief valve on

top of the plexiglass fixtu¡e until the digital display retums to
zero. Keep the vaive open until the pressurc is fully released.
The display will ¡etum to zero.

C. Close the prcssu¡e relief valve (turn clockwise. linger tight).

4.2.t0 Pull the stirrer drawer open to its first stop position. This places rhe
electromagnetic mixer in the drawe¡ underneath ¡he ¡eaction cell.
Now perform these steps:

A. Tum the ROTATION SPEED knob tully open in a clockwise

direction. This brings the acid swirl as high as possible in the
reaction cell aDd ¡emoves any sample stickiüg to the sides of
üe cell when it is dropped to the acid.

B. When *te rotation speed is stabie, lelease the pressu¡e by

opening the prcssu¡e relief vaive one last time so that the
digitai display reads zero.

C. Close the prcssu¡e relief valve (turn clockwise, finger tight).

4.2.1t Feed the stdp chart to the closest heavie¡ solid line using the FEED
button on the recorde¡. This is the minute ma¡k line. They are one
minute apaf at a st¡ip chart speed of 600 mm/hr.

Pélron Indút.i6 Inc, / Horsto¡ ,'lex6 I Qt3) 931t9az

C¡l.iñetd Ope.ltions Work hstrudior
 4.3 Operation for Detemining the CaCO3 Percentage in the sample

4.3.1, Quickly tum the 3-way switch to rhe RIJN position without pausing
between switch seiections. This starts the stdp chart ¡gcording and
releases the sample into the acid. The time and chalt speed will be
prinred ro identill each sample run.

Note: onl! v)hen the 3-way s,,\)itch

The pen on the sfr¡p chaft operates
is ín the RUN mode. Hdrever, the díBital dispkt¡ and bar
g rap h .tlw6J s fanctí on.

Note: When testíng several samples, verify that the RUN sv,üch is
,umed oÍ between samples ín order to consene paper.

As the sample is ¡eleased into the IICL, the pressurc rises quickly and
i¡Dmediately if CaCO, is prcsent. The st¡ip chart pen begins to ¡ecord the
prcssu¡e rise. The p¡essurc dse should pe¿k and level out within tfuee
(3) minutes unless the acid is very cold.

4.3.3 After tfuee (3) minutes record the value shown otr the display. Record
this value as the CaCO3 percentage that will be plotted on the Maste¡
Log.

Observe tlrc chart rccord after flfteen (15) miDutes to dete¡mine the
dolomite pe¡centage. Dolomite reacts much later than CaCO,.

A. If doiomite is prese , you will first notice the C¿CO3 pressure úse.
The ¡eaction will rcmain level fo¡ seve¡al minutes before another
pressure increase occu¡s. The second increase is the dolomite
reaction. Run for approximately 15 minutes or until ¡he pressu¡e
stops incrcasing and becomes level.

B. Record both the CaCO3 and dolomite pressure levels. Subtract the
CaCO3 value from the totai p¡essure level. The remairing value is
the dolomite pe¡centage in üat sample.

.1.3.5 Bleed the pressure from the reaction ceil fixturc.

CAUTION: Pos¡tíon lourself so that pressure ís released AWAv from

lou to prevent acil from contacting Jour eles qnd skin-
4.3.6 Turn the 3-way switch to STOP. This prcvents the strip chan f¡om
ope¡ating.

Pct on l nsLi6 lrc. / Houston , "t¿w I 1117) 931 fin

C'l.inelr Opédttons wo¡k Instdclion
 4.3.7 Tum the ¡otatiol speed knob fully counterciockwise to srop rhe stirring
¡ctioÍ.

4.3.8 Push in the stirrer drawer by rcleasitrg the rctaini¡g lbck on the right
side of the dmwer.

4.3.9 Remove the reactiotr cell. Notice that a vacuum (a negative display
measurement) is crcated if the prcssure rclief valve is closed.

4.3.10 Dismaltle, ciean, and d¡y the equipment between samples. Clean üe
attached reaction fixtüe with a damp cloth or paper towel.

P€ttunlddust.i6In., / Hoston. T*a / O13) 937-?932

CBlcim.é. Opemdons work Lshrctior
¡1m0072 ReYbidr 0
 4.1 Troubleshooting

4.4.I Pressure leaks

A. Pressure leaks arc the grcatest source of prcblems. Inspect the

reaction cylinde¡, O-rings, seals, and prcssure rciief valve; ¡eplace
when necessary. Keep the O-rings and threads otr the feaction
chamber cleaned out and lightly lubdcated with vacuum grease.

B. Test fo¡ leaks by prcssuriDg with a test sample. Let the illstrumeút
stánd for approximately an hour. The reading will decrease if a
Prcssure leak exists.

4.4.2 Degmded peribmance or lack of agreement with calibntion curve

A. Ensu¡e that acid, sample, and machine have had time to stabilize to
room tempeÉturc. Dete¡mine whethe¡ the¡e have been any changes
in room temperan¡re since calib¡ation.

B. Verify the balance calibmtion. EDsu¡e that the balance is clean and
frce of corrosion on weights and pa¡s if a non-elecüonic balatrce is
used. Shield the balance fiom aiI cuÍents and vib¡ation.

C. Check the reactiol cell for contaminants. Ensure that the cell is
clean and dry.

D. Vedfy that the complete sampie is quicldy satu¡ated i¡ the acid with
none sticking to the sides of the reaction cell or sample delivery
spoon.

E. Check for impuIities in reagents. Moisnrre in the sample standard

will introd[ce error.

F. Check lhe recorder lbr normal function. Refer to rhe recorder

manual if a problem is encountered.

P.tron lndnstid lrc. / Ilouslon. Texx I (713) 937'7942

Cslcincie. Opd¡lioG Work Imtruction
Revision 0
 4.5. Strip Chart Setup

,1.5.1 The st¡ip chart has been p¡eset at the factory and shonld not rcqufe
adjusting u¡der normal ci¡cumstances. DO NOI attel¡lpt to adjust uriless
you are sure the p¡oblem is in the reco¡de¡ and you,have checked out
absolutely every other function.

4.5.2 Strip Chart Adjustments

A. The cursor keys for navigatitrg the setup are the buftons with blue
labeling above.

B. The blinkirg item or the digital display shows the item thar may be
set. Cycle though the stdp cha¡t setup selections with the blue up
and down cursor ar¡ows. Pless the ENTER button on the fa¡ ¡ight
(with the arow) to select an item.

C. The¡e a¡e two modes iII setti¡g the strip chart for the caicimeler--
the SET mode and the SETUP mode.

(1) To ente¡ the SETUP mode, tum the power to the OFF
position.

(2) Hold the ENTER button down while turning the power to rhe
ON position.

rJl fo enter rhe StT mode. press Lhe menu ISC buÍon rnd holJ
tor approximately t¡ree (3) seconds until the display reads
SET. The c¡itical ship chaft setup items for operating the
calcimeter are:

. The SETIIP mode

* SETIJP : REM
X SETUP: RCD
* SETLTP = END

. The SET mode

+ SET = RANGE

Pelronhdlstn6 I¡c. / Houton, fdú I Q13) 937-1932

Cahinete.Ope¡ations lvork lnstodior
 (4) Select the following items for SET = RANGE:
. 1: MODE : SCL
. 1: MODE = VOLT
¡ l: RNG = 2V
¡ 1: L = 0.000
. 1:R:1.000
o 1: I : 0.0
. 1:r= 100.0
(5) Select the following items fo¡ SETUP = REM:

. coNT NO. : 1
. 1: RECOR-D

(6) Select the following items for SETUP : RCD:

¡ RECORD = EXT
. CH_TAG = CH (on taC)
¡ SCL_PR = ON
. SPD PR = OFF
. RCtl' PR = ON
. AI-M-PR: OFF
¡ DGT_PR = EXT

(7) Select the lbllowing items for SETUP = END:

. END = STORE (or ABORT)

Note: Thís ís the onb, method to save any selecfion in fhe

SETUP mode. To save and exit selecf STORE. If the
operatíon r)as a training sessíon, select ABORT.

Tew I l7t3) 931t942

Pctrcn Induski6 ¡¡c. / lloostúr,
C¡lcü'etr Ope¡aiion3 Wo.k Iñslruction
10
 Petron Automatic Calcimeter
Calibration Work Instruction .

1.0 Scope
This wo¡k instruction defines the steps to calibÉting the calcimete¡.

2.0 Parts and Tools Checklist

2.1 Calcimeter:

. Petron automatic calcimeter with plexiglass reaction cell

. Sample delivery spoon
. Magnetic spirbar

2.2 Accessories:

. Analytical balance
. Mortar and pestle
'. Spatula
Vacüum g¡ease
. Weigh pape¡
. Hyd¡ochloric acid (10%), rcageDt grade, laboratory standard
. Calcium Carbonate, reagent grade, labo¡atory standard
. Gnduated cylinde¡ (10 mI), o¡ other liquid measuring device

3.0 Description
The parts listed above arc used as followsl

Plexiglass reaction cell with top O-¡ing Vessel that holds the HCL arld sample
during the reaction; retains intemai
prcssure.

A¡ralytical elecfonic balance Accuntely weighs the required amount

of sample.

Sample spoon Holds the 0.5 g¡am CaCOr sample.

Magnetic spinba¡ Agitates the HCL and sample to ensurc

sample reactioll.

Pclon lndürn6 Inc. / Ilouston, Tq6 / (t13) 937-7932

Calcinel.r Calü¡aiio¡ wo.k Insh¡rion
8000071 Rriiion 0
 Moflar and pestle Used to gritrd the fomatio¡ sample
into a powder.

Spatula Used to t¡a¡dfer pqr{dered sample to

the sample delivery spoon on the
electonic balatrce for weighing.

Vacuum srease Lubricates the O-rings and screw

tbreads on the rcaction cell and the
plexiglass fl{tu¡e mai¡tained on the
front of the calcimete¡.

Weigh pape¡ Keeps the sample powde¡ off the

elecúonic bala[ce.

Hydrochloric acid Acid reagent that reacts with calcium

ca¡bonaúe (CaCOJ and dolomite
(CaMglCO.lJ.

Graduated cyli¡der Used to measu¡e the amount of HCL.

(or other liquid me¿suring device)

Petrcn lndustriBlnc,I Honston, Tds / (7ul) 137-79&,

Cálcimeté.Calibdtion Work Instrudion
4.0 Calibration Work Instructions
A¡¡ange a wo¡k a¡ea so that the electonic balance, automatic calcimeter, and
measudng tools and devices are comtbrtably sihraEd in close proxfnity.

Note: Petform at a stable and constunt room rcnperature: ensure that this
is the colíbration temperature that will be maintained during the
operuI¡on.

4-i Sample Preparation

4.1.1 Use only reagent gmde, dry calcium carbonate (CaCOt. Turn the
switch on the back of the calcimeter to the ON position. E¡sure that
the 3-way switch on the front panel is in the STOP posirion. Walm
up for approximately one hou¡.

4.2 Equipment and Process Preparation

4.2.1 Lub cate the O-rings and screw th¡eads on the reaction cell and
fixture with a light coating of vacuum g¡ease pedodically. Ve¡ify
that fhe O-ring seals and p¡essure co¡¡ections are in good
condition. Check fo¡ di¡t o¡ deb¡is on the threads and O- ngs that
rnight prevent a good seal.

4.2.2 Place a weigh paper on the elect¡onic balance to keep any sample
powder off the balance.

4.2.3 Place the sample delivery spoon in the center of the weighi¡g
paper. Close the lid to the electronic balance. Tarc or set the scale
to zero to accu¡ately measure only the weight of the sampie.

1.2.4 With the spatula ta¡sfe¡ exactly 0.5 grams of calib¡ation sample
into the sample delivery spoon on the elect¡onic balance.

P¿iron Industn6 Inc.I Housbn, 1eú / (713) 937-t932

C¡lcL¡eie.C¡libntion Wo.k ldruction
800¡071
 4.2.5 Place the loaded sample delivery spool i¡ position in the
calcimete¡. Keep the sample delivery spoon in a horizontal position.

A. Hook the sample delivery spoon with ttre riveighed sample ro

rhe hanger on Lhe plexiglass reaclion ceLI fixnr¡e Lhar is
attached to the calcimeter, holding the spoon in place agai¡st
¿he electromagnet.

Note: To prevent los¡ng paft of the strmple, hol¿ the sample

delivery spoon snugly against the electoÍurgnet
wh¡le settíng the three-way swítch on the Íront of fhe
calc¡meter to the LOAD posífíon.

B. Itt the 3-way switch irto LOAD position to activate the

elect¡omagnet to hold the sample delivery spoon in place.

4 2.6 Prcpare the reaction cell.

A. First, place the magnetic spinba¡ into the plexiglass reaction

cell.

B. Then measure 10 ml of HCL (10%) into a gmduared cylinde¡.

Transfer the HCL to the ¡eaction cell.

4.2."1 Zero the calcimeter's digital displ¿y using rhe SIGNAL ZERO
potentiometer on the front of the calcimete¡.

Note: This iS scaled from Zero to 100% and is Nery Sensitive and
nay be difficult to set d¡rectll on zero (0.0%). Consider
the calciueter zeroed íf the displ6! is 0.0%, +/- 0.1%. If
the d¡gítal dísplay shows a seríes of asterisks (***) the
pressure yolues are out of range for the strip chart to
record.

Pd.on Indurrig Inc, / Hdüsbn,ldú I l1l3) 911-1942

Calcin¿t¿r Calibmtion W¡rk lnsttucliór
¡000071
 4.2.8 E¡sure that the pressue relief valve on top of the reaction cell
fixtu¡e is in the closed position (tum clockwise finger tight)

4.2.9 Scrcw the plexiglass leaction cell to the fi.dure,'on the calcimeter.
Tighren inugl).

A. The pressu¡e in the reaction ceil will dse immediárely as üe

reaction cell is tightened. This is reflecred on the digirai
display. If this does not occur therc is a pressr¡¡e leak.

B. Bleed the p¡essure by opening the pressure relief valve on top

of the plexiglass fixture urltii the digital display ¡etums ro zero.
Keep ihe valve open untii the prcssure is fuily released. The
display will ¡eh¡m to ze¡o.

C. Close the pressue relief valve (tum clockwise untii fiüger

tigho.

4.2.t0 Pull the sti¡¡er d¡awer open lo its fi¡st stop position. This places the
electlomagoetic müer in the drawer uldemeath the reaction ceil.
Now pe¡form these steps I

Tum the ROTATION SPEED knob tully open in a clockwise

directior. This brings the acid swirl as high as possible in úe
reaction cell aIId rcmoves any sample sticking to the sides of
the cell when it is dropped to the acid.

B. When the rctation speed is stable, release the pressure by

opening the prcssure relief valve one last time so that the
digital display reads zero.

C. Close the p¡essure relief valve (turn clockwise until fiDger

¡ieh0.

1.2.1,1 Feed the st¡ip chaÍ to the closest heavier solid line using rhe FEED
bütton on the rcco¡der. This is the mi¡ute mark line. They arc one
minute apa¡t at a strip chart speed of 600 mm,/fu.

,'t€'5 I Ot3) 931-fi42

C¡lcinel¿. Cdibniion wo.k IEtndion
 4.3 Operq,tion fot Calíbruting With Pure Calcium Carbonate (CaCO) Sample

4.3.1 Quickly tum the 3-way switch to the RUN position without pausing
between switch selections. This starts the stdp ¡hart pcorditrg arld
rcleases the sample into the acid. The time arld cha( speed wiil be
printed ro idenrifv each sample run.

Note: The pen on the stríp charf operaÍes onry when the 3-wcJ sw¡Ích
is in the RUN node. Howewr, the di.gital dísplay and bar
graph always function.

Note: When testing several samples, verifJ that the RUN srrítch ¡s
turnedoÍ bebreen samples in order to conserue paper.
4.3.2 As the calibration sample is ¡eleased into the HCL, the pressüre rises
quickly and immediateiy il CaCO. is present. The st¡ip chan pen begi¡s
to rccord the p¡essurc dse. The prcssu¡e dse shouid peak and level ouf
within tbree (3) mi¡utes unless the acid is very cold.

,+.3.3 Observe the reaction for 1-3 minutes or until it peaks out. wait uniii the
reaction is complete and the pressu¡e stops ¡ising. Adjust the calib¡ation
SPAN potentiometer orl the front of the machine to read 100% on the
digital display.

4.3.1 Bleed the prcssure f¡om the reaction cell fixture.

CAUTION: Posirton Jourself so that pressure is released AWAy Írom

lou to prevent acíd from contactíng lour eJes and skin-
4.3.5 Tum the 3-way switch to STOP. This p¡events the strip chat frcm
oPerating.

Tum the rotation speed knob fully counte¡clockwise to stop the stir¡ing
action.

4.3.'7 Push in the stirrer d¡awer by ¡eleasing the retaining lock on the ¡ight
side of lhe drawer.

4.3.8 Remove the reaction cell. Notice that a vacuum (a negative display
measurcmefit) is created.

Petrun Indurrid Inc. / Honsbn , Tdrs I 1713) 931J942

Cilcinéter Cllibrllion Wo.k Instnclion
&e?tuion 0
 4.3.9 Dismantle, clean, and dry the equipment between samples. Remove the
acid from the attached reaction fixflrre with a clean, dry paper towel-

Note: tf. aÍcr naking a calibraion span a¿ljustr\ent. rhe re(or(1et ¿id
not retum to zero when the pressure'was rpleased, repeat the
calibration process. This wy haye to be repeated seyetq.L
tímes, especiall, if the machine is out of calibratión by a
s¡gn¡rtcant amounÍ, because the zero and span are perfially
¡nteractive. Repeat the calibratíon unt¡l zero and span do not
require furt her edj ustment s.

4.3.10 Check the calibntion every twelve (12) houn and before each use. This
marks üe end oI Lhe calib¡ation work i¡srucrion.

Pd.on lrdütrisInc. / Hóust n, Tds / (713) 93t-794,

Cllcim¿rer Cdibntion Work ¡nslúcti¡n